CN107523877A - The method that graphite matrix surface prepares silicon carbide whisker coating - Google Patents
The method that graphite matrix surface prepares silicon carbide whisker coating Download PDFInfo
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- CN107523877A CN107523877A CN201610452857.6A CN201610452857A CN107523877A CN 107523877 A CN107523877 A CN 107523877A CN 201610452857 A CN201610452857 A CN 201610452857A CN 107523877 A CN107523877 A CN 107523877A
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- Prior art keywords
- silicon carbide
- graphite matrix
- carbide whisker
- matrix surface
- coating
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
This application discloses a kind of method that graphite matrix surface prepares silicon carbide whisker coating, including step：(1), chloroplatinic acid powder is dissolved in absolute ethyl alcohol, prepares catalyst solution；(2), H PSO solution and catalyst solution are mixed, obtain mixed solution；(3), graphite matrix is immersed in mixed solution, then carries out cross-linking reaction；(4), cross-linking products are placed in high temperature process furnances and carry out pyroreaction；(5) unreacted activated carbon and silicon-carbide particle, are removed by floatation, silicon carbide whisker coating is obtained on graphite matrix surface.The silicon carbide whisker coating that the present invention is obtained shows good high-temperature oxidation resistance, and in oxidizing process, coating surface micropore can heal.
Description
Technical field
The application is related to a kind of antioxidant coating, and carborundum is prepared more particularly to a kind of graphite matrix surface
The method of whisker coating.
Background technology
Silicon carbide whisker is a kind of high-modulus, intensity is high, hardness is big, wear-resisting, corrosion-resistant, resistant to elevated temperatures
Lightweight structural material, mainly for the preparation of composites such as ceramic base, Metal Substrate, resin bases, to improve
The performance such as the intensity of material, hardness, wear-resistant, aerospace, atomic energy, automobile, ship, new material,
The industrial circles such as chemistry, electric power, oil, electronics, environment, machinery, metallurgy have extensive purposes.
At present, most common application be silicon carbide whisker activeness and quietness aluminum oxide and silicon nitride manufacture cutting tool,
Pressing mold fills first-class.
Preparing the method for silicon carbide whisker has a lot, most ripe technology be with carbon black, ultrafine silica powder or
Rice husk is raw material, adds Fe, Co, Ni simple substance or the one or more of its compound make catalyst,
It is heated to high temperature in graphite with making heater electric furnace and synthesizes.With conventional heating electric furnace synthesizing silicon carbide whisker,
Not only synthesis temperature is high, low yield, and complex operation, and heater cost is high, loss is big.Cause one
It is that equipment investment is big；Second, raw material heating is uneven, whisker yield is relatively low；Third, the production of whisker
Cost is high, and quality is not relatively high；Fourth, operating difficulties, in preparation process, caused escaping gas is usually
Influence the normal continuous production of high-temperature electric resistance furnace.
The content of the invention
It is an object of the invention to provide a kind of method that graphite matrix surface prepares silicon carbide whisker coating,
To overcome deficiency of the prior art.
To achieve the above object, the present invention provides following technical scheme：
The embodiment of the present application discloses a kind of method that graphite matrix surface prepares silicon carbide whisker coating, including
Step：
(1), chloroplatinic acid powder is dissolved in absolute ethyl alcohol, prepares catalyst solution；
(2), H-PSO solution and catalyst solution are mixed, obtain mixed solution；
(3), graphite matrix is immersed in mixed solution, then carries out cross-linking reaction；
(4), cross-linking products are placed in high temperature process furnances and carry out pyroreaction；
(5) unreacted activated carbon and silicon-carbide particle, are removed by floatation, on graphite matrix surface
Obtain silicon carbide whisker coating.
Preferably, in preparing the method for silicon carbide whisker coating on above-mentioned graphite matrix surface, step (1)
In, the concentration of catalyst solution is 1.5~1.8%.
Preferably, in preparing the method for silicon carbide whisker coating on above-mentioned graphite matrix surface, step (3)
In, impregnation pressure is 0.4~0.5MPa, and dip time is 40~60 minutes
Preferably, in preparing the method for silicon carbide whisker coating on above-mentioned graphite matrix surface, step (3)
In, cross-linking reaction is carried out at 100~110 DEG C 20~30 minutes.
Preferably, in preparing the method for silicon carbide whisker coating on above-mentioned graphite matrix surface, step (4)
In, 8~10 DEG C/min of heating rate, 1800~2000 DEG C of reaction temperature, 60~90min of reaction time.
Preferably, in preparing the method for silicon carbide whisker coating on above-mentioned graphite matrix surface, step (5)
In, a diameter of 0.3~0.4 μm of the silicon carbide whisker of acquisition, draw ratio 50 or so.
Compared with prior art, the advantage of the invention is that：The silicon carbide whisker coating that the present invention is obtained
Good high-temperature oxidation resistance is shown, in oxidizing process, coating surface micropore can heal.
Embodiment
The present invention is described further by the following example：, can be more preferably geographical according to following embodiments
The solution present invention.However, as it will be easily appreciated by one skilled in the art that specific material described by embodiment
The present invention is merely to illustrate than, process conditions and its result, without should be also without limitation on claims
In the described in detail present invention.
Embodiment 1
The method that graphite matrix surface prepares silicon carbide whisker coating
(1), chloroplatinic acid powder is dissolved in absolute ethyl alcohol, prepares catalyst solution, the catalyst is molten
The concentration of liquid is 1.5%；
(2), H-PSO solution and catalyst solution are mixed, obtain mixed solution；
(3), graphite matrix is immersed in mixed solution, impregnation pressure 0.4MPa, dip time is
40 minutes, cross-linking reaction is then carried out at 100 DEG C 20 minutes；
(4), cross-linking products are placed in high temperature process furnances and carry out pyroreaction, 10 DEG C/min of heating rate,
2000 DEG C of reaction temperature, reaction time 60min.
(5) unreacted activated carbon and silicon-carbide particle, are removed by floatation, on graphite matrix surface
Obtain silicon carbide whisker of the content 87% or so, a diameter of 0.3~0.4 μm of whisker, draw ratio 50
Left and right.
The silicon carbide whisker coating obtained shows good high-temperature oxidation resistance, in oxidizing process,
Coating surface micropore can heal.
Obtained coating aoxidizes 8 hours at 1600 DEG C, and oxidation weight loss is only less than 0.8%.
Embodiment 2
The method that graphite matrix surface prepares silicon carbide whisker coating
(1), chloroplatinic acid powder is dissolved in absolute ethyl alcohol, prepares catalyst solution, the catalyst is molten
The concentration of liquid is 1.7%；
(2), H-PSO solution and catalyst solution are mixed, obtain mixed solution；
(3), graphite matrix is immersed in mixed solution, impregnation pressure 0.5MPa, dip time is
40 minutes, cross-linking reaction is then carried out at 100 DEG C 30 minutes；
(4), cross-linking products are placed in high temperature process furnances and carry out pyroreaction, 10 DEG C/min of heating rate,
1800 DEG C of reaction temperature, reaction time 60min.
(5) unreacted activated carbon and silicon-carbide particle, are removed by floatation, on graphite matrix surface
Obtain silicon carbide whisker of the content 87% or so, a diameter of 0.3~0.4 μm of whisker, draw ratio 50
Left and right.
The silicon carbide whisker coating obtained shows good high-temperature oxidation resistance, in oxidizing process,
Coating surface micropore can heal.
Obtained coating aoxidizes 8 hours at 1600 DEG C, oxidation weight loss 0.84%.
Finally, it is to be noted that, term " comprising ", "comprising" or its any other variant meaning
Covering including for nonexcludability so that process, method, article including a series of elements or
Equipment not only includes those key elements, but also the other element including being not expressly set out, or also wraps
Include as this process, method, article or the intrinsic key element of equipment.
Claims (6)
1. a kind of method that graphite matrix surface prepares silicon carbide whisker coating, it is characterised in that including step：
(1), chloroplatinic acid powder is dissolved in absolute ethyl alcohol, prepares catalyst solution；
(2), H-PSO solution and catalyst solution are mixed, obtain mixed solution；
(3), graphite matrix is immersed in mixed solution, then carries out cross-linking reaction；
(4), cross-linking products are placed in high temperature process furnances and carry out pyroreaction；
(5) unreacted activated carbon and silicon-carbide particle, are removed by floatation, silicon carbide whisker coating is obtained on graphite matrix surface.
2. the method that graphite matrix surface according to claim 1 prepares silicon carbide whisker coating, it is characterised in that：In step (1), the concentration of catalyst solution is 1.5~1.8%.
3. the method that graphite matrix surface according to claim 1 prepares silicon carbide whisker coating, it is characterised in that：In step (3), impregnation pressure is 0.4~0.5MPa, and dip time is 40~60 minutes.
4. the method that graphite matrix surface according to claim 1 prepares silicon carbide whisker coating, it is characterised in that：Cross-linking reaction is carried out in step (3), at 100~110 DEG C 20~30 minutes.
5. the method that graphite matrix surface according to claim 1 prepares silicon carbide whisker coating, it is characterised in that：In step (4), 8~10 DEG C/min of heating rate, 1800~2000 DEG C of reaction temperature, 60~90min of reaction time.
6. the method that graphite matrix surface according to claim 1 prepares silicon carbide whisker coating, it is characterised in that：In step (5), a diameter of 0.3~0.4 μm of the silicon carbide whisker of acquisition, draw ratio 50 or so.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610452857.6A CN107523877A (en) | 2016-06-22 | 2016-06-22 | The method that graphite matrix surface prepares silicon carbide whisker coating |
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| CN201610452857.6A CN107523877A (en) | 2016-06-22 | 2016-06-22 | The method that graphite matrix surface prepares silicon carbide whisker coating |
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| CN201610452857.6A Withdrawn CN107523877A (en) | 2016-06-22 | 2016-06-22 | The method that graphite matrix surface prepares silicon carbide whisker coating |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109652857A (en) * | 2019-02-14 | 2019-04-19 | 华北理工大学 | A kind of preparation method of SiC whisker |
| CN115872777A (en) * | 2022-11-30 | 2023-03-31 | 昊石新材料科技南通有限公司 | Preparation method of graphite surface silicon carbide coating based on CVR and CVD |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167623A (en) * | 2011-01-10 | 2011-08-31 | 廖寄乔 | Carbon material oxidation resistant coating and preparation method thereof |
| CN102850087A (en) * | 2012-09-29 | 2013-01-02 | 西安超码科技有限公司 | Method for preparing silicon carbide coating on graphite surface |
| CN103253671A (en) * | 2013-03-14 | 2013-08-21 | 江苏大学 | Method for preparing SiC nanowire |
-
2016
- 2016-06-22 CN CN201610452857.6A patent/CN107523877A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167623A (en) * | 2011-01-10 | 2011-08-31 | 廖寄乔 | Carbon material oxidation resistant coating and preparation method thereof |
| CN102850087A (en) * | 2012-09-29 | 2013-01-02 | 西安超码科技有限公司 | Method for preparing silicon carbide coating on graphite surface |
| CN103253671A (en) * | 2013-03-14 | 2013-08-21 | 江苏大学 | Method for preparing SiC nanowire |
Non-Patent Citations (1)
| Title |
|---|
| 陈旸，王成国，高冉冉，朱波: "SiC晶须制备工艺的研究", 《无机材料学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109652857A (en) * | 2019-02-14 | 2019-04-19 | 华北理工大学 | A kind of preparation method of SiC whisker |
| CN109652857B (en) * | 2019-02-14 | 2020-08-04 | 华北理工大学 | Preparation method of SiC whisker |
| CN115872777A (en) * | 2022-11-30 | 2023-03-31 | 昊石新材料科技南通有限公司 | Preparation method of graphite surface silicon carbide coating based on CVR and CVD |
| CN115872777B (en) * | 2022-11-30 | 2023-10-27 | 昊石新材料科技南通有限公司 | Preparation method of graphite surface silicon carbide coating |
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Application publication date: 20171229 |