CN110028338A - A kind of ZrB2-SiC-B2O3-SiO2-Zr(H3PO4)2The preparation method of coating - Google Patents
A kind of ZrB2-SiC-B2O3-SiO2-Zr(H3PO4)2The preparation method of coating Download PDFInfo
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- CN110028338A CN110028338A CN201910429128.2A CN201910429128A CN110028338A CN 110028338 A CN110028338 A CN 110028338A CN 201910429128 A CN201910429128 A CN 201910429128A CN 110028338 A CN110028338 A CN 110028338A
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- coating
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- zrb
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- 238000000576 coating method Methods 0.000 title claims abstract description 48
- 239000011248 coating agent Substances 0.000 title claims abstract description 47
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 235000011007 phosphoric acid Nutrition 0.000 title claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910007948 ZrB2 Inorganic materials 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 9
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 9
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 9
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 9
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 9
- 239000007770 graphite material Substances 0.000 claims abstract description 8
- VWZIXVXBCBBRGP-UHFFFAOYSA-N boron;zirconium Chemical compound B#[Zr]#B VWZIXVXBCBBRGP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000001680 brushing effect Effects 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract 6
- 238000001035 drying Methods 0.000 claims description 7
- 239000011812 mixed powder Substances 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 abstract description 15
- 238000007254 oxidation reaction Methods 0.000 abstract description 15
- 238000000034 method Methods 0.000 abstract description 11
- 230000003026 anti-oxygenic effect Effects 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 9
- 239000011159 matrix material Substances 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000003963 antioxidant agent Substances 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- MPNNOLHYOHFJKL-UHFFFAOYSA-N peroxyphosphoric acid Chemical compound OOP(O)(O)=O MPNNOLHYOHFJKL-UHFFFAOYSA-N 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5076—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with masses bonded by inorganic cements
- C04B41/5092—Phosphate cements
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
Abstract
The present invention relates to a kind of ZrB2‑SiC‑B2O3‑SiO2‑Zr(H3PO4)2The preparation method of coating.The coating is with ZrB2、SiC、B2O3、SiO2、H3PO4For raw material, after adjusting ratio academic title slurry in the way of brushing by slurry brush on graphite material surface, thickness can be adjusted by the method for repeatedly brushing and adjusting slurry viscosity.This method preparation process is simple, is suitable for complicated shape basis material.The coating can use in 1500 DEG C of high-temperature oxidation environment, significantly improve the antioxygenic property of graphite material, have good high-temperature oxidation resistance.
Description
Technical field
The present invention relates to a kind of preparation methods of oxidation-resistant ceramic coating.
Background technique
Graphite material and other carbon-based materials, such as C/C composite material have a variety of excellent performances, but in high temperature
It is easy to oxidize under the conditions of oxygen-containing, significantly limit its application range.In order to meet graphite material in high-temperature oxidation environment
Requirement, it is necessary to improve its antioxygenic property.
Currently used for improve Oxidation Resistance of Graphite Material main path there are two types of.One is matrix modifications, i.e., in stone
Antioxidant is added in black matrix reduces the oxidation rate of material;Another kind is surface coating method, i.e., graphite material surface applies
One layer of antioxidant coating is covered, opens it with oxidizing gas isolation, prevents gas from entering to improve antioxygenic property.
For ZrB2- SiC base ceramic material, with excellent high-temperature oxidation resistance.Due to ZrB2It is basic with SiC
It constitutes, which all has good antioxygenic property within the temperature range of from room temperature to 1600 DEG C.Therefore, ZrB2-
The composition of SiC is suitable for use as the composition material of fire-resistant oxidation resistant coating.But ZrB2SiC ceramic is difficult to be sintered, and is preparing
It is difficult to obtain fine and close structure during coating, limits its application as antioxidant coating.Currently, common preparation
ZrB2The method of-SiC coating is to prepare one layer of SiC transition zone using investment, then passes through investment, thermal spraying, brushing etc.
Method further prepares outer coating.In order to further increase ZrB2- SiC coating antioxygenic property generally requires to combine a variety of
Method prepares laminated coating.Preparation process is more complex, and the period is longer, higher cost, and most method be difficult to be suitable for for
The component of special shape.
Summary of the invention
Invention provides a kind of ZrB with good oxidation resistance energy2-SiC-B2O3-SiO2- Zr(H3PO4)2It applies
The preparation method of layer.
ZrB of the invention2-SiC-B2O3-SiO2-Zr(H3PO4)2The preparation method of coating is to sequentially include the following steps:
By ZrB2, SiC, B2O3、SiO2, H3PO4 be configured to slurry, then by brush in the way of by slurry brush in graphite material
Surface, the brush second layer again as needed after drying at room temperature.So continue, brushes laminated coating as needed.
In the method, the volume ratio of ZrB2 and SiC should be between 1:9 ~ 9:1.B2O3And SiO2Molar ratio in 1:4 ~ 2:
Between 1.B2O3And SiO2Volume content be no more than ZrB2 and SiC total volume 50%.H3PO4 concentration 1wt% ~ 85wt% it
Between, the ratio between gross mass of the quality of H3PO4 used and mixed powder is between 1:10 ~ 20:1.
Advantages of the present invention:
One, ZrB of the invention2-SiC-B2O3-SiO2-Zr(H3PO4)2Preparation technology of coating is simple, easy to use, can be direct
Using spread coating in component surface prepares coating, and coating layer thickness can according to need and be adjusted by the method repeatedly brushed
Section.Slurry viscosity is adjustable, passes through the thickness of the adjustable signal layer coating of adjusting of viscosity.The coating uses spread coating, fits
For basis material of various shapes.
Two, ZrB prepared by the present invention2-SiC-B2O3-SiO2-Zr(H3PO4)2Coating structure is fine and close, after brushing just through drying
It can be used for hot environment, be not required to using preceding carry out high-temperature process.Coating after drying has good in high-temperature oxidation environment
Antioxygenic property, can be used for a long time in 1500 DEG C of high-temperature oxidation environment.
Detailed description of the invention
Fig. 1 is the ZrB prepared in specific embodiment2-SiC-B2O3-SiO2-Zr(H3PO4)2Coating is after drying at room temperature
Surface SEM photograph.
Fig. 2 is in specific embodiment in the ZrB of graphite matrix surface preparation2-SiC-B2O3-SiO2-Zr(H3PO4)2It applies
Macro morphology of the layer after 1500 DEG C of oxidation 60min.
Specific embodiment
A kind of ZrB in present embodiment2-SiC-B2O3-SiO2-Zr(H3PO4)2The preparation method of coating is according to the following steps
It carries out:
By 42g ZrB2、9.6g SiC、2.5g B2O3、2.6g SiO2It is added in ball grinder, ethyl alcohol is added as ball-milling medium,
Then it is mixed using ball mill, utilizes rotary evaporator that will cross 200 mesh after the mixture drying of the above powder after mixing 8h
Sieve.Then the powder obtained after mixing is mixed with the ratio that 10g powder corresponds to 4ml concentrated phosphoric acid, phosphoric acid concentration 85%.
The powder that phosphoric acid is added is sufficiently stirred, powder and phosphoric acid are sufficiently mixed, the slurry of mixed powder is made.Pass through brushing
Method slurry is brushed after graphite matrix shows, at room temperature it is dry for 24 hours.Then second is carried out on its surface to brush
Painting prepares second layer coating, then dry for 24 hours in room temperature condition.It so repeats, until four layers of coating are made.
Coating after brushing is after drying at room temperature, and coating structure is fine and close, with substrate combinating strength height.Fig. 1 show room
ZrB after temperature is dry2-SiC-B2O3-SiO2-Zr(H3PO4)2The surface SEM photograph of coating.Through peroxophosphoric acid treated coating knot
Structure is fine and close, and there are a large amount of glass phases.Due to the use of concentrated phosphoric acid, Zr (H is formd in coating3PO4)2, it is also possible to it forms
SiHP3O10.The presence of glass phase substantially increases coating consistency, and consistency coating can be effectively by matrix and external oxidation ring
Border separates.
By four layers of ZrB obtained2-SiC-B2O3-SiO2-Zr(H3PO4)2It is heated to 1500 DEG C in the air of coating, and protects
After warm 60min, coating structure keeps complete, is effectively protected graphite matrix, avoids the oxidation of graphite matrix.After oxidation
Coating macro morphology is as shown in Fig. 2, the diameter of disc-shaped graphite matrix therein is 50mm.
Claims (7)
1. a kind of ZrB2-SiC-B2O3-SiO2-Zr(H3PO4)2The preparation method of coating, feature is in the ZrB2-SiC-B2O3-
SiO2-Zr(H3PO4)2The preparation method of coating is to sequentially include the following steps:
By ZrB2、SiC、B2O3、SiO2、H3PO4Be configured to slurry, then by brush in the way of by slurry brush in graphite material table
Face, the brush second layer again as needed after drying at room temperature;So continue, brushes laminated coating as needed.
2. a kind of ZrB according to claim 12-SiC-B2O3-SiO2-Zr(H3PO4)2The preparation method of coating, feature
It is that the volume ratio of ZrB2 and SiC in raw material should be between 1:9 ~ 9:1.
3. a kind of ZrB according to claim 12-SiC-B2O3-SiO2-Zr(H3PO4)2The preparation method of coating, feature
It is B in raw material2O3And SiO2Molar ratio between 1:4 ~ 2:1.
4. a kind of ZrB according to claim 12-SiC-B2O3-SiO2-Zr(H3PO4)2The preparation method of coating, feature
It is B in raw material2O3And SiO2Total volume content be no more than ZrB2 and SiC total volume 50%.
5. a kind of ZrB according to claim 12-SiC-B2O3-SiO2-Zr(H3PO4)2The preparation method of coating, feature
It is that H3PO4 concentration is between 1wt% ~ 85wt% in raw material, the ratio between gross mass of the quality of H3PO4 used and mixed powder is 1:
Between 10 ~ 20:1.
6. a kind of ZrB according to claim 12-SiC-B2O3-SiO2-Zr(H3PO4)2The preparation method of coating, feature
It is ZrB in raw material2、SiC、B2O3、SiO2It to be first uniformly mixed before being mixed with H3PO4.
7. a kind of ZrB according to claim 12-SiC-B2O3-SiO2-Zr(H3PO4)2The preparation method of coating, feature
Be the coating after brushing will no more than 60 DEG C at a temperature of dry 1-48h after carry out the preparation of next layer of coating again.
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CN201910429128.2A CN110028338A (en) | 2019-05-22 | 2019-05-22 | A kind of ZrB2-SiC-B2O3-SiO2-Zr(H3PO4)2The preparation method of coating |
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CN201910429128.2A CN110028338A (en) | 2019-05-22 | 2019-05-22 | A kind of ZrB2-SiC-B2O3-SiO2-Zr(H3PO4)2The preparation method of coating |
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Citations (9)
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---|---|---|---|---|
CN1062961A (en) * | 1990-12-26 | 1992-07-22 | 华兴航空机轮公司 | Carbon/carbon compound material brake disc high-temperature oxidation resistant coating |
US5420084A (en) * | 1993-01-28 | 1995-05-30 | Pechiney Recherche | Coatings for protecting materials against reactions with atmosphere at high temperatures |
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US6632762B1 (en) * | 2001-06-29 | 2003-10-14 | The United States Of America As Represented By The Secretary Of The Navy | Oxidation resistant coating for carbon |
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CN105198492A (en) * | 2015-09-25 | 2015-12-30 | 东南大学 | Oxidation-resistant coating and preparation method thereof |
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-
2019
- 2019-05-22 CN CN201910429128.2A patent/CN110028338A/en active Pending
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CN1062961A (en) * | 1990-12-26 | 1992-07-22 | 华兴航空机轮公司 | Carbon/carbon compound material brake disc high-temperature oxidation resistant coating |
US5420084A (en) * | 1993-01-28 | 1995-05-30 | Pechiney Recherche | Coatings for protecting materials against reactions with atmosphere at high temperatures |
US6071615A (en) * | 1996-04-23 | 2000-06-06 | Man Technologie Aktiengesellschaft | Protective coating for workpieces, especially of carbon composite material, workpieces with a protective coating of this type, and process for producing such protective coating |
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Application publication date: 20190719 |
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