CN109896868A - It is a kind of to effectively improve and CfThe antioxidant coating of binding performance between Zr-B - Google Patents
It is a kind of to effectively improve and CfThe antioxidant coating of binding performance between Zr-B Download PDFInfo
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- CN109896868A CN109896868A CN201910170788.3A CN201910170788A CN109896868A CN 109896868 A CN109896868 A CN 109896868A CN 201910170788 A CN201910170788 A CN 201910170788A CN 109896868 A CN109896868 A CN 109896868A
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Abstract
The present invention relates to carbon fibre reinforced ceramics based composites technical fields, and disclose a kind of can effectively improve and CfThe antioxidant coating of binding performance between Zr-B, the raw material including following parts by weight proportion: 30-50 parts of silicon powders, 7-9 parts of carbon fiber powders, 5g glass powder, 2.33 parts of waterglass, 0.5 part of soybean lecithin, 6 parts of bisphenol A type epoxy resins, 2.77 parts of isophorone diamine.The present invention solves CfThe antioxidant coating of/Zr-B composite material surface, under high temperature environment, due between interface cementation power weaken, the interface Yi Fasheng pyrolytic or generate unwanted new interface phase the technical issues of.
Description
Technical field
The present invention relates to carbon fibre reinforced ceramics based composites technical field, specially it is a kind of can effectively improve with
CfThe antioxidant coating of binding performance between Zr-B.
Background technique
Carbon fibre reinforced ceramics based composites possess good mechanical property and hot property, inert conditions at high temperature
Under, still keeping the mechanical properties such as intensity, modulus not in the environment of more than 2000 DEG C reduces, and thermal expansion coefficient is low, thermal conductivity
High, gasification temperature height, thermal shock resistance are good, therefore, are with a wide range of applications in aerospace craft thermal protection system.
Wherein, fibre reinforced zirconium boride ceramic base (Cf/ Zr-B) composite material be than fibre reinforced silicon oxide carbide make pottery
Porcelain base (Cf/ Si-O-C) the more excellent carbon fibre reinforced ceramics based composites of composite property, basis material is free of
Oxygen atom is avoided that and carbothermic reduction reaction occurs at high temperature with reinforced phase carbon fiber, however as CfIn/Zr-B composite material
The carbon fiber of reinforced phase, under the aerobic environment higher than 400 DEG C, oxygen easily occurs for active site caused by carbon fiber surface defect
Change, easily causes material failure, while the ZrB as body portion2Although itself has good antioxygenic property,
The ZrO of generation is aoxidized under high temperature2Glass phase can reduce the bond strength of carbon fiber and basis material, equally can also material be made to lose
Effect.
Although CfThe basis material of/Zr-B composite material is coated with carbon fiber, but carbon fiber axle to and radial thermal expansion
Coefficient differs greatly, under high temperature, when temperature steeply rises or sharply declines, since carbon fiber and basis material thermal expansion are
Thermal stress caused by number mismatches reaches and carbon fiber will be made to get loose with basis material after certain threshold value to separate, this will for oxygen and
Carbon fiber contact provides channel, meanwhile, the C/Zr-B composite material porosity as light porous material reaches 40%, high hole
Rate is also that oxygen enters material internal, and generation is contacted with carbon fiber by basis material defect produced during the preparation process
Oxidation reaction provides possibility, therefore, improves CfThe oxidation resistance of/Zr-B composite material has very important practical meaning
Justice.
Currently, there are mainly three types of the anti-oxidation methods taken carbon fibre reinforced ceramics based composites: matrix modification method,
Fiber coat method, surface covering method.For Cf/ Zr-B composite material, oxidation are mainly the oxidation deactivation of carbon fiber in material,
Therefore coating protection, the channel of cutting oxygen contact carbon fiber, to improve material individually can be carried out to carbon fiber surface
Antioxygenic property, still, material internal to carbon fiber carry out coating and individual carbon fibers coating it is very difficult, coating it is small
Crackle is difficult to control, and coating declines carbon fiber intensity itself.Surface covering method is at present to Cf/ Zr-B composite material
Oxidation resistant main method is using in CfThe covering of/Zr-B composite material surface it is fine and close can self-healing antioxidant coating, with oxygen
The property changed is gas-insulated to reach antioxidation.
To make Cf/ Zr-B composite material can effectively use for a long time under aerobic conditions, and antioxidant coating itself is internal
The binding performance and antioxidant coating and C of structurefBinding performance between/Zr-B composite material does not need only to have certain
Intensity, and be also required to that there is good physical chemistry compatibility, otherwise, during heating is with cooling, anti-oxidant painting
Between internal structure of layer itself, antioxidant coating and CfPyrolytic can occur between/Zr-B composite material or generate to be not required to
The interface phase wanted.
The present invention provides a kind of can effectively improve and CfThe antioxidant coating of binding performance between Zr-B, it is intended to solve Cf/
The antioxidant coating of Zr-B composite material surface, under high temperature environment, since cementation power weakens between interface, the interface Yi Fasheng
The technical issues of pyrolytic or generation unwanted new interface phase.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, it can be effectively improved and C the present invention provides a kind offBinding performance is anti-between Zr-B
Oxide covering solves CfThe antioxidant coating of/Zr-B composite material surface is made due to bonding between interface under high temperature environment
Firmly weaken, the interface Yi Fasheng pyrolytic or generate unwanted new interface phase the technical issues of.
(2) technical solution
To achieve the above object, the invention provides the following technical scheme:
It is a kind of to effectively improve and CfThe antioxidant coating of binding performance between Zr-B, including following parts by weight proportion
Raw material: 30-50 parts of silicon powders, 7-9 parts of carbon fiber powders, 5 parts of glass powders, 2.33 parts of waterglass, 0.5 part of soybean lecithin, 6 parts pairs
Phenol A type epoxy resin, 2.77 parts of isophorone diamine.
Preferably, the glass powder is by 1g average grain diameter≤100nm SnO2, 2g average grain diameter≤100nm B2O3、2g
Average grain diameter≤100nm SiO2Composition.
Preferably, average grain diameter≤50um of average grain diameter≤50um of the silicon powder, carbon fiber powder.
Preferably, the antioxidant coating includes the raw material of following parts by weight proportion: 40g average grain diameter≤50um
Silicon powder, 8g average grain diameter≤50um carbon fiber powder, 5g glass powder, 50mL dehydrated alcohol, 1mL waterglass, 0.5g soybean lecithin
Rouge, 6gE03 trade mark bisphenol A type epoxy resin, 20mL butanone, 3mL isophorone diamine.
Preferably, the antioxidant coating preparation method the following steps are included:
S1. 30-50 parts of silicon powders, 7-9 parts of carbon fiber powders are taken, it is spare；
S2. the standby raw material in step S1 is subjected to ball milling, matrix component is prepared；
S3. with average grain diameter≤100nm SnO2, average grain diameter≤100nm B2O3, average grain diameter≤100nm
SiO2For raw material, glass powder is prepared；
S4. using E03 trade mark bisphenol A type epoxy resin and butanone as raw material, adhesion component is prepared；
S5. the matrix component in step S2, the glass powder in step S3 are added together with the adhesion component in step S4
Into reaction kettle, 2h is reacted at 120-180 DEG C, stops stirring, and isophorone diamine is added, antioxidant coating is prepared；
S6. first by Cf/ Zr-B composite material, which is placed in dehydrated alcohol, is cleaned by ultrasonic 1h, is dried in vacuo 2h at 60 DEG C,
It is spare；
S7. the antioxidant coating in step S5 is packed into spray gun, C in step s 6fThe spraying of/Zr-B composite material surface
3mm after the completion of spraying, is placed at 60-80 DEG C and toasts 1-2h, be warming up to 100-150 DEG C, toast 1h at 100-150 DEG C.
Preferably, in the step S5, after stopping stirring, at 120-180 DEG C, 1h is kept the temperature.
Preferably, in the step S7, spray gun and CfThe spacing control of/Zr-B composite material exists in 300mm, pressure control
0.25-0.5MPa。
(3) beneficial technical effect
Compared with prior art, the present invention has following beneficial technical effect:
After tested, the antioxidant coating and C that the present invention preparesfPeel strength between/Zr-B composite material is
62.4N/cm, after 1400 DEG C of oxidation test 9h, the antioxidant coating and CfThere is no high temperature between/Zr-B composite material
It decomposes, also without generating new interface phase, and basis material does not find to be oxidized sign, to solve Cf/ Zr-B composite wood
Expect surface antioxidant coating, under high temperature environment, due between interface cementation power weaken, the interface Yi Fasheng pyrolytic or
The technical issues of generating unwanted new interface phase.
Specific embodiment
Embodiment one:
Antioxidant coating includes following raw material: 40g average grain diameter≤50um silicon powder, 8g average grain diameter≤50um carbon fiber
It is double to tie up powder, 5g glass powder, 50mL dehydrated alcohol, 1mL waterglass (ρ 2.33g/mL), 0.5g soybean lecithin, the 6gE03 trade mark
Phenol A type epoxy resin, 20mL butanone (ρ 0.805g/cm3), 3mL isophorone diamine (ρ 0.924g/cm3)；
Wherein, glass powder is by 1g average grain diameter≤100nm SnO2, 2g average grain diameter≤100nm B2O3, 2g is averaged grain
Diameter≤100nm SiO2Composition；
The preparation method of above-mentioned antioxidant coating the following steps are included:
S1. 40g average grain diameter≤50um silicon powder, 8g average grain diameter≤50um carbon fiber powder are weighed, it is spare；
S2. by the standby raw material and 10mL dehydrated alcohol in step S1, under 300r/min, ball milling 12h is added later
1mL waterglass, 0.5g soybean lecithin and 40mL dehydrated alcohol, continue at ball milling 2h under 300r/min, and matrix group is prepared
Point；
S3. 1g average grain diameter≤100nm SnO is weighed2, 2g average grain diameter≤100nm B2O3, 2g average grain diameter≤
The SiO of 100nm2, it is configured to glass powder；
S4. 6gE03 trade mark bisphenol A type epoxy resin is dissolved in 20mL butanone solvent, adhesion component is prepared；
S5. the matrix component in step S2, the glass powder in step S3 are added together with the adhesion component in step S4
Into reaction kettle, under 150 DEG C, 300r/min, 2h is reacted, stops stirring, after keeping the temperature 1h at 150 DEG C, the different Fo Er of 3mL is added
Ketone diamines, after stirring 20min under 150 DEG C, 300r/min, antioxidant coating is prepared in discharging；
S6. first by Cf/ Zr-B composite material, which is placed in dehydrated alcohol, is cleaned by ultrasonic 1h, is dried in vacuo 2h at 60 DEG C,
It is spare；
S7. the antioxidant coating in step S5 is packed into spray gun, C in step s 6fThe spraying of/Zr-B composite material surface
3mm, spray gun and CfIn 300mm, pressure is controlled after the completion of 0.25MPa, spraying, is placed in for the spacing control of/Zr-B composite material
1h is toasted at 80 DEG C, with the heating rate of 5 DEG C/min, 150 DEG C is warming up to, toasts 1h at 150 DEG C, anti-oxidant painting is prepared
Layer；
S8. the antioxidant coating in step S7 is tested for the property, as a result are as follows: antioxidant coating and Cf/ Zr-B is compound
Peel strength 62.4N/cm between material, after 1400 DEG C of oxidation test 9h, antioxidant coating and Cf/ Zr-B composite material
Between there is no pyrolytic, also without generating new interface phase, and basis material does not find to be oxidized sign.
Embodiment two:
Antioxidant coating includes following raw material: 30g average grain diameter≤50um silicon powder, 9g average grain diameter≤50um carbon
Fiber powder, 5g glass powder, 50mL dehydrated alcohol, 1mL waterglass, 0.5g soybean lecithin, 6gE03 trade mark bisphenol type epoxy tree
Rouge, 20mL butanone, 3mL isophorone diamine；
Wherein, glass powder is by 1g average grain diameter≤100nm SnO2, 2g average grain diameter≤100nm B2O3, 2g is averaged grain
Diameter≤100nm SiO2Composition；
The preparation method of above-mentioned antioxidant coating the following steps are included:
S1. 30g average grain diameter≤50um silicon powder, 9g average grain diameter≤50um carbon fiber powder are weighed, it is spare；
S2. by the standby raw material and 10mL dehydrated alcohol in step S1, under 320r/min, ball milling 10h is added later
1mL waterglass, 0.5g soybean lecithin and 40mL dehydrated alcohol, continue at ball milling 2h under 320r/min, and matrix group is prepared
Point；
S3. 1g average grain diameter≤100nm SnO is weighed2, 2g average grain diameter≤100nm B2O3, 2g average grain diameter≤
The SiO of 100nm2, it is configured to glass powder；
S4. 6gE03 trade mark bisphenol A type epoxy resin is dissolved in 20mL butanone solvent, adhesion component is prepared；
S5. the matrix component in step S2, the glass powder in step S3 are added together with the adhesion component in step S4
Into reaction kettle, under 120 DEG C, 350r/min, 2h is reacted, stops stirring, after keeping the temperature 1h at 120 DEG C, the different Fo Er of 3mL is added
Ketone diamines, after stirring 20min under 120 DEG C, 350r/min, antioxidant coating is prepared in discharging；
S6. first by Cf/ Zr-B composite material, which is placed in dehydrated alcohol, is cleaned by ultrasonic 1h, is dried in vacuo 2h at 60 DEG C,
It is spare；
S7. the antioxidant coating in step S5 is packed into spray gun, C in step s 6fThe spraying of/Zr-B composite material surface
3mm, spray gun and CfIn 300mm, pressure is controlled after the completion of 0.35MPa, spraying, is placed in for the spacing control of/Zr-B composite material
2h is toasted at 80 DEG C, with the heating rate of 5 DEG C/min, 120 DEG C is warming up to, toasts 1h at 120 DEG C, anti-oxidant painting is prepared
Layer；
S8. the antioxidant coating in step S7 is tested for the property, as a result are as follows: antioxidant coating and Cf/ Zr-B is compound
Peel strength 63.5N/cm between material, after 1400 DEG C of oxidation test 9h, antioxidant coating and Cf/ Zr-B composite material
Between there is no pyrolytic, also without generating new interface phase, and basis material does not find to be oxidized sign.
Embodiment three:
Antioxidant coating includes following raw material: 50g average grain diameter≤50um silicon powder, 7g average grain diameter≤50um carbon
Fiber powder, 5g glass powder, 50mL dehydrated alcohol, 1mL waterglass, 0.5g soybean lecithin, 6gE03 trade mark bisphenol type epoxy tree
Rouge, 20mL butanone, 3mL isophorone diamine；
Wherein, glass powder is by 1g average grain diameter≤100nm SnO2, 2g average grain diameter≤100nm B2O3, 2g is averaged grain
Diameter≤100nm SiO2Composition；
The preparation method of above-mentioned antioxidant coating the following steps are included:
S1. 50g average grain diameter≤50um silicon powder, 7g average grain diameter≤50um carbon fiber powder are weighed, it is spare；
S2. by the standby raw material and 10mL dehydrated alcohol in step S1, under 280r/min, ball milling 10h is added later
1mL waterglass, 0.5g soybean lecithin and 40mL dehydrated alcohol, continue at ball milling 2h under 280r/min, and matrix group is prepared
Point；
S3. 1g average grain diameter≤100nm SnO is weighed2, 2g average grain diameter≤100nm B2O3, 2g average grain diameter≤
The SiO of 100nm2, it is configured to glass powder；
S4. 6gE03 trade mark bisphenol A type epoxy resin is dissolved in 20mL butanone solvent, adhesion component is prepared；
S5. the matrix component in step S2, the glass powder in step S3 are added together with the adhesion component in step S4
Into reaction kettle, under 180 DEG C, 250r/min, 2h is reacted, stops stirring, after keeping the temperature 1h at 180 DEG C, the different Fo Er of 3mL is added
Ketone diamines, after stirring 20min under 180 DEG C, 250r/min, antioxidant coating is prepared in discharging；
S6. first by Cf/ Zr-B composite material, which is placed in dehydrated alcohol, is cleaned by ultrasonic 1h, is dried in vacuo 2h at 60 DEG C,
It is spare；
S7. the antioxidant coating in step S5 is packed into spray gun, C in step s 6fThe spraying of/Zr-B composite material surface
3mm, spray gun and CfIn 300mm, pressure is controlled after the completion of 0.5MPa, spraying, is placed in for the spacing control of/Zr-B composite material
1h is toasted at 60 DEG C, with the heating rate of 5 DEG C/min, 100 DEG C is warming up to, toasts 1h at 100 DEG C, be prepared anti-oxidant
Coating；
S8. the antioxidant coating in step S7 is tested for the property, as a result are as follows: antioxidant coating and Cf/ Zr-B is compound
Peel strength 62.1N/cm between material, after 1400 DEG C of oxidation test 9h, antioxidant coating and Cf/ Zr-B composite material
Between there is no pyrolytic, also without generating new interface phase, and basis material does not find to be oxidized sign.
Claims (7)
- It can be effectively improved and C 1. a kind offThe antioxidant coating of binding performance between Zr-B, which is characterized in that including following parts by weight The raw material of number proportion: 30-50 parts of silicon powders, 7-9 parts of carbon fiber powders, 5 parts of glass powders, 2.33 parts of waterglass, 0.5 part of soybean lecithin Rouge, 6 parts of bisphenol A type epoxy resins, 2.77 parts of isophorone diamine.
- 2. antioxidant coating according to claim 1, which is characterized in that the glass powder is by 1g average grain diameter≤100nm SnO2, 2g average grain diameter≤100nm B2O3, 2g average grain diameter≤100nm SiO2Composition.
- 3. antioxidant coating according to claim 1, which is characterized in that average grain diameter≤50um of the silicon powder, carbon fiber Tie up average grain diameter≤50um of powder.
- 4. antioxidant coating according to claim 1, which is characterized in that the raw material including following parts by weight proportion: 40g Average grain diameter≤50um silicon powder, 8g average grain diameter≤50um carbon fiber powder, 5g glass powder, 50mL dehydrated alcohol, 1mL water glass Glass, 0.5g soybean lecithin, 6gE03 trade mark bisphenol A type epoxy resin, 20mL butanone, 3mL isophorone diamine.
- 5. antioxidant coating according to claim 1, which is characterized in that the preparation method of the antioxidant coating include with Lower step:S1. 30-50 parts of silicon powders, 7-9 parts of carbon fiber powders are taken, it is spare；S2. the standby raw material in step S1 is subjected to ball milling, matrix component is prepared；S3. with average grain diameter≤100nm SnO2, average grain diameter≤100nm B2O3, average grain diameter≤100nm SiO2For original Material prepares glass powder；S4. using E03 trade mark bisphenol A type epoxy resin and butanone as raw material, adhesion component is prepared；S5. the matrix component in step S2, the glass powder in step S3 are added to instead together with the adhesion component in step S4 It answers in kettle, 2h is reacted at 120-180 DEG C, stop stirring, isophorone diamine is added, antioxidant coating is prepared；S6. first by Cf/ Zr-B composite material, which is placed in dehydrated alcohol, is cleaned by ultrasonic 1h, and 2h is dried in vacuo at 60 DEG C, spare；S7. the antioxidant coating in step S5 is packed into spray gun, C in step s 6f/ Zr-B composite material surface sprays 3mm, After the completion of spraying, it is placed at 60-80 DEG C and toasts 1-2h, be warming up to 100-150 DEG C, toast 1h at 100-150 DEG C.
- 6. antioxidant coating according to claim 5, which is characterized in that in the step S5, after stopping stirring, in 120- At 180 DEG C, 1h is kept the temperature.
- 7. antioxidant coating according to claim 5, which is characterized in that in the step S7, spray gun and Cf/ Zr-B is compound In 300mm, pressure is controlled in 0.25-0.5MPa for the spacing control of material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910170788.3A CN109896868A (en) | 2019-03-07 | 2019-03-07 | It is a kind of to effectively improve and CfThe antioxidant coating of binding performance between Zr-B |
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| CN201910170788.3A CN109896868A (en) | 2019-03-07 | 2019-03-07 | It is a kind of to effectively improve and CfThe antioxidant coating of binding performance between Zr-B |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113861727A (en) * | 2021-09-29 | 2021-12-31 | 上海利尔耐火材料有限公司 | Continuous casting tundish dry material antioxidant coating |
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| DE102012216190A1 (en) * | 2012-09-12 | 2014-04-10 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Composite e.g. fiber composite materials or composite coatings e.g. paint coatings, useful in a component, comprises a matrix material, and microcapsules comprising a shell material consisting of a cell wall and/or a cell membrane |
| CN106752644A (en) * | 2016-12-26 | 2017-05-31 | 上海东洋炭素有限公司 | One kind solidification felt surface self-healing anti-oxidation coating and preparation method thereof |
| CN108342062A (en) * | 2017-01-25 | 2018-07-31 | 翁秋梅 | A kind of hydridization dynamic aggregation object composition and its application |
| CN108485516A (en) * | 2018-04-28 | 2018-09-04 | 兆山科技（北京）有限公司 | ceramic surface material and surface coating |
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2019
- 2019-03-07 CN CN201910170788.3A patent/CN109896868A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| EP1433021B1 (en) * | 2001-08-28 | 2011-04-20 | Gentex Corporation | Electrochromic medium having a self-healing cross-linked polymer gel and associated electrochromic device |
| DE102012216190A1 (en) * | 2012-09-12 | 2014-04-10 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Composite e.g. fiber composite materials or composite coatings e.g. paint coatings, useful in a component, comprises a matrix material, and microcapsules comprising a shell material consisting of a cell wall and/or a cell membrane |
| CN106752644A (en) * | 2016-12-26 | 2017-05-31 | 上海东洋炭素有限公司 | One kind solidification felt surface self-healing anti-oxidation coating and preparation method thereof |
| CN108342062A (en) * | 2017-01-25 | 2018-07-31 | 翁秋梅 | A kind of hydridization dynamic aggregation object composition and its application |
| CN108485516A (en) * | 2018-04-28 | 2018-09-04 | 兆山科技（北京）有限公司 | ceramic surface material and surface coating |
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| CN113861727A (en) * | 2021-09-29 | 2021-12-31 | 上海利尔耐火材料有限公司 | Continuous casting tundish dry material antioxidant coating |
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