CN1297515C - Preparation method of charcoal material surface coating for resisting high temperature oxidation - Google Patents
Preparation method of charcoal material surface coating for resisting high temperature oxidation Download PDFInfo
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- CN1297515C CN1297515C CNB2005100127304A CN200510012730A CN1297515C CN 1297515 C CN1297515 C CN 1297515C CN B2005100127304 A CNB2005100127304 A CN B2005100127304A CN 200510012730 A CN200510012730 A CN 200510012730A CN 1297515 C CN1297515 C CN 1297515C
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Abstract
The present invention relates to a preparation method of a charcoal material surface coating for resisting high temperature oxidation, which is used for cleaning and drying the charcoal material surface. Silicon powder, boron powder, water and adhesives are mixed to prepare slurry according to weight proportion of 43.5 to 50.5: 3 to 10: 44.5 to 45: 1.0 to 2.5; then, the slurry is coated on the charcoal material surface which is cleanly washed in a dipping way, a spraying way or a brushing way; the thickness of the coating slurry is from 200 microns to 240 microns; the charcoal material surface with the slurry is dried and then is put in a vacuum resistance furnace which is heated to 400 to 500 DEGC; the heat-insulation time lasts for 10-20 minutes; then the furnace is heated to 1420 DETC to 1500 DEGC, and the heat-insulation time lasts for 20 to 30 minutes; after cooled, a high temperature anti-oxidation ceramic coating is obtained. The present invention has the advantages of simple technology, high efficiency and favorable repeatability, and the present invention largely reduces the cost of the charcoal materials, is easy to amplify the whole technological process, and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind ofly prepare the method for high-temperature oxidation resistant coating, belong to raw material of wood-charcoal material protection field at charcoal material surface.
Background technology
Carbon material has good thermotolerance, and chemical stability and electroconductibility are widely used in the high temperature field as structure and engineering materials.But, carbon material just begins to take place oxidizing reaction in the oxidizing atmosphere more than 400 ℃, make its every physics and the rapid deterioration of mechanical property, therefore, it is to prolong its working life that the raw material of wood-charcoal material is carried out the oxidation protection processing, improves the essential measure of its job stability and reliability.
It is a kind of main method that solves raw material of wood-charcoal material high temperature (＞1200 ℃) oxidation protection that the raw material of wood-charcoal material is carried out the coating processing.SiC coating thermostability height, good with the carbon matrix chemical compatibility, thermal expansivity is approaching.It is the main ceramic coating material that is used for raw material of wood-charcoal material oxidation protection at present.Preparation SiC coating main method has at present: entrapping method, and chemical Vapor deposition process, plasma spraying method, chemical vapor infiltration etc., but the SiC coating of this several method preparation generally contains a lot of microporositys and tiny crack, and resistance of oxidation is not strong.In order to improve the SiC anti-oxidation of coating, people take diverse ways to come the packing crackle again, for example use sol-gel shutoff SiC coating repeatedly.(Journal of Material Science, 1991,26 (4) such as Gee; 1093) applied borate glass again on the SiC coating, borate glass at high temperature has lower viscosity and good flowability, the tiny crack in the SiC coating that can heal.(Carbon, 1995,33 (4) such as Piquero; 455) adopt B
4The C undercoat adds SiC external coating (EC) system and carries out oxidation protection research.So just make whole process complicated, reduced its economic benefit.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of low cost is provided, has good oxidation-resistance, the preparation method of the simple charcoal material surface coating for resisting high temperature oxidation of technology
The object of the present invention is achieved like this: according to a certain percentage silica flour, boron powder, water, binding agent mixed preparing form slurry, slurry is fully ground in ball mill, make wherein each component uniform distribution.Adopt dip-coating, spraying or spread coating that this pulp bales is overlayed on the charcoal material surface that cleans up in advance, drying is 10～16 hours in 100 ℃-150 ℃ environment, obtains the exsiccant cladding.At last in vacuum resistance furnace, Heating temperature is higher than 20～100 ℃ of the fusing points (1410 ℃) of Si, insulation 20～30min, because there is a large amount of microporositys in raw material of wood-charcoal material inside, under capillary action power, feed liquid Si in the time of raw material of wood-charcoal material uniformly penetrating and carbon matrix reaction generate certain thickness gradient SiC coating, a spot of boron is uniformly distributed in the gradient SiC coating.The Gradient distribution of SiC coating has promoted the Chemical bond of coating and body material, has avoided owing to concentrating of thermal stresses causes coating stripping.The boron of disperse can become B by oxidation transformation in the coating
2O
3Fill the micropore of SiC coating, make the raw material of wood-charcoal material realize self-healing anti-oxidation.Prepared oxidation resistant coating has thermal-shock resistance and good high-temperature (1300 ℃) antioxidant property.
Preparation method of the present invention may further comprise the steps: (1). and charcoal material surface is cleaned, and the distilled water ultrasonic cleaning is used in decontamination, puts into the loft drier oven dry then;
(2). silica flour, boron powder, water, binding agent are silica flour by weight: boron powder: water: binding agent=43.5～50.5: 3～10: 44.5～45: 1.0～2.5 carry out the mixed preparing form slurry, slurry is fully ground in ball mill, make its each component uniform distribution, adopt dip-coating, spraying or spread coating this pulp bales to be overlayed on the charcoal material surface that cleans up, coating slurry thickness is 200 μ m～240 μ m, drying is 10～16 hours in 100 ℃-150 ℃ environment, obtains the exsiccant cladding;
(3). the above-mentioned cladding that makes is put into vacuum resistance furnace, at first stove is heated to 400～500 ℃ with 5～10 ℃/minute rate of heating, be incubated 10～20 minutes, and then stove is heated to 1420 ℃～1500 ℃ with 15～20 ℃/minute rate of heating, being incubated 20～30 minutes. outage stops heating, treat stove cooling back taking-up sample, can obtain the high-temperature oxidation resistant ceramic coating.
Above-mentioned used silicon particle size is 5～47 μ m, and boron powder degree is 3～10 μ m; Binding agent is polyvinyl alcohol (PVA), acrylamide (AM) or polyvinyl formal (PVA).
Advantage of the present invention:
1. technological process is simple relatively, good reproducibility.
2. adopt the Gradient distribution of liquid siliconising technology realization SiC coating, promoted the Chemical bond of coating and body material, avoided owing to concentrating of thermal stresses causes coating stripping.
3. the boron of disperse can become B by oxidation transformation in the coating
2O
3Fill the micropore of SiC coating, make the raw material of wood-charcoal material realize self-healing anti-oxidation.
4. Zhi Bei oxidation resistant coating has thermal-shock resistance and good high-temperature (1300 ℃) antioxidant property.
Embodiment
Embodiment 1
Si, B, H
2O, polyvinyl alcohol are 50.5: 3: 45 by weight: 1.5 are mixed with slurry, fully grind 1 hour in ball mill, make each component uniform distribution in the slurry.Adopt dip coating that this pulp bales is overlayed on the graphite material surface that cleans up, coating slurry thickness is 200 μ m.In 100 ℃ baking oven dry 16 hours then, obtain the exsiccant cladding.The exsiccant cladding is put into plumbago crucible, then crucible is put into vacuum resistance furnace, banking vacuumizes the energising heating.With 5 ℃/minute rate of heating stove being heated to 400 ℃, being incubated 20 minutes, and then stove is heated to 1450 ℃, be incubated 25 minutes with 20 ℃/minute rate of heating. outage stops heating, treats stove cooling back taking-up sample.Do anti-oxidant test in 1300 ℃ air, without the graphite oxidation of coating 1 hour, weight loss was 40%; After coating was handled, oxidation was after 30 hours, and weight loss is 0.1%.
Embodiment 2
Si, B, H
2O, polyvinyl alcohol are 45.5: 8: 45 by weight: 1.5 are mixed with slurry, fully grind 1 hour in ball mill, make each component uniform distribution in the slurry.Adopt spread coating that this pulp bales is overlayed on the graphite material surface that cleans up, coating slurry thickness is 230 μ m.In 120 ℃ baking oven dry 14 hours then, obtain the exsiccant cladding.The exsiccant cladding is put into plumbago crucible, then crucible is put into vacuum resistance furnace, banking vacuumizes the energising heating.With 8 ℃/minute rate of heating stove being heated to 450 ℃, being incubated 15 minutes, and then stove is heated to 1500 ℃, be incubated 20 minutes with 15 ℃/minute rate of heating. outage stops heating, treats stove cooling back taking-up sample.Do anti-oxidant test in 1300 ℃ air, without the graphite oxidation of coating 1 hour, weight loss was 40%; After coating was handled, oxidation was after 30 hours, and weight loss is 0.06%.
Embodiment 3
Si, B, H
2O, acrylamide, be 43.5: 10: 45.5 by weight: 1.0 are mixed with slurry, fully grind 1 hour in ball mill, make each component uniform distribution in the slurry.Adopt spraying method that this pulp bales is overlayed on the carbon/carbon composite surface that cleans up, coating slurry thickness is 240 μ m.In 150 ℃ baking oven dry 10 hours then, obtain the exsiccant cladding.The exsiccant cladding is put into plumbago crucible, then crucible is put into vacuum resistance furnace, banking vacuumizes the energising heating.With 10 ℃/minute rate of heating stove is heated to 500 ℃, is incubated 10 minutes, and then stove is heated to 1440 ℃, be incubated 30 minutes with 18 ℃/minute rate of heating.Outage stops heating, treats stove cooling back taking-up sample.Do anti-oxidant test in 1300 ℃ air, without the graphite oxidation of coating 1 hour, weight loss was 40%; After coating was handled, oxidation was after 30 hours, and weight loss is 0.04%.
Embodiment 4
Si, B, H
2O, polyvinyl formal, be 48.5: 5: 44 by weight: 2.5 are mixed with slurry, and slurry was fully ground 1 hour in ball mill, make wherein each component uniform distribution. and all the other carry out the heat shock resistance experiment with 1. pairs of prepared samples of embodiment.Earlier furnace is raised to 1020 ℃ during experiment, oxidation dropped into sample rapidly in 20 ℃ of water of room temperature after 30 minutes, and through 10 thermal cycle impact tests, coating is complete, does not see coating cracking.The sample weight rate of loss is 0.8%.
Claims (4)
1, a kind of preparation method of charcoal material surface coating for resisting high temperature oxidation is characterized in that comprising the steps:
(1) charcoal material surface is cleaned, the distilled water ultrasonic cleaning is used in decontamination, puts into the loft drier oven dry then;
(2) silica flour, boron powder, water, binding agent are silica flour by weight: boron powder: water: binding agent=43.5～50.5: 3～10: 44.5～45: 1.0～2.5 carry out the mixed preparing form slurry, slurry is fully ground in ball mill, make its each component uniform distribution, adopt dip-coating, spraying or spread coating this pulp bales to be overlayed on the charcoal material surface that cleans up, coating slurry thickness is 200 μ m～240 μ m, drying is 10～16 hours in 100 ℃-150 ℃ environment, obtains the exsiccant cladding;
(3) the above-mentioned cladding that makes is put into vacuum resistance furnace, at first stove is heated to 400～500 ℃ with 5～10 ℃/minute rate of heating, be incubated 10～20 minutes, and then stove is heated to 1420 ℃～1500 ℃ with 15～20 ℃/minute rate of heating, be incubated 20～30 minutes, outage stops heating, treats stove cooling back taking-up sample, can obtain the high-temperature oxidation resistant ceramic coating.
2, the preparation method of a kind of charcoal material surface coating for resisting high temperature oxidation as claimed in claim 1 is characterized in that described silicon particle size is 5～47 μ m.
3, the preparation method of a kind of charcoal material surface coating for resisting high temperature oxidation as claimed in claim 1 is characterized in that described boron powder degree is 3～10 μ m.
4, the preparation method of a kind of charcoal material surface coating for resisting high temperature oxidation as claimed in claim 1 is characterized in that described binding agent is polyvinyl alcohol, acrylamide or polyvinyl formal.
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| CNB2005100127304A CN1297515C (en) | 2005-08-11 | 2005-08-11 | Preparation method of charcoal material surface coating for resisting high temperature oxidation |
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| CNB2005100127304A CN1297515C (en) | 2005-08-11 | 2005-08-11 | Preparation method of charcoal material surface coating for resisting high temperature oxidation |
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| CN1297515C true CN1297515C (en) | 2007-01-31 |
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Families Citing this family (7)
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| CN103204701B (en) * | 2013-04-15 | 2014-10-29 | 上海应用技术学院 | Anti-oxidation treatment method for surface of carbon material |
| CN104909840B (en) * | 2015-06-05 | 2019-05-03 | 南通扬子碳素股份有限公司 | The manufacturing method of resistance to oxidation carbon product |
| CN106045523B (en) * | 2016-07-29 | 2018-07-06 | 张宁 | A kind of method based on Bayer process production aluminum nitride ceramic powder |
| CN109666886A (en) * | 2018-12-28 | 2019-04-23 | 河南科技大学 | A kind of preparation method of molybdenum base material surface oxidation-resistant coating |
| CN112404162A (en) * | 2019-08-21 | 2021-02-26 | 宝鸡富源凯达工贸有限公司 | Efficient rolling processing method for large-diameter seamless pipe made of titanium and titanium alloy |
| CN110540416B (en) * | 2019-10-11 | 2022-10-18 | 山东铭特陶瓷材料有限公司 | High-strength and long-service-life stopper rod and preparation method thereof |
| CN113860915B (en) * | 2021-10-18 | 2022-11-22 | 中钢新型材料股份有限公司 | Borosilicate glass coating on graphite substrate and preparation method thereof |
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| CN1235941A (en) * | 1998-05-19 | 1999-11-24 | 中国科学院山西煤炭化学研究所 | Method for preparing high temperature anti-oxidation carbon base composite material |
| JP2002249371A (en) * | 2001-02-20 | 2002-09-06 | Nippon Steel Corp | Magnesia carbon refractory and furnace utilizing it |
| JP2004002133A (en) * | 2002-03-28 | 2004-01-08 | Toyo Tanso Kk | Production process of carbon/silicon carbide composite material, and carbon/silicon carbide composite material by the production process |
| RU2232738C1 (en) * | 2002-10-09 | 2004-07-20 | Федеральное государственное унитарное предприятие "Всероссийский научно-исследовательский институт авиационных материалов" | High temperature coating |
| CN1611635A (en) * | 2003-10-28 | 2005-05-04 | 东洋炭素株式会社 | Silicon carbide-coated carbonaceous material and carbonaceous material to be coated with silicon carbide |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1235941A (en) * | 1998-05-19 | 1999-11-24 | 中国科学院山西煤炭化学研究所 | Method for preparing high temperature anti-oxidation carbon base composite material |
| JP2002249371A (en) * | 2001-02-20 | 2002-09-06 | Nippon Steel Corp | Magnesia carbon refractory and furnace utilizing it |
| JP2004002133A (en) * | 2002-03-28 | 2004-01-08 | Toyo Tanso Kk | Production process of carbon/silicon carbide composite material, and carbon/silicon carbide composite material by the production process |
| RU2232738C1 (en) * | 2002-10-09 | 2004-07-20 | Федеральное государственное унитарное предприятие "Всероссийский научно-исследовательский институт авиационных материалов" | High temperature coating |
| CN1611635A (en) * | 2003-10-28 | 2005-05-04 | 东洋炭素株式会社 | Silicon carbide-coated carbonaceous material and carbonaceous material to be coated with silicon carbide |
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