• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Composition and shaping of ceramic material with low coefficient of thermal expansion and high resistance to thermal shock. The present invention is a composition and shaping of ceramic material comprising at least one frit and at least one inorganic raw material. Some of the advantages are that it requires a thermal treatment not higher than 1180ºC, that the duration of said thermal treatment is not more than 60 minutes, that after the thermal treatment has a coefficient of thermal expansion of less than 25 x 10-7ºC-1 in the temperature range between 25ºC and 500ºC and that has a high resistance to thermal shock, supporting at least 10 consecutive cycles of thermal shock between 600ºC and 25ºC without the formation of cracks or structural changes. Composition of ceramic material that is formed by uniaxial pressing, band pressing, cast molding, extrusion, injection molding or lamination.
    公开号:ES2687800A1
    申请号:ES201730419
    申请日:2017-03-27
    公开日:2018-10-29
    发明作者:Carlos CONCEPCIÓN HEYDORN；Francisco Sanmiguel Roche；Óscar RUIZ VEGA；Vicente FERRANDO CATALÁ
    申请人:Torrecid SA；
    IPC主号:
    专利说明:

    Object of the invention
    The present invention relates to a composition and forming of ceramic material that has a low coefficient of thermal expansion (CDT) and a high resistance to thermal shock or sudden temperature changes, once subjected to a heat treatment with a maximum temperature of 1180 ° C and with a maximum duration of 60 minutes.
    Thanks to these two properties, the ceramic material object of the invention is intended to
    10 those applications that require stability at high temperatures and that are subject to heating and cooling cycles. Examples of applications, but not limited to, are ceramic tiles, radiators, heaters, heaters, high temperature particle filters, kitchen surfaces and countertops and work surfaces in laboratories.
    The present invention is encompassed within ceramic materials that require prior heat treatment and that are intended for high temperature or thermal shock applications. Description of the state of the art
    Ceramic materials with low thermal expansion coefficient are especially useful
    20 in applications where heating and cooling cycles take place as well as sudden temperature changes, also known as thermal shock.
    In fact, in the prior art prior to the present invention, ceramic material compositions are described which, after a heat treatment, are characterized by a low coefficient of thermal expansion.
    Thus, patent US8257831B2 protects a composition of ceramic material composed essentially of SiO2, Al2O3 and Li2O including P2O5 and characterized in that, once subjected to a thermal treatment of fusion, nucleation and crystallization, it has a coefficient of thermal expansion between 10x107ºC1 and 50x107 ° C in the temperature range of 25 ° C to 100 ° C. Likewise, US8257831B2 patent is characterized by
    30 use heat treatment temperatures between 600ºC and 1500ºC and with a duration


    the same between 2 hours and 40 hours. In addition, the presence of P2O5 in the composition reduces the chemical resistance of the final product.
    On the other hand, patent application WO2004094334A2 describes a composition of ceramic material containing as main phase the compound of formula CaAl4O7 as a result of a heat treatment between 1450 ° C and 1600 ° C and characterized by having a coefficient of thermal expansion lower than 10x107ºC1 in the temperature range between 25ºC and 800ºC and a high resistance to thermal shock. In addition, as described in WO2004094334A2, the heat treatment time is 6 hours. In addition, the composition according to the patent application
    WO2004094334A2 includes Fe2O3 that would color it unnecessarily or, in case of using pigments, forcing pigmentation corrections.
    Also, patent application WO2011008938A1 discloses a composition of ceramic material of formula MgxAl2 (1 + x) Ti (1 + x) O5 (0≤x <1) as a result of heat treatment between 1200 ° C and 1700 ° C, preferably between 1400 ° C and 1600 ° C , of a mixture comprising the raw materials, expressed in oxides, TiO2, Al2O3, MgO and SiO2. The ceramic material is characterized by a coefficient of thermal expansion less than 30.0x107K1 in the temperature range between 30ºC and 1000ºC. Additionally, said application WO2011008938A1 preferably includes the use of frits as a source of SiO2 due to its industrial availability as well as feldspar as a source of Al2O3. As for the time of
    The heat treatment, as indicated in the examples, is not less than 34 hours. In addition, the raw materials based on TiO2 and Al2O3 are refractory, that is, high melting point, requiring high temperatures, preferably between 1400 ° C and 1600 ° C to achieve correct sintering and therefore the target properties.
    The ceramic materials described in the previous patents have the drawbacks
    25 particulars indicated in addition to the common one that all require temperatures above 1200ºC, in some cases reaching 1600ºC, and high heat treatment times, not less than 2 hours.
    Based on these limitations in the current state of the art, the objective of the present invention is a composition of ceramic material of low thermal expansion coefficient 30 and high resistance to thermal shock characterized by solving existing technical problems and requiring a heat treatment with a maximum temperature of 1180ºC and a


    Duration not exceeding 60 minutes. This decrease in temperature and time of heat treatment also provides a reduction in energy consumption and therefore in cost and environmental impact. Description of the invention
    Throughout the invention and the claims the word "comprises" and its variants are not intended to exclude other technical characteristics, additives, components or steps. For those skilled in the art, other objects, advantages and features of the invention will be derived partly from the description and partly from the practice of the invention.
    The present invention is a ceramic material comprising at least one frit and at
    10 minus an inorganic raw material. Some of the advantages are that it requires a heat treatment at a maximum temperature of 1180ºC, that the duration of said heat treatment is not more than 60 minutes, which, after the heat treatment, has a coefficient of thermal expansion of less than 25 x107ºC1 in the temperature range between 25 ° C and 500 ° C and which has a high resistance to thermal shock.
    The term "heat treatment" as used in the present invention refers to a thermal cycle that makes it possible to transform a shaped powder product into a compact and coherent one, as a result of the physical-chemical bonding of the initial components and which can additionally cause chemical reactions of transformation of the initial components into new chemical species
    The frits used in the present invention have the function of lowering the maximum heat treatment temperature and acting as a binder between the other ceramic components of the material. For this purpose, the frits have a coefficient of thermal expansion between 18x107ºC1 and 50x107ºC1 in the temperature range between 25ºC and 500ºC and are in the composition of the ceramic material in a percentage by weight
    25 between 15% and 45%, preferably between 15% and 35%. The main components of frits, expressed in oxides, are indicated below. The final value of each component of the frit will depend on the final thermal expansion coefficient to be achieved.
    Element% by weight


    SiO2 5060% Al2O3 825% Li2O 110% B2O3 530% CaO 0.110% MgO 0.15% TiO2 02.5% ZnO 010% BaO 010% ZrO2 03%
    Na2O 02%
    K2O 02% It should be noted that although the main elements of the frit are expressed in oxides, in the formulation of the frit both oxides and inorganic salts (carbonates, silicates, nitrates, feldspars, among others) of the corresponding cations can be used.
    In the present invention, "fried" is understood as the result of a mixture of inorganic compounds that has undergone a melting and subsequent cooling process to obtain an amorphous glassy compound, that is, without a crystalline structure.
    Another aspect of the present invention is that the ceramic material contains in its composition at least one inorganic raw material in a weight percentage between 55% and 85%.
    The term "inorganic raw material" as used in the present invention refers to any chemical compound other than the frits which is incorporated directly into the composition of the ceramic material object of the invention and selected from magnesium carbonate, calcium carbonate, spodumene, montmorillonite clays, preferably bentonite, kaolinitic clays, preferably kaolin, wollastonite, dolomite, cordierite,
    15 kaolinite, illite, nepheline, zinc oxide, aluminum oxide, titanium oxide, magnesium silicate, zirconium silicate, zirconium oxide, feldspars, sodium aluminosilicate, potassium aluminosilicate, magnesium aluminosilicate, boric acid or mixture from them.
    In a preferred embodiment, the inorganic raw material of the ceramic material comprises spodumene -LiAl (SiO3) 2 in a weight percentage comprised between 55% and 85%.


    In another preferred embodiment the ceramic material composition contains at least one ceramic pigment, with a particle size D100 of up to 5 micrometers if, additionally, it is required to provide chromatic and / or optical properties to the composition. In this case, the ceramic pigments are found in the composition of ceramic material in a weight percentage between 0% and 10% and are selected from simple oxides, mixed oxides and crystalline structures of any composition.
    The ceramic material object of the invention can be shaped by any of the existing industrial methods. Examples, by way of example but not limitation, are uniaxial pressing, band pressing, casting molding, extrusion, injection molding and lamination among others. In order to facilitate the forming, the composition may also include specific additives to facilitate said process, in a weight percentage comprised between 0% and 5%. Examples of additives, by way of example but not limitation, are acrylic derivatives, polyvinyl alcohol and their derivatives and cellulose derivatives.
    The present invention also includes the option of applying, on the surface of the ceramic material formed and prior to heat treatment, a composition called "surface layer" intended to increase properties such as chemical resistance, resistance to cleaning agents, scratch resistance and / or resistance to corrosion, as well as to reduce roughness. Said surface layer is applied by the different deposition techniques of ceramic materials such as fillet, bell, disc, gun, screen printing, inkjet, etc. The surface layer composition may contain a ceramic pigment with a D100 particle size of up to 5 micrometers and in a weight percentage between 5% and 15%, silicon dioxide with a D100 particle size of up to 2 micrometers and in a weight percentage between 0% and 10%, zirconium silicate with a D100 particle size of up to 5 micrometers and a weight percentage between 5% and 15%, zinc oxide with a D100 particle size of up to 5 micrometers and in a weight percentage between 0% and 10%, a silicon alkoxide that is liquid at room temperature, also known as organosilane, in a weight percentage comprised between 70% and 95% or a mixture thereof. Finally, it can also contain water whose content will vary depending on the application technique.
    In a preferred embodiment of the invention, the forming and heat treatment of the ceramic material composition is carried out by uniaxial pressing and using a


    process according to the usual production methods in the manufacture of ceramic tiles comprising the following stages:
    (1) Joint milling of a ceramic material composition according to the invention,
    additives for grinding and water until a D100 particle size of up to 40 microns is achieved.
    (2) Addition of at least one ceramic pigment, if required, and additives for forming by uniaxial pressing, if necessary.
    (3) Atomization of the previous mixture to obtain atomized particles with a granulometric distribution D100 between 100 micrometers and 600 micrometers.
    10 Atomization means an industrial process that allows the transformation of suspended solids into spherical and hollow particles. The process is characterized by spraying a suspension or dispersion, normally aqueous, of the material through a nozzle in the opposite direction to a stream of hot air. As a consequence, the formation of spherical and hollow particles of the material that is called atomizing occurs.
    15 (4) Uniaxial pressing in order to achieve pieces of ceramic material object of invention either smooth or with a certain relief and of a thickness of 3 mm or more.
    (5) Optionally, a composition called "surface layer" can be applied on the surface of the previously formed part.
    (6) Drying of the shaped part at a temperature between 100ºC and 200ºC.
    20 (7) Heat treatment of the piece formed at a maximum temperature of 1180ºC and a time not exceeding 60 minutes.
    As indicated above, the ceramic material object of the present invention has a thermal expansion coefficient of less than 25x107 ° C in the temperature range between 25 ° C and 500 ° C. The measurement of the thermal expansion coefficient 25 (also known by the acronym CDT) is widely known by a person skilled in the art and is carried out by means of a dilatometer (of the BAHR brand type Model DIL801L THERMO ANALYSE or the like). For this, a piece of ceramic material of dimensions 10 cm x 10 cm is prepared and cooked at the heat treatment temperature in accordance with the present invention. Once the cooking is done, a piece of the piece of 5 is cut


    cm long and 3 cm wide and polished until it adopts a cylindrical shape. Once the cylinder is obtained, it is introduced into the dilatometer to measure the CDT in the desired temperature range.
    In accordance with the present invention, the ceramic material composition resulting from the
    5 heat treatment is characterized by supporting at least 10 consecutive cycles of thermal shock between 600 ° C and 25 ° C without the formation of cracks or structural changes. For the measurement of the resistance to thermal shock, the ceramic material object of the invention is formed in a test tube of 10 cm x 10 cm and 4 mm thick and is subjected to the corresponding heat treatment according to the present invention. Once the treatment
    10 thermal, the evaluation of resistance to thermal shock begins. For this, the piece is placed in an oven and heated to 600 ° C, keeping at that temperature for 10 minutes. It is then removed from the oven and suddenly placed in a water bath at 25 ° C for 5 minutes. After this time, the bathroom part is removed and an inspection is performed to detect the presence of cracks or other defects. If the piece
    15 remains unchanged, the heating cycle is repeated at 600 ° C, immersion in a water bath at 25 ° C and evaluation until the presence of cracks or structural changes is detected. If the piece resists 10 consecutive cycles, it is considered to have a high resistance to thermal shock.
    In certain applications such as laboratory work surfaces and
    20 outdoor applications, it is also very important that the ceramic material does not absorb liquids to avoid effects such as frost rupture, degradation by chemical agents, low stain resistance, etc. In this sense, the ceramic material object of the present invention is characterized by having a water absorption of less than 1%. The average water absorption allows to evaluate the impermeability of the material. The method
    Measurement consists of submerging a piece of ceramic material of dimensions 5 cm x 5 cm and 6 mm thick and of known mass (m0), in a water bath at a temperature of 25 ° C for 24 hours. After that time the piece is dried at 25 ° C for 15 minutes to remove surface water and weighed again, noting its mass (m1). Finally the ratio between (m1m0) / m0 expressed as a percentage, indicates the percentage of absorption
    30 of water
    Preferred forms of realization


    To complete the description that is being made and in order to help a better understanding of its characteristics, several examples of realization of the ceramic material object of the present invention are attached to the present specification.
    All the examples of embodiment described are by way of example and not limitation.
    5 Seven ceramic material compositions according to the present invention called C1, C2, C3, C4, C5, C6 and C7 respectively were prepared. In composition C3 a blue ceramic pigment was included which allows the ceramic material to be colored. All compositions are expressed as percentage by weight.
    Components C1C2C3C4
    Frit 1 (CDT = 45x107 ° C) 24%31.5%twenty%25%
    Fried 2 (CDT = 18x107 ° C) fifteen%
    Spodumene 70%55%56%fifty%
    Cordierite
    Bentonite one%one%one%one%
    Dolomite 10%
    ZnO 4%3%4%
    Kaolin 3.5%5%5%
    ZrSiO4 5%5%0.5%
    Blue ceramic pigment Cobalt spinel structure 4.5%
    Components C5C6C7
    Frit 1 (CDT = 45x107 ° C) 9%fifteen%fifteen%
    Fried 2 (CDT = 18x107 ° C) 36%
    Spodumene 84%85%
    Cordierite 47%
    Bentonite one%0.5%
    Dolomite 0.5%
    ZnO
    Kaolin 2%
    ZrSiO4 5%


    Blue ceramic pigment Cobalt spinel structure
    Examples 1,2, 3, 4, 5, 6 and 7. Formed by uniaxial pressing using the usual technical means in the manufacture of ceramic tiles.
    From the compositions C1, C2, C3, C4, C5, C6 and C7 described above,
    5 made a forming of each of them using an industrial uniaxial press commonly used in the manufacture of ceramic tiles, in order to get pieces of 30 cm x 30 cm and 10 mm thick, called respective P1, P2, P3, P4 , P5, P6 and P7. Part P1 was obtained from composition C1, P2 from composition C2, P3 from composition C3, P4 from composition C4,
    10 P5 from composition C5, P6 from C6 and P7 from composition C7.
    The process of forming and heat treatment of the compositions C1, C2, C3, C4 C5, C6 and C7 comprised the following steps:
    (1) Grinding of each composition C1 to C7 with additives for grinding and water until a D100 particle size of up to 40 micrometers is achieved.
    15 (2) Addition of 2% by weight of the mixture according to step 1 of acrylic binder as a forming additive, except in composition C7 that 2% of said acrylic binder and 1% of polyvinyl alcohol was added.
    (3) Atomization of the previous mixture to obtain atomized particles with a D100 granulometric distribution between 100 micrometers and 600 micrometers.
    20 (4) Uniaxial pressing with a pressure of 400 Kg / cm2 to get pieces of 30 cm x 30 cm and a thickness of 10mm.
    (5) Drying the pieces at a temperature of 150 ° C for 20 minutes.
    (6) Heat treatment of parts in an industrial gas oven commonly used
    in the manufacture of ceramic tiles at a maximum temperature of 1120ºC and with a duration of 50 minutes.


    Once the indicated heat treatment was carried out, each piece of ceramic material had the following properties. As indicated, all the pieces passed the thermal shock resistance test, after at least 10 consecutive cycles.
    Properties P1P2P3P4
    CDT (α25ºC500ºC) (x107ºC1) 11.99twenty18.5025
    Heat shock resistance 10101010
    Water absorption (%) 0.085%0.065%0.050%0.050%
    Stain resistance (ISO 1054514: 1995) 4555
    Chemical resistance (UNEEN ISO1054513) A classA classA classA class
    Properties P5P6P7
    CDT (α25ºC500ºC) (x107ºC1) 25.0113.7512.10
    Heat shock resistance 101010
    Water absorption (%) 0.15%0.050%0.050
    Stain resistance (ISO 1054514: 1995) 544
    Chemical resistance (UNEEN ISO1054513) A classA classA class
    5 Example 8. Formed by uniaxial pressing using the usual technical means in the manufacture of ceramic tiles with application of a surface layer.
    Additionally, another piece (P8) consisting of the composition of ceramic material C1 was prepared on which, once formed by uniaxial pressing, a surface layer composition was applied. The composition of the surface layer made as a
    10 example, indicated below:
    Surface layer components % in weigh
    ZrSiO4 5
    SiO2 (Cabosil®, Cabot Corporation) 5
    Water hydrolyzed epoxysilane 90


    The forming procedure for said compositions comprised the following steps:
    (1) Joint milling of composition C1 with milling additives and water until a D100 particle size of up to 40 micrometers is achieved.
    5 (2) Addition of 2% by weight of the mixture according to step 1 of acrylic binder as forming additive.
    (3) Atomization of the previous mixture to achieve atomized particles with a D100 granulometric distribution between 100 micrometers and 600 micrometers.
    (4) Uniaxial pressing with a pressure of 400 Kg / cm2 to get pieces of 30 cm x 30 10 cm and a thickness of 10 mm.
    (5) Application of the composition of the surface layer by airbrushing by depositing a weight of 7.5 g / m2 on the surface of the piece formed in step (4).
    (6) Drying the piece at a temperature of 150 ° C for 20 minutes.
    (7) Heat treatment of the part in an industrial gas oven commonly used
    15 in the manufacture of ceramic tiles at a maximum temperature of 1120ºC and with a duration of 50 minutes.
    The following table shows the properties of the part obtained from example 1 (P1) and example 8 (P8).
    Properties P1P8
    CDT (α25ºC500ºC) (x107ºC1) 11.9911.89
    Heat shock resistance 1010
    Water absorption (%) 0.085%0.060%
    Roughness (micrometers) 5.152.85
    Stain resistance (ISO 1054514: 1995) 45
    Chemical resistance (UNEEN ISO1054513) A classA class


    The results indicate that the P8 part, which contains the surface layer, improves stain resistance and decreases the surface roughness by 2.3 micrometers. On the other hand, both pieces passed the thermal shock resistance test.
    5 Examples 9 and 10. Formed by extrusion.
    From the compositions C1 and C3 described above, a forming of each of them was carried out by extrusion using the conventional manufacturing procedures generally used in the industry in order to achieve laminated pieces of 30 cm x 30 cm and 5 mm of thickness, respectively named P9 and P10.
    10 Part P9 was prepared from composition C1 and P10 from composition C3. Once both pieces were formed, a heat treatment was carried out at a temperature of 1170ºC and with a duration of 55 minutes.
    The following table shows the properties of the parts obtained according to the invention.
    Property P9P10
    CDT (α25ºC500ºC) (x107ºC1) 12.4014.10
    Heat shock resistance 1010
    Water absorption (%) 0.080%0.060%

    权利要求:
    Claims (7)
    [1]
    1. A composition of ceramic material to conform characterized in that it comprises:
    At least one frit in a weight percentage between 15% and 45% with a thermal expansion coefficient between 18x107 ° C and 50x107 ° C in the range of 5 temperatures between 25 ° C and 500 ° C, and
    At least one inorganic raw material in a weight percentage between 55% and 85%.
    [2]
    2. The composition according to claim 1, wherein the inorganic raw material comprises spodumene in a weight percentage between 55% and 85%.
    The composition according to any of the preceding claims, wherein the percentage by weight of the frit is between 15% and 35%.
    [4]
    4. The composition according to any of the preceding claims, comprising at least one ceramic pigment with a D100 particle size of up to 5 micrometers and in a weight percentage comprised between 0% and 10%.
    5. Atomized particle for uniaxial pressing characterized in that it comprises: a composition of ceramic material according to claims 1 to 4,
    grinding additives,additives for forming by uniaxial pressing,a granulometric distribution D100 comprised
    20 micrometers
    [6]
    6. Procedure for obtaining an atomized particle characterized in that it comprises:
    between 100 micrometers and 600
    for uniaxial pressing
    (one) Joint milling of the ceramic material composition according to claims 1 to 4 with additives for grinding and water until a D100 particle size of up to 40 micrometers is achieved,
    (2) Addition of additives for forming by uniaxial pressing, and

    (3) Atomization of the previous mixture to obtain atomized particles with a D100 granulometric distribution between 100 micrometers and 600 micrometers.
    [7]
    7. A shaped ceramic material characterized in that it comprises:
    5 a composition of ceramic material according to any one of claims 1 to4, and
    ºC1
    a coefficient of thermal expansion less than 25x107 in the temperature range between 25ºC and 500ºC
    [8]
    8. Method for obtaining a shaped ceramic material according to claim 10, characterized in that it comprises at least the following steps:
    (one) Mixing of a ceramic material composition according to claims 1 to 4,
    (2) Forming the mixture, and
    (3) Heat treatment of the mixture formed at a maximum temperature of 1180 ° C and a duration not exceeding 60 minutes to obtain a ceramic material with a
    15 coefficient of thermal expansion less than 25 x107ºC1 in the temperature range between 25ºC and 500ºC.
    [9]
    9. Method according to claim 8, wherein the step of forming the mixture is performed by uniaxial pressing and / or band pressing and / or casting and / or extrusion molding and / or injection molding and / or lamination.
    Method according to claim 8, characterized in that the step of forming the mixture comprises at least:
    (one) Obtaining atomized particles for uniaxial pressing according to claim 6, and
    (2) Uniaxial pressing of said atomized particles.
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    同族专利:
    公开号 | 公开日
    ES2687800B1|2019-08-06|
    US20210101837A1|2021-04-08|
    EP3584233A4|2020-12-02|
    WO2018178436A1|2018-10-04|
    EP3584233A1|2019-12-25|
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    优先权:
    申请号 | 申请日 | 专利标题
    ES201730419A|ES2687800B1|2017-03-27|2017-03-27|COMPOSITION AND CONFORMING OF CERAMIC MATERIAL OF LOW COEFFICIENT OF THERMAL DILATATION AND ELEVATED RESISTANCE TO THERMAL SHOCK|ES201730419A| ES2687800B1|2017-03-27|2017-03-27|COMPOSITION AND CONFORMING OF CERAMIC MATERIAL OF LOW COEFFICIENT OF THERMAL DILATATION AND ELEVATED RESISTANCE TO THERMAL SHOCK|
    PCT/ES2018/070161| WO2018178436A1|2017-03-27|2018-03-06|Composition and shaping of a ceramic material with low thermal expansion coefficient and high resistance to thermal shock|
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