CN115403399A - Graphite fiber heat-insulation composite material for high-purity semiconductor and preparation method thereof - Google Patents
Graphite fiber heat-insulation composite material for high-purity semiconductor and preparation method thereof Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 140
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 99
- 239000010439 graphite Substances 0.000 title claims abstract description 99
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 239000002131 composite material Substances 0.000 title claims abstract description 78
- 238000009413 insulation Methods 0.000 title claims abstract description 47
- 239000004065 semiconductor Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 87
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 85
- 239000004917 carbon fiber Substances 0.000 claims abstract description 85
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical group [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000005011 phenolic resin Substances 0.000 claims abstract description 24
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 24
- 238000005087 graphitization Methods 0.000 claims abstract description 21
- 239000000853 adhesive Substances 0.000 claims abstract description 16
- 230000001070 adhesive effect Effects 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 11
- 239000011230 binding agent Substances 0.000 claims abstract description 9
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 18
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- 238000002791 soaking Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000000746 purification Methods 0.000 claims description 11
- 239000000178 monomer Substances 0.000 claims description 9
- 238000009960 carding Methods 0.000 claims description 8
- 239000011810 insulating material Substances 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 8
- 229920000297 Rayon Polymers 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 6
- 239000000460 chlorine Substances 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 6
- 238000003754 machining Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 230000005855 radiation Effects 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000003763 carbonization Methods 0.000 claims description 4
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 4
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 230000003247 decreasing effect Effects 0.000 claims description 2
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- 208000005156 Dehydration Diseases 0.000 claims 1
- 230000018044 dehydration Effects 0.000 claims 1
- 238000006297 dehydration reaction Methods 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 12
- 239000012774 insulation material Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 abstract description 5
- 229910010271 silicon carbide Inorganic materials 0.000 abstract description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 3
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 abstract description 3
- 229910052710 silicon Inorganic materials 0.000 abstract description 3
- 239000010703 silicon Substances 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
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- 239000010935 stainless steel Substances 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
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- C04B35/83—Carbon fibres in a carbon matrix
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Abstract
The invention belongs to the technical field of high-purity graphite fiber heat-insulation composite materials, and particularly relates to a graphite fiber heat-insulation composite material for a high-purity semiconductor and a preparation method thereof. Comprises carbon fiber filaments and a binder; the carbon fiber filaments are arranged according to a preset direction; the density of the graphite fiber filaments formed after the carbon fiber filaments are subjected to graphitization treatment is gradually reduced from inside to outside according to the preset density; the adhesive is phenolic resin, and the adhesive is liquid and/or powder; more than 90% of the graphite fiber filaments are arranged along the circumferential direction of the product or parallel to the axial direction of the graphite fiber cylindrical product. Solves the technical problems of low purity and poor heat insulation effect of thermal field heat insulation materials in the existing semiconductor silicon crystal bar and silicon carbide crystal bar.
Description
Technical Field
The invention belongs to the technical field of high-purity graphite fiber heat-insulation composite materials, and particularly relates to a novel graphite fiber heat-insulation composite material for a high-purity semiconductor and a preparation method thereof.
Background
In the process of preparing high-quality crystals by using a crystal growing furnace in the third-generation silicon carbide crystal field in the second-generation semiconductor field, the graphite fiber heat-insulating material with high efficiency, energy conservation, high purity and high quality is urgently needed to be improved, so that the energy consumption of enterprises is reduced, the crystal quality is improved, and the production cost is saved. However, the heat insulating material in the prior art has low purity, high heat conductivity, long product manufacturing period, short service life and other factors, which restrict the rapid development of the field of semiconductor crystal growth in China.
Disclosure of Invention
The invention provides a graphite fiber heat-insulating composite material for a high-purity semiconductor, which solves the technical problems of low purity, poor heat-insulating effect and easy cracking of thermal field heat-insulating materials in the existing semiconductor silicon crystal bar and silicon carbide crystal bar.
In order to accomplish the above object, according to one aspect of the present invention, there is provided a graphite fiber thermal insulation composite for high purity semiconductor, comprising,
carbon fiber filaments and a binder;
the carbon fiber filaments are arranged according to a preset direction; the density of the graphite fiber filaments formed after the carbon fiber filaments are subjected to graphitization treatment is gradually reduced from inside to outside according to the preset density;
the adhesive is phenolic resin, and the adhesive is liquid and/or powder;
more than 90% of the graphite fiber filaments are arranged along the circumferential direction of the product or parallel to the axial direction of the graphite fiber cylindrical product.
Further, the graphite fiber filament of the graphite fiber heat-insulation composite material for the high-purity semiconductor is subjected to pre-oxidation treatment or carbonization treatment by selecting one or more of PAN-based fiber filament, pitch-based fiber filament, viscose-based fiber filament or phenolic resin-based fiber filament.
Furthermore, the carbon fiber yarns are fixed to form a carbon bridge connection after pyrolysis of phenolic resin.
Furthermore, the density of the graphite fiber heat insulation and preservation cylinder is gradually reduced from the internal high-temperature area to the external low-temperature area, so that the heat conduction of the internal high-temperature area mainly based on radiation and the solid heat conduction of the fiber in the external low-temperature area are reduced.
Furthermore, in the graphitization treatment of the graphite fiber heat-insulating composite material for the high-purity semiconductor, the curing molding temperature is 150 ℃, the graphitization treatment temperature is more than 2000 ℃, and the purification treatment temperature is 2600 ℃.
In another aspect of the present invention, there is provided a method for preparing a graphite fiber heat-insulating composite material for high-purity semiconductors, comprising the steps of (1) cutting a carbon fiber tow by a desired length using a filament cutter; (2) Opening the cut carbon fiber tows to obtain completely dispersed monomer carbon fiber yarns; (3) Forming a directional fiber net by the dispersed carbon fiber yarns through directional water flow, and then dehydrating through a drying channel; (4) Forming the dehydrated carbon fiber net by an automatic rounding forming machine, rolling and adding phenolic resin in the forming process, and finally forming a cylindrical carbon fiber heat insulation material with a preset size; (5) Putting the formed cylindrical carbon fiber heat-insulating composite material and the mold into an oven with the temperature of more than 150 ℃, and curing and molding for 5 hours to form a shrunk carbon fiber heat-insulating composite material; (6) Placing the cured carbon fiber heat-insulating composite material into a graphitization furnace at the temperature of more than 2000 ℃ for high-temperature treatment for 8 hours to obtain a graphite fiber heat-insulating composite material; (7) machining the appearance; (8) Soaking the processed graphite fiber heat-insulating composite material in hydrofluoric acid with the concentration of 30% for 24h, taking out and drying; (9) And (3) putting the graphite fiber heat-insulating composite material subjected to soaking and drying control by hydrofluoric acid into a high-temperature purification furnace at 2600 ℃, carrying out high-temperature treatment for 15 hours, and introducing chlorine or/and Freon gas in the technological process to obtain a finished product of the graphite fiber heat-insulating composite material for the high-purity semiconductor.
The invention also provides a preparation method of the graphite fiber heat-insulation composite material for the high-purity semiconductor, which comprises the following steps of (1) cutting the carbon fiber tows according to the required length by using a filament cutter; (2) Opening the cut carbon fiber tows to obtain completely dispersed monomer carbon fiber yarns; (3) Adding the dispersed monomer carbon fiber into powder phenolic resin, mixing, forming an ordered fiber net by a stirring opener and a directional airflow carding machine, and forming the formed fiber net by an automatic rounding machine; (4) Putting the formed cylindrical carbon fiber heat-insulating composite material and the mold into an oven with the temperature of more than 150 ℃, and curing and molding for 5 hours to form a contracted carbon fiber heat-insulating composite material; (5) Placing the cured carbon fiber heat-insulating composite material into a graphitization furnace at the temperature of more than 2000 ℃ for high-temperature treatment for 8 hours to obtain a graphite fiber heat-insulating composite material; (6) machining the appearance according to requirements; (7) Soaking the processed graphite fiber heat-insulating composite material with 30% hydrofluoric acid for 24h, taking out and drying (8), placing the graphite fiber heat-insulating composite material subjected to soaking and drying by the hydrofluoric acid into a high-temperature purification furnace at 2600 ℃ for high-temperature treatment for 15 hours, and introducing chlorine or/and freon gas to obtain the graphite fiber heat-insulating composite material for the high-purity semiconductor.
Compared with the prior art, the invention has the beneficial effects that: the invention adopts the ordered arrangement of graphite fibers and the decreasing arrangement of the density from the inside to the outside of the cylinder, and the purification treatment is carried out at 2600 ℃ by introducing chlorine or/and Freon gas at high temperature. Therefore, the graphite fiber heat-insulating material has better heat-insulating effect and higher purity, and the problem of circumferential cracking due to the orderly arrangement of the fibers is solved, and the effect is obvious particularly in a third-generation semiconductor silicon carbide crystal induction heating furnace.
Drawings
FIG. 1A is a schematic structural diagram of a graphite fiber heat-insulating composite material for high-purity semiconductors according to the present invention, which is arranged in order.
FIG. 1B is a schematic structural diagram of the graphite fiber thermal insulation composite material in a disordered arrangement.
FIG. 2 is a diagram showing the results of the thermal insulation effect test under the same conditions as the thermal insulation material of the present invention and the randomly arranged carbon fiber.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
The terms "first" and "second," and the like, in the description and in the claims of embodiments of the present invention are used for distinguishing between different objects and not for describing a particular order of the objects. For example, the first parameter set and the second parameter set, etc. are used to distinguish different parameter sets, rather than to describe a particular order of parameter sets.
In the description of the embodiments of the present invention, the meaning of "a plurality" means two or more unless otherwise specified. For example, a plurality of elements refers to two elements or more.
The term "and/or" herein is an association relationship describing an associated object, and means that there may be three relationships, for example, a display panel and/or a backlight, which may mean: there are three cases of a display panel alone, a display panel and a backlight at the same time, and a backlight alone. The symbol "/" herein denotes a relationship in which the associated object is or, for example, input/output denotes input or output.
In the embodiments of the present invention, words such as "exemplary" or "for example" are used to mean serving as examples, illustrations or descriptions. Any embodiment or design described as "exemplary" or "e.g.," an embodiment of the present invention is not necessarily to be construed as preferred or advantageous over other embodiments or designs. Rather, use of the word "exemplary" or "such as" is intended to present concepts related in a concrete fashion.
The term is used herein to describe one or more of the alternatives in the process chain that require a high or low degree of purity depending on the customer.
As shown in fig. 1a,1b and fig. 2, in one aspect of the present invention, there is provided a graphite fiber thermal insulation composite for high purity semiconductors comprising carbon fiber filaments and a binder; the carbon fiber filaments are arranged according to a preset direction; the density of the graphite fiber heat-insulation material formed by graphitizing the carbon fiber filaments is gradually reduced from inside to outside according to the preset density; the adhesive is phenolic resin, and the adhesive is liquid and/or powder; more than 90% of the graphite fiber filaments are arranged along the circumferential direction of the product or parallel to the axial direction of the graphite fiber heat-insulation cylinder product. More than 90% of graphite fiber filaments are arranged along the circumferential direction of the product or in the direction parallel to the axial direction of the graphite fiber cylinder product, the binder is selectively used, and simultaneously graphitization treatment is carried out, so that the technical problems of low purity, poor heat insulation effect and easiness in cracking of thermal field heat insulation materials in the conventional semiconductor silicon crystal bar and silicon carbide crystal bar are effectively solved.
Illustratively, the graphite fiber heat insulation composite material for the high-purity semiconductor comprises carbon fiber filaments and a binder; the carbon fiber filaments are arranged according to a preset direction; the density of the graphite fiber filaments formed after the carbon fiber filaments are subjected to graphitization treatment is gradually reduced from inside to outside according to the preset density; the adhesive is phenolic resin, and the adhesive is liquid and/or powder; more than 90% of the graphite fiber filaments are arranged along the circumferential direction of the product or parallel to the axial direction of the graphite fiber cylindrical product. The graphite fiber of the graphite fiber heat-insulation composite material is one or more of PAN (polyacrylonitrile) -based fiber, pitch-based fiber, viscose-based fiber or phenolic resin-based fiber, and is subjected to pre-oxidation treatment or carbonization treatment to obtain carbon fiber or directly selects carbonized carbon fiber.
Illustratively, the graphite fiber heat insulation composite material for the high-purity semiconductor comprises carbon fiber filaments and a binder; the carbon fiber filaments are arranged according to a preset direction; the density of the graphite fiber filaments formed after the carbon fiber filaments are subjected to graphitization treatment is gradually reduced from inside to outside according to the preset density; the adhesive is phenolic resin, and the adhesive is liquid and/or powder; more than 90% of the graphite fiber filaments are arranged along the circumferential direction of the product or parallel to the axial direction of the graphite fiber cylindrical product. The carbon fiber wires are fixed with each other and are connected through a carbon bridge formed after phenolic resin is pyrolyzed.
Illustratively, the graphite fiber heat insulation composite material for the high-purity semiconductor comprises carbon fiber filaments and a binder; the carbon fiber filaments are arranged according to a preset direction; the density of the graphite fiber filaments formed after the carbon fiber filaments are subjected to graphitization treatment is gradually reduced from inside to outside according to the preset density; the adhesive is phenolic resin, and the adhesive is liquid and/or powder; more than 90% of the graphite fiber filaments are arranged along the circumferential direction of the product or parallel to the axial direction of the graphite fiber cylindrical product. The density of the graphite fiber filament is 0.2g/cm from the inside 3 Gradually decreases to 0.08g/cm outside 3 And the device is used for reducing the heat conduction of the inner high-temperature area mainly based on radiation and the heat conduction of the outer low-temperature area fiber solid.
In one embodiment of the present invention, the graphite fiber thermal insulation composite for high purity semiconductors comprises carbon fiber filaments and a binder; the carbon fiber thread is pressedArranging according to a preset direction; the density of the graphite fiber filaments formed after the carbon fiber filaments are subjected to graphitization treatment is gradually reduced from inside to outside according to the preset density; the adhesive is phenolic resin, and the adhesive is liquid and/or powder; more than 90% of the graphite fiber filaments are arranged along the circumferential direction of the product or parallel to the axial direction of the graphite fiber cylindrical product. The density of the graphite fiber filament is 0.2g/cm from the inside 3 Gradually decreases to 0.08g/cm outside 3 And the device is used for reducing the heat conduction of the inner high-temperature area mainly based on radiation and the heat conduction of the outer low-temperature area fiber solid. In the graphitization treatment of the graphite fiber heat-insulation composite material, the curing and molding temperature is 150 ℃, the graphitization treatment temperature is 2000 ℃, and the purification treatment temperature is 2600 ℃.
Illustratively, the phenolic resin particle size is about 20um of powdered phenolic resin.
Illustratively, the carbon fiber filaments are staple fiber viscose-based carbon fibers with diameters of 7-10um and lengths of 1-2mm.
In another aspect of the invention, a preparation method of a high-purity graphite fiber heat-insulation composite material is provided, which comprises the following steps of (1) cutting 3kg of viscose-based carbon fiber filaments into pieces with the length of 1-2mm; (2) Putting the cut carbon fiber tows into a dispersion opening carding machine for opening treatment to obtain completely dispersed monomer carbon fiber yarns; (3) Placing the dispersed carbon fiber filaments in a water flow carding machine, forming a directional fiber net with the width of 350mm under the directional water flow through the directional water flow of the water flow carding machine and the relation between the diameter and the length of the fiber filaments, and then removing about 80% of water through a drying channel, namely forming the directional fiber net through the directional water flow, wherein the fiber length is larger than the fiber diameter, and the fiber tends to be parallel to the water surface under the action of water buoyancy; (4) Forming the dehydrated carbon fiber net by an automatic rounding forming machine, adding phenolic resin while rolling to form a cylindrical carbon fiber heat insulating material with the outer diameter phi 450mm, the inner diameter phi 290mm and the height L350 mm; (5) The formed cylindrical carbon fiber heat-insulation composite material is filled into a stainless steel mold with the outer diameter phi 440mm, the inner diameter phi 290mm and the height L350mm, fixed and filled into an oven with the temperature of more than 150 ℃, and the temperature is raised by 5 ℃ per minute for curing and forming for 5 hours to form the shrunk carbon fiber heat-insulation composite material; (6) Placing the cured carbon fiber heat-insulation composite material into a vacuum graphitization furnace at the temperature of 2000 ℃ for high-temperature treatment for 8 hours, and introducing 900L/h argon gas in the treatment process to obtain a quasi-graphite fiber heat-insulation composite material; (7) Machining to form an outer diameter phi 402mm, an inner diameter phi 298mm and a height L304mm; (8) Soaking the processed graphite fiber heat-insulating composite material in hydrofluoric acid with the concentration of 30% for 24h, taking out and drying; (9) And (3) putting the hydrofluoric acid soaking and drying control graphite fiber heat-insulation composite material into a high-temperature purification furnace at 2600 ℃ for high-temperature treatment for 15 hours, introducing 50L/furnace and chlorine gas or/and Freon gas in the process, and obtaining the high-purity graphite fiber heat-insulation composite material with the outer diameter phi 400mm, the inner diameter phi 300mm and the height L300mm after high shrinkage. And (10) vacuumizing and packaging.
Illustratively, the phenolic resin is a powdered phenolic resin with a particle size of about 20um
Illustratively, the carbon fiber is short fiber viscose-based carbon fiber with the diameter of 7-10um and the length of 1-2mm
Illustratively, the gas auxiliary materials are 200KG of water, 20L of argon, 2KG of 30% hydrofluoric acid and 50L of chlorine.
The device comprises required equipment, a fiber cutting machine, carbon fiber dispersing and opening equipment, a water flow fiber carding machine, a circular mold, a drying tunnel at 200 ℃, processing equipment, a vacuum carbonization/graphitization furnace at 2000 ℃, a hydrofluoric acid soaking liquid storage tank, a purification furnace at 2600 ℃ and a vacuum thermal conductivity test furnace.
In one embodiment of the present invention, as shown in fig. 1a,1b and fig. 2, the method for preparing the graphite fiber thermal insulation composite material for high purity semiconductor comprises the steps of (1) cutting 3kg of viscose-based carbon fiber yarn to a length of 1-2mm; (2) Putting the cut carbon fiber tows into a dispersion opening carding machine for opening treatment to obtain completely dispersed monomer carbon fiber yarns; adding the dispersed monomer carbon fiber into powder phenolic resin, mixing, forming a fiber net by an opener and a directional carding machine, and forming the formed fiber net by an automatic rounding machine to form an outer diameter
Inner diameter
A cylindrical carbon fiber heat insulating material having a height L350 mm; (3) The formed cylindrical carbon fiber heat insulation composite material is filled in the outer diameter
Inner diameter
Fixing the stainless steel mold with the height of L350mm in a baking oven with the temperature of more than 150 ℃, heating the stainless steel mold to 5 ℃ per minute, and curing and molding the stainless steel mold for 5 hours to form the shrunk carbon fiber composite heat-insulating material; (4) Placing the cured carbon fiber heat-insulation composite material into a vacuum graphitization furnace at the temperature of 2000 ℃ for high-temperature treatment for 8 hours, and introducing 900L/h argon gas in the treatment process to obtain a quasi-graphite fiber heat-insulation composite material; (5) Machining to form the outside diameter
Inner diameter
Height L304mm; (6) Soaking the processed graphite fiber heat-insulating composite material for 24 hours by using hydrofluoric acid with the concentration of 30 percent, and taking out and drying; (7) Putting the graphite fiber heat-insulation composite material subjected to soaking and drying control by hydrofluoric acid into a high-temperature purification furnace at 2600 ℃ for high-temperature treatment for 15 hours, and introducing 50L/furnace chlorine gas in the technical process to obtain the graphite fiber heat-insulation composite material with high-shrinkage external diameter
Inner diameter
A graphite fiber heat-insulating composite material for high-purity semiconductors with the height L of 300 mm. And (8) vacuumizing and packaging.
Through a vacuum thermal conductivity test furnace (steady-state flat plate method thermal conductivity test), a heat-preservation cylinder samples 100 x 50mm thickness, main performance tests are carried out, the ambient temperature is 10 ℃, the RH ambient humidity is 80 percent, and the orderly arranged graphite fiber thermal insulation composite product 100 x 100 is sampled* The 50mm (thickness) samples are the experimental group. Comparative experiment data is carried out, the graphite fiber heat insulation material is shown in figure 1, and the density of the composite is 0.14g/cm 3 . According to the 30-minute steady state data at 1200 ℃ sampled in FIG. 1, the external temperature of the graphite fiber insulation material of the present invention is 112 ℃. The coefficient of thermal expansion of the fibers in the parallel direction is less than 2.3x10 -6 K, compressive strength 0.2MPa.
The main performance test is carried out by a vacuum thermal conductivity test furnace (steady-state flat plate method thermal conductivity test), a heat-preservation cylinder is sampled with the thickness of 100 x 50mm, the samples with the ambient temperature of 10 ℃ and the RH ambient humidity of 80 percent are sampled with the thickness of 100 x 50mm, the comparative experimental data are carried out, the carbon fiber thermal insulation material is shown in figure 2, and the density is 0.14g/cm 3 According to the 30 minute steady state data at 1200 ℃ sampled in FIG. 2, the external temperature of the carbon fiber insulation was 373 deg.C (calculated from the mixed linear 1/2 of the vertical and parallel data sources). The thermal expansion coefficient of the carbon fiber in the parallel direction is 2.6x10 -6 K, and a compressive strength of 0.8MPa. The two are compared, it can be known that in the embodiment of the application, the temperature difference is 261 ℃ at 1200 ℃, the higher the temperature is, the more obvious the heat preservation effect is, the ash content of the domestic common carbon fiber heat preservation material is about 20ppm, and the total non-carbon elements of the product treated by introducing chlorine in the process of soaking by hydrofluoric acid and then heating at 2600 ℃ are lower than 1 ppm. GDMS (glow discharge mass spectrometry) was used to test the main element content: b0.01, fe0.07, mg0.14, al0.05, si0.5, P<0.08,Ca0.04,Cu<0.1 unit ppm wt, compared with the prior art, the performance of each aspect is obviously improved, and the method has unexpected technical effect and obvious progress.
The thermal conductivity of the graphite fiber thermal insulation material for the high-purity semiconductor is reduced to the maximum extent by uniformly arranging the fibers along the circumferential direction, and the anisotropy of the radial and axial thermal conductivities of the fibers is determined by the physical properties of the internal crystal structure of the fibers. In the above, the fibers are arranged in the circumferential direction, and the thermal conductivity can be extremely reduced. Meanwhile, the density of the graphite fiber is gradually reduced from inside to outside, so that the heat conduction of an internal high-temperature area mainly based on radiation and the solid heat conduction of fibers in an external low-temperature area are reduced.
While the present invention has been described with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, which are illustrative and not restrictive, and it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. A graphite fiber heat insulation composite material for a high-purity semiconductor is characterized in that: the graphite fiber heat-insulating composite material for the high-purity semiconductor comprises,
carbon fiber filaments and a binder;
the carbon fiber filaments are arranged according to a preset direction, and the density of the graphite fiber filaments formed by the carbon fiber filaments after graphitization treatment is gradually reduced from inside to outside according to the preset direction;
the adhesive is phenolic resin, and the adhesive is liquid and/or powder;
more than 90% of the graphite fiber filaments are arranged along the circumferential direction of the product or parallel to the axial direction of the graphite fiber cylindrical product.
2. The graphite fiber thermal insulation composite material for a high purity semiconductor according to claim 1, characterized in that: the graphite fiber filament of the graphite fiber heat-insulation composite material for the high-purity semiconductor is subjected to pre-oxidation treatment or carbonization treatment by selecting one or more of PAN-based fiber filament, pitch-based fiber filament, viscose-based fiber filament or phenolic resin-based fiber filament.
3. The graphite fiber thermal insulation composite material for a high purity semiconductor as claimed in claim 1, wherein: the carbon fiber wires are fixed with each other and are connected through a carbon bridge formed after phenolic resin is pyrolyzed.
4. The graphite fiber thermal insulation composite material for a high purity semiconductor according to claim 1, characterized in that: the graphite fiber heat insulation and preservation cylinder has the density decreasing from the internal high-temperature area to the external low-temperature area, and is used for reducing the heat conduction of the internal high-temperature area mainly based on radiation and the solid heat conduction of the fiber in the external low-temperature area.
5. The graphite fiber thermal insulation composite material for high purity semiconductors according to any one of claims 1 to 4, characterized in that: during graphitization treatment, the curing and molding temperature of the graphite fiber heat-insulation composite material is 150 ℃, the graphitization treatment temperature is more than 1600 ℃, and the purification treatment temperature is 2600 ℃.
6. A preparation method of a graphite fiber heat-insulation composite material for a high-purity semiconductor is characterized by comprising the following steps: the method comprises the following steps of (1) cutting a carbon fiber tow according to a required length by using a filament cutter; (2) Dispersing and opening the cut carbon fiber tows to obtain completely dispersed monomer carbon fiber yarns; (3) Forming a directional fiber net by the dispersed carbon fiber yarns through directional water flow, and then performing dehydration treatment through a drying channel; (4) Forming the dehydrated carbon fiber net by an automatic rounding forming machine, adding phenolic resin while rounding in the forming process, and finally forming a cylindrical carbon fiber heat-insulating material with a preset size; (5) Putting the formed cylindrical carbon fiber heat-insulating composite material and the mold into an oven with the temperature of more than 150 ℃, and curing and molding for 5 hours to form a shrunk carbon fiber heat-insulating composite material; (6) Placing the cured carbon fiber heat-insulating composite material into a graphitization furnace with the temperature of more than 2000 ℃ for high-temperature treatment for 8 hours to obtain a graphite fiber heat-insulating composite material; (7) machining the appearance; (8) Soaking the processed graphite fiber heat-insulating composite material in hydrofluoric acid with the concentration of 30% for 24h, taking out and drying; (9) And (3) putting the graphite fiber heat-insulating composite material subjected to soaking and drying control by hydrofluoric acid into a high-temperature purification furnace at 2600 ℃, treating at high temperature for 15 hours, and introducing chlorine or/and freon gas in the process to obtain a finished product of the graphite fiber heat-insulating composite material for the high-purity semiconductor.
7. A preparation method of a graphite fiber heat-insulation composite material for a high-purity semiconductor is characterized by comprising the following steps: the method comprises the following steps of (1) cutting a carbon fiber tow according to a required length by using a filament cutter; (2) Dispersing and opening the cut carbon fiber tows to obtain completely dispersed monomer carbon fiber yarns; (3) Adding the dispersed monomer carbon fiber into powder phenolic resin, uniformly mixing, forming an ordered fiber net by a stirring opener and a directional airflow carding machine, and forming the formed fiber net by an automatic rounding machine; (4) Putting the formed cylindrical carbon fiber heat-insulating composite material and the mold into an oven with the temperature of more than 150 ℃, and curing and molding for 5 hours to form a contracted carbon fiber heat-insulating composite material; (5) Placing the cured carbon fiber heat-insulating composite material into a graphitization furnace with the temperature of more than 2000 ℃ for high-temperature treatment for 8 hours to obtain a graphite fiber heat-insulating composite material; (6) machining the appearance according to requirements; (7) Soaking the processed graphite fiber heat-insulating composite material in 30% hydrofluoric acid for 24h, taking out and drying (8), putting the graphite fiber heat-insulating composite material subjected to soaking and drying in the hydrofluoric acid into a high-temperature purification furnace at 2600 ℃ for high-temperature treatment for 15 h, and introducing chlorine gas or/and freon gas to obtain the graphite fiber heat-insulating composite material for the high-purity semiconductor.
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|---|---|---|---|---|
| JPH02208264A (en) * | 1989-02-04 | 1990-08-17 | Osaka Gas Co Ltd | Formed heat-insulation material and production thereof |
| JPH02258245A (en) * | 1988-08-19 | 1990-10-19 | Osaka Gas Co Ltd | Molded heat insulation material and manufacture thereof |
| JP2005097010A (en) * | 2003-09-22 | 2005-04-14 | Showa Denko Kk | Carbon material, production method therefor and its application |
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| JPH02258245A (en) * | 1988-08-19 | 1990-10-19 | Osaka Gas Co Ltd | Molded heat insulation material and manufacture thereof |
| JPH02208264A (en) * | 1989-02-04 | 1990-08-17 | Osaka Gas Co Ltd | Formed heat-insulation material and production thereof |
| JP2005097010A (en) * | 2003-09-22 | 2005-04-14 | Showa Denko Kk | Carbon material, production method therefor and its application |
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Application publication date: 20221129 |