CN103724052A - Preparation method of high-temperature anti-oxidation coating for carbon-ceramic brake disc - Google Patents
Preparation method of high-temperature anti-oxidation coating for carbon-ceramic brake disc Download PDFInfo
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- CN103724052A CN103724052A CN201310740086.7A CN201310740086A CN103724052A CN 103724052 A CN103724052 A CN 103724052A CN 201310740086 A CN201310740086 A CN 201310740086A CN 103724052 A CN103724052 A CN 103724052A
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Abstract
The invention relates to a preparation method of a high-temperature anti-oxidation coating for a carbon-ceramic brake disc. The method mainly comprises the following steps: with magnesium nitrate, aluminum nitrate, ethyl orthosilicate and the like as raw materials, preparing sol as an inner coating material; with phosphate as a raw material, preparing a solution as an outer coating material; and uniformly coating the sol and the solution on the surface of the carbon-ceramic brake disc material, so as to obtain the coating which is good in binding force with a matrix and compact by high-temperature treatment. By adopting the method, the problem of oxidation of the carbon-ceramic brake disc coating at high temperature is effectively solved, and the coating has good water resistance and seawater resistance. Meanwhile, the method has the advantages of simple preparation technology, short preparation period, good repeatability and the like.
Description
Technical field
The present invention relates to the preparation method of a kind of carbon pottery brake flange high-temperature oxidation resistant coating, particularly relate to that a kind of preparation process is simple, cost is low and the manufacture method of the carbon of excellent performance pottery aircraft brake material inoxidzable coating.
Background technology
Carbon pottery brake material has that density is low, heatproof is high, intensity is high, stable friction performance, and especially static friction coefficient is high, under hygrometric state and briny environment frictional behaviour decay little, recover the advantage such as fast, can increase substantially the work-ing life of braking efficiency and brake material.Therefore carbon pottery brake material is the aircraft brake material of new generation that has competitive power.Aircraft is the in the situation that of normal landing and overload landing, the temperature rise of brake secondary volume can reach 600～800 ℃, when termination is taken off, temperature can be considerably beyond 1200 ℃, aircraft brake pair is to work under the oxidizing condition of thermal shocking repeatedly, oxidation can make the friction and wear behavior of brake material and heat physical properties reduce, especially can significantly reduce the intensity of carbon pottery brake material, have a strong impact on the connection reliability of brake material and wheel system, catastrophic failure even occurs.Therefore prepare carbon pottery aircraft brake material inoxidzable coating significant.
In carbon pottery brake flange, contain the carbon phase (RESEARCH OF PYROCARBON and carbon fiber) of 50-60wt%, the SiC ceramic phase of about 40-50wt%.Do not having under oxidation protection condition, carbon is easily oxidized owing to containing a large amount of active sites, friction and wear behavior and heat physical properties are reduced, also can significantly reduce brake flange intensity, have a strong impact on reliability and takeoff and landing security that brake flange is connected with wheel system.Must development 600～800 ℃ can passivation carbon phase active site protective coating, to improve resistance of oxidation.Meanwhile, carbon pottery brake flange is comprised of carbon fiber, RESEARCH OF PYROCARBON, SiC pottery and remaining Si etc., and the matrix cracking that heterogeneous material thermal expansion mismatch produces can become the diffusion admittance of oxygen, must develop the inoxidzable coating with high temperature self-healing capability.
Chinese patent mandate publication number CN1718560A discloses a kind of carbon fibre reinforced silicon carbide material inoxidzable coating and preparation method thereof, and the method is SiC tack coat, self-healing layer and SiC erosion resistance layer.This invention, by adopting the self-healing layer that can produce self-healing effect in compared with large-temperature range to improve the antioxidant effect of coating, makes C/SiC composite element in compared with large-temperature range, have good antioxidant property.But the preparation method of coating is chemical Vapor deposition process, complex process, to having relatively high expectations of experimental installation; Compound coating is three layers, and preparation cycle is longer.
Summary of the invention
The technical problem solving
For fear of the deficiencies in the prior art part; the present invention proposes a kind of preparation method of carbon pottery brake flange high-temperature oxidation resistant coating; the problem such as overcome that the preparation material cost existing in existing coating technology is high, resistance of oxidation is weak under complicated process of preparation and sea conditions; that a kind of raw material is simple and easy to get; preparation technology is simple; not high to preparation environmental requirement, and at high temperature material is carried out to the preparation method of protection against oxidation effectively.
Technical scheme
A preparation method for carbon pottery brake flange high-temperature oxidation resistant coating, is characterized in that step is as follows:
Step 1: the carbon brake flange ultrasonic cleaning in water of making pottery is removed to surface contaminant, put into 120～180 ℃ of dry 2～4h of baking oven, obtain dried carbon pottery brake flange and take out and dry in the air to room temperature;
Step 2: by the brushing of magnalium silicon sol on step carbon pottery brake flange surface, be placed in the dry 5-20h of 50-150 ℃ of baking oven, then high-temperature heat treatment under argon gas or vacuum condition, temperature rise rate: 5～10 ℃/min, at 1200 ℃～1500 ℃ insulation 0.5～2h, after furnace cooling, obtain high temperature self-healing glass coating;
Step 3: by phosphate solution brushing on the high temperature self-healing glass coating on carbon pottery brake flange surface, be placed in the dry 5-20h of 50-150 ℃ of baking oven, then high-temperature heat treatment under argon gas or vacuum condition, temperature rise rate: 5～10 ℃/min, at 600 ℃～900 ℃ insulation 0.5～2h, insulation finishes directly from stove, to take out afterwards, is cooled to room temperature and obtains the high-temperature oxidation resistant coating of phosphoric acid salt passivation.
Being prepared as of described magnalium silicon sol: the magnesium nitrate and the citric acid that are first 1～1.5:2～3 by mol ratio are dissolved in the water, and are prepared into magnesium nitrate solution; The aluminum nitrate and the citric acid that by mol ratio, are 1～1.5:3～4 are dissolved in the water, and are prepared into aluminum nitrate solution; By adding dehydrated alcohol and water to be hydrolyzed in tetraethoxy, be prepared into silicon sol again; Wherein the mol ratio of tetraethoxy, dehydrated alcohol and water is 1～1.5 ︰ 3～4 ︰ 1～1.5; Under agitation condition, magnesium nitrate solution, aluminum nitrate solution are joined in silicon sol, drip hydrochloric acid or ammoniacal liquor and regulate PH=1～3, prepare magnalium silicon sol; The mol ratio of described magnesium nitrate, aluminum nitrate and tetraethoxy is 1～3:3～6:4～8.
Being prepared as of described phosphoric acid salt passivating coating: the aluminum phosphate, manganous phosphate, zinc phosphate, calcium phosphate, phosphoric acid, boric acid and the water that are 1～3:2～5:8～10:0.1～0.5:20～30:5～10:30～40 by mass ratio are placed in beaker stirring and dissolving, obtain phosphate solution.
Described phosphoric acid salt is aluminum phosphate, manganous phosphate, zinc phosphate or calcium phosphate.
Beneficial effect
The preparation method of a kind of carbon pottery brake flange high-temperature oxidation resistant coating that the present invention proposes, using magnesium nitrate, aluminum nitrate, tetraethoxy etc. as raw material, be prepared into colloidal sol as undercoat material, using phosphoric acid salt as raw material, be prepared into solution as external coating (EC) material, colloidal sol and solution are evenly coated on to carbon pottery brake material surface, through pyroprocessing, obtain with matrix in conjunction with good and fine and close coating.The method efficiently solves at high temperature oxidized problem of carbon pottery brake-disc coating, and coating has good water-fast and seawater ability.Meanwhile, the present invention has the advantages such as preparation technology is simple, preparation cycle is short, favorable repeatability.
The invention has the beneficial effects as follows: (1) coating evenly, fine and close and be combined with matrix; (2) coating oxidation proof properties and thermal shock resistance excellence; (3) coating resisting sea water erosion ability is strong; (4) preparation technology of coating process is simple, and the cycle is short, cost is low, convenient and easy, is suitable for preparation of industrialization.
Accompanying drawing explanation
Fig. 1: the preparation process of magnalium silicon sol;
Fig. 2: the preparation process of phosphate solution;
Fig. 3: the SEM photo of coating sample surface micro-topography;
Fig. 4: the SEM photo of coating sample section microscopic appearance;
Fig. 5: at 700 ℃, be oxidized the SEM photo of coatingsurface microscopic appearance after 10 hours in air;
Fig. 6: at 700 ℃, be oxidized the SEM photo of coating section microscopic appearance after 10 hours in air;
Fig. 7: coating sample and the oxidation dynamic curve without coating sample.
Embodiment
Now in conjunction with the embodiments, the invention will be further described for accompanying drawing:
Embodiment 1:
The preparation of magnalium silicon sol:
The magnesium nitrate and the citric acid that by mol ratio, are 1:2 are dissolved in the water, and the mass ratio of citric acid and water is that 0.5:1 is prepared into magnesium nitrate solution; The aluminum nitrate and the citric acid that by mol ratio, are 1:3 are dissolved in the water, and the mass ratio of citric acid and water is that 0.7:1 is prepared into aluminum nitrate solution; By adding dehydrated alcohol, water to be hydrolyzed in appropriate tetraethoxy, prepare silicon sol again, wherein the mol ratio of tetraethoxy, dehydrated alcohol and water is 1:4:1.Under the condition constantly stirring, magnesium nitrate solution, aluminum nitrate solution are joined in silicon sol successively, drip hydrochloric acid or ammoniacal liquor and regulate PH=1, prepare magnalium silicon sol, seal stand-by.
The preparation of phosphate solution:
By mass ratio, be that 2:3:8:0.3:25:8:32 aluminum phosphate, manganous phosphate and zinc phosphate, phosphoric acid, boric acid and water are placed in beaker stirring and dissolving, obtain phosphate solution, seal stand-by.
Step 1: the preparation of carbon pottery brake flange sample:
The carbon brake flange of making pottery is processed into 15 × 15 × 10mm
3sample, in tap water, ultrasonic cleaning is removed surface contaminant, puts into 120 ℃ of dry 4h of baking oven, and dried carbon pottery brake flange sample is taken out and dried in the air to room temperature, prepares to brush.
Step 2: the preparation of high temperature self-healing glass coating:
By the magnalium silicon sol of the preparation carbon pottery brake flange specimen surface that evenly brushing is prepared in step 1; be placed in the dry 15h of 60 ℃ of baking ovens; then by coated brake flange sample high-temperature heat treatment under argon shield condition; temperature rise rate: 5 ℃/min; at 1300 ℃ of insulation 2h, after furnace cooling, obtain high temperature self-healing glass coating.
Step 3: the preparation of phosphoric acid salt passivating coating:
By the evenly carbon pottery brake flange specimen surface of brushing after step 2 thermal treatment of the phosphate solution of preparation, be placed in the dry 10h of 90 ℃ of baking ovens, then by coated brake flange sample high-temperature heat treatment under argon gas condition, temperature rise rate: 5 ℃/min, at 650 ℃ of insulation 1h, directly from stove, take out and be placed in room temperature and obtain phosphoric acid salt passivating coating after cooling.
To the coating sample of preparing with without coating sample, carry out 700 ℃ of oxidation experiments examinations, result shows: 10 hours coating sample weightlessness of 700 ℃ of oxidations of dry state is～0.14%, and uncoated sample weightlessness is～56.75%; Coating sample is directly～0.4% in 10 hours weightlessness of 700 ℃ of oxidations soak 10min in fresh water after; Coating sample is directly～0.7% in 10 hours weightlessness of 700 ℃ of oxidations soak 10min in seawater after; After 700 ℃ of thermal shocks of coating sample 50 times, coating is complete, without peeling off, and flawless.Show that this coating has good anti-oxidation effect, has good resisting sea water erosion performance.
Embodiment 2:
The preparation of magnalium silicon sol:
The magnesium nitrate and the citric acid that by mol ratio, are 1:2.5 are dissolved in the water, and the mass ratio of citric acid and water is 0.6:1, is prepared into magnesium nitrate solution; The aluminum nitrate and the citric acid that by mol ratio, are 1:4 are dissolved in the water, and the mass ratio of citric acid and water is 0.8:1, is prepared into aluminum nitrate solution; By adding dehydrated alcohol, water to be hydrolyzed in appropriate tetraethoxy, prepare silicon sol again, wherein the mol ratio of tetraethoxy, dehydrated alcohol and water is 1:3:1.5.Under the condition constantly stirring, magnesium nitrate solution, aluminum nitrate solution are joined in silicon sol successively, drip hydrochloric acid or ammoniacal liquor and regulate PH=3, prepare magnalium silicon sol, seal stand-by.
The preparation of phosphate solution:
Aluminum phosphate, manganous phosphate and the zinc phosphate, phosphoric acid, boric acid and the water that by mass ratio, are 2.5:3.5:9:0.4:25:8.5:35 are placed in beaker stirring and dissolving, obtain phosphate solution, seal stand-by.
Step 1: the preparation of carbon pottery brake flange sample:
The carbon brake flange of making pottery is processed into 15 × 15 × 10mm
3sample, in tap water, ultrasonic cleaning is removed surface contaminant, puts into 150 ℃ of dry 3h of baking oven, and dried carbon pottery brake flange sample is taken out and dried in the air to room temperature, prepares to brush.
Step 2: the preparation of high temperature self-healing glass coating:
By the magnalium silicon sol of the preparation carbon pottery brake flange specimen surface that evenly brushing is prepared in step 1; be placed in the dry 10h of 70 ℃ of baking ovens; then by coated brake flange sample high-temperature heat treatment under argon shield condition; temperature rise rate: 10 ℃/min; at 1400 ℃ of insulation 1h, after furnace cooling, obtain high temperature self-healing glass coating.
Step 3: the preparation of phosphoric acid salt passivating coating:
By the evenly carbon pottery brake flange specimen surface of brushing after step 2 thermal treatment of the phosphate solution of preparation, be placed in the dry 10h of 100 ℃ of baking ovens, then by coated brake flange sample high-temperature heat treatment under argon gas condition, temperature rise rate: 10 ℃/min, at 750 ℃ of insulation 1h, directly from stove, take out and be placed in room temperature and obtain phosphoric acid salt passivating coating after cooling.
To the coating sample of preparing with without coating sample, carry out 700 ℃ of oxidation experiments examinations, result shows: 10 hours coating sample weightlessness of 700 ℃ of oxidations of dry state is～0.39%, and uncoated sample weightlessness is～56.75%; Coating sample is directly～0.65% in 10 hours weightlessness of 700 ℃ of oxidations soak 10min in fresh water after; Coating sample is directly～0.96% in 10 hours weightlessness of 700 ℃ of oxidations soak 10min in seawater after; After 700 ℃ of thermal shocks of coating sample 50 times, coating is complete, without peeling off, and flawless.Show that this coating has good anti-oxidation effect and good resisting sea water erosion performance.
Claims (4)
1. a preparation method for carbon pottery brake flange high-temperature oxidation resistant coating, is characterized in that step is as follows:
Step 1: the carbon brake flange ultrasonic cleaning in water of making pottery is removed to surface contaminant, put into 120～180 ℃ of dry 2～4h of baking oven, obtain dried carbon pottery brake flange and take out and dry in the air to room temperature;
Step 2: by the brushing of magnalium silicon sol on step carbon pottery brake flange surface, be placed in the dry 5-20h of 50-150 ℃ of baking oven, then high-temperature heat treatment under argon gas or vacuum condition, temperature rise rate: 5～10 ℃/min, at 1200 ℃～1500 ℃ insulation 0.5～2h, after furnace cooling, obtain high temperature self-healing glass coating;
Step 3: by phosphate solution brushing on the high temperature self-healing glass coating on carbon pottery brake flange surface, be placed in the dry 5-20h of 50-150 ℃ of baking oven, then high-temperature heat treatment under argon gas or vacuum condition, temperature rise rate: 5～10 ℃/min, at 600 ℃～900 ℃ insulation 0.5～2h, insulation finishes directly from stove, to take out afterwards, is cooled to room temperature and obtains the high-temperature oxidation resistant coating of phosphoric acid salt passivation.
2. the preparation method of carbon pottery brake flange high-temperature oxidation resistant coating according to claim 1, is characterized in that being prepared as of described magnalium silicon sol: the magnesium nitrate and the citric acid that by mol ratio, are first 1～1.5:2～3 are dissolved in the water, and are prepared into magnesium nitrate solution; The aluminum nitrate and the citric acid that by mol ratio, are 1～1.5:3～4 are dissolved in the water, and are prepared into aluminum nitrate solution; By adding dehydrated alcohol and water to be hydrolyzed in tetraethoxy, be prepared into silicon sol again; Wherein the mol ratio of tetraethoxy, dehydrated alcohol and water is 1～1.5 ︰ 3～4 ︰ 1～1.5; Under agitation condition, magnesium nitrate solution, aluminum nitrate solution are joined in silicon sol, drip hydrochloric acid or ammoniacal liquor and regulate PH=1～3, prepare magnalium silicon sol; The mol ratio of described magnesium nitrate, aluminum nitrate and tetraethoxy is 1～3:3～6:4～8.
3. the preparation method of carbon pottery brake flange high-temperature oxidation resistant coating according to claim 1, it is characterized in that being prepared as of described phosphoric acid salt passivating coating: the aluminum phosphate, manganous phosphate, zinc phosphate, calcium phosphate, phosphoric acid, boric acid and the water that by mass ratio, are 1～3:2～5:8～10:0.1～0.5:20～30:5～10:30～40 are placed in beaker stirring and dissolving, obtain phosphate solution.
4. the preparation method of carbon pottery brake flange high-temperature oxidation resistant coating according to claim 1, is characterized in that described phosphoric acid salt is aluminum phosphate, manganous phosphate, zinc phosphate or calcium phosphate.
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| CN201310740086.7A CN103724052A (en) | 2013-12-27 | 2013-12-27 | Preparation method of high-temperature anti-oxidation coating for carbon-ceramic brake disc |
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| CN201310740086.7A CN103724052A (en) | 2013-12-27 | 2013-12-27 | Preparation method of high-temperature anti-oxidation coating for carbon-ceramic brake disc |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1889822A2 (en) * | 2006-08-18 | 2008-02-20 | Honeywell International Inc. | Two piece carbon-carbon pressure plate design for aircraft brakes |
| CN101318835A (en) * | 2008-07-17 | 2008-12-10 | 孙文革 | Oxidization protection processing method for aviation brake of carbon/carbon composite material |
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2013
- 2013-12-27 CN CN201310740086.7A patent/CN103724052A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1889822A2 (en) * | 2006-08-18 | 2008-02-20 | Honeywell International Inc. | Two piece carbon-carbon pressure plate design for aircraft brakes |
| CN101318835A (en) * | 2008-07-17 | 2008-12-10 | 孙文革 | Oxidization protection processing method for aviation brake of carbon/carbon composite material |
Non-Patent Citations (2)
| Title |
|---|
| 吴雅惠 等: ""BaO–Al2O3–SiO2环境隔离涂层的制备与耐腐蚀性能表征"", 《硅酸盐学报》, vol. 37, no. 8, 31 August 2009 (2009-08-31), pages 1299 - 1305 * |
| 江东亮 等: "《无机非金属材料手册》", 31 July 2009, article "无机非金属材料手册", pages: 511 * |
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Application publication date: 20140416 |