CN105347848A - Preparation method for composite material graphite heater used at high temperature - Google Patents
Preparation method for composite material graphite heater used at high temperature Download PDFInfo
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- CN105347848A CN105347848A CN201510675208.8A CN201510675208A CN105347848A CN 105347848 A CN105347848 A CN 105347848A CN 201510675208 A CN201510675208 A CN 201510675208A CN 105347848 A CN105347848 A CN 105347848A
- Authority
- CN
- China
- Prior art keywords
- tinsel
- graphite heater
- graphite
- high temperature
- heater
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 69
- 239000010439 graphite Substances 0.000 title claims abstract description 69
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 10
- 229910052715 tantalum Inorganic materials 0.000 claims description 16
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 238000002203 pretreatment Methods 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000005554 pickling Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 3
- 238000009499 grossing Methods 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims description 3
- 238000010583 slow cooling Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 8
- 238000003763 carbonization Methods 0.000 abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 238000002955 isolation Methods 0.000 abstract description 3
- 229910052786 argon Inorganic materials 0.000 abstract description 2
- 230000005587 bubbling Effects 0.000 abstract description 2
- 239000001307 helium Substances 0.000 abstract description 2
- 229910052734 helium Inorganic materials 0.000 abstract description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 abstract description 2
- 238000013467 fragmentation Methods 0.000 abstract 1
- 238000006062 fragmentation reaction Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 8
- 229910003468 tantalcarbide Inorganic materials 0.000 description 7
- 229910004448 Ta2C Inorganic materials 0.000 description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 5
- 230000006698 induction Effects 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 239000010937 tungsten Substances 0.000 description 4
- 229910004166 TaN Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000007669 thermal treatment Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/145—Carbon only, e.g. carbon black, graphite
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B6/00—Heating by electric, magnetic or electromagnetic fields
- H05B6/02—Induction heating
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/013—Heaters using resistive films or coatings
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B2206/00—Aspects relating to heating by electric, magnetic, or electromagnetic fields covered by group H05B6/00
- H05B2206/02—Induction heating
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Inorganic Chemistry (AREA)
- Resistance Heating (AREA)
Abstract
The invention discloses a preparation method for a composite material graphite heater used at a high temperature. The method comprises the following steps: (A) pretreatment of a graphite heater; (B) pretreatment of tinsel; (C) attaching of tinsel; and (D) high temperature heat treatment. With the method, the graphite heater is perfectly converted into the metallic carbide-graphite composite material graphite heater. The composite material graphite heater retains the heating function of the graphite heater, has the high temperature corrosion resistance of metallic carbide, realizes physical isolation of graphite from an internal to-be-heated element and eradicates volatilization of carbon on the inner surface of graphite. The method overcomes problems like fragmentation, bubbling and incapability of intact bonding due to direct carbonization of the tinsel in an inert atmosphere, e.g., argon, helium and vacuum.
Description
Technical field
The present invention relates to the preparation method of the graphite heater used in elevated heating processes, particularly relate to a kind of preparation method of high temperature composite graphite heater.
Background technology
Graphite is a kind of crystalline carbon, fusing point 3652 DEG C, boiling point 4827 DEG C, and chemical property torpescence is corrosion-resistant, should not react with acid, alkali etc.High purity graphite has that intensity is high, good thermal shock, high temperature resistant, anti-oxidant, specific resistance is little, corrosion-resistant, be easy to the advantages such as precision sizing.High purity graphite can be used for processing and fabricating an electric heating element, single crystal growing furnace well heater, smelt with and semi-conductor crucible.
When graphite is as heating member, generally there are two kinds of type of heating, are respectively resistance-type and induction.Be used alone pure graphite and do heating member, under some particular surroundings, have its limitation.Such as, during with graphite heating body heating tungsten crucible, under high temperature, the volatilization of (more than 2100 DEG C) graphite part, reacts with tungsten crucible, at tungsten crucible Surface Creation wolfram varbide, causes tungsten crucible to ftracture.For another example, with graphite heater heating, when growth or epitaxial semiconductor body monocrystalline or monocrystal thin films material, easily the introducing carbon impurity at crystal, has a strong impact on electricity and the optical property of material.
Tantalum is rare refractory metal, fusing point 2996 DEG C, linear expansivity 6.5 × 10-6(0-100 DEG C), thermal conductivity 54W/ (MK) (25 DEG C).The toughness of tantalum is strong, has good ductility, not easily broken.Tantalum, mainly as heat-resistant high-strength material, in vacuum high temperature furnace, can be used as Holder Fasteners, thermoshield, well heater and radiator element etc.Under high temperature, tantalum and nitrogen react and generate TaN, TaN fusing point 3090 DEG C.Under high temperature, tantalum contacts with carbon, and reaction generates TaC or Ta2C etc.TaC and Ta2C all has very high chemical stability and good high-temperature behavior, and fusing point is respectively 3875 DEG C and 3500 DEG C, can the high temperature of resistance to less than 3000 DEG C.But TaN, TaC and Ta2C material fragility is large, very easily ftractures under the impact of high/low temperature.
If graphite can be combined with TaC, TaN, make with graphite is base material, with the compound heating member that TaC, Ta2C or TaN are shield, then both can effectively stop, isolate high temperature under the volatilization of carbon, the difficult problem that TaC, Ta2C, TaN material fragility easily splits can be solved again.
Summary of the invention
The object of the invention is to be reacted by heating unit to solve graphite heater of the prior art and other material crucible or other material, the problem causing crucible or gone bad by heating unit or damage, specifically provides a kind of preparation method of NEW TYPE OF COMPOSITE material graphite heater.
In order to achieve the above object, the technical scheme that the present invention takes is: a kind of preparation method of high temperature composite graphite heater, and it is characterized in that, the method is carried out according to following steps:
(A). graphite heater pre-treatment: graphite heater is carried out internal surface polished finish, surface smoothing, in mirror effect, then purges clean surfaces externally and internally;
(B). tinsel pre-treatment: roll tinsel, ensures that the surfacing of tantalum paper tinsel is smooth, carries out pickling and washing to tinsel, ensure that tinsel is clean;
(C). tinsel attaches: tinsel is attached to graphite heater internal surface, attaches completely, make tinsel not play drum;
(D). high-temperature heat treatment: the graphite heater having attached tinsel is moved into high-temperature heater, vacuumize, fill reactant gases, intensification, control in-furnace temperature between 2000-2200 DEG C, pressure is between 100 ~ 900mbar, constant temperature time is between 5 ~ 20 hours, then slow cooling is to room temperature, takes out and namely obtains composite graphite heater.
From stove, take out the graphite heater after thermal treatment, this graphite heater has been transformed into the composite graphite heater of inner liner metal carbide.
Prepare the action principle of composite graphite heater: under high temperature, reactant gases environment, chemical reaction is there is between the carbon of graphite heater internal surface, tinsel and reactant gases, tinsel is transformed into fine and close carbide completely, the simultaneously thermal expansion process of tinsel under Yin Gaowen, realization fits tightly with graphite heater internal surface, and graphite internal surface is completely closed.
The beneficial effect that the present invention produces is: take present method graphite heater perfection can be changed into refractory carbide-graphite composite graphite heater.This composite graphite heater had both remained the heating function of graphite heater, was provided with again the high-temperature corrosion-resistance performance of metallic carbide.This graphite heater can realize graphite with inner by the physical isolation of heating unit, can stop the carbon volatilization of graphite internal surface under high temperature.This preparation method can eliminate tinsel cracked, the bubbling that directly carbonization causes in inert atmosphere (as argon gas, helium) or vacuum and the problem such as cannot completely to fit.
Accompanying drawing explanation
Fig. 1 is the preparation flow figure of composite graphite heater of the present invention;
Fig. 2 is composite graphite heater structural representation of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described:
The present invention is in preparation (B) step, (C) step and (D) step, and tinsel is tantalum paper tinsel, and thickness is within the scope of 0.05 ~ 0.2mm, and purity is more than 99.9%.In preparation (D) step, reactant gases is high pure nitrogen, and purity is more than 99.9%.
Graphite heater in the present invention is generally cylindrical shape, also can be Polygons tubular or other complicated shape, may be used for induction heating, also can be used for resistance-type heating.
Embodiment: with reference to Fig. 1, a kind of high temperature composite graphite heater preparation method carries out according to following steps:
Step 100(A), graphite heater pre-treatment: graphite heater is carried out internal surface polished finish, makes surface smoothing, in mirror effect, then purges clean surfaces externally and internally.
Step 110(B), tantalum paper tinsel pre-treatment: adopt rolling machine to roll tantalum paper tinsel, ensures that the surfacing of tantalum paper tinsel is smooth, pickling and washing are carried out to tinsel, in the present embodiment, pickling employing concentration is the dilute hydrochloric acid of 20 ﹪, washes as deionized water, ensures that tinsel is clean.
Step 120(C), tantalum paper tinsel attaches: tantalum paper tinsel is attached to graphite heater internal surface, and ensure as far as possible to attach completely, tantalum paper tinsel does not play drum.
Step 120(D), high-temperature heat treatment: moved in High Temperature Furnaces Heating Apparatus by the graphite heater having attached tantalum paper tinsel, this High Temperature Furnaces Heating Apparatus can be induction type or resistance-type process furnace, and the present embodiment is induction type high-temperature heater.Be evacuated to 1 × 10
-4below mbar, fills high pure nitrogen.Heat up, temperature rise rate controls within the scope of 2 ~ 20 DEG C/min.In the present embodiment, progressively heat up with 10 DEG C/min speed.Utilize infrared pyrometer to control in-furnace temperature between 2000-2200 DEG C, the present embodiment is about 2100 DEG C.Control process furnace internal pressure between 100 ~ 900mbar, the present embodiment is about 500mbar.The thermostatically heating time, the present embodiment was constant temperature 10 hours between 5 ~ 20 hours.Then slow cooling is to room temperature, and rate of temperature fall controls within the scope of 2 ~ 10 DEG C/min, and in the present embodiment, rate of temperature fall is 5 DEG C/min.
The graphite heater after thermal treatment is taken out from stove.Through inspecting and X-ray diffraction analysis, utilize the graphite heater that this preparation method obtains, internal surface be converted into completely densification, smooth, do not split, not broken layer of tantalum carbide, the smooth layer of carbonization 1 and graphite 2 fit tightly.It is matrix that this graphite heater has become with graphite, the composite graphite heater (as shown in Figure 2) of the smooth layer of liner carbonization.In following application process, due to the existence of the smooth layer of carbonization, well heater achieves graphite with inner by the physical isolation of heating unit, has stopped the carbon volatilization of graphite internal surface under high temperature simultaneously.
Claims (3)
1. a high temperature preparation method for composite graphite heater, is characterized in that, the method is carried out according to following steps:
(A). graphite heater pre-treatment: graphite heater is carried out internal surface polished finish, surface smoothing, in mirror effect, then purges clean surfaces externally and internally;
(B). tinsel pre-treatment: roll tinsel, ensures that the surfacing of tantalum paper tinsel is smooth, carries out pickling and washing to tinsel, ensure that tinsel is clean;
(C). tinsel attaches: tinsel is attached to graphite heater internal surface, attaches completely, make tinsel not play drum;
(D). high-temperature heat treatment: the graphite heater having attached tinsel is moved into high-temperature heater, vacuumize, fill reactant gases, intensification, control in-furnace temperature between 2000-2200 DEG C, pressure is between 100 ~ 900mbar, constant temperature time is between 5 ~ 20 hours, then slow cooling is to room temperature, takes out and namely obtains composite graphite heater.
2. the preparation method of a kind of high temperature composite graphite heater as claimed in claim 1, it is characterized in that, in described (B) step, (C) step and (D) step, tinsel is tantalum paper tinsel, thickness is within the scope of 0.05 ~ 0.2mm, and purity is more than 99.9%.
3. the preparation method of a kind of high temperature composite graphite heater as claimed in claim 1, is characterized in that, in described (D) step, reactant gases is high pure nitrogen, and purity is more than 99.9%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510675208.8A CN105347848B (en) | 2015-10-19 | 2015-10-19 | A kind of preparation method of high temperature composite graphite heater |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510675208.8A CN105347848B (en) | 2015-10-19 | 2015-10-19 | A kind of preparation method of high temperature composite graphite heater |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105347848A true CN105347848A (en) | 2016-02-24 |
| CN105347848B CN105347848B (en) | 2018-04-06 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510675208.8A Active CN105347848B (en) | 2015-10-19 | 2015-10-19 | A kind of preparation method of high temperature composite graphite heater |
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| Country | Link |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108419307A (en) * | 2018-04-17 | 2018-08-17 | 北京强度环境研究所 | A kind of control method of graphite heater |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87100500A (en) * | 1986-01-29 | 1987-08-19 | 通用电器公司 | Re-sintered boron-rich polycrystalling cabic boron nitride and manufacture method thereof |
-
2015
- 2015-10-19 CN CN201510675208.8A patent/CN105347848B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87100500A (en) * | 1986-01-29 | 1987-08-19 | 通用电器公司 | Re-sintered boron-rich polycrystalling cabic boron nitride and manufacture method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 孙汉文: "《原子光谱分析》", 31 July 2002, 高等教育出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108419307A (en) * | 2018-04-17 | 2018-08-17 | 北京强度环境研究所 | A kind of control method of graphite heater |
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| Publication number | Publication date |
|---|---|
| CN105347848B (en) | 2018-04-06 |
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