CN103435372A - Graphite carbon sleeve gradient anti-oxidation coating and preparation method thereof - Google Patents
Graphite carbon sleeve gradient anti-oxidation coating and preparation method thereof Download PDFInfo
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- CN103435372A CN103435372A CN2013103479526A CN201310347952A CN103435372A CN 103435372 A CN103435372 A CN 103435372A CN 2013103479526 A CN2013103479526 A CN 2013103479526A CN 201310347952 A CN201310347952 A CN 201310347952A CN 103435372 A CN103435372 A CN 103435372A
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Abstract
The invention relates to a graphite carbon sleeve gradient anti-oxidation coating and a preparation method thereof. The preparation method comprises the following steps: the surface of a graphite carbon sleeve is pretreated; polyaluminocarbosilane (PACS) serves as a precursor for preparing the graphite carbon sleeve gradient anti-oxidation coating; the PACS has the advantages of high ceramic production rate and good effects of anti-oxidation and high temperature resistance; the pre-treated graphite carbon sleeve is immersed in a xylene solution of the PACS under the vacuum condition, kept under the vacuum condition for 1-10 min, macerated under the condition of pressurizing 10 MPa, dried and placed in an electric furnace, raised to 1,100-1,600 DEG C, and is cracked for preparing the graphite carbon sleeve gradient anti-oxidation coating.
Description
Technical field
The present invention relates to a kind of preparation method of graphite anti-oxidation composite coating, being specifically related to a kind of employing high-pressure impregnation SiC ceramic precursor is that polyaluminocarbosilane (PACS) is dissolved in xylene solution, and then the technique of cracking prepares the method for graphite carbon sleeve gradient oxidation resistant coating.
Background technology
The graphite sleeves of rollers at furnace bottom of silicon steel production use, because its good thermotolerance, self lubricity and suitable hardness are widely used.But it is poor that its deadly defect is antioxidant property, particularly extremely short work-ing life in the high-temperature zone more than 920 ℃, what impact was produced normally carries out, and production cost also is difficult to bear, and therefore improves the anti-oxidant problem of graphite carbon sleeve most important.
The coat of silicon carbide on graphite carbon sleeve surface has good high-temperature oxidation resistance in the operation interval of graphite carbon sleeve, is the effective anti-oxidation barrier of graphite carbon sleeve.In order to improve the bonding force between coating and graphite carbon sleeve substrate, make oxidation resistant coating there is excellent anti-oxidant and thermal shock resistance, a kind of effective means is that the bonding interface of coating and graphite matrix is configured to thermal stresses mitigation type gradient cladding.Adopting the high-pressure impregnation cracking technology to make the SiC component is a kind of simple and effective method in the inner Gradient distribution of graphite carbon sleeve.The advantages such as it is simple that high-pressure impregnation cracking technology (PIP) has technique, and cost is low, can prepare large-scale and complex-shaped composite element, and material composition and structure are controlled, and the PIP method is easy to suitability for industrialized production.Usually the impregnating by pressure technique adopted, its pressure is too low, and generally lower than 1.5MPa, the impregnation pressure adopted such as patent CN100534951C is 1.2～0.5MPa, and oxidation resistance temperature is the highest only reaches 950 ℃; The impregnation pressure that in patent CN1117479A, the metallic cementation processing adopts is 0.4～0.6MPa, has improved the wear-resistant and snappiness of graphite carbon sleeve, and the high-temperature oxidation resistant effect is not provided to concrete data; In patent CN100425571C, the phosphoric acid salt impregnation pressure is 0.6MPa, and dipping efficiency is not high, and apparent porosity is up to 15%; The impregnation pressure that patent CN101696121B adopts is 1～1.5MPa, slightly high, and dipping efficiency is than the improve greatly of other patent report, but the high-temperature oxidation resistant temperature is still on the low side; This too low impregnation pressure is little to the formation effect of gradient cladding, and this patent adopts high-pressure impregnation, and effect significantly improves.
Summary of the invention
The object of the present invention is to provide a kind of not only preparation cost low, and the preparation method of graphite carbon sleeve gradient oxidation resistant coating simple to operate, that preparation cycle is short.
The invention provides a kind of preparation method of graphite carbon sleeve gradient oxidation resistant coating, graphite carbon sleeve is carried out to surface preparation; The presoma for preparing graphite carbon sleeve gradient oxidation resistant coating with polyaluminocarbosilane (PACS) conduct, it is high that polyaluminocarbosilane (PACS) has a ceramic yield, anti-oxidant and the good advantage of high-temperature resistant result, pre-treatment is flooded to the xylene solution of polyaluminocarbosilane (PACS) under complete graphite carbon sleeve vacuum, after vacuum state keeps 1～10min, 2～10MPa impregnating by pressure, put into electric furnace after oven dry and be warming up to 1100 ℃～1600 ℃, the standby graphite carbon sleeve gradient oxidation resistant coating of cracking.
For achieving the above object, the technical solution used in the present invention is specific as follows:
A kind of graphite carbon sleeve gradient coating for resisting oxidation preparation method, the preparation method is as follows: (1), graphite carbon sleeve pre-treatment: graphite carbon sleeve is carried out to surface preparation, first surface finish, then cleaned, finally carry out drying; (2), solution preparation: polyaluminocarbosilane (PACS) is dissolved in to dimethylbenzene, and heated and stirred is mixed with the polyaluminocarbosilane (PACS) of 30wt.%～60wt.%/xylene solution; (3), impregnation stage: impregnation stage is divided into vacuum impregnation and impregnating by pressure, vacuum impregnation is by through step 1) graphite carbon sleeve pre-treatment sample piece after processing is placed in impregnating autoclave, vacuumize, the above-mentioned PACS/ xylene solution prepared is injected to tank, keep vacuum impregnation 1～10min under vacuum state; Impregnating by pressure is: the 2～10MPa that pressurizes after vacuum impregnation, keep pressure impregnation 1～5 hour, and flood complete the taking-up afterwards from impregnating autoclave; (4), baking stage: the graphite carbon sleeve after dipping that will take out is dried; (5), roasting cleavage stages: pass through again inert atmosphere after oven dry at 500～1600 ℃ of lower sintering, roasting insulation 2～4 hours; (6), repeating step (3) is to step (5) 3-7 time, finally obtains the graphite carbon sleeve gradient coating for resisting oxidation.
In described step (4) baking stage, bake out temperature is 50-200 ℃; Drying time is 3-8 hour; Preferably bake out temperature is 100-200 ℃; Drying time is 5-8 hour; More preferably bake out temperature is 100 ℃; Drying time is 5 hours;
In described step (5) roasting cleavage stages, graphite carbon sleeve after drying is put into to atmosphere furnace, pass into rare gas element as shielding gas, the temperature rise rate of controlled atmosphere furnace is 0.1～2 ℃/min subsequently, and furnace temperature is risen to 500-1000 ℃ of insulation 1～2 hour; Then continue to heat up, temperature rise rate is 0.1～2 ℃/min, furnace temperature is risen to 1100-1600 ℃ and be incubated 1～2 hour again, is down to room temperature with the speed of 2-10 ℃/min subsequently, after blow-on, takes out, and obtains the graphite carbon sleeve gradient coating for resisting oxidation;
Preferably pass into rare gas element as shielding gas, the temperature rise rate of controlled atmosphere furnace is 1～2 ℃/min subsequently, and furnace temperature is risen to 800-1000 ℃ of insulation 1～2 hour; Then continue to heat up, temperature rise rate is 1～2 ℃/min, furnace temperature is risen to 1400-1600 ℃ and be incubated 1～2 hour again, is down to room temperature with the speed of 2-8 ℃/min subsequently;
More preferably pass into rare gas element as shielding gas, the temperature rise rate of controlled atmosphere furnace is 2 ℃/min subsequently, and furnace temperature is risen to 800 ℃ of insulations 2 hours; Then continue to heat up, temperature rise rate is 2 ℃/min, furnace temperature is risen to 1500 ℃ and be incubated 2 hours again, is down to room temperature with the speed of 5 ℃/min subsequently;
At described step (3) impregnation stage: vacuum impregnation is by through step 1) graphite carbon sleeve pre-treatment sample piece after processing is placed in impregnating autoclave, is evacuated to 0 to negative 1MPa; Limited being evacuated to-0.1 is to-0.8MPa, and preferably-0.1 to-0.8MPa, choosing-0.18MPa is more arranged;
Preferably at described step (3) impregnation stage: vacuum impregnation is by through step 1) graphite carbon sleeve pre-treatment sample piece after processing is placed in impregnating autoclave, be evacuated to negative 0.1MPa, the above-mentioned PACS/ xylene solution prepared is injected to tank, keep vacuum impregnation 10min under vacuum state; Impregnating by pressure is: the 5MPa that pressurizes after vacuum impregnation, keep pressure impregnation 3 hours, and flood complete the taking-up afterwards from impregnating autoclave.
Preferably, in described step (5) roasting cleavage stages, the graphite carbon sleeve after drying is put into to atmosphere furnace, pass into rare gas element as shielding gas, the temperature rise rate of controlled atmosphere furnace is 0.1 ℃/min subsequently, and furnace temperature is risen to 650 ℃ of insulations 2 hours; Then continue to heat up, temperature rise rate is 2 ℃/min, furnace temperature is risen to 1400 ℃ and be incubated 2 hours again, is down to room temperature with the speed of 5 ℃/min subsequently, after blow-on, takes out, and obtains the graphite carbon sleeve gradient coating for resisting oxidation;
For step 6), preferably repeating step (3), to step (5) 3-5 time, more selects 3-4 time or 5 times or 7 times most preferably 3 times.
The present invention also provides a kind of graphite carbon sleeve gradient coating for resisting oxidation prepared as preceding method; prepared graphite carbon sleeve gradient coating for resisting oxidation is protected graphite material 1000 hours in 1100 ℃ of still airs; oxidation weight loss is less than 0.53wt.%; 1100 ℃ of anti-thermal shocks do not come off for 100 times, and use temperature reaches 2000 ℃.
Technique of the present invention is simple, easy to operate, lower than the vapour deposition process cost; Adopt under vacuum state and inject steeping fluid, there is good perviousness, can infiltrate trickle hole and the top coat in graphite matrix surface, strengthen oxidation-resistance; Adopt 2～10MPa impregnating by pressure, there is high dipping efficiency, the immersion graphite carbon sleeve matrix inside that steeping fluid under high pressure can be more deep, progressively fill the graphite carbon sleeve internal void, form gradient cladding, there is pinning effect, not only strengthened oxidation-resistance, and also helpful to heat-shock resistance; Method of the present invention has solved the poor problem of coating heat-shock resistance, and than the standby transition layer technique of traditional RESEARCH OF PYROCARBON or BN legal system, operation greatly reduces, and dipping efficiency obviously improves, and the dipping number of times significantly reduces.The graphite carbon sleeve gradient oxidation resistant coating even compact of gained, have good anti-oxidant and high-temperature resistant result.
The present invention obtains the graphite carbon sleeve gradient coating for resisting oxidation by vacuum/high-pressure impregnation.This coating effective constituent SiC can immerse graphite carbon sleeve inside, in material internal and surperficial distribution gradient, plays pinning effect, and good with graphite carbon sleeve substrate bonding strength, and density is high, and even thickness, without through-wall crack and micropore.The single coating that the gained coating is distribution gradient, technique is simple, easy to operate, and reaction time is short, and cost is low.And the presoma of graphite carbon sleeve gradient coating for resisting oxidation has adopted polyaluminocarbosilane (PACS), greatly improved the high thermal resistance of ceramic yield and coating.The technique preparation is simple, and easy to operate, raw material is easy to get, and preparation cost is lower.Prepared graphite carbon sleeve gradient coating for resisting oxidation can be protected graphite material 1000 hours in 1100 ℃ of still airs, and oxidation weight loss is less than 0.53wt.%, and 1100 ℃ of anti-thermal shocks do not come off for 100 times.
In conjunction with technical solution of the present invention, the technique effect reached also comprises:
1) described SiC oxidation resistant coating, the advantage such as its presoma is polyaluminocarbosilane (PACS), has a ceramic yield high, and anti-oxidant and high-temperature resistant result is good;
2) described steeping fluid, its concentration 30wt.%～60wt.%, improved dipping efficiency, reduced the dipping number of times; Described dipping number of times can be according to dipping concentration and impregnation pressure adjustment, conveniently, flexibly; And impregnation sintering has guaranteed homogeneity and the compactness of gained coating repeatedly, avoid the existence of dipping " blind area ";
3) described sintering process, at 1100 ℃～1600 ℃, be incubated 1～4 hour, makes the complete crystallization of gained SiC coating, improves its coating compactness and mechanical property;
4) described have high dipping efficiency, steeping fluid under high pressure can the hole of more deep immersion graphite carbon sleeve matrix inside in, when progressively filling the graphite carbon sleeve internal void, form gradient cladding, there is pinning effect, not only strengthened oxidation-resistance, and also helpful to heat-shock resistance; High-pressure impregnation has solved the poor problem of coating heat-shock resistance, than traditional RESEARCH OF PYROCARBON or BN, prepares transition layer technique, and operation greatly reduces, and the dipping efficiency obviously improve, the dipping number of times significantly reduce;
5) preparation technology of described gradient cladding all adopts impregnation technology, do not need to adopt such as vapour deposition process, gas phase siliconising method etc., have that technique is simple, cost is low, easy to operate, can prepare the advantages such as large-scale and complex-shaped composite element, material composition and structure be controlled, and be easy to suitability for industrialized production.
6) the present invention is equally applicable to the preparation of all carbonaceous material oxidation resistant coating.
Above these sintering temperatures and time, impregnating process comprise impregnation pressure and have synergy mutually between the time, not isolated parameter, can not by prior art, openly be caused whole invention not possess creativeness because of one of them or some parameters, consider that invention possesses the whether creative main integral body of the technical scheme from invention and considers, the present invention is just by the combination of above-mentioned parameter feature, its synergy has obtained unforeseeable technique effect, make invention possess creativeness, the parameter index value of specifically putting down in writing referring to comparative example in table 1.
The accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention (take is for 3 times example repeatedly);
Silicon carbide gradient oxidation resistant coating graphite carbon sleeve surface (XRD) collection of illustrative plates that Fig. 2 is the embodiment of the present invention 1 preparation, wherein X-coordinate is diffraction angle 2 θ, unit is °; Ordinate zou is diffraction peak intensity, and unit is a.u..
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment 1:
1) pre-treatment of graphite carbon sleeve: graphite carbon sleeve is carried out to surface finish, polished finish, then clean up, put into baking oven and dry;
2) get polyaluminocarbosilane (PACS), be dissolved in dimethylbenzene, be mixed with the xylene solution of the PACS of 40wt.% through 70 ℃ of heated and stirred;
3) graphite sample piece is placed in to impregnating autoclave, is evacuated down to-0.1MPa, the solution that is 40wt.% by above-mentioned concentration injects tank, keep the vacuum state dipping after 5 minutes, the 2MPa that adds high pressure dipping 2 hours then takes out graphite carbon sleeve from impregnating autoclave, dries 4 hours for 200 ℃;
4) graphite carbon sleeve after drying is put into to atmosphere furnace, pass into argon gas as shielding gas, the temperature rise rate of controlled atmosphere furnace is that 0.1 ℃/min is warming up to 650 ℃ of insulations 2 hours subsequently, then be warming up to 1400 ℃ of insulations 2 hours with 2 ℃/min, be down to room temperature with the speed of 2 ℃/min subsequently, take out the graphite carbon sleeve with the SiC gradient protective coating after blow-on, after cleaning, drying, repeat above-mentioned technique, infiltration pyrolysis is 7 times repeatedly, dipping concentration is 40wt.%, soaks once and burns once, and sintering schedule is identical; The SiC gradient protective coating that obtains graphite carbon sleeve after 7 infiltration pyrolysis is the graphite carbon sleeve gradient coating for resisting oxidation; Prepared compound coating can be protected graphite carbon sleeve 1000 hours in 1100 ℃ of still airs, oxidation weight loss 0.51wt.%, and 1100 ℃ of anti-thermal shocks do not come off for 100 times.
Embodiment 2:
The pre-treatment of graphite carbon sleeve and the preparation of dipping solution are identical with embodiment 1, and dipping, oven dry, pyroprocessing and vacuum tightness, impregnation pressure (2MPa) are also identical; Impregnation concentration is changed into: 60wt.%, the infiltration pyrolysis number of times changes into 3 times, and 3 times impregnating cracking technology is all corresponding with embodiment 1; The SiC gradient protective coating that obtains graphite carbon sleeve after 3 infiltration pyrolysis is the graphite carbon sleeve gradient coating for resisting oxidation.Prepared gradient cladding can be protected graphite material 1000 hours in 1100 ℃ of still airs, oxidation weight loss 0.52wt.%, and 1100 ℃ of anti-thermal shocks do not come off for 100 times.
Embodiment 3:
The pre-treatment of graphite carbon sleeve and the preparation of dipping solution are identical with embodiment 1, and dipping, oven dry, pyroprocessing and vacuum tightness are also identical; Change impregnation concentration into 60wt.%, impregnation pressure changes 5MPa into, and the infiltration pyrolysis number of times changes into 3 times, and 3 times impregnating cracking technology is all corresponding with embodiment 1; Obtain the SiC gradient protective coating of graphite carbon sleeve after 3 infiltration pyrolysis.Prepared gradient cladding can be protected graphite material 1000 hours in 1100 ℃ of still airs, oxidation weight loss 0.50wt.%, and 1100 ℃ of anti-thermal shocks do not come off for 100 times.
By gained with the SiC gradient protective coating, be (ARLX ' TRA type) x-ray diffractometer analytic sample graphite carbon sleeve for of graphite carbon sleeve gradient coating for resisting oxidation, the diffraction peak (seeing Fig. 2) that discovery coating gained collection of illustrative plates is graphite, silicon carbide and micro-silicon-dioxide.
Comparative example, design parameter sees the following form 1, table 1 parameter comparison table:
The obtaining of above parameter index value has benefited from technical scheme limiting sintering temperature and time, impregnating process comprises impregnation pressure and has synergy mutually between the time, makes invention technical scheme integral body obtain unforeseeable technique effect.In above-mentioned table 1, the content of record, the graphite carbon sleeve antioxidant property that can reflect embodiment of the present invention 1-3 from work-ing life significantly improves, and simple, easy to operate by the known technique of preparation technology, reaction time is short, and cost is low; High-temperature resistant result can show from the use temperature of table 1 well, and heat-shock resistance can the folding strength index from table 1 be considered etc.In a word, technical scheme of the present invention, solved Related Technical Issues, obtained good technique effect.
Be only below the preferred embodiment of the present invention, protection scope of the present invention also not only is confined to above-described embodiment, with the present invention, conceives various process programs without substantial differences all in protection scope of the present invention.The present invention elaborates it by embodiment, and still, any form that does not exceed the claim protection domain that those skilled in the art made on this basis and the variation of details, all belong to invention which is intended to be protected.
Claims (8)
1. a graphite carbon sleeve gradient coating for resisting oxidation preparation method is characterized in that:
(1) graphite carbon sleeve pre-treatment: graphite carbon sleeve is carried out to surface preparation, first surface finish, then cleaned, finally carry out drying;
(2) solution preparation: polyaluminocarbosilane (PACS) is dissolved in to dimethylbenzene, and heated and stirred is mixed with the polyaluminocarbosilane (PACS) of 30wt.%～60wt.%/xylene solution;
(3) impregnation stage: impregnation stage is divided into vacuum impregnation and impregnating by pressure, vacuum impregnation is that the graphite carbon sleeve pre-treatment sample piece after step (1) is processed is placed in to impregnating autoclave, vacuumize, the above-mentioned polyaluminocarbosilane (PACS) for preparing/xylene solution is injected to tank, keep vacuum impregnation 1～10min under vacuum state; Impregnating by pressure is: the 2～10MPa that pressurizes after vacuum impregnation, keep the pressure impregnation 1～5 hour of 2～10MPa, and flood after complete and take out from impregnating autoclave;
(4) baking stage: the graphite carbon sleeve after dipping that will take out is dried;
(5) roasting cleavage stages: pass through inert atmosphere after oven dry at 500～1600 ℃ of lower sintering, roasting insulation 2～4 hours, obtain the graphite carbon sleeve gradient coating for resisting oxidation again;
(6) repeating step (3), to step (5) 3-7 time, finally obtains the graphite carbon sleeve gradient coating for resisting oxidation.
2. the method for claim 1, it is characterized in that: in described step (4) baking stage, bake out temperature is 50-200 ℃; Drying time is 3-8 hour; At described step (2) solution preparation in the stage, solution preparation temperature 50-80 ℃.
3. as claim 1 or the described method of 2 any one, it is characterized in that: in described step (5) roasting cleavage stages, graphite carbon sleeve after drying is put into to atmosphere furnace, pass into rare gas element as shielding gas, the temperature rise rate of controlled atmosphere furnace is 0.1～2 ℃/min subsequently, and furnace temperature is risen to 500-1000 ℃ of insulation 1～2 hour; Then continue to heat up, temperature rise rate is 0.1～2 ℃/min, furnace temperature is risen to 1100-1600 ℃ and be incubated 1～2 hour again, is down to room temperature with the speed of 2-10 ℃/min subsequently, after blow-on, takes out, and obtains the graphite carbon sleeve gradient coating for resisting oxidation.
4. method as claimed in claim 3 is characterized in that: at described step (3) impregnation stage: vacuum impregnation is that the graphite carbon sleeve pre-treatment sample piece after step (1) is processed is placed in to impregnating autoclave, is evacuated to 0 to-1MPa.
5. as claim 1 or the described method of 4 any one, it is characterized in that: at described step (3) impregnation stage: vacuum impregnation is by through step 1) graphite carbon sleeve pre-treatment sample piece after processing is placed in impregnating autoclave, be evacuated to-0.1MPa, the above-mentioned PACS/ xylene solution prepared is injected to tank, keep vacuum impregnation 10min under vacuum state; Impregnating by pressure is: the 5MPa that pressurizes after vacuum impregnation, keep pressure impregnation 3 hours, and flood complete the taking-up afterwards from impregnating autoclave.
6. as claim 1 or the described method of 3 any one, it is characterized in that:
In described step (5) roasting cleavage stages, the graphite carbon sleeve after drying is put into to atmosphere furnace, pass into rare gas element as shielding gas, the temperature rise rate of controlled atmosphere furnace is 0.1 ℃/min subsequently, and furnace temperature is risen to 650 ℃ of insulations 2 hours; Then continue to heat up, temperature rise rate is 2 ℃/min, furnace temperature is risen to 1400 ℃ and be incubated 2 hours again, is down to room temperature with the speed of 5 ℃/min subsequently, after blow-on, takes out, and obtains the graphite carbon sleeve gradient coating for resisting oxidation.
7. as claim 1,2 or 4 described methods, it is characterized in that: for step (6), repeating step (3) is to step (5) 3 times or 5 times or 7 times.
8. the graphite carbon sleeve gradient coating for resisting oxidation prepared as method as described in claim 1-7 any one; it is characterized in that: prepared graphite carbon sleeve gradient coating for resisting oxidation is protected graphite material 1000 hours in 1100 ℃ of still airs; oxidation weight loss is less than 0.53wt.%; 1100 ℃ of anti-thermal shocks do not come off for 100 times, and use temperature reaches 2000 ℃.。
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103820627A (en) * | 2014-01-02 | 2014-05-28 | 中国平煤神马集团开封炭素有限公司 | Graphitic carbon sleeve production method |
| CN107141023A (en) * | 2017-05-04 | 2017-09-08 | 上海弘竣实业有限公司 | A kind of graphite surface carbonization silicon infiltration handling process |
| CN107814590A (en) * | 2017-11-07 | 2018-03-20 | 中国科学院山西煤炭化学研究所 | A kind of preparation method of fusedsalt reactor graphite surface SiC coatings |
| CN112624797A (en) * | 2020-12-15 | 2021-04-09 | 湖南德智新材料有限公司 | Graphite surface gradient silicon carbide coating and preparation method thereof |
| CN113698232A (en) * | 2021-08-19 | 2021-11-26 | 武汉钢铁有限公司 | Low-temperature carbon sleeve resistant to ammonia gas corrosion and abrasion and production method thereof |
| CN115198253A (en) * | 2022-07-05 | 2022-10-18 | 苏州步科斯新材料科技有限公司 | Preparation method of graphite matrix surface tantalum carbide coating |
| CN115304391A (en) * | 2022-08-16 | 2022-11-08 | 三一集团有限公司 | Graphite felt-based composite material and preparation method thereof |
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2013
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103820627A (en) * | 2014-01-02 | 2014-05-28 | 中国平煤神马集团开封炭素有限公司 | Graphitic carbon sleeve production method |
| CN103820627B (en) * | 2014-01-02 | 2015-11-25 | 中国平煤神马集团开封炭素有限公司 | A kind of graphite charcoal cover production method |
| CN107141023A (en) * | 2017-05-04 | 2017-09-08 | 上海弘竣实业有限公司 | A kind of graphite surface carbonization silicon infiltration handling process |
| CN107814590A (en) * | 2017-11-07 | 2018-03-20 | 中国科学院山西煤炭化学研究所 | A kind of preparation method of fusedsalt reactor graphite surface SiC coatings |
| CN112624797A (en) * | 2020-12-15 | 2021-04-09 | 湖南德智新材料有限公司 | Graphite surface gradient silicon carbide coating and preparation method thereof |
| CN113698232A (en) * | 2021-08-19 | 2021-11-26 | 武汉钢铁有限公司 | Low-temperature carbon sleeve resistant to ammonia gas corrosion and abrasion and production method thereof |
| CN113698232B (en) * | 2021-08-19 | 2023-07-18 | 武汉钢铁有限公司 | Low-temperature carbon sleeve resistant to ammonia corrosion and abrasion and production method thereof |
| CN115198253A (en) * | 2022-07-05 | 2022-10-18 | 苏州步科斯新材料科技有限公司 | Preparation method of graphite matrix surface tantalum carbide coating |
| CN115304391A (en) * | 2022-08-16 | 2022-11-08 | 三一集团有限公司 | Graphite felt-based composite material and preparation method thereof |
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