CN1300260C - Precursor of carbon/carbon composite material anti-oxidation coating - Google Patents
Precursor of carbon/carbon composite material anti-oxidation coating Download PDFInfo
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- CN1300260C CN1300260C CNB2004100030427A CN200410003042A CN1300260C CN 1300260 C CN1300260 C CN 1300260C CN B2004100030427 A CNB2004100030427 A CN B2004100030427A CN 200410003042 A CN200410003042 A CN 200410003042A CN 1300260 C CN1300260 C CN 1300260C
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- carbon
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 41
- 239000011248 coating agent Substances 0.000 title claims abstract description 41
- 238000000576 coating method Methods 0.000 title claims abstract description 41
- 239000002243 precursor Substances 0.000 title abstract description 7
- 230000003064 anti-oxidating effect Effects 0.000 title abstract description 6
- 239000002131 composite material Substances 0.000 title abstract description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004327 boric acid Substances 0.000 claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 4
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 34
- 150000001722 carbon compounds Chemical class 0.000 claims description 31
- 230000003647 oxidation Effects 0.000 claims description 10
- 238000007254 oxidation reaction Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 229960001866 silicon dioxide Drugs 0.000 claims description 3
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 claims description 3
- 229910000165 zinc phosphate Inorganic materials 0.000 claims description 3
- 238000005470 impregnation Methods 0.000 abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 abstract description 5
- 239000001301 oxygen Substances 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 230000001934 delay Effects 0.000 abstract description 2
- 230000035876 healing Effects 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract description 2
- 230000035699 permeability Effects 0.000 abstract 2
- 230000007547 defect Effects 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- MFXMOUUKFMDYLM-UHFFFAOYSA-L zinc;dihydrogen phosphate Chemical compound [Zn+2].OP(O)([O-])=O.OP(O)([O-])=O MFXMOUUKFMDYLM-UHFFFAOYSA-L 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 34
- 238000007598 dipping method Methods 0.000 description 13
- 239000000203 mixture Substances 0.000 description 13
- 239000008367 deionised water Substances 0.000 description 12
- 229910021641 deionized water Inorganic materials 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 12
- 238000005303 weighing Methods 0.000 description 11
- 239000007864 aqueous solution Substances 0.000 description 9
- OTRAYOBSWCVTIN-UHFFFAOYSA-N OB(O)O.OB(O)O.OB(O)O.OB(O)O.OB(O)O.N.N.N.N.N.N.N.N.N.N.N.N.N.N.N Chemical compound OB(O)O.OB(O)O.OB(O)O.OB(O)O.OB(O)O.N.N.N.N.N.N.N.N.N.N.N.N.N.N.N OTRAYOBSWCVTIN-UHFFFAOYSA-N 0.000 description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 7
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 7
- 235000011194 food seasoning agent Nutrition 0.000 description 7
- 239000011701 zinc Substances 0.000 description 7
- 229910052725 zinc Inorganic materials 0.000 description 7
- 239000003610 charcoal Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 229960000935 dehydrated alcohol Drugs 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 208000037656 Respiratory Sounds Diseases 0.000 description 3
- 230000002950 deficient Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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Abstract
本发明涉及涂布液体的前驱体，特别是碳/碳复合材料抗氧化涂层前驱体，其特征是：选用化学纯代替部分蒸馏水做溶剂，按重量百分比将二氧化硅20～40%，磷酸5～25%，磷酸二氢锌40～65%，硼酸1～10%，配制；溶胶浸渍抗氧化涂层表面未发现裂纹、孔洞等缺陷。涂层与碳结合性好，具有高致密性、高愈合能力。而多种高溶点低氧渗透率物质引入提高了涂层抗氧渗透能力，延缓氧气与碳/碳复合材料接触的时间，从而提高了涂层的抗氧化能力。The invention relates to a precursor of a coating liquid, in particular to a precursor of a carbon/carbon composite material anti-oxidation coating, which is characterized in that: chemically pure water is selected as a solvent to replace part of distilled water, and 20-40% of silicon dioxide, 5-25% of phosphoric acid, 40-65% of zinc dihydrogen phosphate, and 1-10% of boric acid are prepared by weight percentage; no defects such as cracks and holes are found on the surface of the anti-oxidation coating after sol impregnation. The coating has good bonding with carbon, high density and high healing ability. The introduction of a variety of high melting point and low oxygen permeability substances improves the anti-oxygen permeability of the coating, delays the contact time between oxygen and the carbon/carbon composite material, and thus improves the anti-oxidation ability of the coating.
Description
Technical field:
The present invention relates to the presoma of coating liquid, specifically is the presoma of the low temperature oxidation resistant coating of carbon/carbon compound material.
Background technology:
Solution dipping method, the phenomenon that the coating behind the existence dipping and the thermal expansivity of carbon/carbon compound material differ greatly, referring to Fig. 1, cause defectives such as crackle, hole to produce, reduced the compactness of coating, make oxygen molecule penetrate coating easily and arrive the carbon/carbon material surface, react, cause oxidation with carbon.Solution dipping method is difficult to multiple composition with difference in functionality effectively is dissolved in a kind of solution simultaneously, in the composition modulation, bigger restriction is arranged, and in order to overcome this type of defective, often need to fill crackle or adjust coated component through repeatedly flooding, this has not only increased the thickness of coating, also increase the step of preparation technology of coating, thereby reduced technology, the economic advantages of this type coating.
Summary of the invention:
The objective of the invention is: a kind of presoma that is used for the carbon/carbon compound material oxidation resistant coating is provided, and this utilizes this persursor material can prepare the deficiency that overcomes aforesaid method.This presoma effectively mixes multiple starting material with coated component of difference in functionality, is dissolved in together, make coating precursor have bigger selection allotment property, allocate at the performance and the environment for use of carbon/carbon compound material as much as possible, thereby reduce the dipping number of times, reduce holiday, improve coating compactness and with the suitability of carbon/carbon compound material, improve the resistance of oxidation of carbon/carbon compound material.
Technical scheme of the present invention is:
The composition of carbon/carbon compound material oxidation resistant coating presoma: selecting for use chemical pure alcohol instead of part distilled water to make solvent, is that 99% phosphoric acid 5～25%, purity are that 99% primary zinc phosphate 40～65% and purity are that 99% boric acid 1～10% is formulated by weight percentage with silicon-dioxide 20～40%, purity.Select for use alcohol (chemical pure) instead of part distilled water to make solvent, by weight percentage with silicon-dioxide 20～40%, phosphoric acid 5～25% (purity is 99%), primary zinc phosphate 40～65% (purity is 99%), boric acid 1～10% (purity is 99%), formulated.
Preparation to the sol impregnation coating
1. prepare 2～4% boric acid spirit solutions, and add the TEOS of 15～20% systems ratio;
2. prepare 20～50% phosphate aqueous solutions;
3. will be 1., 2. prepare the stirring that is mixed of solution;
4. the ammonium pentaborate aqueous solution for preparing 5～10% concentration, and mix with 3. colloidal sol;
5. prepare 35～55% phosphoric acid dihydro zinc aqueous solution;
6. by 1: 1～1: 4 volume ratio will 4., 5. mixing;
7. at 150 ℃～200 ℃ baking carbon/carbon compound materials, immerse 6. middle 24h then;
8. take out the dipping carbon/carbon compound material, seasoning;
9. 0.5 ℃/1 ℃/min is warming up to 150 ℃～200 ℃, baking 1～4h.
The advantage and the positively effect of invention:
1, carbon/carbon compound material oxidation resistant coating preparation technology has been simplified in this invention, increases the coating precursor composition, has suppressed the rapid reaction of coating precursor composition under solution state, has improved the wetting property of coating precursor and carbon/carbon compound material.
2, the introducing of LMP material has improved carbon/carbon compound material coating self-healing ability in the coating, reduced the difference of coating and carbon/carbon compound material thermal expansivity, referring to Fig. 2, can cross SEM and observe, defectives such as crackle, hole are not found on the sol-impregnation anti-oxidation coating on sliding surface.Coating and carbon associativity are good, have high compactness, high healing ability.And multiple high melting-point low oxygen permeation rate material introducing has improved coating antioxygen penetrating power, delays the time that oxygen contacts with carbon/carbon compound material, thereby has improved anti-oxidation of coating.
3,650 ℃, 50h oxidative mass loss 19% of independent solution impregnation or composite solution dipping carbon/carbon compound material, and 650 ℃ in sample, the 50h oxidative mass loss of sol impregnation preparation are 1.89%, have demonstrated fully the remarkable of antioxidant effect of the present invention.
Description of drawings:
Fig. 1: the design sketch of the carbon/carbon compound material oxidation resistant coating of existing solution dipping method preparation
Fig. 2: the design sketch of the carbon/carbon compound material oxidation resistant coating of sol impregnation method preparation of the present invention
Embodiment:
Embodiment 1
Preparation to the sol impregnation coating:
1. take by weighing the boric acid of 1.5g, be dissolved in the dehydrated alcohol of 50ml, the TEOS of measuring 10ml is dissolved in the solution.
2. dilute in the phosphoric acid solution adding 20ml deionized water with 30ml 85%.
3. will be 1. and the solution of producing 2. mix stirring, make colloidal sol.
4. the 10g ammonium pentaborate is dissolved in the 100ml deionized water, and with the solution of 10ml with 3. in the colloidal sol produced mix, be stirred to leave standstill transparent.
5. the phosphoric acid dihydro zinc aqueous solution for preparing 40wt%.
6. the colloidal sol of producing in will be 4. by 1: 1 volume ratio mixes with 5. middle solution, and it is transparent to be stirred to colloidal sol.
7. the carbon/carbon compound material sample for preparing is toasted 2h in 150 ℃, immerse in the colloidal sol for preparing rapidly, dipping time is 24h.
8. take out impregnated carbon/carbon compound material sample and be placed on the charcoal felt, place loft drier seasoning 24h.
9. the sample in inciting somebody to action 8. is placed in the loft drier and is raised to 180 ℃ of baking 3h furnace cooling afterwards gradually with 0.5 ℃/min speed.
Embodiment 2:
Preparation to the sol impregnation coating:
1. take by weighing the boric acid of 1.0g, be dissolved in the dehydrated alcohol of 50ml, the TEOS of measuring 10ml is dissolved in wherein.
2. dilute in the phosphoric acid solution adding 20ml deionized water with 10ml 85%.
3. will be 1. and the solution of producing 2. mix, be stirred to the transparent colloidal sol of making, leave standstill 24h.
4. take by weighing the 10g ammonium pentaborate and be dissolved in the 100ml deionized water, and in the colloidal sol in adding 10ml solution 3., be stirred to transparent.
5. the phosphoric acid dihydro zinc aqueous solution for preparing 40 (wt) %.
6. the colloidal sol of producing in will be 4. by 2: 3 volume ratio mixes with 5. middle solution, and it is transparent to be stirred to colloidal sol.
7. the carbon/carbon compound material sample for preparing is toasted 2h in 180 ℃, immerse in the colloidal sol for preparing rapidly, dipping time is 24h.
8. take out impregnated carbon/carbon compound material sample and be placed on the charcoal felt, place loft drier seasoning 24h.
9. the sample in inciting somebody to action 8. is placed in the loft drier and is raised to 180 ℃ of baking 3h, last furnace cooling gradually with 0.5 ℃/min speed.
Embodiment 3:
Preparation to the sol impregnation coating:
1. take by weighing the boric acid of 1.5g, be dissolved in the dehydrated alcohol of 50ml, the TEOS of measuring 10ml is dissolved in wherein.
2. dilute in the phosphoric acid solution adding 20ml deionized water with 10ml 85%.
3. will be 1. and the solution of producing 2. mix, be stirred to the transparent colloidal sol of making.
4. take by weighing the 10g ammonium pentaborate and be dissolved in the 100ml deionized water, and in the colloidal sol in adding 10ml solution 3., be stirred to transparent.
5. the phosphoric acid dihydro zinc aqueous solution for preparing 40wt%.
6. the colloidal sol of producing in will be 4. by 1: 3 volume ratio mixes with 5. middle solution, and it is transparent to be stirred to colloidal sol.
7. the carbon/carbon compound material sample for preparing is toasted 2h in 180 ℃, immerse in the colloidal sol for preparing rapidly, dipping time is 24h.
8. take out impregnated carbon/carbon compound material sample and be placed on the charcoal felt, place loft drier seasoning 24h.
9. the sample in inciting somebody to action 8. is placed in the loft drier and is raised to 180 ℃ of baking 3h, last furnace cooling gradually with 0.5 ℃/min speed.
Embodiment 4:
Preparation to the sol impregnation coating:
1. take by weighing the boric acid of 1.5g, be dissolved in the dehydrated alcohol of 50ml, the TEOS of measuring 10ml is dissolved in wherein.
2. dilute in the phosphoric acid solution adding 20ml deionized water with 5ml 85%.
3. will be 1. and the solution of producing 2. mix, be stirred to the transparent colloidal sol of making.
4. take by weighing the 10g ammonium pentaborate and be dissolved in the 100ml deionized water, and in the colloidal sol in adding 10ml solution 3., be stirred to transparent.
5. the phosphoric acid dihydro zinc aqueous solution for preparing 50wt%.
6. the colloidal sol of producing in will be 4. by 1: 1 volume ratio mixes with 5. middle solution, and it is transparent to be stirred to colloidal sol.
7. the carbon/carbon compound material sample for preparing is toasted 2h in 150 ℃, immerse in the colloidal sol for preparing rapidly, dipping time is 24h.
8. take out impregnated carbon/carbon compound material sample and be placed on the charcoal felt, place loft drier seasoning 24h.
9. the sample in inciting somebody to action 8. is placed in the loft drier and is raised to 200 ℃ of baking 3h, last furnace cooling gradually with 0.5 ℃/min speed.
Embodiment 5:
Preparation to the sol impregnation coating:
1. take by weighing the boric acid of 1.5g, be dissolved in the dehydrated alcohol of 50ml, the TEOS of measuring 10ml is dissolved in wherein.
2. dilute in the phosphoric acid solution adding 20ml deionized water with 5ml 85%.
3. will be 1. and the solution of producing 2. mix, be stirred to the transparent colloidal sol of making.
4. take by weighing the 10g ammonium pentaborate and be dissolved in the 100ml deionized water, and in the colloidal sol in adding 10ml solution 3., be stirred to transparent.
5. the phosphoric acid dihydro zinc aqueous solution for preparing 40wt%.
6. the colloidal sol of producing in will be 4. by 1: 3 volume ratio mixes with 5. middle solution, and it is transparent to be stirred to colloidal sol.
7. the carbon/carbon compound material sample for preparing is toasted 2h in 180 ℃, immerse in the colloidal sol for preparing rapidly, dipping time is 24h.
8. take out impregnated carbon/carbon compound material sample and be placed on the charcoal felt, place loft drier seasoning 24h.
9. the sample in inciting somebody to action 8. is placed in the loft drier and rises to 180 ℃ of baking 3h, last furnace cooling gradually with 0.5 ℃/min speed.
Embodiment 6:
Preparation to the sol impregnation coating:
1. take by weighing the boric acid of 1.3g, be dissolved in the dehydrated alcohol of 50ml, the TEOS of measuring 10ml is dissolved in wherein.
2. dilute in the phosphoric acid solution adding 20ml deionized water with 10ml 85%.
3. will be 1. and the solution of producing 2. mix, be stirred to the transparent colloidal sol of making.
4. take by weighing the 10g ammonium pentaborate and be dissolved in the 100ml deionized water, and in the colloidal sol in adding 10ml solution 3., be stirred to transparent.
5. the phosphoric acid dihydro zinc aqueous solution for preparing 40wt%.
6. the colloidal sol of producing in will be 4. by 1: 3 volume ratio mixes with 5. middle solution, and it is transparent to be stirred to colloidal sol.
7. the carbon/carbon compound material sample for preparing is toasted 2h in 180 ℃, immerse in the colloidal sol for preparing rapidly, dipping time is 24h.
8. take out impregnated carbon/carbon compound material sample and be placed on the charcoal felt, place loft drier seasoning 24h.
9. the sample in inciting somebody to action 8. is placed in the loft drier and rises to 200 ℃ of baking 3h, last furnace cooling gradually with 0.5 ℃/min speed.
Claims (1)
1, the presoma of carbon/carbon compound material oxidation resistant coating, it is characterized in that: selecting for use chemical pure alcohol instead of part distilled water to make solvent, is that 99% phosphoric acid 5～25%, purity are that 99% primary zinc phosphate 40～65% and purity are that 99% boric acid 1～10% is formulated by weight percentage with silicon-dioxide 20～40%, purity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100030427A CN1300260C (en) | 2004-01-13 | 2004-01-13 | Precursor of carbon/carbon composite material anti-oxidation coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100030427A CN1300260C (en) | 2004-01-13 | 2004-01-13 | Precursor of carbon/carbon composite material anti-oxidation coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1640852A CN1640852A (en) | 2005-07-20 |
| CN1300260C true CN1300260C (en) | 2007-02-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100030427A Expired - Fee Related CN1300260C (en) | 2004-01-13 | 2004-01-13 | Precursor of carbon/carbon composite material anti-oxidation coating |
Country Status (1)
| Country | Link |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100455548C (en) * | 2007-06-12 | 2009-01-28 | 陕西科技大学 | A kind of carbon/carbon composite material solvothermal modification method |
| CN101318835B (en) * | 2008-07-17 | 2011-09-14 | 孙文革 | Oxidation protection processing method for carbon/carbon composite material aviation brake piece |
| CN111233498A (en) * | 2020-03-06 | 2020-06-05 | 中南大学 | A kind of environmental barrier coating and its preparation method and application |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6455159B1 (en) * | 2000-02-18 | 2002-09-24 | Honeywell International Inc. | Oxidation protection for carbon/carbon composites and graphites |
| CN1378524A (en) * | 1999-10-14 | 2002-11-06 | 维苏维尤斯·克鲁斯布公司 | Carbon-containing refractory article having protective coating |
| US6555173B1 (en) * | 2000-11-08 | 2003-04-29 | Honeywell International Inc. | Carbon barrier controlled metal infiltration layer for enhanced oxidation protection |
| US6668984B2 (en) * | 2000-12-06 | 2003-12-30 | Honeywell Advanced Composites Inc. | Oxidation protection for carbon/carbon composite and graphite friction materials |
-
2004
- 2004-01-13 CN CNB2004100030427A patent/CN1300260C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1378524A (en) * | 1999-10-14 | 2002-11-06 | 维苏维尤斯·克鲁斯布公司 | Carbon-containing refractory article having protective coating |
| US6455159B1 (en) * | 2000-02-18 | 2002-09-24 | Honeywell International Inc. | Oxidation protection for carbon/carbon composites and graphites |
| US6555173B1 (en) * | 2000-11-08 | 2003-04-29 | Honeywell International Inc. | Carbon barrier controlled metal infiltration layer for enhanced oxidation protection |
| US6668984B2 (en) * | 2000-12-06 | 2003-12-30 | Honeywell Advanced Composites Inc. | Oxidation protection for carbon/carbon composite and graphite friction materials |
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| CN1640852A (en) | 2005-07-20 |
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