CN104250107B - A kind of Carbon foam surface in situ synthesizes Si3N4The method of coating - Google Patents
A kind of Carbon foam surface in situ synthesizes Si3N4The method of coating Download PDFInfo
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- CN104250107B CN104250107B CN201310495482.8A CN201310495482A CN104250107B CN 104250107 B CN104250107 B CN 104250107B CN 201310495482 A CN201310495482 A CN 201310495482A CN 104250107 B CN104250107 B CN 104250107B
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Abstract
The present invention relates to one kind Si is synthesized in foam carbon material surface in situ3N4The method of coating, belongs to new material technology field.Specifically include following steps：(1) phenolic resin is used as base stock, and the homogeneous phenol formaldehyde foam matrix of stomata is obtained by normal pressure physical blowing method.(2) using tetraethyl orthosilicate as primary raw material, required sol solution is made using its hydrolyzed under acidic conditions.(3) the phenol formaldehyde foam matrix of step (1) is cleaned by ultrasonic, drying, immersed in the sol solution of step (2), the dip coating under the conditions of ultrasonic oscillation, obtain collosol coating sample.(4) the collosol coating sample of step (3) is placed in atmosphere hot pressing furnace, at 1400 DEG C, in nitrogen atmosphere, insulation 4h reactions are burnt till, and Carbon foam surface in situ synthesis Si is made3N4The sample of coating.
Description
Technical field
The present invention relates to one kind Si is synthesized in foam carbon material surface in situ3N4The method of coating, belong to new material technology neck
Domain.
Background technology
Foam carbon material as a kind of novel charcoal material, unique pore space structure assign its low-density, high intensity, conduction,
The superior performance such as heat conduction, thermostabilization, chemically stable, is widely used in the fields such as aerospace, metallurgy, chemical industry, environmental protection, electronics.But
It is the weakness of oxidizable corrosion in high temperature oxidative atmosphere, has a strong impact on the performance of foam carbon material excellent properties, and then restricts it
In the application of various fields.Therefore, need a kind of effective antioxidant defense method badly, do not influence foam carbon material structure and property
On the premise of energy, the oxidation of foam carbon material is prevented.
At present, the antioxidant defense of foam carbon material mainly includes two kinds of matrix modification and coating, and coating is most
For effective antioxidant defense measure.Si3N4It is passivated because of its unique mechanics, optics, electrical properties and preferably, anti-oxidant
Performance, and a kind of important coating and thin-film material.Though prior art is related to Si3N4In the antioxidant coating of Carbon Materials
Research, but be to carry out being compounded to form certain composite coating for matrix of carbon/carbon composite materials surface and with SiC etc. mostly, and use
In the anti-oxidant Si of porous foam carbon material3N4Coating yet there are no correlation technique report.
The present invention is based on Si3N4The gas-solid mechanism formed, it is proposed that a kind of technique is simple, easily controllable, and low temperature easily adulterates
Sol impregnation combination high-temperature ammonolysis processing prepare Si3N4The new method of coating, greatly improve the inoxidizability of foam carbon material
Can, provide certain theoretical foundation and experiment in the large-scale development in the fields such as aerospace, chemical industry, electronics, environmental protection and application for it
With reference to.
The content of the invention
The main object of the present invention is to provide a kind of in foam carbon material surface in situ synthesis Si3N4The method of coating.
The present invention uses tetraethyl orthosilicate as primary raw material, is glued by the hydrolysis of acid condition and normal temperature are still aging
Spend uniform sol solution；Then the phenol formaldehyde foam obtained by normal pressure physical blowing is immersed into above-mentioned sol solution, ultrasonic oscillation
Under the conditions of to phenol formaldehyde foam matrix coating；Finally fully dry coating sample is placed in atmosphere hot pressing furnace, nitrogen gas
4h reactions are incubated in atmosphere at 1400 DEG C to burn till.
It is of the invention a kind of in foam carbon material surface in situ synthesis Si3N4The method of coating, it the advantage is that technique is simple,
Easily operated, cost is low, and coating consistency is high, and antioxidant effect is good.
Specific step of preparation process and principle are as follows：
(1) appropriate thermosetting phenolic resin is weighed, sodium acid carbonate, Tween 80, right is sequentially added under the conditions of strong magnetic agitation
Toluenesulfonic acid, three's adding proportion are respectively 5wt%, 6wt% and 20wt% of phenolic resin quality, and strong magnetic agitation mixing is several
Minute, mixture is placed in baking oven several minutes of drying under 80 DEG C or so, foamed solidification, obtains phenol formaldehyde foam matrix.
(2) measure respectively appropriate volume than tetraethyl orthosilicate and absolute ethyl alcohol, strong magnetic agitation mixing at room temperature.To
The deionized water of appropriate volume is added in the mixture, and the pH value of mixed liquor is adjusted with 10% nitric acid, strong magnetic agitation is certain
Time.Finally, the sucrose solution of certain volume is added to said mixture, strong magnetic agitation a few hours, is stood at room temperature old
Change a couple of days, obtain required sol solution.
(3) the phenol formaldehyde foam matrix of step (1) is cleaned by ultrasonic, after drying, immersed in the sol solution of step (2),
Certain time surface is impregnated under the conditions of ultrasonic oscillation and obtains coating.After fully being dried per secondary coating, dipping next time is carried out
Coating, impregnate repeatedly for several times, obtain collosol coating sample.
(4) the collosol coating sample of step (3) is placed in atmosphere hot pressing furnace, under certain temperature, in nitrogen atmosphere, insulation
A few hours react, and obtain Carbon foam surface in situ synthesis Si3N4Coating sample.To reduce collosol coating and phenol formaldehyde foam matrix heat
Generation caused by expansion coefficient difference the defects of peeling, micro-crack, warming machine are made as：Heated up first with 10 DEG C/min speed
To 300 DEG C, 500 DEG C then are warming up to 5 DEG C/min speed, is finally warming up to 1400 DEG C with 2 DEG C/min speed, insulation
4h, room temperature is naturally cooled to, antioxidant coating Carbon foam sample is made.
Brief description of the drawings
The foam carbon material surface in situ synthesis Si of Fig. 1 present invention3N4The process chart of coating；
The gained Si of Fig. 2 embodiments one3N4Coating XRD spectrum；
The gained Si of Fig. 3 embodiments one3N4Coating SEM photograph；
The gained Si of Fig. 4 embodiments one3N4Coating cross section SEM photograph；
Embodiment
Embodiment one：
(1) 10g thermosetting phenolic resins are weighed, sodium acid carbonate, Tween 80 are sequentially added under the conditions of strong magnetic agitation, to first
Benzene sulfonic acid, three's adding proportion are respectively 5wt%, 6wt% and 20wt% of phenolic resin quality, and strong magnetic agitation mixing 3~
5min, mixture is placed in 80 DEG C or so 5~10min of lower drying in baking oven, foamed solidification, obtains phenol formaldehyde foam matrix.
(2) volume ratio is measured respectively as 10：3 tetraethyl orthosilicate and absolute ethyl alcohol, at room temperature strong magnetic agitation mixing.
The deionized water that volume ratio is tetraethyl orthosilicate 33vol% is added into the mixture, and mixed liquor is adjusted with 10% nitric acid
PH value be 3.5, strong magnetic agitation 30min.Finally, it is tetraethyl orthosilicate 27vol% to add volume ratio to said mixture
Sucrose solution, strong magnetic agitation 4h, still aging 72h, obtains required sol solution at room temperature.
(3) the phenol formaldehyde foam matrix of step (1) is cleaned by ultrasonic, after drying, immersed in the sol solution of step (2),
Dip coating 20min under conditions of ultrasonic wave.After fully being dried per secondary coating, dip coating next time is carried out, is impregnated repeatedly
For several times, obtain applying the collosol coating sample that hierachy number is followed successively by 1,2,3.
(4) the collosol coating sample of the different coating number of step (3) is placed in atmosphere hot pressing furnace, at 1400 DEG C, nitrogen
In gas atmosphere, insulation 4h reactions, Carbon foam surface in situ synthesis Si is obtained3N4The sample of coating.To reduce collosol coating and phenolic aldehyde
Generation caused by foam base plate thermal expansion coefficient difference the defects of peeling, micro-crack, warming machine are made as：First with 10 DEG C/min
Speed be warming up to 300 DEG C, be then warming up to 500 DEG C with 5 DEG C/min speed, be finally warming up to 2 DEG C/min speed
1400 DEG C, 4h is incubated, naturally cools to room temperature, antioxidant coating Carbon foam sample is made.
Claims (1)
1. a kind of Carbon foam surface in situ synthesizes Si3N4The method of coating, it is characterised in that：Methods described includes following steps,
(1) preparation of phenol formaldehyde foam matrix
Appropriate thermosetting phenolic resin is weighed, sodium acid carbonate, Tween 80 are sequentially added under the conditions of strong magnetic agitation, to toluene sulphur
Acid, three's adding proportion are respectively 5wt%, 6wt% and 20wt% of phenolic resin quality, and strong stirring mixed for several minutes will
Mixture is placed in baking oven and dried several minutes at 80 DEG C, foamed solidification, obtains phenol formaldehyde foam matrix,
(2) preparation of sol solution
Measure respectively appropriate volume than tetraethyl orthosilicate and absolute ethyl alcohol, strong magnetic agitation mixing at room temperature；To the mixing
The deionized water of appropriate volume is added in thing, and the pH value of mixed liquor, strong magnetic agitation certain time are adjusted with 10% nitric acid；Most
Afterwards, certain volume sucrose solution is added to said mixture, strong magnetic agitation a few hours, at room temperature still aging a couple of days, obtained
To required sol solution,
(3) preparation of collosol coating sample
The phenol formaldehyde foam matrix of step (1) is cleaned by ultrasonic, drying, immersed in the sol solution of step (2), in ultrasonic oscillation
Under the conditions of impregnate certain time surface obtain coating；After fully being dried per secondary coating, dip coating next time is carried out, is soaked repeatedly
Stain for several times, obtains collosol coating sample,
(4) preparation of antioxidant coating Carbon foam
The collosol coating sample of step (3) is placed in atmosphere hot pressing furnace, under certain temperature, in nitrogen atmosphere, is incubated a few hours
Reaction, obtains antioxidant coating sample；To be peeled off caused by reduction collosol coating and phenol formaldehyde foam matrix thermal expansion coefficient difference,
The generation of the defects of micro-crack, warming machine are made as：300 DEG C first are warming up to 10 DEG C/min speed, then with 5 DEG C/min speed
Rate is warming up to 500 DEG C, is finally warming up to 1400 DEG C with 2 DEG C/min speed, is incubated 4h, naturally cools to room temperature, and antioxygen is made
Change coating Carbon foam sample.
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| CN201310495482.8A CN104250107B (en) | 2013-06-28 | 2013-10-22 | A kind of Carbon foam surface in situ synthesizes Si3N4The method of coating |
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| CN201310265163 | 2013-06-28 | ||
| CN201310265163.8 | 2013-06-28 | ||
| CN2013102651638 | 2013-06-28 | ||
| CN201310495482.8A CN104250107B (en) | 2013-06-28 | 2013-10-22 | A kind of Carbon foam surface in situ synthesizes Si3N4The method of coating |
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| CN104250107B true CN104250107B (en) | 2017-12-08 |
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| CN108658598A (en) * | 2018-05-15 | 2018-10-16 | 潘荣强 | A kind of preparation method of Carbon foam |
| CN114604870A (en) * | 2022-02-24 | 2022-06-10 | 南京智汇环境气象产业研究院有限公司 | Method for preparing foam carbon material from wood block |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1887940A (en) * | 2006-06-26 | 2007-01-03 | 北京航空航天大学 | Carbon-base brake material for track vehicle |
| CN102515851A (en) * | 2011-12-26 | 2012-06-27 | 天津大学 | Preparation method for silicon-nitride-based coating on surface of porous ceramic |
| CN103011836A (en) * | 2012-12-03 | 2013-04-03 | 北京中材人工晶体研究院有限公司 | Carbon material surface coat composition and preparation method of coat |
| CN103030135A (en) * | 2013-01-05 | 2013-04-10 | 航天材料及工艺研究所 | Preparation method of antioxidant high-heat-conductivity foamy carbon material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH0753622B2 (en) * | 1988-05-12 | 1995-06-07 | 東芝セラミックス株式会社 | Carbonaceous composite material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1887940A (en) * | 2006-06-26 | 2007-01-03 | 北京航空航天大学 | Carbon-base brake material for track vehicle |
| CN102515851A (en) * | 2011-12-26 | 2012-06-27 | 天津大学 | Preparation method for silicon-nitride-based coating on surface of porous ceramic |
| CN103011836A (en) * | 2012-12-03 | 2013-04-03 | 北京中材人工晶体研究院有限公司 | Carbon material surface coat composition and preparation method of coat |
| CN103030135A (en) * | 2013-01-05 | 2013-04-10 | 航天材料及工艺研究所 | Preparation method of antioxidant high-heat-conductivity foamy carbon material |
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