• 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:
    The present invention relates to a vapor phase diamond deposition equipment comprising: - a vacuum reactor (1) comprising a reaction chamber connected to a vacuum source, - a substrate holder (3) disposed in the reactor according to the invention. the invention comprises a system for holding the filaments (4) in a vertical position. The filaments (5) are positioned inside the substrates to be treated (6), in order to make it possible to produce diamond deposits on their internal face.
    公开号:CH710471A1
    申请号:CH01941/14
    申请日:2014-12-15
    公开日:2016-06-15
    发明作者:Provent Christophe；Rats David
    申请人:Neocoat Sa；
    IPC主号:
    专利说明:

    Technical area
    The present invention relates to the field of diamond deposition on the inner surface of a substrate, particularly to diamond deposition in the vapor phase.
    State of the art
    Diamond is a material with exceptional properties such as its high hardness, its high Young's modulus or its high thermal conductivity. It can be synthesized in a thin layer using the chemical vapor deposition (CVD) method by thermally or plasma activating a gaseous mixture containing at least one precursor of carbon and hydrogen. The activation of the gas phase makes it possible to create radical species such as atomic hydrogen or the methyl radical with a concentration sufficient to ensure the rapid growth of a diamond layer of high crystalline quality.
    [0003] Various applications of the diamond layers require the coating of tubular or hollow substrates inside with a layer of polycrystalline diamond, which can not, or very difficultly, be achieved with the techniques generally used.
    The use of a thermal activation of the reaction gas mixture by hot filament (HFCVD for Hot Filament Chemical Vapor Deposition) is known. This technique allows deposits on large surfaces (> 0.5m <2>) but the vertical or horizontal filament arrangements used allow to deposit diamond only on 2D substrates. It is possible to deposit inside objects such as rings or portions of open spheres, but the deposits are uniform only about ten millimeters in depth, which strongly limits the potential applications.
    The use of plasma technology for the deposition of polycrystalline diamond is known. However, the known devices use either a microwave cavity or a two-dimensional plasma sheet, and have the same limitations on the shape of the substrates as the hot filament technique.
    It is known to generate a plasma inside a tube for depositing diamond inside thereof. However, the substrate material must be transparent to microwaves, which limits its use to materials such as silica or alumina.
    The present invention aims to solve these problems.
    Disclosure of the invention
    More specifically, the invention relates to an equipment and a deposit method implementing this equipment, as mentioned in the claims.
    Brief description of the drawings
    Other details of the invention will appear more clearly on reading the description which follows, given with reference to the accompanying drawing in which:<tb> fig. 1 <SEP> is a view representing a diamond deposition equipment according to the invention,<tb> fig. 2 <SEP> gives illustrations of examples of substrates that can advantageously be coated with diamond according to the invention,<tb> fig. 3 <SEP> gives an illustration of the position of the filaments inside the substrate to be coated, here shown in section,<tb> figs. 4, 5 and 6 <SEP> give illustrations of the different possible configurations of the arrangement of the filaments in the deposition equipment of FIG. 1 in order to obtain uniform diamond deposits according to the section of the substrate to be coated,
    Embodiment of the invention
    As mentioned above, it is possible to produce polycrystalline diamond deposits by advantageously implementing hot filament chemical vapor deposition technology on the inner surface of various substrates. which will be defined below.
    According to the invention, these deposits are made on the inner surface of tubular substrates by implementing hot filament deposition technology with equipment as proposed in FIG. 1.
    This deposition system 1 comprises a vacuum reactor 2, a substrate holder 3, a system for arranging the filaments 4, filaments 5 and a substrate 6 is introduced thereto.
    The substrate shown diagrammatically in profile view in FIG. 2. 1 has a height, H, and a length, D. The substrate may be of rectangular section of length, D, and width, d, as shown in FIG. 2. 2, or of elliptical section length, D, and width, d, as shown in FIG. 2. 3, or have any other type of polygonal section as shown in FIG. 2. 4.
    The distance between the filament and the surface to be coated, S, is described in FIG. 3 is generally between 1 to 100mm, typically 20mm. It significantly influences the temperature of the surface and therefore the rate of growth and the thickness of diamond deposited. It is therefore necessary to obtain a uniform layer on the circumference of the substrate that the arrangement of the filaments has a geometry close to the section of the substrate to be coated.
    The filament holding system 4 is designed to accommodate one or more filaments 5 held on a suitable mechanical part 7 as described in FIGS. 4, 5 and 6. The mechanical piece for holding the filaments has a length, D ", equal to the length, D, of the substrate minus the distance to the filaments, S, and a width, of, equal to d minus S.
    When the substrate section to be coated is rectangular as described in FIG. 2. 2, the filament holding system installed in the deposition reactor has a rectangular shape as described in FIG. 4.
    When the substrate section to be coated is elliptical as described in FIG. 2. 3, the filament holding system installed in the deposition reactor has an elliptical shape of length as described in FIG. 5.
    When the section of the substrate to be coated is polygonal as described in FIG. 2. 4, the filament holding system installed in the deposition reactor has a polygonal shape as described in FIG. 6.
    By implementing this installation, it can thus perform a polycrystalline diamond deposit on a hollow part as proposed in FIG. 2, This hollow part is defined by its height, H, whose dimension is between 10 and 1000mm and its length, D, and its width, d, whose dimensions are between 40mm and 400mm.
    Such a part can be made using at least one material chosen from the following materials: refractory metals and derivatives, transition metals and derivatives, titanium-based alloys, cemented carbides, silicon-based alloys , glasses, oxides (fused silica, alumina), other materials coated with a thin layer of the above-mentioned materials.
    In a particular example, the substrate is niobium, rectangular in shape as described in FIG. 2. 2 (H = 200 mm, d = 60 mm and D = 100 mm), only inoculated by a method of the state of the art.
    Before the deposition, a filament holding system is installed in the vacuum reactor. The filament holding member has a rectangular geometry as described in FIG. 4 with the dimensions D '= 60mm, and d = 20mm, the filaments have a length of 500mm and are located 20mm from the inner surface of the substrate.
    A 5 μm layer of microcrystalline diamond doped with boron is deposited using the hot filament chemical vapor deposition method by means of an installation as described above with the following deposition conditions:Filing time = 40 hoursSubstrate temperature = 800 ° C,Working pressure = 100 mbar.
    A control of the thickness of the deposited layer (measurement on metallographic sections) and the quality of the deposit (measurement by Raman spectrometry) shows that the variation of uniformity (calculated by the formula = (min-max) / average) is less than 10% over the entire area deposited.
    According to a second particular example, the substrate is fused silica, circular in shape as described in FIG. 2. 3 (H = 400 mm, d = 80 mm and D = 80 mm), only inoculated by a method of the state of the art.
    Before the deposition, a filament holding system is installed in the vacuum reactor. The filament holding member has a circular geometry as described in FIG. With the dimensions D = 30mm and 30mm, the filaments have a length of 500mm and are located 25mm from the inner surface of the substrate.
    A layer of 300 nm nanocrystalline diamond is deposited using the hot filament chemical vapor deposition method by means of an installation as described above with the following deposition conditions:Filing time = 4 hoursSubstrate temperature = 750 ° C,Working pressure = 30 mbar.
    A control of the thickness of the deposited layer (measurement on metallographic sections) and the quality of the deposit (measurement by Raman spectrometry) shows that the variation of uniformity (calculated by the formula = (min-max) / average) is less than 10% over the entire area deposited.
    According to a third particular example, the substrate is made of titanium base alloy (Ti-4AI-6V), of hexagonal shape as described in FIG. 2. 4 (H = 300mm, d = 100mm and D = 100mm), only seeded by a method of the state of the art.
    Before the deposition, a filament holding system is installed in the vacuum reactor. The filament holding member has a hexagonal geometry as described in FIG. 6 with dimensions D = 60mm, and of = 60mm, the filaments have a length of 500mm and are located 20mm from the inner surface of the substrate.
    A 2 micron layer of microcrystalline diamond is deposited using the hot filament chemical vapor deposition method by means of an installation as described above with the following deposition conditions:Filing time = 20 hoursSubstrate temperature = 770 ° C,Working pressure = 50 mbar.
    A control of the thickness of the deposited layer (measurement on metallographic sections) and the quality of the deposit (measurement by Raman spectrometry) shows that the variation of uniformity (calculated by the formula = (min-max) / average) is less than 10% over the entire area deposited.
    Thus, by implementing the hot filament chemical vapor deposition technology by means of an installation as proposed above, it is possible to deposit a layer of polycrystalline diamond whose thickness is between 50nm and 50um and whose uniformity variation (calculated by the formula = (min-max) / average) is less than 10% over the entire deposited surface.
    权利要求:
    Claims (10)
    [1]
    A vapor phase diamond deposition apparatus using hot filaments comprising:A vacuum reactor comprising a reaction chamber connected to a vacuum source,A substrate holder disposed in the reactor,- A device for maintaining tension filaments positioned inside tubular parts of free section.
    [2]
    2. Equipment according to claim 1, comprising a filament holding system for arranging the filaments in an elliptical, polygonal or free geometry similar to that of the inner surface of the tubular part to be coated.
    [3]
    3. Polycrystalline diamond deposition process implementing equipment according to one of claims 1 to 2, characterized in that it is carried out at a temperature between 600 and 1000 ° C.
    [4]
    4. deposition process according to claim 3, characterized in that it is formed on the inner surface of tube-type hollow parts, having a section of elliptical, polygonal or free shape.
    [5]
    5. deposition process according to claim 4, characterized in that the inner walls of the substrate can be smooth or structured.
    [6]
    6. Method according to claim 5, characterized in that the treated part consists of at least one substrate selected from the following materials: refractory metals and derivatives, transition metals and derivatives, titanium-based alloys, cemented carbides, alloys silicon-based, glasses, oxides (fused silica, alumina).
    [7]
    7. Method according to claim 5, characterized in that the substrate may be made of any material coated with a thin layer of materials cited in claim 6.
    [8]
    8. Part obtained by a method according to one of claims 3 to 7, characterized in that it comprises a polycristailin diamond deposit having a thickness whose value is between 50nm and 50um and whose uniformity variation (calculated by the formula = (min-max) / average) is less than 20% over the entire area deposited.
    [9]
    9. Part according to claim 8, characterized in that the diamond deposit is of the nanocrystalline diamond type having a grain size of between 1 and 100 nm, typically around 20 nm, to obtain an average roughness of less than 200 nm. preferably less than 50 nm.
    [10]
    10. Part according to claim 8, characterized in that the diamond deposition is of the microcrystalline diamond type having a grain size of between 20 nm and 10 μm, typically around 100 nm.
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    同族专利:
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    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    DE19809675C1|1998-03-06|1999-11-25|Fraunhofer Ges Forschung|Apparatus and method for diamond coating of tubular components of limited length|
    EP1036861A1|1999-03-16|2000-09-20|Basf Aktiengesellschaft|Diamond coated electrodes|
    DE19922665A1|1999-05-18|2000-11-23|Fraunhofer Ges Forschung|Three-dimensional base body used in the production of a bearing or sealing component has a fine crystalline diamond structure with a specified surface roughness|
    EP1411143A1|2002-10-14|2004-04-21|CSEM Centre Suisse d'Electronique et de Microtechnique|Process for producing tubular pieces with an internal diamond coating|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    CH01941/14A|CH710471B1|2014-12-15|2014-12-15|Hot filament vapor phase diamond deposition equipment for coating the inner surface of hollow parts.|CH01941/14A| CH710471B1|2014-12-15|2014-12-15|Hot filament vapor phase diamond deposition equipment for coating the inner surface of hollow parts.|
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