CN101514473B - Method for preparing yttrium silicate coat by cathode rotation hydrothermal electrophoretic deposition - Google Patents
Method for preparing yttrium silicate coat by cathode rotation hydrothermal electrophoretic deposition Download PDFInfo
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- CN101514473B CN101514473B CN2009100212165A CN200910021216A CN101514473B CN 101514473 B CN101514473 B CN 101514473B CN 2009100212165 A CN2009100212165 A CN 2009100212165A CN 200910021216 A CN200910021216 A CN 200910021216A CN 101514473 B CN101514473 B CN 101514473B
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Abstract
The invention relates to a method for preparing an yttrium silicate coat by cathode rotation hydrothermal electrophoretic deposition. A cathode rotation hydrothermal electrophoretic deposition method is used for preparing an yttrium silicate antioxidant coat on the surface of carbon/carbon-carborundum composite. Yttrium silicate powder is used as raw material to be respectively made into the yttrium silicate coats with compact structure, microcrack and different thickness in certain powder material proportion, under certain temperature and voltage and at different cathode rotation speeds. The method has the advantages of simple technical control and uniform coat, avoids repeated operation to certain extent and can be used for product with complex surface, and the method can obtain the yttrium silicate coat with controllable structure and good performance under low temperature.
Description
Technical field
The present invention relates to a kind of preparation method of iridium silicate coating layer, be specifically related to a kind of method of preparing yttrium silicate coat by cathode rotation hydrothermal electrophoretic deposition.
Background technology
Carbon/carbon compound material becomes the focus of people's research gradually in recent years.Because the carbon/carbon compound material thermal expansivity is low, density is low, anti-ablation, corrosion-resistant, stable friction factor, the heat-conductivity conducting performance is good and characteristics such as high strength, high-modulus, the characteristic that goes up not down with temperature rising mechanical property particularly, so it is applied to Aeronautics and Astronautics and civilian industry field.Yet, its many above-mentioned character is only under inert atmosphere or be lower than under 450 ℃ the condition and could keep, oxidation weight loss will make the mechanical property of carbon/carbon compound material obviously descend, thereby limit it as the widespread use of high-temperature refractory under oxidizing atmosphere.Therefore, solving carbon/carbon compound material high temperature oxidation protection question is the prerequisite that makes full use of its performance.
Oxidation resistant coating is considered to solve the effective ways of carbon/carbon compound material high temperature oxidation protection question, but because the special physicochemical characteristic of carbon/carbon compound material, many high temperature ceramic material can't directly use as high temperature coating, therefore adopt the compound coating method of transition layer/external coating (EC) (high temperature ceramic material) mostly, in transition layer, because SiC and carbon/carbon compound material have good physical chemistry consistency, so generally adopted.Because the yttrium silicate material has excellent physical and chemical performances such as high-melting-point, low Young's modulus, low thermal coefficient of expansion, low vaporization at high temperature rate, low high-temperature oxygen rate of permeation and resistance to chemical attack, makes one of its desirable top layer material that becomes graphite, C/C and C/C-SiC matrix material and the contour performance material at high temperature of SiC structural ceramics oxidation resistant coating.
Up to the present, the technology of preparing of iridium silicate coating layer mainly contains hot isostatic pressing method, molten slurry coating sintering method, plasma spraying method and original position forming method etc.But because above method all needs at high temperature just can prepare more satisfactory coating.And higher preparation temperature may cause certain damage to matrix, so low temperature preparation technology's exploitation is one of direction of endeavouring of investigator always.Its characteristics of negative electrode rotation water heat electrophoresis deposition method at first are with electro-deposition techniques and hydrothermal technique combination, and the reacting activation energy that utilizes localized hyperthermia that ultrasonic wave produces in reaction system and high pressure effectively to reduce the yttrium silicate suspended particles, make it in the hydro-thermal electrophoresis process, react more complete and abundant.Phase transformation and the embrittlement adopting this method can avoid adopting conventional high-temperature to apply and cause solve in the coating preparation process thermal damage to matrix to a certain extent; Secondly, deposition process is non-streamlined process, can form uniform settled layer at the matrix surface of complex-shaped or porous surface, and the accurate control coating composition of energy, thickness and porosity, make heterogeneous compound coating of simple efficient production and graded ceramics coating become possibility; Moreover water heat electrophoresis deposition is that the orientation of charged particle moves, a large amount of gases affect coatings that produce in the time of can be because of the brine electrolysis solvent and the bonding force of matrix.By the negative electrode high speed rotating, avoid traditional hydrothermal method to need repeatedly to apply the shortcoming that just can obtain the coating of compact and uniform structure in addition, realized under controlled condition, obtaining fine and close, iridium silicate coating layer that have micro-flaw, different thickness.In addition, negative electrode rotation water heat electrophoresis deposition method also has characteristics such as simple to operation, that cost is low, depositing operation is easy to control.
Adopting electrodip process to prepare in the research of iridium silicate coating layer, Chr.Argirusis, T.Damjanovic, M.Stojanovic, G.Borchardt (Chr.Argirusis, T.Damjanovic, M.Stojanovic, G.Borchardt.Current Research inAdvanced Materials and Processes, 2005, pp.451-456) wait human 70wt%Y
2Si
2O
7And 30wt%Y
2SiO
5After nano-powder fully disperseed in b propanol, the deposition voltage deposit of 60V 1-3 minute, preparing thickness on the C/C-Si-SiC matrix material was the compound external coating (EC) of yttrium silicate of 15-30 μ m.This coating plays C/C in 1500 ℃ still air and reaches 100 hours protection.Huang Jianfeng (Huang Jian-Feng, Zeng Xie-Rong, Li He-Jun, Ceramics International, 2006 (32): 417-421.Huang Jian-Feng, ZengXie-Rong, Li He-Jun, Journal of Material Science, 2004 (39): 7383-7385) waiting the yttrium silicate nano powder with gradient composition is spraying raw material, adopts the Y of plasma spraying method in SiC undercoat surface preparation
2O
32SiO
2/ Y
2O
31.5SiO
2/ Y
2O
3SiO
2Gradient composite coating has been brought into play different components yttrium silicate properties of materials preferably, and material weightlessness is lower than 2% behind 1600 ℃ of following oxidation 116h; Y in this coating system
2O
3And SiO
2Distribution gradient has greatly been alleviated the thermal stresses of coating inside, outer field Y
2O
3SiO
2(Y
2SiO
5) then play the effect of thermal barrier coating, reduced internally coated service temperature, help improving anti-oxidation of coating.The water heat electrophoresis deposition method of utilizing of Huang Jianfeng, Deng Fei etc. (Huang Jianfeng, Deng Fei etc., a kind of water heat electrophoresis deposition method of gradient iridium silicate coating layer [P] .CN1904144.) success has been prepared even, fine and close yttrium silicate gradient cladding on the carbon/carbon composite material base body.
Summary of the invention
The object of the present invention is to provide a kind of technology controlling and process simple, coating is even, can avoid the method for the preparing yttrium silicate coat by cathode rotation hydrothermal electrophoretic deposition of repetitive operation, preparation method of the present invention prepares under relatively low temperature with matrix bond is good, antioxidant property is high, compact structure, even, the iridium silicate coating layer that coat-thickness is controlled.
For achieving the above object, the technical solution used in the present invention is:
1) at first, selects the analytically pure yttrium silicate (Y of 0.05-5 micron for use
2Si
2O
7) powder, analytically pure Virahol and iodine is starting material, according to Y
2Si
2O
7: the ratio of Virahol=2.5-5g: 150ml is mixed with suspension, under 1000-2000r/min behind the mechanical stirring 8-12h, after in suspension, introducing iodine and stir 8-12h in the ratio of 0.5-1.5g/L, place ultrasonic wave standby behind vibration 10-60min under the power of 100-500W;
2) secondly, above-mentioned suspension being added in the water heat electrophoresis deposition reactor, is anode with the Graphite Electrodes, with depositing in advance of can rotating the carbon/carbon compound material of 50-100 micron thickness SiC coating be negative electrode;
3) then, after the carbon/carbon compound material of having treated to deposit in advance 50-100 micron thickness SiC coating is fixed in negative electrode, sealing water heat electrophoresis deposition reactor, simultaneously the water heat electrophoresis deposition reactor is heated to 100-300 ℃, the control deposition voltage is 50-300V, and the negative electrode rotating speed is controlled to be 20-100r/min, deposition 10-60min, stop heating after water heat electrophoresis deposition is finished, treat to take out the carbon/carbon compound material that deposits yttrium silicate after water heating kettle is cooled to room temperature;
4) last, the carbon/carbon compound material that deposits yttrium silicate with distilled water wash is placed on the dry yttrium silicate (Y that obtains in 60-100 ℃ the loft drier
2Si
2O
7) carbon/carbon compound material that applies of coating.
The present invention adopts negative electrode rotation water heat electrophoresis deposition method at carbon/anti-oxidant external coating (EC) of carbon fiber reinforced silicon carbide matrix composite surface preparation yttrium silicate, utilize the yttrium silicate powder to be raw material, according to certain powder proportioning, under certain temperature and voltage, different negative electrode speed of rotation can be prepared iridium silicate coating layer compact structure, that have micro-flaw, different thickness respectively.The advantage of this method is that technology controlling and process is simple, and coating is even, avoids repetitive operation to a certain extent, can be used for surperficial complex product, and can obtain controllable structure and well behaved iridium silicate coating layer at low temperatures.
Description of drawings
Fig. 1 is the sem photograph of the coating section of the embodiment of the invention 1 preparation.
Embodiment
Embodiment 1: at first, select 5 microns analytically pure yttrium silicate (Y for use
2Si
2O
7) powder, analytically pure Virahol and iodine is starting material, according to Y
2Si
2O
7: the ratio of Virahol=2.5g: 150ml is mixed with suspension, under 1500r/min behind the mechanical stirring 8h, after introducing iodine stir 12h in suspension in the ratio of 0.5g/L, places ultrasonic wave standby behind vibration 60min under the power of 500W; Secondly, above-mentioned suspension being added in the water heat electrophoresis deposition reactor, is anode with the Graphite Electrodes, with depositing in advance of can rotating the carbon/carbon compound material of 100 micron thickness SiC coatings be negative electrode; Then, after the carbon/carbon compound material of having treated to deposit in advance 50-100 micron thickness SiC coating is fixed in negative electrode, sealing water heat electrophoresis deposition reactor, simultaneously the water heat electrophoresis deposition reactor is heated to 220 ℃, the control deposition voltage is 300V, and the negative electrode rotating speed is controlled to be 20r/min, deposition 60min, stop heating after water heat electrophoresis deposition is finished, treat to take out the carbon/carbon compound material that deposits yttrium silicate after water heating kettle is cooled to room temperature; At last, the carbon/carbon compound material that deposits yttrium silicate with distilled water wash is placed on the dry yttrium silicate (Y that obtains in 100 ℃ the loft drier
2Si
2O
7) carbon/carbon compound material that applies of coating.Obtain yttrium silicate (Y as shown in Figure 1
2Si
2O
7) carbon/carbon compound material that applies of coating.As can be seen from Figure 1, thick about 100 microns of yttrium silicate external coating (EC), compact and uniform structure combines well with undercoat.
Embodiment 2: at first, select 0.05 micron analytically pure yttrium silicate (Y for use
2Si
2O
7) powder, analytically pure Virahol and iodine is starting material, according to Y
2Si
2O
7: the ratio of Virahol=5g: 150ml is mixed with suspension, under 2000r/min behind the mechanical stirring 12h, after introducing iodine stir 10h in suspension in the ratio of 1.5g/L, places ultrasonic wave standby behind vibration 10min under the power of 100W; Secondly, above-mentioned suspension being added in the water heat electrophoresis deposition reactor, is anode with the Graphite Electrodes, with depositing in advance of can rotating the carbon/carbon compound material of 50 micron thickness SiC coatings be negative electrode; Then, after the carbon/carbon compound material of having treated to deposit in advance 50-100 micron thickness SiC coating is fixed in negative electrode, sealing water heat electrophoresis deposition reactor, simultaneously the water heat electrophoresis deposition reactor is heated to 100 ℃, the control deposition voltage is 50V, and the negative electrode rotating speed is controlled to be 100r/min, deposition 10min, stop heating after water heat electrophoresis deposition is finished, treat to take out the carbon/carbon compound material that deposits yttrium silicate after water heating kettle is cooled to room temperature; At last, the carbon/carbon compound material that deposits yttrium silicate with distilled water wash is placed on the dry yttrium silicate (Y that obtains in 60 ℃ the loft drier
2Si
2O
7) carbon/carbon compound material that applies of coating.
Embodiment 3: at first, select 0.5 micron analytically pure yttrium silicate (Y for use
2Si
2O
7) powder, analytically pure Virahol and iodine is starting material, according to Y
2Si
2O
7: the ratio of Virahol=4g: 150ml is mixed with suspension, under 1000r/min behind the mechanical stirring 10h, after introducing iodine stir 8h in suspension in the ratio of 1g/L, places ultrasonic wave standby behind vibration 30min under the power of 300W; Secondly, above-mentioned suspension being added in the water heat electrophoresis deposition reactor, is anode with the Graphite Electrodes, with depositing in advance of can rotating the carbon/carbon compound material of 80 micron thickness SiC coatings be negative electrode; Then, after the carbon/carbon compound material of having treated to deposit in advance 50-100 micron thickness SiC coating is fixed in negative electrode, sealing water heat electrophoresis deposition reactor, simultaneously the water heat electrophoresis deposition reactor is heated to 300 ℃, the control deposition voltage is 200V, and the negative electrode rotating speed is controlled to be 60r/min, deposition 40min, stop heating after water heat electrophoresis deposition is finished, treat to take out the carbon/carbon compound material that deposits yttrium silicate after water heating kettle is cooled to room temperature; At last, the carbon/carbon compound material that deposits yttrium silicate with distilled water wash is placed on the dry yttrium silicate (Y that obtains in 80 ℃ the loft drier
2Si
2O
7) carbon/carbon compound material that applies of coating.
The iridium silicate coating layer that the present invention can prepare under relatively low temperature with matrix bond is good, antioxidant property is high, coat-thickness is controlled; avoided the sedimentary repetitive operation coatings prepared of conventional electrophoretic at high temperature effectively to protect simultaneously to carbon/carbon compound material, at the oxidation weight loss of oxidation sample after 200 hours under 1600 ℃ the high temperature less than 0.5%.
Claims (1)
1. the method for a preparing yttrium silicate coat by cathode rotation hydrothermal electrophoretic deposition is characterized in that:
1) at first, selects the analytically pure yttrium silicate (Y of 0.05-5 micron for use
2Si
2O
7) powder, analytically pure Virahol and iodine is starting material, according to Y
2Si
2O
7: the ratio of Virahol=2.5-5g: 150ml is mixed with suspension, under 1000-2000r/min behind the mechanical stirring 8-12h, after in suspension, introducing iodine and stir 8-12h in the ratio of 0.5-1.5g/L, place ultrasonic wave standby behind vibration 10-60min under the power of 100-500W;
2) secondly, above-mentioned suspension being added in the water heat electrophoresis deposition reactor, is anode with the Graphite Electrodes, with depositing in advance of can rotating the carbon/carbon compound material of 50-100 micron thickness SiC coating be negative electrode;
3) then, after the carbon/carbon compound material of having treated to deposit in advance 50-100 micron thickness SiC coating is fixed in negative electrode, sealing water heat electrophoresis deposition reactor, simultaneously the water heat electrophoresis deposition reactor is heated to 100-300 ℃, the control deposition voltage is 50-300V, and the negative electrode rotating speed is controlled to be 20-100r/min, deposition 10-60min, stop heating after water heat electrophoresis deposition is finished, treat to take out the carbon/carbon compound material that deposits yttrium silicate after water heating kettle is cooled to room temperature;
4) last, the carbon/carbon compound material that deposits yttrium silicate with distilled water wash is placed on the dry yttrium silicate (Y that obtains in 60-100 ℃ the loft drier
2Si
2O
7) carbon/carbon compound material that applies of coating.
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|---|---|---|---|
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| CN101514473B true CN101514473B (en) | 2010-12-29 |
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| CN106495745B (en) * | 2016-09-28 | 2019-04-09 | 陕西科技大学 | A kind of preparation method of the crystal whisker toughened yttrium silicate of β-yttrium silicate/YAS coating |
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Assignee: Morgan Special Ceramic Technology Co., Ltd. Assignor: Shaanxi University of Science and Technology Contract record no.: 2011320010060 Denomination of invention: Method for preparing yttrium silicate coat by cathode rotation hydrothermal electrophoretic deposition Granted publication date: 20101229 License type: Exclusive License Open date: 20090826 Record date: 20110617 |
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