Evaporator comprising a sintered body with a conductive coating.

专利摘要:
The invention relates to an evaporator comprising a porous sintered body (6) with an electrically conductive coating. The sintered body has an open porosity in the range of 10 to 90%. The electrically conductive coating is connected to the surface of the pores and is part of a heating device in an evaporator. In this case, it lines up the pores which are located in the interior of the sintered body (6) so that, when the sintered body is electrically contacted and subjected to a current, this current flows at least partially through the interior of the sintered body and the interior of the sintered body is heated. Furthermore, the invention relates to a method for producing an evaporator, comprising a porous sintered body with an electrically conductive coating. The inventive evaporator may e.g. be used as a component in an electric cigarette or in a medical inhaler.
公开号:CH714241A2
申请号:CH01116/18
申请日:2018-09-18
公开日:2019-04-15
发明作者:Dang Cuong Phan Dr；Gold Julia；Rindt Matthias；schmid Susanne；Beerhorst Thomas
申请人:Schott Ag；
IPC主号:

专利说明:

description
Field of the Invention The invention generally relates to a sintered body coated with an electrically conductive coating. In particular, the invention relates to an evaporator unit comprising a liquid storage device and a heating unit for storing and controlled dispensing of evaporable substances. The evaporator unit can be used in particular in electronic cigarettes, in the administration devices for medicaments, room humidifiers and / or heatable evaporators for releasing substances into the room air, such as, for example, fragrances or insect repellents.
Electronic cigarettes, also referred to below as e-cigarettes, are increasingly used as an alternative to tobacco cigarettes. Typically, the electronic cigarettes comprise a mouthpiece and an evaporator unit and an electrical energy source that is operatively connected to the evaporator unit. The evaporator unit has a liquid reservoir which is connected to a heating element.
Certain drugs, particularly drugs for the treatment of respiratory tract and / or oral and / or nasal mucosa, are advantageously administered in the vaporized form, e.g. as an aerosol. Vaporizers according to the invention can be used for storing and dispensing such medicaments, in particular in administration devices for such medicaments.
[0004] Thermally heatable evaporators are increasingly being used to provide an ambience with fragrances. In particular, these can be bars, hotel lobbies and / or vehicle interiors, for example the interiors of motor vehicles, in particular passenger cars. A liquid reservoir is also connected to a heating element in the evaporator unit used here. The liquid reservoir contains a liquid, which is usually a carrier liquid such as propylene glycol or glycerin, in which additives such as fragrance and aroma substances and / or nicotine and / or medicines are dissolved and / or generally contained. The carrier liquid is bound by adsorption processes on the inner surface of the liquid storage device. A separate liquid reservoir is optionally provided to supply liquid to the liquid storage.
In general, the liquid stored in the liquid storage is evaporated by heating the / a heating element, desorbed from the wetted surface of the liquid storage and can be inhaled by the user. Temperatures of over 200 ° C can be reached.
The liquid reservoir must therefore have a high absorption capacity and a high adsorption effect, but at the same time the liquid must be dispensed quickly at high temperatures.
Different materials for use as liquid storage are known from the prior art. For example, the liquid reservoir can be formed by a porous or fibrous, organic polymer. Corresponding liquid stores can be produced quite simply, but there is a risk here that, for example, the polymeric material will be heated too high and decompose if the liquid store runs dry. This not only has a disadvantageous effect on the service life of the liquid store or the evaporator unit, but there is also the risk that decomposition products of the fluid to be evaporated or even the liquid store are released and inhaled by the user.
Electronic cigarettes with porous liquid stores made from organic polymers are known from the prior art. Due to the low temperature stability of the polymeric material, there is therefore a need to maintain a minimum distance between the heating element and the liquid reservoir. This prevents the evaporator unit and thus the electronic cigarette from being compact. As an alternative to maintaining a minimum distance, a wick can be used which leads the liquid to be evaporated to the heating coil by capillary action. This wick is usually made of glass fibers. Although these have high temperature stability, the individual glass fibers can easily break. The same applies if the liquid reservoir itself is made of glass fibers. There is therefore a risk that the user inhales loose or loosened fiber fragments. Alternatively, wicks made of cellulose fibers, cotton or bamboo fibers can also be used. Although these have a lower risk of breakage than wicks made of glass fibers, they are less temperature-stable.
Therefore, evaporator units are increasingly used, whose liquid storage consists of porous glasses or ceramics. Due to the higher temperature stability of these liquid stores, a more compact design of the vaporizer and thus also of the electronic cigarette as a whole can be realized.
The local evaporation can be achieved in practice by a low pressure combined with a high temperature. In the case of an electronic cigarette, the low pressure is realized, for example, by the suction pressure when pulling the cigarette during consumption, so the pressure is regulated by the consumer. The temperatures in the liquid storage required for the evaporation are generated by a heating unit. Temperatures of more than 200 ° C are usually reached to ensure rapid evaporation.
Usually the heating power is provided by an electrical heating coil operated by means of a battery or accumulator. The heating power required depends on the volume to be evaporated and the effectiveness of the heating. To prevent the liquid from decomposing due to high temperatures, the heat transfer from
CH 714 241 A2 of the heating coil to the liquid by non-contact radiation. For this purpose, the heating coil is attached as close as possible to the evaporation surface, preferably without touching it. However, if the coil touches the surface, the liquid is often overheated and decomposed.
Overheating of the surface can, however, also occur in the case of heat transport by means of contactless radiation. The overheating usually occurs locally on the surface of the evaporator opposite the heating coil.
This is the case when a large amount of steam is required in operation and the liquid transport to the surface of the evaporator is not fast enough. Thus, the energy supply from the heating element cannot be used for evaporation, the surface dries out and can be locally heated to temperatures far above the evaporation temperature and / or the temperature stability of the liquid reservoir is exceeded. Precise temperature setting and / or control is therefore essential. However, the resulting complex structure of the electronic cigarette is disadvantageous, which manifests itself, among other things, in high production costs. In addition, the temperature control may reduce the steam development and thus the maximum possible steam intensity.
[0014] EP 2 764 783 A1 describes an electronic cigarette with an evaporator which has a porous liquid store made of a sintered material. The heating element can be designed as a heating spiral or as an electrically conductive coating, the coating being deposited only on parts of the lateral surfaces of the liquid reservoir. Evaporation is thus also locally limited here.
[0015] US 2011/0 226 236 A1 describes an inhaler in which the liquid reservoir and the heating element are integrally connected to one another. Liquid storage and heating element form a flat composite material. The liquid reservoir, for example made of an open-pore sintered body, acts as a wick and directs the liquid to be evaporated to the heating element. The heating element is applied to one of the surfaces of the liquid reservoir, for example in the form of a coating. Here too, the evaporation takes place locally limited on the surface, so that there is also a risk of overheating.
To avoid this problem, evaporator units are known from the prior art, in which the evaporation occurs not only on the surface of the liquid storage device, but over its entire volume. The vapor develops not only locally on the surface, but in the entire volume of the liquid storage. The vapor pressure within the liquid reservoir is thus largely constant and capillary transport of the liquid to the surface of the liquid reservoir is no longer necessary. Accordingly, the rate of evaporation is no longer minimized by capillary transport. A suitable evaporator requires an electrically conductive and porous material. If an electrical voltage is applied, the entire volume of the evaporator heats up and the evaporation takes place everywhere in the volume.
Corresponding evaporators are described in US 2014/0 238 424 A1 and US 2014/0 238 423 A1. Liquid storage and heating element are combined in one component, for example in the form of a porous body made of metal or a metal mesh. The disadvantage here, however, is that the ratio of pore size to electrical resistance cannot be easily adjusted in the porous bodies described. After the conductive coating has been applied, a subsequent sintering can lead to a degradation of the coating.
However, the materials described in the abovementioned prior art are not suitable or are suitable only to a limited extent in order to produce composites by means of a sintering process which have both a high, adjustable porosity and good electrical conductivities. In general, ceramics are also difficult to coat continuously due to their fine porosity and rough surface.
OBJECT OF THE INVENTION It is therefore an object of the invention to provide a sintered body coated with an electrical coating, which is particularly suitable for use as an evaporator in electronic cigarettes and / or administration devices for medicaments and / or thermally heated evaporators of fragrances and which does not have the disadvantages described above. In particular, the invention strives for good heatability and simple adjustability of the electrical resistance and porosity of the liquid reservoir. Another object of the invention is to provide a method for producing a corresponding coated sintered body.
Brief Description of the Invention The object of the invention is already achieved by the subject matter of the independent claims. Advantageous embodiments and developments of the invention are the subject of the dependent claims.
[0021] The evaporator according to the invention or the evaporator unit according to the invention comprises a sintered body and an electrically conductive coating. By means of adsorptive interactions, a carrier liquid is stored in the porous evaporator, which can contain, for example, fragrance and aroma substances and / or medicines, including active substances and / or nicotine dissolved in suitable liquids. When an electrical voltage is applied, the electrically conductive coating in the evaporator generates high temperatures, so that the carrier liquid is evaporated, desorbed from the wetted surface of the evaporator and the steam can be inhaled by the user.
CH 714 241 A2 The sintered body can consist of glass or glass ceramic and has an open porosity in the range from 10 to 90% based on the volume of the sintered body.
Preferably at least 90%, in particular at least 95% of the total pore volume is present as open pores. The open porosity can be determined using measuring methods in accordance with DIN EN ISO 1183 and DIN 66 133. According to one embodiment of the invention, the sintered body has an open porosity in the range of at least 20%, preferably 20% to 90%, particularly preferably 50 to 80% and in particular in the range of 60 to 80%. The porosity according to the invention ensures a high adsorption capacity of the sintered body. According to one embodiment, the sintered body can absorb at least 50% of its open pore volume of propylene glycol at a temperature of 20 ° C. and an adsorption time of 3 hours. At the same time, the sintered body has good mechanical stability. In particular, sintered bodies with a relatively low porosity show high mechanical stability, which can be particularly advantageous for some applications. According to another embodiment, the open porosity is 20 to 50%.
[0025] The sintered body preferably contains only a small proportion of closed pores. As a result, the sintered body has only a small dead volume, i.e. a volume that does not contribute to the absorption of the liquid to be evaporated. The sintered body preferably has a proportion of closed pores of less than 15% or even less than 10% of the total volume of the sintered body. To determine the proportion of closed pores, the open porosity can be determined as described above. The total porosity is calculated from the density of the body. The difference between the total porosity and the open porosity then results as the proportion of the closed pores. According to one embodiment of the invention, the sintered body even has a proportion of closed pores of less than 5% of the total volume. Closed pores can be created by pores in the granulate that is used for sintering, by the sintering process or by coating very small open pores with the electrically conductive coating. Open pores can be closed by the electrically conductive coating in particular if the corresponding pores are very small and / or the layer thickness of the electrically conductive coating is very thick.
The electrically conductive coating is preferably non-positively and cohesively connected to the surface of the sintered body. Here, not only the pores on the lateral surfaces of the porous sintered body, but also the pores in the interior of the sintered body are provided with the electrically conductive coating. The open pores are thus provided with the electrically conductive coating over the entire volume of the sintered body. This has the consequence that when a voltage is applied to the sintered body coated according to the invention, the current flows through the entire volume of the sintered body and the entire volume of the sintered body is thus heated. The electrically conductive coating is thus deposited on the surface of the sintered body and connected to the surface of the sintered body, the electrically conductive coating lining the pores which are located inside the sintered body, so that when the sintered body and, at least partially or in sections, is electrically contacted When a current is applied, this current at least partially flows through the interior of the sintered body and heats the interior of the sintered body.
Thus, heating is carried out over the entire current-carrying body volume of the sintered body and, accordingly, the liquid to be evaporated is evaporated in the entire volume of the sintered body. The vapor pressure is the same everywhere in the sintered body and the steam develops not only locally on the surface of the sintered body, which form its outer surfaces, but also inside the sintered body. The electrically conductive coating is applied to the surface of the sintered body and forms at least part of its pore surface.
Unlike in evaporators, which have a local heating device, for example a heating coil or an electrically conductive coating only on the lateral surfaces of the sintered body, a capillary transport to the surface of the sintered body is not necessary. This prevents the evaporator from running dry if the capillary action is too low and thus also prevents local overheating. This has an advantageous effect on the life of the evaporator unit. In addition, decomposition processes of the liquid to be evaporated can occur if the evaporator overheats locally. On the one hand, this can be problematic since, for example, the active substance content of a medicament to be evaporated is thus reduced. On the other hand, decomposition products are inhaled by the user, which can pose health risks. In the evaporator according to the invention, however, there is no such danger.
Alternatively, the sintered body can also be heated by an inductive or capacitive coupling of the electrically conductive coating.
In a preferred embodiment of the invention, the entire surface of the sintered body formed by the open pores is covered with the electrically conductive coating. Accordingly, the term “entire surface” also includes, for example in the case of a cylindrical sintered body, the surface of the sintered body which is formed by the pores in the interior of the body. The entire coated surface is therefore generally larger than the outer surface of the body.
[0031] The coated sintered body can have different geometries depending on the area of application. For example, the sintered body can be fully or hollow cylindrical, plate-shaped, prismatic, polyhedral or ring-shaped. The respective shape can already be determined by the shape of the green body before sintering, on the basis of the
CH 714 241 A2 high mechanical stability of the sintered body, however, mechanical processing of the sintered body after its sintering is also possible.
The electrically conductive coating can in particular be a metal such as silver, gold, platinum or chrome or be formed by a metal oxide. In one embodiment of the invention, the metal oxide is a metal oxide from the group consisting of indium tin oxide (ITO), zinc oxide (AZO) doped with aluminum, fluorine tin oxide (FTO) or antimony tin oxide (ATO). Metal oxides have been found to be particularly advantageous here, in particular due to the good adhesion to glass and the good wetting behavior of the liquid to be evaporated on the metal oxide. In addition, the above-mentioned metal oxides, in particular ITO, have high chemical and mechanical stability and are insoluble in water and alcohol, so that they are inert to the solvent of the liquid to be evaporated. In addition, the above-mentioned metal oxides are stable to temperatures up to 2000 ° C. The coating preferably contains ITO and / or is an ITO coating.
When used as an evaporator in electronic cigarettes, the electrically conductive coated sintered body preferably has an electrical conductivity in the range from 0.001 to 10 ⁶ S / m. A conductivity in the range from 10 to 600 S / m has proven to be particularly advantageous. Conductivities in the areas described above are particularly advantageous in the case of relatively small vaporizers, such as those used in electronic cigarettes. The stated conductivities are high enough to ensure sufficient heat development for the evaporation. At the same time, excessive heating capacities, which can lead to overheating and thus to decomposition of the liquid components, are avoided.
[0034] The sintered body according to the invention can be used both as an evaporator in electronic cigarettes and as an evaporator in medical inhalers. The two applications place different demands on the evaporator. This applies in particular with regard to the required heating power of the evaporator. The electrical resistance and thus the heating power of the evaporator can be set via the layer thickness of the electrically conductive coating and the electrical conductivity of the coated sintered body thus achieved. This is advantageous since the optimal heating output depends on the dimensions of the sintered body and the voltage source used in each case. For example, vaporizers that are used in electronic cigarettes have a small size of a few cm and are usually operated with one or more voltage sources with a voltage of 1 V to 12 V, preferably with a voltage of 1 to 5 V. These voltage sources can be standard batteries or standard accumulators. According to one embodiment, the evaporator is operated with an operating voltage in the range from 3 to 5 V. Electrical resistances in the range from 0.2 to 5 ohms and a heating power of up to 80 W have proven to be particularly advantageous. In contrast, inhalers for the medical sector, for example, will also be operated at voltages of 110 V, 220 V / 230 V or even 380 V. Electrical resistances up to 3000 ohms and powers up to 1000 W are advantageous here. Depending on the embodiment of an evaporator unit or its use, other operating voltages, for example greater than 12 V to less than 110 V, resistors, e.g. greater than 5 ohms and power ranges, e.g. suitable than 80 W.
[0035] According to one embodiment of the invention, the layer thickness of the electrically conductive coating is in the range from 1 nm to 800 μm. Layer thicknesses in the range from 200 nm to 200 μm or 200 nm to 10 μm have proven to be particularly advantageous. If the layer thickness is too large, there may be a risk of pore closure due to the electrically conductive coating. The layer thickness also depends on the material used. Layers based on metal oxides usually have a significantly greater layer thickness than layers made of a metal.
One embodiment of the invention provides an electrically conductive coating made of a deposited metal, for example silver, gold, platinum or chromium, with a layer thickness in the range from 1 nm to 1 μm, preferably in the range from 10 nm to 100 nm.
[0037] The electrically conductive coating can have a homogeneous layer thickness within the sintered body. However, the present invention also relates to sintered bodies whose electrically conductive coating has inhomogeneous layer thicknesses within the sintered body. This applies in particular to coatings based on metal oxides with a relatively large layer thickness. According to a development of the invention, the layer thickness of the electrically conductive coating has a gradient within the sintered body. For example, the layer thickness can decrease from the outside to the inside.
In addition to the layer thickness described above, the desired electrical resistance can be set by the electrical conductivity of the coated sintered body. The electrical conductivity of the coated sintered body depends on the coating material used or on its electrical conductivity. In one embodiment of the invention, the coated sintered body has 0.001 to 106 S / m, preferably 10 to 600 S / m.
[0039] According to one embodiment of the invention, the pores have an average pore size in the range from 1 μm to 5000 μm. The pore size of the open pores of the sintered body is preferably in the range from 100 to 800 μm, particularly preferably in the range from 200 to 600 μm. Pores with appropriate sizes are advantageous because they are small enough to generate a sufficiently large capillary force and thus ensure the replenishment of liquid to be evaporated, in particular during the operation of the evaporator, and at the same time they are large enough to allow a rapid
CH 714 241 A2
Allow steam to be dispensed. If the pores are too small, there is also the danger that the electrically conductive coating can completely or partially close them.
[0040] A further development of the invention provides an at least bimodal distribution of the pore sizes. Here, the sintered body has small and large pores, each with a discrete pore size distribution. The small pores enable a large capillary force and thus for a good and quick absorption of the liquid in the sintered body. However, since small pores release the steam only slowly, the sintered body also has large pores which ensure that the steam is released quickly. The pore size and the ratio of large to small pores can be adjusted via the manufacturing process of the sintered body by using salts with different grain sizes in the appropriate ratio as pore formers. The adsorption or desorption behavior of the sintered body can be adjusted via the ratio of large to small pores. Depending on the application, the proportion of large pores is in the range of 5 to 95% of the total number of pores. This development of the invention preferably has small pores in the range from 100 to 300 μm and large pores in the range from 500 to 700 μm.
[0041] According to one embodiment of the invention, the sintered body consists of glass. Glasses with a relatively low alkali content have been found to be particularly advantageous. A low alkali content, in particular a low sodium content, is advantageous from several points of view. On the one hand, corresponding glasses have a relatively high transformation temperature T _g , so that after the electrically conductive coating has been applied, it can be baked at relatively high temperatures. In particular in the case of electrically conductive coatings based on oxide, high penetration temperatures have an advantageous effect on the density of the electrically conductive coating and the electrical conductivity of the sintered body. The glasses preferably have a transformation temperature T _g in the range from 300 ° C. to 900 ° C., preferably 500 ° C. to 800 ° C.
On the other hand, glasses with a relatively low alkali content show a low alkali diffusion even at high temperatures, so that sintering can take place at relatively high temperatures or the baking of a coating can take place without this or its properties changing negatively , The low alkali diffusion of the glasses is also advantageous in the operation of the sintered body as an evaporator, since no escaping components interact with the electrically conductive coating or with the liquid to be evaporated. The latter is particularly relevant when using the coated sintered body as an evaporator in medical inhalers. An alkaline proportion of the glass of at most 11% by weight or even at most 6% by weight has proven to be particularly advantageous.
[0043] The sintered body is exposed to large temperature fluctuations both during its manufacture and during operation. During the operation of the evaporator, this results from numerous heating cycles. The sintered body must therefore have not only a high mechanical but also a high thermal load capacity. It is therefore advantageous if the sintered body has a linear thermal expansion coefficient a _2O -3oo ° c of asintered body <11 * 10 "® K" ¹ , preferably less than 8 * 10 "® K" ¹ . In order to keep thermal stresses between the sintered body and the electrically conductive coating as low as possible, it can be advantageous, depending on the coating, if the sintered body has a linear thermal expansion coefficient a2O-3oo ° c in the range from 1 to 10 * 10 “® K“ ¹ , which is electrical conductive coating has a linear thermal expansion coefficient a2O-3oo ° c in the range from «coating to 1 to 20 * 10" ® K " ¹ and / or the difference between the two thermal expansion coefficients Δ a _2O -3oo ° c =« 20-300 ° cschicht - «20-300 ° c sintered body 0 to 20 * 10" ® K " ¹ , preferably 0 to 10 * 10" ® K " ¹ , also preferably 0 to 5 * 10" ® K " ¹ .
One embodiment of the invention provides a metallic, electrically conductive coating, preferably silver, and a glass sintered body with a linear thermal expansion coefficient in the range from 8 * 10 "® K" ¹ to 20 * 10 "® K" ¹ .
According to a further development of the invention, the coated sintered body has an electrically conductive coating made of ITO and a glass sintered body with a linear thermal expansion coefficient in the range from 3 * 10 "® K" ¹ to 8 * 10 "® K" ¹ . Corresponding thermal expansion coefficients or differences have been found to be advantageous in particular when using metal oxide-based electrically conductive coatings. These coatings are usually applied to the sintered body with a greater layer thickness than, for example, metallic coatings.
Surprisingly, despite the a _2O -3oo ° c differences between glass and coating, crack-free or at least low-crack layers can also be obtained when using metal oxides as an electrically conductive coating with a relatively large layer thickness. In particular, crack-free or low-crack layers can be obtained if these are baked on at high temperatures, preferably at temperatures in the range from 300 to 900 ° C., after being deposited on the sintered body. It has been found that appropriate ITO coatings do not tend to crack and do not delaminate even when an evaporator is in operation, that is to say under cyclical thermal loading. The electrical conductivity of the coated sintered body and thus the evaporation capacity of the evaporator thus also remain constant or at least largely constant over the life of the evaporator. Another advantage of a low-crack coating is that, even when the evaporator is operating, there is as little as possible a release of metal oxide and / or glass particles or flakes, in particular with a particle size <5 μm, which could otherwise be inhaled by the user.
According to another development of the invention, the electrically conductive coating and / or an intermediate zone to the sintered body has a gradient with respect to the linear thermal expansion coefficient. The
CH 714 241 A2 linear coefficient of thermal expansion increases from the surface of the coating that is in contact with the sintered body to the free surface of the coating. The / this gradient of the a2o-3oo ° c of the electrically conductive coating allows thermal stresses between the sintered body and the coating to be absorbed.
Preferably, the sintered body has a lower a ₂ o-3oo ° C than the electrically conductive coating. This ensures that the coating is not subjected to tensile stress in heating mode. A tensile stress on the coating can have a disadvantageous effect on the development of cracks in the coating or on the enlargement of existing cracks and / or delamination of the layer.
Since there is due to the inventive design of the evaporator as a volume evaporator to local overheating, for example, the surface or the areas that are in closer and / or direct contact with a heating element or parts of a heating element in conventional evaporators, and thus overall A large number of glasses are suitable for achieving lower maximum temperatures than the evaporators known from the prior art. The associated selection of different glasses means that the appropriate glass can be selected for the respective electrically conductive coating with regard to thermal expansion coefficients, chemical resistance or a possible penetration temperature.
When using the coated sintered body as an evaporator in an electronic cigarette or as a medical inhaler, any substances which may be hazardous to the user should not be released from the glass. Therefore, the glasses used preferably do not have the following elements or only in very small, unavoidable traces: arsenic, antimony, cadmium and / or lead. In particular, the arsenic, antimony, cadmium and / or lead content is less than 500 ppm.
An embodiment of the invention provides the following glass composition for the porous sintered body in% by weight:
Sio ₂ 30 to 85 B2O3 3 to 20 Al2O3 Obis 15 Na ₂ O 3 to 15 K ₂ O 3 to 15 ZnO Obis 12 TiO ₂ 0.5 to 10 CaO Obis 0.1 In a further embodiment of the invention, the glass of the porous sintered body has the following composition in% by weight: SiO ₂ 58 to 65 B2O3 6 to 10.5 Al2O3 14 to 25 MgO 0 to 3 CaO 0 to 9 BaO 3 to 8 ZnO 0 to 2, with the proviso that the sum of the contents of MgO, CaO and BaO is characterized in that it is in the range from 8 to 18% by weight.In a further embodiment of the invention, the glass of the porous sintered body has the following composition in% by weight: SiO2 61
CH 714 241 A2
b ₂ 0 ₃ 10 Al2O3 18 MgO 2.8 CaO 4.8 BaO 3.3
[0054] Glaziers of this embodiment have the following properties:
«20-300 c 3.2 · 10 ^_6 / K
Tg 717 ° C density 2.43 g / cm ³
[0055] According to a further embodiment of the invention, the porous sintered body has the following glass composition in% by weight:
SiO ₂ 55 to 75 Na ₂ O Obis 15 K ₂ O 2 to 14 AI ₂ O ₃ Obis 15 MgO 0 to 4 CaO 3 to 12 BaO Obis 15 ZnO 0 to 5 TiO ₂ Obis 2
[0056] One embodiment provides a sintered body with the following glass composition in% by weight:
SiO ₂ 64-74 Na ₂ O 6-10 K ₂ O 6-10 CaO 5-9 BaO 0-4 ZnO 2-6 TiO ₂ 0-2
With glasses in this composition range, a porous glass body with the following properties can be obtained:
«20-300 ° c 9.4 · 10 ⁶ / K
T _g 533 ° C
CH 714 241 A2
density 2.55 g / cm3
Another embodiment provides a porous glass body with the following composition in% by weight:
Sio ₂ 75-85 B2O3 8-18 Al2O3 0.5-4.5 Na ₂ O 1.5-5.5 K ₂ O 0-2
A porous glass body with the following properties can be obtained with this composition:
"20-300 c 3.25 to 10 ^_6 / K
T _g 525 ° C
Density 2.2 g / cm ³ In a further embodiment of the invention, the glass of the porous sintered body has the following composition in% by weight:
SiO ₂ 50 to 65 AI ₂ O ₃ 15 to 20 B ₂ O ₃ 0 to 6 Li ₂ O 0 to 6 Na ₂ O 8 to 15 K ₂ O 0 to 5 MgO 0 to 5 CaO 0 to 7, preferably 0 to 1 ZnO 0 to 4, preferably 0 to 1 ZrO ₂ 0 to 4 TiO ₂ 0 to 1, preferably free of TiO ₂
The glass may further contain 0 to 1% by weight: P ₂ O ₅ , SrO, BaO; and refining agents at 0 to 1% by weight: SnO ₂ , CeO ₂ or _As2 O ₃ , R CI, sulfate or other refining agents.
According to a further development of the invention, the glass of the porous sintered body is a ceramizable lithium aluminosilicate glass. One embodiment provides the following glass composition in% by weight:
SiO ₂ 55-69 AI ₂ O ₃ 15-25 Li ₂ O 3-5 Na ₂ O + K ₂ O 0-30 MgO + CaO + SrO + BaO 0-5
CH 714 241 A2
ZnO 0-4 TiO ₂ 0-5 ZrO ₂ 0-5 TiO ₂ + ZrO ₂ + SnO ₂ 2-6 p ₂ o ₅ 0-8 F 0-1 B ₂ O ₃ 0-2 W20-300 ° C 3.3-5.7 as glass
The glass has an a _2O -3oo ° C in the range from 3.3 * 10 ⁶ K ¹ to 5.7 * 10 "® K ¹ .
As an alternative, the glass of the porous sintered body has the following composition in% by weight:
SiO ₂ 57-66 AI ₂ O ₃ 15-23 Li ₂ O 3-5 Na ₂ O + K ₂ O 3-25 MgO + CaO + SrO + BaO 1-4 ZnO 0-4 TiO ₂ 0-4 ZrO ₂ 0-5 TiO ₂ + ZrO ₂ + SnO ₂ 2-6 p ₂ o ₅ 0-7 F 0-1 B ₂ C> 3 0-2
The glass of this embodiment has an a ₂ o-3oo ° c in the range of 4.7 * 10 "®K ^{1 to} 5.7 * 10" ®K ¹ . The following glass composition in% by weight has proven to be particularly advantageous:
SiO ₂ 57-63 AI ₂ O ₃ 15-22 Li ₂ O 3.5-5 Na ₂ O + K ₂ O 5-20 MgO + CaO + SrO + BaO 0-5 ZnO 0-3 TiO ₂ 0-3 ZrO ₂ 0-5 TiO ₂ + ZrO ₂ + SnO ₂ 2-5 P ₂ O ₅ 0-5 F 0-1
CH 714 241 A2
B2O3
Another development of the invention provides for the use of a porous sintered body made of soda-lime glass. In particular, the soda-lime glass is a glass with the following composition in% by weight:
SiO2 40-81 Al2O3 0-6 B2O3 0-5 Li ₂ O + Na ₂ O + K ₂ O 5-30 MgO + CaO + SrO + BaO + ZnO 5-30 T1O2 + ZrO ₂ 0-7 P2O5 0-2
Glasses of this embodiment have an a ₂ o-3oo ° C in the range from 5.5 * 10 ⁶ K ¹ to 9.7 * 10 ⁶ K ¹ .
A soda-lime glass with the following composition is preferably used for the porous sintered body:
S1O2 50-81 Al2O3 0-5 B2O3 0-5 Li ₂ O + Na ₂ O + K ₂ O 5-28 MgO + CaO + SrO + BaO + ZnO 5-25 TiO ₂ + ZrO ₂ 0-6 P2O5 0-2
Glasses of this embodiment have an a ₂ o-3oo ° C in the range from 4.9 * 10 ⁶ K ¹ to 10.3 * 10 ⁶ K ¹ .
In a particularly preferred embodiment of this development, the glass porous sintered body consists of a soda-lime glass with the following composition in% by weight:
S1O2 55-76 Al2O3 0-5 B2O3 0-5 Li ₂ O + Na ₂ O + K ₂ O 5-25 MgO + CaO + SrO + BaO + ZnO 5-20 T1O2 + ZrO ₂ 0-5 P2O5 0-2
According to a further embodiment, the glass of the sintered body contains the following components in% by weight:
SiO ₂ 1 to 85
B2O3 0 to 60
AI2O3 0 to 30
CH 714 241 A2
Li ₂ O 0 to 5 Na ₂ O 0 to 20 K ₂ O 0 to 15 ZnO 0 to 62 TiO ₂ 0 to 10 CaO 0 to 35 BaO 0 to 60 MgO 0 to 10 SrO 0 to 30 La ₂ O ₃ 0 to 40 Fe ₂ O ₃ 0 'to 10 MnO ₂ 0 to 5 Bi ₂ O ₃ 0 to 85 Cs ₂ O 0 to 20 SnO 0 to 5 ZrO ₂ 0 to 10 Y ₂ O ₃ 0 to 15 F 0 'to 7
According to one embodiment, the glasses can contain coloring oxides such as Nd ₂ O ₃ , Fe ₂ O ₃ , CoO, NiO, V ₂ O ₅ , MnO ₂ , TiO ₂ , CuO and / or CeO ₂ . Alternatively or additionally, 0-2% by weight of AS ₂ O ₃ , Sb ₂ O ₃ , SnO ₂ , SO ₃ , Cl, F and / or CeO _{2 can} be added as refining agents. Another embodiment provides for the glass to be added alternatively or additionally.
In a further development of the invention, the coated sintered body has one or more further coatings in addition to the electrically conductive coating. For example, a coated sintered body that has been galvanically coated with a metal as an electrically conductive layer can have a so-called starter coating between the surface of the sintered body and the electrically conductive metal layer.
In the case of metals as an electrically conductive coating and a sintered body made of glass, the problem can arise that the surface tensions of glass and metal can differ considerably and it is therefore difficult to achieve good adhesion of the electrically conductive coating to the glass surface. A further development of the invention therefore provides for an oxide layer to be applied between the sintered body and the metallic coating. This layer acts as an adhesion promoter, so that particularly good adhesion of the metallic coating can be achieved. Furthermore, the surface of the sintered body can be changed by an additional coating, the zeta potential of the surface and thus adapted to the zeta potential of the liquid to be evaporated. Alternatively or additionally, a further layer, for example a protective or passivation layer, can also be deposited on the electrically conductive coating.
Alternatively or additionally, the electrically conductive coating or the body can contain a further component, for example an antibacterial and / or antimicrobial component. Silver, ZnO or TiO ₂ are suitable as antibacterial or antimicrobial components. Silver as a component of the conductive coating has the advantage of being conductive on the one hand and also having an antibacterial effect on the other.
The sintered body coated according to the invention can be used as a heating element in an evaporator. Here, the necessary electronic contacting can take place mechanically, for example by means of spring forces or by means of a form fit, or in a material manner, for example by means of a soldered connection. For example, a silver conductive paste can be used as the solder. Contacting via intermediate layers is also possible.
A corresponding vaporizer can be, for example, part of an electronic cigarette, a medical inhaler, a fragrance dispenser, a room humidifier or a device for dispensing substances such as e.g. Insecticides or insect repellents or for related applications.
CH 714 241 A2 Furthermore, the invention relates to a method for producing a sintered body coated with an electrically conductive coating. The method according to the invention comprises at least the following method steps
a) providing a sintered body made of glass or glass ceramic with an open porosity in the range of 10 to 90% and
b) coating the surface of the sintered body formed by the open pores, including the surface of pores in the interior of the sintered body, with an electrically conductive coating.
The sintered body in step a) can be provided by a method in which first fine-grained glass powder with average grain sizes in the range from approximately 20 μm to 600 μm, preferably a maximum of 300 μm, is mixed with a high-melting salt and a binder. The grain size of the salt used is adapted to the desired pore size of the sintered body. 5 to 80% by weight of fine-grained glass powder is added to this mixture and the mass is pressed into shape. The resulting molded body is heated to the sintering temperature of the glass and sintered. The melting temperature of the salt used is above the corresponding sintering temperature, so that the grain structure of the salt is retained. After the sintering process, the salt is washed out with a suitable solvent. The salts NaCl and K ₂ SO ₄ have been found to be particularly suitable. Other salts such as KCl, MgSO ₄ , Li ₂ SO ₄ , Na ₂ SO ₄ are also conceivable. In addition to aspects such as costs, environmental compatibility or the like, the choice of salt depends on the glass used and its temperature requirement for sintering. In one embodiment of the invention, 20 to 85% by weight of salt with a grain size of 30 to 5000 μm are mixed with 5 to 85% by weight of glass powder with a grain size in the range of 1 to 500 μm and with an aqueous polyethylene glycol solution and mixed thoroughly. The mixture obtained in this way can either be dried or, in the moist state, 5 to 80% by weight of glass powder (based on the mass of the mixture) can be added. The mixture is pressed into shape and sintered at the sintering temperature of the glass used. The salt is then washed out, so that a porous sintered body is obtained.
In this way, a highly porous, open-pore sintered body is obtained. Since the individual glass grains are firmly connected to one another by the sintering process, the sintered body, despite the high porosity, has good mechanical strength compared to a corresponding glass fiber material, for example a wick made of glass fiber cord. There are therefore no loose or easily detachable particles within the sintered body which, when used as a liquid store in an electronic cigarette and / or an administration device for medicaments and / or thermally heated evaporators for fragrances, can be released and inhaled by the user. Due to the high mechanical stability of the sintered body, liquid stores can be provided which can even have porosities of more than 80% by volume.
[0081] In one embodiment of the invention, a sintered body made of glass is provided in step a). A sintered body made of glass with an alkali content of <15% by weight, preferably <10% by weight and particularly preferably <5% by weight has proven to be advantageous. Glasses with a correspondingly low alkali content Corresponding glasses have a high softening temperature, so that in step a) sintering can take place at high temperatures. Alumosilicate glasses and borosilicate glasses have been found to be particularly advantageous.
In step b), the electrically conductive layer can be obtained by condensation or separation of solid from a dispersion, condensation or removal of solid from a solution (for example sol-gel), condensation or removal of solid from the gas phase or by a galvanic process be deposited on the surface of the sintered body. The respective coating method depends on the coating material used and the desired layer thickness.
In one embodiment of the invention, a metallic layer is deposited electrolytically. For example, a silver coating can be deposited on the porous sintered body by deposition from a silver solution. The silver content of the solution used for this is preferably 10 to 20% by weight or 15 to 20% by weight. Alternatively, silver can be deposited by reduction from solution, for example by reducing a silbenitrate solution with sugar or by precipitation reactions.
A further development of the method according to the invention provides that an electrically conductive coating in the form of a metal oxide indium tin oxide (ITO), aluminum oxide doped zinc oxide (AZO), fluorine tin oxide (FTO) and antimony tin oxide (ATO) is applied in step b). The metal oxide in step b) is preferably deposited by condensation or precipitation from a solution or dispersion, particularly preferably from a dispersion.
[0085] The coating of the sintered body by means of an immersion process has proven to be particularly advantageous. In a corresponding embodiment of the above-mentioned development of the invention, the immersion process comprises at least the following process steps:
a2) provision of the sintered body b2) provision of a dispersion or solution of the metal oxide
CH 714 241 A2 c2) immersing the sintered body in the dispersion provided in step b2) for a predefined immersion time ^ immersion d2) drying the coated sintered body obtained in step c2) e2) baking the layer obtained by steps c2) and d2) a period of time t _A fire at a predefined penetration temperature T _penetration .
The layer thickness of the electrically conductive coating deposited by means of immersion is preferably 200 nm to 200 μm, particularly preferably 200 nm to 10 μm and can be adjusted via the solids content of the dispersion or solution used in step b). The solids content is preferably 1 to 50% by weight, particularly preferably 20 to 35% by weight. Alternatively or additionally, the desired layer thickness of the deposited layer can be obtained via the number of dipping processes of the sintered body. One embodiment provides that steps c2) and d2) are carried out several times, preferably two to three times. In a further development of the invention, the sintered body is immersed for different lengths in the various immersion processes. In this way, a gradient in the electrical conductivity of the coating can be achieved.
In step e2), the layer is preferably burned in at a penetration temperature T _penetration in the range from 60 to 1000 ° C., particularly preferably in the range from 300 to 900 ° C. Very dense layers can be obtained, especially at high penetration temperatures. In this way, low-crack or even crack-free coatings can be obtained even with large layer thicknesses. The coating remains crack-free or crack-free even at different a ₂ o-3oo ° c of sintered body and coating under cyclical thermal stress. It is assumed that the high penetration temperatures form a diffusion zone between the metal oxide and the sintered body, which absorbs the a ₂ o-3oo ° c differences. The baking of the electrically conductive coating in step e2) can take place under inert gas, under vacuum or under a slightly reducing atmosphere, for example in a 3 to 50% hydrogen atmosphere or under carbon monoxide.
The method described above or its embodiments described above can also be used for coating porous ceramics. In this case, a porous sintered body made of a ceramic is provided in step a) instead of a sintered body made of glass or glass ceramic. It has proven to be advantageous if the ceramic provided is the same or at least similar to the porous bodies made of glass or glass ceramic with regard to their porosity and / or pore size.
The electrically conductive layers deposited on the pore surface of a porous ceramic by means of this method are comparable with the electrically conductive layers of the sintered body made of glass or glass ceramic according to the invention. This applies in particular to features such as the electrically conductive materials used, the layer thicknesses, the electrical conductivities and / or the electrical resistances of the electrically conductive layers. Furthermore, an evaporator head with a sintered body according to the invention is the subject of the present invention. This has at least one housing, the sintered body according to the invention and electrical contacts for connecting the sintered body to an electrical energy source.
DETAILED DESCRIPTION OF THE INVENTION The invention is described in more detail below using exemplary embodiments and figures. Show it:
Fig. 1 a schematic representation of a conventional evaporator, Fig. 2 1 shows a schematic representation of a sintered body with electrical contacting on the lateral surfaces of the sintered body, Fig. 3 1 shows a schematic illustration of an evaporator with a sintered body coated according to the invention as the heating element, Fig. 4 3 shows a schematic illustration of a sintered body coated according to the invention in cross section, Fig. 5 an SEM image of a first embodiment, Fig. 6 a light microscope image of a second embodiment, Fig. 7 1 shows a schematic representation of a development of the invention with a bimodal pore size distribution, Fig. 8 the pore size distribution of a third exemplary embodiment,
CH 714 241 A2
9a and 9b show the schematic representation of a sintered body coated according to the invention as a component in an evaporator and
10 shows thermal images of a conventional evaporator and of an evaporator with a sintered body coated according to the invention as a heating element.
Tables 1 and 2 show the compositions of the porous sintered body of various exemplary embodiments. Due to their different compositions, the individual exemplary embodiments have different coefficients of thermal expansion. Examples 8 to 10 have, for example, expansion coefficients in the range from 3.2 * 10 "® K" ¹ to 3.8 * 10 "® K" ¹ and are particularly suitable for porous sintered bodies with an electrically conductive coating based on a metal oxide, for example with ITO. In addition, the glasses 8 to 10 are free or at least largely free of sodium, which affects not only the coefficient of thermal expansion but also the transition temperature T _g . These are above 700 ° C and allow high penetration temperatures during the coating process with ITO, so that crack-free or at least largely crack-free, electrically conductive coatings with a particularly high mechanical stability can be obtained.
Glasses 2 to 7, on the other hand, have a relatively high sodium content and correspondingly higher thermal expansion coefficients. They are therefore particularly suitable for the production of porous sintered bodies which are to be coated with a metallic coating. In addition, the glasses of the exemplary embodiments 2 to 7 can be chemically hardened on account of the high sodium content. For example, the sintered body can be chemically prestressed 5 before coating. This increases the mechanical stability of the porous sintered body
1 2 3 4 5 6 7 SiO ₂ 64.0 62.3 62.2 52 60.7 62 61.1 B2O3 8.30.2 4.5 Al2O3 4.0 16.7 18.1 17 16.9 17 19.6 Li ₂ O 5.2 N32O 6.5 11.8 9.7 12 12.2 13 12.1 K ₂ O 7.0 3.8 0.1 4 4.1 3.5 0.9 SrO 0.1 CaO 0.6 60.3 0.1 SnO ₂ 0.4 0.1 0.2 TIO ₂ 4.0 0.8 0.6SÓ2O3 0.6 As2O30.7CI " 0.1 P ₂ O ₅0.1 MgO3.741.2ZrO ₂ 0.1 3.6 1.5 1.5 C © 020.1 0.30.3 ZnO 5.50.1 3.5 Tg [° C]607 505 556 623600 «20-300 ° C [K ¹ ]8.6 * 10 "® 8.5 * 10 "® 9.7 * 10 "® 8.3 * 10 "®8.9 * 10 "® Density [g / cm ³ ]2.4 2.5 2.6 2.42.4
CH 714 241 A2
Table 1: working examples 1 to 7
8th 9 10 11 12 Sio ₂ 59.7 58.8 62.5 74.3 72.8 B2O3 7.8 10.3 10.3 Al2O3 17.1 14.6 17.5 1.3 0.2 Li ₂ ONa ₂ O 13.2 13.9 K ₂ O 0.3 0.1 SrO 7.7 3.8 0.7 BaO 0.1 5.7 CaO 4.2 4.7 7.6 10.7 9.0 SnO ₂ TiO ₂ Sb ₂ O ₃ 0.2 As2O30.7 heP2O5MgO1.2 1.4 0.2 4.0 ZrO ₂ Οθ0 ₂ ZnO
T _g [° C] 719 705573 564 «20-300 ° C [K ¹ ] 3.8 * 10 ^-6 3.73 * 10 ⁶ 3.2 * 10 ^-6 9 * 10 ⁶ 9.5 * 10 ' Density [g / cm ³ ] 2.51 2.49 2.38
Table 2: Embodiments 8 to 12 In FIG. 1 an example of a conventional evaporator with a porous sintered body 2 as a liquid reservoir is shown. Due to the capillary forces of the porous sintered body 2, the liquid 1 to be evaporated is absorbed by the porous sintered body 2 and transported further in all directions of the sintered body 2. The capillary forces are symbolized by the arrows 4. A heating coil 3 is positioned in the upper section of the sintered body 2 in such a way that the corresponding section 2a of the sintered body 2 is heated by thermal radiation. The heating coil 3 is therefore brought very close to the lateral surfaces of the sintered body 2 and should not touch the lateral surfaces if possible. In practice, however, direct contact between the heating wire and the outer surface is often unavoidable.
The evaporation of the liquid 1 takes place in the heating area 2a. This is represented by the arrows 5. The rate of evaporation depends on the temperature and the ambient pressure. The higher the temperature and the lower the pressure, the faster the liquid evaporates in the heating area 2a.
Since the evaporation of the liquid 1 takes place only locally on the lateral surfaces of the heating area 2a of the sintered body, the heating of this local area must take place with relatively high heating powers in order to achieve rapid evaporation within 1 to 2 seconds. Therefore high temperatures of more than 200 ° C have to be used. High heating outputs, in particular in a locally narrowly limited area, can, however, lead to local overheating and thus possibly to decomposition of the liquid 1 to be evaporated and of the material of the liquid reservoir or wick.
CH 714 241 A2 [0097] Furthermore, high heating outputs can also lead to evaporation that is too rapid, so that additional liquid 1 cannot be made available for evaporation quickly enough by the capillary forces. This also leads to overheating of the jacket surfaces of the sintered body in the heating area 2a. Therefore, a unit, for example a voltage, power and / or temperature setting, control or regulation unit (not shown here) can be installed, but this is at the expense of the battery life and limits the maximum amount of evaporation. Disadvantages of the evaporator shown in FIG. 1 and known from the prior art are thus the local heating method and the associated ineffective heat transport, the complex and expensive control unit and the risk of overheating and decomposition of the liquid to be evaporated.
2 shows an evaporator unit known from the prior art, in which the heating element 30 is arranged directly on the sintered body 20. In particular, the heating element 30 is firmly connected to the sintered body 20. Such a connection can be achieved in particular by designing the heating element 30 as a sheet resistor. For this purpose, a ladder-shaped, electrically conductive coating is applied to the sintered body 20 in the manner of a sheet resistance. A coating applied directly to the sintered body 20 as a heating element 30 is advantageous, inter alia, in order to achieve good thermal contact, which enables rapid heating. However, the evaporator unit shown in FIG. 2 also has only a locally limited evaporation surface, so that here too there is a risk of the surface overheating.
3 schematically shows the structure of an evaporator with a sintered body 6 according to the invention. Like the porous sintered body 2 in FIGS. 1 and 2, it is immersed in the liquid 1 to be evaporated. Capillary forces (represented by arrows 4) transport the liquid to be evaporated into the entire volume of the sintered body 6. The sintered body 6 has an electrically conductive coating, the surface formed by the open pores having the electrically conductive one Coating is provided. Thus, when an electrical voltage is applied, the sintered body 6 is heated in the entire volume with a large surface area. Thus, in contrast to the evaporator shown in Fig. 2, the liquid 1 is not only on the lateral surfaces of the sintered body, i.e. formed in a locally limited part of the sintered body 6, but in the entire volume of the sintered body 6. A capillary transport to the jacket surfaces or heated surfaces or elements of the sintered body 6 is therefore not necessary. There is also no risk of local overheating. Since the evaporation in volume is much more efficient than using a heating coil in a locally limited heating area, the evaporation can take place at significantly lower temperatures and a lower heating output. A lower electrical power requirement is advantageous in that the usage time per battery charge increases or smaller accumulators or batteries can be installed.
4 shows the structure of a coated sintered body 6 with open porosity using a schematic cross section through an exemplary embodiment. The coated sintered body 6 has a porous, sintered glass matrix 7 with open pores 8a, 8b. A part of the open pores 8b forms with its pore surface the outer surfaces of the sintered body, while another part of the pores 8a form the inside of the sintered body. All pores of the sintered body have an electrically conductive coating 9.
5 is an SEM image of a sintered body with an electrically conductive coating. The surface of the pores 8 is coated with an ITO layer 9 as an electrically conductive coating. The sintered glass matrix 7 is an aluminum-borosilicate glass with the following composition:
alkali oxides 1 to 11% by weight alkaline earth oxides 1 to 13% by weight B2O3 1 to 20% by weight Al2O3 1 to 17% by weight SiO ₂ 50 to 96% by weight
A glass with the above composition melts very slowly and in a wide temperature range. It is therefore particularly suitable for the production of porous materials using the melting and sintering processes. Glasses from this composition range can have melting temperatures of more than 1000 ° C, which allows the electrically conductive coating to burn in at temperatures up to 900 ° C and which has a positive effect on the coating properties such as density and prevents cracks in the coating. The low linear thermal expansion coefficient (a2o-3oo ° c) of glass reduces thermally induced stresses and thus increases the mechanical stability of the material against temperature differences, such as occur during switching on and off in the evaporator. In addition, the electrically conductive coated glass as a radiator is permanently resistant to temperatures up to 600 ° C.
6 shows an optical micrograph of a sintered body coated with an ITO layer.
CH 714 241 A2 From optical and electron microscopic measurements it was possible to measure on the sintered body shown that the ITO layer has a layer thickness of 200 nm to 2000 nm and surprisingly shows no cracks. This is surprising because the glass (3.3 * 10 "® K" ¹ ) and ITO (7.2 * 10 "® K" ¹ ) have different linear coefficients of thermal expansion.
7 shows the structure of a coated sintered body 60 according to a development of the invention using a schematic cross section. The coated sintered body 60 has a porous, sintered glass matrix 70 with open pores 80, 81, the pores having a bimodal pore size distribution with large pores 80 and small pores 81. A part of the open pores 8b forms with its pore surface the lateral surfaces of the sintered body, while another part of the pores form the inside of the sintered body. All pores of the sintered body have an electrically conductive coating 90. The small pores 81 enable the liquid to be evaporated to be readily and rapidly absorbed into the sintered body, while the large pores 80 enable the steamer to be released quickly. Depending on the application, the ratio of large to small pores and their pore size can be used to set the absorption behavior and the desorption properties during operation of the evaporator.
8 shows the pore size distribution of an exemplary embodiment of the development shown schematically in FIG. 7. The pore size distribution of the porous sintered body has a maximum at approximately 200 μm and a maximum at approximately 600 μm, the proportion of small pores (200 μm) in this exemplary embodiment corresponding to the proportion of large pores (600 μm). The pore size can be adjusted in the manufacturing process by the grain size of the salt used as the pore former, the ratio of large to small pores correspondingly via the ratio of the grain sizes used and their grain size distributions.
9a and 9b schematically show a sintered body 3 coated according to the invention as a component in a possible evaporator. The evaporator has a reservoir with the liquid 1 to be evaporated. The evaporation chamber 11 is separated from the liquid 1 to be evaporated by a steel wall 12. The liquid 1 to be evaporated comes into contact with the coated sintered body 3 through openings (12a, 12b) in the steel wall. The latter sucks in the liquid 1 to be evaporated by capillary forces. By applying a voltage 10 to the electrically conductive coated sintered body 3, the latter is heated in volume, so that the liquid 1 is evaporated in the entire volume of the sintered body 3. The steam is generated until the pores of the sintered body 3 and / or the reservoir no longer contain liquid 1 or the current flow is switched off. When the evaporator is switched off, the pores are sucked full of liquid again by the capillary force, so that when the evaporator is switched on again by the user, sufficient liquid 1 is again available for evaporation.
The maximum possible amount of steam that can be generated is equal to the amount of liquid stored or storable in the porous sintered body 3. The amount of steam that can be generated can thus be controlled, for example, by the dimensions of the sintered body 3 and its porosity. Small sintered bodies with a high porosity have proven to be particularly advantageous with regard to the effectiveness of the evaporation process and the energy consumption and flow of liquid or filling speed.
Fig. 10 shows thermal images of a conventional evaporator (10 b) and an evaporator with a sintered body coated according to the invention as a heating element (10a). While in the evaporator with a sintered body coated according to the invention as the heating element, the evaporation temperatures are in the range of only 127 to 135 ° C, a conventional evaporator with a spiral heating wire as heating element requires evaporation temperatures in the range of 252 to 274 ° C to generate the same or at least a similar amount of steam ,
Table 3 shows the evaporation parameters in a conventional evaporator and in an evaporator with a sintered body coated according to the invention as an exemplary embodiment. The respective vaporizers were operated in a structure analogous to an electronic cigarette. The power was determined by measuring the applied voltage and flowing current with the help of electrotechnical measuring devices, the amount of steam generated was determined by the weight loss of the liquid.
Conventional evaporator embodiment Dimensions OD = 5 mm, ID = 3 mm, length 12 mm Hollow cylinder with OD = 6 mm, ID = 2 mm, length of the cylinder 5 mm Applied voltage 4 V 4 V Required heating output 16 W. 2 W operating temperatur 252-274 ° C 127-135 ° C Amount of steam [milligrams / min Max. 72 minute 72
Table 3: Comparison of evaporators
CH 714 241 A2 As can be seen from Table 3, both evaporators are of a comparable size. In order to generate the same amount of steam as a conventional evaporator, an evaporator with a sintered body coated according to the invention requires a significantly lower heating output and lower evaporation temperatures.
In the exemplary embodiment, the evaporation temperature is significantly below the decomposition temperatures of the typically used, evaporable substances, so that there is also no so-called “coking” of the evaporator by decomposition products, which means that corresponding decomposition products are not to be expected to be released. This increases the life of the evaporator.
Because of the lower heating power required, the evaporator with a sintered body coated according to the invention is also far superior to a conventional evaporator with regard to the energy efficiency and the service life of the electrical energy source.

权利要求:
Claims (35)
[1]
claims
1. Evaporator, comprising a sintered body and an electrically conductive coating, the sintered body being formed by glass or glass ceramic, has an open porosity in the range from 10 to 90%, the electrically conductive coating with the surface of the sintered body, which passes through the open pores is formed, is connected, the electrically conductive coating is part of a heating device of the evaporator, the electrically conductive coating being deposited on the surface of the sintered body and connected to the surface of the sintered body, the electrically conductive coating lining pores which are located inside the Sintered body are so that when an electrical contact is made with the sintered body and a current is applied, this current at least partially flows through the interior of the sintered body and heats the interior of the sintered body.
[2]
2. Evaporator according to claim 1, wherein the sintered body has an open porosity in the range 10 to 90%, preferably from 50 to 80%.
[3]
3. Evaporator according to one of the preceding claims, wherein the open pores of the sintered body have a pore size in the range from 1 μm to 5000 μm, preferably 100 to 800 μm and particularly preferably in the range from 200 to 600 μm.
[4]
4. Evaporator according to one of the preceding claims, wherein the sintered body has closed pores in addition to the open pores, the proportion of closed pores in the total volume of the pores preferably being at most 10% and very particularly preferably at most 5%.
[5]
5. Evaporator according to one of the preceding claims, wherein the pores of the sintered body have an at least bimodal pore size distribution.
[6]
6. Evaporator according to claim 5, wherein the sintered body has large pores with a pore size in the range from 500 to 700 μm and small pores with a pore size in the range from 100 to 300 μm and / or the proportion of the large pores is 5 to 95%.
[7]
7. Evaporator according to one of the preceding claims, wherein the sintered body is formed from glass, preferably from a glass with an alkali content <11% by weight, particularly preferably from a glass with an alkali content <6% by weight.
[8]
8. Evaporator according to claim 7, wherein the glass has a transformation temperature T _g in the range from 300 to 900 ° C, preferably 500 to 800 ° C.
[9]
9. Evaporator according to one of the two preceding claims, wherein the glass is an aluminum borosilicate glass, preferably an aluminum borosilicate glass containing the following components
SiO ₂ : 50 to 85% by weight B ₂ O ₃ : 1 to 20% by weight AI ₂ O ₃ : 1 to 17% by weight
ZNa ₂ O + K ₂ O: 1 to 11% by weight
ZMgO + CaO + BaO + SrO: 1 to 13% by weight.
[10]
10. Evaporator according to one of claims 8 or 9, wherein the sintered body has a linear thermal expansion coefficient a _2O - ₃ oo ° c sintered body of at most 20 * 10 "® K" ^1, preferably less than 11 * 10 "® K" ¹ , particularly preferably less 8 * 10 "® K" ¹ , the electrically conductive coating has a linear thermal expansion coefficient rr.2o-3oo ° c coating in the range from 1 * 10 "® to 20 * 10" ® K “ ¹ and / or the difference between the two thermal expansion coefficient Δαα ₂₀ - ₃₀ ο ° ο = α _2Ο - _3Ο ο ° c coating - a _2O - _3O o ° c sintered body o to 20 * 10 "® K ¹ , preferably 0 to 5 * 10-6 K" ¹ .
[11]
11. Evaporator according to one of the preceding claims, wherein the sintered body provided with the electrically conductive coating has an electrical conductivity in the range from 0.001 to 10 ⁶ S / m, preferably in the range from 10 to 600 S / m.
CH 714 241 A2
[12]
12. Evaporator according to one of the preceding claims, wherein the electrically conductive coating by a metal oxide, preferably by a metal oxide from the group consisting of indium tin oxide (ITO), aluminum-doped zinc oxide (AZO), fluorotin oxide (FTO) and / or antimony tin oxide (ATO ) is formed.
[13]
13. Evaporator according to claim 12, wherein the layer thickness of the electrically conductive coating is 1 nm to 1000 μm, preferably 200 nm to 200 μm.
[14]
14. Evaporator according to one of the preceding claims 1 to 11, wherein the electrically conductive coating is formed by a metal, preferably by silver, gold, platinum and / or chromium.
[15]
15. Evaporator according to claim 14, wherein the layer thickness of the electrically conductive coating is 1 nm to 1000 μm, preferably 10 nm to 100 nm.
[16]
16. Vaporizer according to one of the preceding claims, wherein the vaporizer is a component of an electronic cigarette or a component of a medical inhaler.
[17]
17. Evaporator according to one of the preceding claims, wherein the sintered body to which the electrically conductive coating is applied has an electrical resistance in the range from 0.2 to 5 ohms, and with a voltage in the range from 1 to 12 V and / or with a heating power of 1 to 80 W is operated.
[18]
18. Evaporator according to one of claims 1 to 16, wherein the sintered body to which the electrically conductive coating is applied has an electrical resistance in the range from 0.2 ohms to 3000 ohms, and the evaporator with a voltage in the range from 110 to 380 V and / or is operated with a heating power of 10 to 1000 W.
[19]
19. Evaporator according to one of the preceding claims, wherein the evaporator has a mechanical electrical contact or an electrical contact through an electrically conductive connector or an integral electrically conductive connection, preferably a soldered connection.
[20]
20. Evaporator according to one of the preceding claims, wherein the electrically conductive coating in addition to the electrically conductive component has at least one further, preferably antimicrobial and / or antibacterial component, particularly preferably silver, ZnO and / or TiO ₂ .
[21]
21. Use of an evaporator according to one of the preceding claims as a component in an electronic cigarette, a medical inhaler, a fragrance dispenser or a room humidifier.
[22]
22. A method for producing an evaporator, in particular an evaporator according to claim 1, comprising at least the following process steps:
a) providing a sintered body made of glass, ceramic or glass ceramic with an open porosity in the range of 10 to 90% and
b) coating the surface of the sintered body formed by the open pores, including the surface of pores in the interior of the sintered body, with an electrically conductive coating.
[23]
23. The method according to claim 22, wherein in step a) a sintered body made of glass, preferably a sintered body made of glass with an alkali content <11% by weight, particularly preferably a sintered body made of aluminum borosilicate glass is provided.
[24]
24. The method according to any one of the preceding claims 22 to 23, wherein in step b) the electrically conductive layer by condensation or removal of solid from a dispersion, condensation or removal of solid from a solution, condensation or removal of solid from the gas phase or by a galvanic process is deposited on the entire surface of the sintered body formed by the surface of the open pores.
[25]
25. The method according to claim 24, wherein the electrically conductive coating deposited in step b) by a metal oxide, preferably a metal oxide selected from the group metal oxide from the group consisting of indium tin oxide (ITO), aluminum doped zinc oxide (AZO), fluorine tin oxide (FTO ) and / or antimony tin oxide (ATO), particularly preferably formed by ITO.
[26]
26. The method according to claim 25, wherein the metal oxide in step b) is deposited by condensation or precipitation from a solution or dispersion, preferably from a dispersion.
[27]
27. The method according to claim 26, wherein the metal oxide by a dipping process, preferably by a dipping process, comprising at least the following process steps a2) providing the sintered body b2) providing a dispersion or solution of the metal oxide c2) immersing the sintered body in the one provided in step c2) dispersion for a predefined _time, dive ^ and d2) burn in the obtained by the step c2) layer for a predefined time period t _firing at a predetermined firing temperature T brand _a ·
[28]
28. The method according to claim, wherein in step d2) a firing temperature T _A brand in the range of 60 to 1000 ° C, preferably 300 to 900 ° C is selected 27th
CH 714 241 A2
[29]
29. The method according to claim 27 or 28, wherein the baking of the electrically conductive coating takes place under inert gas, under vacuum or under a reducing atmosphere.
[30]
30. The method according to any one of the preceding claims 27 to 29, wherein the layer thickness of the deposited electrically conductive coating is 1 nm to 800 μm, preferably 200 nm to 200 μm, particularly preferably 200 nm to 10 μm.
[31]
31. The method according to any one of the preceding claims 27 to 30, wherein the solids content of the dispersion provided in step c2) is 1 to 50% by weight, preferably 20 to 35% by weight.
[32]
32. The method according to any one of the preceding claims 27 to 31, wherein steps c2) and / or d2) are carried out several times, preferably 2 to 3 times.
[33]
33. The method according to any one of the preceding claims 23 to 27, wherein the electrically conductive coating deposited in step b) is formed by a metal, preferably by silver, gold, platinum and / or chromium.
[34]
34. The method according to claim 33, wherein the metal is electrolytically deposited from a solution or dispersion or galvanically.
[35]
35. Evaporator head with a sintered body according to one of claims 1 to 20 in a housing, and electrical contacts for connecting the sintered body.

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同族专利:

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公开号 | 公开日

---

CN109608048A|2019-04-12|

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US10617154B2|2020-04-14|

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JP6576535B2|2019-09-18|

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DE102017123000B4|2021-05-12|

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GB2567319A|2019-04-10|

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DE102017123000A1|2019-04-04|

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CH714241B1|2019-08-15|

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US20190098935A1|2019-04-04|

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GB2567319B|2019-10-16|

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JP2019062895A|2019-04-25|

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法律状态:

优先权:

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申请号 | 申请日 | 专利标题

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DE102017123000.9A|DE102017123000B4|2017-10-04|2017-10-04|Sintered body with conductive coating, method for producing a sintered body with conductive coating and its use|

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