CN100577892C - Water heat electrophoresis deposition method of gradient iridium silicate coating layer - Google Patents

Water heat electrophoresis deposition method of gradient iridium silicate coating layer Download PDF

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CN100577892C
CN100577892C CN200610043155A CN200610043155A CN100577892C CN 100577892 C CN100577892 C CN 100577892C CN 200610043155 A CN200610043155 A CN 200610043155A CN 200610043155 A CN200610043155 A CN 200610043155A CN 100577892 C CN100577892 C CN 100577892C
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CN1904144A (en
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黄剑锋
邓飞
曹丽云
李贺军
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Abstract

This invention relates to a kind of water-thermo electrophoresis deposition process which use gradient silicic acid yttrium smear layer. This process applies wet chemistry method to synthesize gradient component and three kinds of expected crystal phase structure silicic acid yttrium micropower, then dispersing them in liquid medium, applying water-thermo electrophoresis deposition process in low temperature to gain satisfactory gradient silicic acid yttrium smear layer, solving the problem of heat injury of basis body in the process. The feature is: cohering strength of smear layer and basis body exceed 28MPa; excellent antioxygen performance; valid protection to carbon material at 1600 DEG C can last 260hours; oxidizing weight loss is below 2%.

Description

A kind of water heat electrophoresis deposition method of gradient iridium silicate coating layer
Technical field
The present invention relates to a kind of preparation method of iridium silicate coating layer, particularly a kind of water heat electrophoresis deposition method of gradient iridium silicate coating layer.
Background technology
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 ideal 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.The further investigation of yttrium silicate high-temperature oxidation resistant coating material is used more widely at aerospace, military affairs and numerous areas such as civilian for structured material prerequisite and guarantee is provided.
The technology of preparing of present reported iridium silicate coating layer mainly contains hot isostatic pressing method, slip coating-sintering process, plasma spraying method and original position forming method etc.Hot isostatic pressing method is to be coated in matrix surface after original powder is mixed, and obtains coatings prepared by regulating processing parameters such as required atmosphere, pressure, temperature in hot isostatic press.As Ogura Y etc. (Ogura Y, Kondo M, and Mormoto T.Proceedings of theTenth International Conference on Composite Materials, Canada is 1995.767-774) with Y 2O 3, SiO 2Deng being raw material, adopt first hot isostatic pressing method in the C/C-SiC surface preparation Y 2SiO 5External coating (EC).Adopt this method can make material be subjected to the pressure that all directions equate, be expected to finally obtain the coating of high compaction.It is with Y that slip coating-sintering process prepares iridium silicate coating layer 2O 3And SiO 2And fusing assistant etc. is mixed with and is mixed and made into slip with solvent (as ethanol) etc. after meeting necessarily required powder, add suitable dispersion agent and binding agent again, after fully stirring, brush in the surface of matrix or with the matrix direct impregnation and in slip, form coating, oven dry is at a certain temperature heat-treated under the high temperature inert atmosphere the most finally and is promptly got coating afterwards.As Webster J D etc. (Webster J D, Westwood M E, Hayes H.Journal ofthe European Ceramic Society, 1998,18:2345-2350) with the tetramethylammonium hydroxide be dispersion agent, in water with Y 2O 3And SiO 2Be formulated as slip, again the C/C-SiC matrix is immersed in the slip form coating and oven dry after, under argon shield, finally obtain Y in 1600 ℃ of sintering 3h 2SiO 5And Y 2SiO 5/ Y 2Si 2O 7Two kinds of external coating (EC)s (thickness 100 μ m).This method technology is comparatively simple, and the thickness of coating is more easy to control.Weak point is that the homogeneity of coating is wayward, and compactness difficulty reaches requirement.It is with the ion bombardment solid yttrium silicate surface of quickening that sputtering method prepares iridium silicate coating layer, and ion and solid surface atom exchange momentum deposit to matrix surface after making the atom of solid surface leave solid.As (Sekigawa T such as Sekigawa T, Takeda F, and Taguchi M.Proceedings of the 8th Symposium onPerformance Materials for severe Environments, Tokyo, 1997.307) adopt sputtering method in the C/C-SiC surface preparation Y 2SiO 5Coating (thickness 100 μ m).In addition, owing to plasma can produce high temperature, plasma jet can be heated to molten state with the raw material for preparing, and makes it to quicken to spray to matrix surface and form coating.As (Huang J F such as Huang J F, Li H J, and Zeng X R.Carbon, 2004,42 (11):, adopt plasma spraying method to prepare Y in the research of C/C-SiC matrix surface 2356-2359) by rationally adjusting the proportioning and the parameters Optimization of powder 4Si 3O 12/ Y 2Si 2O 7/ Y 2SiO 5And Y 4Si 3O 12/ Y 2Si 2O 7/ Y 2SiO 5/ glass coating.The original position forming method is the method for a kind of in-situ preparing silicate coating of Huang Jianfeng etc. (Huang Jianfeng, Li Hejun, once mediate banyan .CN Patent, ZL200410029115.X, 2004) research and development design.Its ultimate principle is by mixing elemental silicon and good metal oxide compound wetting with it, being coated in advance, preparation has the internally coated specimen surface of SiC, preoxidation for some time under certain temperature and oxidizing atmosphere, then can original position generate that antioxidant property is good, oxygen permeability is low, resistant to elevated temperatures silicate external coating (EC).This method requires the enough densifications of SiC undercoat, can effectively protect in preoxidation process matrix.The common feature of aforesaid method is all to need at high temperature just can prepare more satisfactory iridium silicate coating layer, and higher preparation temperature may cause certain damage to matrix.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, provide a kind of not only technology controlling and process simple, coating is evenly fine and close, the product that can be used for the surface tissue complexity, and can obtain the water heat electrophoresis deposition method of the gradient iridium silicate coating layer of controllable structure and well behaved iridium silicate coating layer at low temperatures.
For achieving the above object, the technical solution used in the present invention is:
1) Y 4Si 3O 12The preparation of coating
1.1 according to Y 4Si 3O 12Powder: the ratio formulated suspension of Virahol=0.5～5g: 100ml; Under 1000～2000r/min, behind mechanical stirring 6～12h, in this suspension, introduce iodine, place the ultrasonic wave container 15～60min that under 100～500W power, vibrates, continue to stir behind 24～36h suspension stand-by by the suspension of 0.5～2g: 100ml;
1.2 with Y 4Si 3O 12Suspension join in the water heating kettle that has electrode, with the conducting base is negative electrode, the control hydrothermal temperature is that 80～200 ℃, deposition voltage are that 50～300V, depositing time are that 5～60min carries out water heat electrophoresis deposition, and deposition is finished and treated to take out sample after water heating kettle is cooled to room temperature;
1.3 promptly finish matrix Y after sample being placed 50～80 ℃ the dry 30～60min of loft drier 4Si 3O 12The preparation of coating;
2) Y 4Si 3O 12/ Y 2Si 2O 7The preparation of gradient cladding
2.1 according to Y 2Si 2O 7Powder: the ratio formulated suspension of Virahol=0.5～5g: 100ml; Under 1000～2000r/min, behind mechanical stirring 6～12h, in this suspension, introduce iodine, place the ultrasonic wave container 15～60min that under 100～500W power, vibrates, continue to stir behind 24～36h suspension stand-by by the suspension of 0.5～2g: 100ml;
2.2 with Y 2Si 2O 7Suspension join in the water heating kettle that has electrode, and to deposit Y 4Si 3O 12The coating sample be negative electrode, the control hydrothermal temperature is that 80～200 ℃, deposition voltage are that 50～300V, depositing time are that 5～60min carries out water heat electrophoresis deposition, deposition is finished and is treated to take out sample after water heating kettle is cooled to room temperature;
2.3 promptly finish Y after sample being placed 50～80 ℃ the dry 30～60min of loft drier 4Si 3O 12/ Y 2Si 2O 7The preparation of coating;
3) Y 4Si 3O 12/ Y 2Si 2O 7/ Y 2SiO 5The preparation of gradient cladding
3.1 according to Y 2SiO 5Powder: the ratio formulated suspension of Virahol=0.5～5g: 100ml; Under 1000～2000r/min, behind mechanical stirring 6～12h, in this suspension, introduce iodine, place the ultrasonic wave container 15～60min that under 100～500W power, vibrates, continue to stir behind 24～36h suspension stand-by by the suspension of 0.5～2g: 100ml;
3.2 with Y 2SiO 5Suspension join in the water heating kettle that has electrode, and to deposit Y 4Si 3O 12/ Y 2Si 2O 7The coating sample is a negative electrode, and the control hydrothermal temperature is that 80～200 ℃, deposition voltage are that 50～300V, depositing time are that 5～60min carries out water heat electrophoresis deposition, and deposition is finished and treated to take out sample after water heating kettle is cooled to room temperature;
3.3 after sample being placed 50～80 ℃ the dry 30～60min of loft drier, finally can obtain Y 4Si 3O 12/ Y 2Si 2O 7/ Y 2SiO 5The coating of gradient.
Conducting base of the present invention is C/C, SiC, titanium or metal alloy.
Y of the present invention 4Si 3O 12Powder is synthetic by following technology
1) according to Y: Si=2: 3 mol ratio is mixed in the yttrium nitrate aqueous solution of 1.25mol/L and the sodium silicate aqueous solution of 1.87mol/L in the same container; Mechanical stirring 10～30min is placed on the 10～60min that vibrates in the ultrasonic wave container of ultrasonic power 0＜P≤500W under 1000～2000r/min;
2) get with 1) in the concentration of same amount be the aqueous sodium hydroxide solution of the yttrium nitrate aqueous solution of 1.25mol/L and 3.75mol/L by 1: 3 mixed in molar ratio in same container, mechanical stirring 10～30min is placed on the 10～60min that vibrates in the ultrasonic wave container of ultrasonic power 0＜P≤500W under 1000～2000r/min;
3) with above-mentioned 1) and 2) vibration after have sedimentary liquid mixing in same container, mechanical stirring 10～90min is placed on the 10～60min that vibrates in the ultrasonic wave container of ultrasonic power 0＜P≤500W under 1000～2000r/min, filter after the vibration, the distilled water wash precipitation is placed in the loft drier at 50～100 ℃ of drying 30～90min for 3～5 times;
4) speed muller with 5000～10000r/min obtains powder to dried throw out grinding 1～3h, powder after grinding is mixed with the mass ratio of dehydrated alcohol by 1: 10, and the lithium fluoride of the quality 2～6% of adding grinding back powder, mechanical stirring 10～30min is placed on the 10～20min that vibrates in the ultrasonic wave container under 1000～2000r/min; Dry 30～60min in the baking oven that is placed on 40～60 ℃ is finished in vibration;
5) dried powder is moved into corundum crucible and places High Temperature Furnaces Heating Apparatus, be incubated 1～4h after rising to 800～1200 ℃ with 2～6 ℃/min to cool to room temperature with the furnace, take out crucible, promptly get Y 4Si 3O 12Powder.
Y of the present invention 2Si 2O 7Powder is synthetic by following technology
1) according to Y: Si=2: 3 mol ratio is got the yttrium nitrate aqueous solution of 2.5mol/L and the sodium silicate aqueous solution of 3.75mol/L is mixed in the same container, and mechanical stirring 10～30min is placed on the 10～60min that vibrates in the ultrasonic wave container of ultrasonic power 0＜P≤500W under 1000～2000r/min;
2) get 1) in the concentration of 0.5 times of amount be the aqueous sodium hydroxide solution of the yttrium nitrate aqueous solution of 1.25mol/L and 3.75mol/L by 1: 3 mixed in molar ratio in same container, mechanical stirring 10～30min is placed on the 10～60min that vibrates in the ultrasonic wave container of ultrasonic power 0＜P≤500W under 1000～2000r/min;
3) with above-mentioned 1) and 2) vibration after have sedimentary liquid mixing in same container, mechanical stirring 10～90min is placed on the 10～60min that vibrates in the ultrasonic wave container of ultrasonic power 0＜P≤500W under 1000～2000r/min, filter after the vibration, the distilled water wash precipitation is placed in the loft drier at 50～100 ℃ of drying 30～90min for 3～5 times;
4) speed muller with 5000～10000r/min obtains powder to dried throw out grinding 1～3h, powder after grinding is mixed with the mass ratio of dehydrated alcohol by 1: 10, and the lithium fluoride of the quality 2～6% of adding grinding back powder, mechanical stirring 10～30min is placed on the 10～20min that vibrates in the ultrasonic wave container under 1000～2000r/min; Dry 30～60min in the baking oven that is placed on 40～60 ℃ is finished in vibration;
5) dried powder is moved into corundum crucible and places High Temperature Furnaces Heating Apparatus, cool to room temperature with the furnace after being incubated 1～4h after rising to 800～1200 ℃ with 2～6 ℃/min, take out crucible, promptly get Y 2Si 2O 7Powder.
Y of the present invention 2SiO 5Powder is synthetic by following technology
1) according to Y: Si=2: 3 mol ratio is got the yttrium nitrate aqueous solution of 1.25mol/L and the sodium silicate aqueous solution of 1.87mol/L is mixed in the same container, and mechanical stirring 10～30min is placed on the 10～60min that vibrates in the ultrasonic wave container of ultrasonic power 0＜P≤500W under 1000～2000r/min;
2) get 1) in the concentration of 2 times of amounts be the aqueous sodium hydroxide solution of the yttrium nitrate aqueous solution of 2.5mol/L and 7.5mol/L by 1: 3 mixed in molar ratio in same container, mechanical stirring 10～30min is placed on the 10～60min that vibrates in the ultrasonic wave container of ultrasonic power 0＜P≤500W under 1000～2000r/min;
3) with above-mentioned 1) and 2) vibration after have sedimentary liquid mixing in same container, mechanical stirring 10～90min is placed on the 10～60min that vibrates in the ultrasonic wave container of ultrasonic power 0＜P≤500W under 1000～2000r/min, filter after the vibration, the distilled water wash precipitation is placed in the loft drier at 50～100 ℃ of drying 30～90min for 3～5 times;
4) speed muller with 5000～10000r/min obtains powder to dried throw out grinding 1～3h, powder after grinding is mixed with the mass ratio of dehydrated alcohol by 1: 10, and the lithium fluoride of the quality 2～6% of adding grinding back powder, mechanical stirring 10～30min is placed on the 10～20min that vibrates in the ultrasonic wave container under 1000～2000r/min; Dry 30～60min in the baking oven that is placed on 40～60 ℃ is finished in vibration;
5) dried powder is moved into corundum crucible and places High Temperature Furnaces Heating Apparatus, cool to room temperature with the furnace after being incubated 1～4h after rising to 800～1200 ℃ with 2～6 ℃/min, take out crucible, promptly get Y 2SiO 5Powder.
The present invention adopts the wet chemistry method composition gradient to become to be grouped into and expects three kinds of yttrium silicate superfine powders of crystal phase structure, afterwards it is scattered in the liquid medium, adopt the water heat electrophoresis deposition method good gradient iridium silicate coating layer of obtained performance easily at low temperatures, solved the thermal damage problem of matrix in the coating preparation process simultaneously effectively.Coatings prepared and matrix bond mortise intensity are greater than 28MPa, and the antioxidant property excellence can effectively be protected the raw material of wood-charcoal material to reach 260 hours under 1600 ℃ oxidizing atmosphere, and oxidation weight loss is less than 2%.Operation is simple for the inventive method, is particularly useful for the matrix of surface tissue complexity.
Embodiment
Embodiment 1: step 1: yttrium silicate superfine powder synthetic
1, Y 4Si 3O 12Synthesizing of superfine powder
1.1 according to Y: Si=2: 3 mol ratio is mixed in the yttrium nitrate aqueous solution of 1.25mol/L and the sodium silicate aqueous solution of 1.87mol/L in the same container; Mechanical stirring 10min is placed on the 10min that vibrates in the ultrasonic wave container of 100W under 1000r/min;
1.2 get with 1.1 in the concentration of same amount be the aqueous sodium hydroxide solution of the yttrium nitrate aqueous solution of 1.25mol/L and 3.75mol/L by 1: 3 mixed in molar ratio in same container, mechanical stirring 10min is placed on the 10min that vibrates in the ultrasonic wave container of 100W under 1000r/min;
1.3 will have sedimentary liquid mixing in same container after above-mentioned 1.1 and 1.2 vibrations, mechanical stirring 10min is placed on the 10min that vibrates in the ultrasonic wave container of 100W under 1000r/min, filter after the vibration, the distilled water wash precipitation is placed in the loft drier at 50 ℃ of dry 30min for 3 times;
1.4 the speed muller with 5000r/min obtains powder to dried throw out grinding 1h, powder after grinding is mixed with the mass ratio of dehydrated alcohol by 1: 10, and the lithium fluoride of the quality 2% of adding grinding back powder, mechanical stirring 10min is placed on the 10min that vibrates in the ultrasonic wave container under 1000r/min; Dry 30min in the baking oven that is placed on 40 ℃ is finished in vibration;
1.5 dried powder is moved into corundum crucible and places High Temperature Furnaces Heating Apparatus, rise to 800 ℃ with 2 ℃/min after insulation 1h cool to room temperature with the furnace, take out crucible, promptly get Y 4Si 3O 12Powder;
2.Y 2Si 2O 7Synthesizing of superfine powder
2.1 according to Y: Si=2: 3 mol ratio is got the yttrium nitrate aqueous solution of 2.5mol/L and the sodium silicate aqueous solution of 3.75mol/L is mixed in the same container, and mechanical stirring 10min is placed on the 10min that vibrates in the ultrasonic wave container of 100W under 1000r/min;
2.2 the concentration of getting in 2.1 0.5 times be the aqueous sodium hydroxide solution of the yttrium nitrate aqueous solution of 1.25mol/L and 3.75mol/L by 1: 3 mixed in molar ratio in same container, mechanical stirring 10min is placed on the 10min that vibrates in the ultrasonic wave container of 100W under 1000r/min;
2.3 will have sedimentary liquid mixing in same container after above-mentioned 2.1 and 2.2 vibrations, mechanical stirring 10min is placed on the 10min that vibrates in the ultrasonic wave container of 100W under 1000r/min, filter after the vibration, the distilled water wash precipitation is placed in the loft drier at 50 ℃ of dry 30min for 3 times;
2.4 the speed muller with 5000r/min obtains powder to dried throw out grinding 1h, powder after grinding is mixed with the mass ratio of dehydrated alcohol by 1: 10, and the lithium fluoride of the quality 2% of adding grinding back powder, mechanical stirring 10min is placed on the 10min that vibrates in the ultrasonic wave container under 1000r/min; Dry 30min in the baking oven that is placed on 40 ℃ is finished in vibration;
2.5 dried powder is moved into corundum crucible and places High Temperature Furnaces Heating Apparatus, cool to room temperature with the furnace behind the insulation 1h after rising to 800 ℃ with 2 ℃/min, take out crucible, promptly get Y 2Si 2O 7Powder;
3.Y 2SiO 5Synthesizing of superfine powder
3.1 according to Y: Si=2: 3 mol ratio is got the yttrium nitrate aqueous solution of 1.25mol/L and the sodium silicate aqueous solution of 1.87mol/L is mixed in the same container, and mechanical stirring 10min is placed on the 10min that vibrates in the ultrasonic wave container of 100W under 1000r/min;
3.2 the concentration of getting in 3.1 2 times be the aqueous sodium hydroxide solution of the yttrium nitrate aqueous solution of 2.5mol/L and 7.5mol/L by 1: 3 mixed in molar ratio in same container, mechanical stirring 10min is placed on the 10min that vibrates in the ultrasonic wave container of 100W under 1000r/min;
3.3 will have sedimentary liquid mixing in same container after above-mentioned 3.1 and 3.2 vibrations, mechanical stirring 10min is placed on the 10min that vibrates in the ultrasonic wave container of 100W under 1000r/min, filter after the vibration, the distilled water wash precipitation is placed in the loft drier at 50 ℃ of dry 30min for 3 times;
3.4 the speed muller with 5000r/min obtains powder to dried throw out grinding 1h, powder after grinding is mixed with the mass ratio of dehydrated alcohol by 1: 10, and the lithium fluoride of the quality 2% of adding grinding back powder, mechanical stirring 10min is placed on the 10min that vibrates in the ultrasonic wave container under 1000r/min; Dry 30min in the baking oven that is placed on 40 ℃ is finished in vibration;
3.5 dried powder is moved into corundum crucible and places High Temperature Furnaces Heating Apparatus, cool to room temperature with the furnace behind the insulation 1h after rising to 800 ℃ with 2 ℃/min, take out crucible, promptly get Y 2SiO 5Powder;
Step 2: water heat electrophoresis deposition prepares gradient iridium silicate coating layer
1.Y 4Si 3O 12The preparation of coating
1.1 according to Y 4Si 3O 12The ratio formulated suspension of powder: Virahol=0.5g: 100ml; Under 1000r/min, behind the mechanical stirring 6h, in this suspension, introduce iodine, place the ultrasonic wave container 15min that under 100W power, vibrates, continue to stir behind the 24h suspension stand-by by the suspension of 0.5g: 100ml;
1.2 with Y 4Si 3O 12Suspension join in the water heating kettle that has electrode, with conducting base (C/C, SiC, titanium or metal alloy) is negative electrode, the control hydrothermal temperature is that 80 ℃, deposition voltage are that 50V, depositing time are that 5min carries out water heat electrophoresis deposition, and deposition is finished and treated to take out sample after water heating kettle is cooled to room temperature;
1.3 promptly finish matrix Y after sample being placed 50 ℃ the dry 30min of loft drier 4Si 3O 12The preparation of coating;
2.Y 4Si 3O 12/ Y 2Si 2O 7The preparation of gradient cladding
2.1 according to Y 2Si 2O 7The ratio formulated suspension of powder: Virahol=0.5g: 100ml; Under 1000r/min, behind the mechanical stirring 6h, in this suspension, introduce iodine, place the ultrasonic wave container 15min that under 100W power, vibrates, continue to stir behind the 24h suspension stand-by by the suspension of 0.5g: 100ml;
2.2 with Y 2Si 2O 7Suspension join in the water heating kettle that has electrode, and to deposit Y 4Si 3O 12The coating style be negative electrode, the control hydrothermal temperature is that 80 ℃, deposition voltage are that 50V, depositing time are that 5min carries out water heat electrophoresis deposition, deposition is finished and is treated to take out sample after water heating kettle is cooled to room temperature;
2.3 promptly finish Y after sample being placed 50 ℃ the dry 30min of loft drier 4Si 3O 12/ Y 2Si 2O 7The preparation of coating;
3.Y 4Si 3O 12/ Y 2Si 2O 7/ Y 2SiO 5The preparation of gradient cladding
3.1 according to Y 2SiO 5The ratio formulated suspension of powder: Virahol=0.5g: 100ml; Under 1000r/min, behind the mechanical stirring 6h, in this suspension, introduce iodine, place the ultrasonic wave container 15min that under 100～500W power, vibrates, continue to stir behind the 24h suspension stand-by by the suspension of 0.5～2g: 100ml;
3.2 with Y 2SiO 5Suspension join in the water heating kettle that has electrode, and to deposit Y 4Si 3O 12/ Y 2Si 2O 7The coating style is a negative electrode, and the control hydrothermal temperature is that 80 ℃, deposition voltage are that 50V, depositing time are that 5min carries out water heat electrophoresis deposition, and deposition is finished and treated to take out sample after water heating kettle is cooled to room temperature;
3.3 after sample being placed 50 ℃ the dry 30min of loft drier, finally can obtain Y 4Si 3O 12/ Y 2Si 2O 7/ Y 2SiO 5The coating of gradient.
Embodiment 2
Step 1: yttrium silicate superfine powder synthetic
1, Y 4Si 3O 12Synthesizing of superfine powder
1.1 according to Y: Si=2: 3 mol ratio is mixed in the yttrium nitrate aqueous solution of 1.25mol/L and the sodium silicate aqueous solution of 1.87mol/L in the same container; Mechanical stirring 30min is placed on the 60min that vibrates in the ultrasonic wave container of 500W under 2000r/min;
1.2 get with 1.1 in the concentration of same amount be the aqueous sodium hydroxide solution of the yttrium nitrate aqueous solution of 1.25mol/L and 3.75mol/L by 1: 3 mixed in molar ratio in same container, mechanical stirring 30min is placed on the 60min that vibrates in the ultrasonic wave container of 500W under 2000r/min;
1.3 will have sedimentary liquid mixing in same container after above-mentioned 1.1 and 1.2 vibrations, mechanical stirring 90min is placed on the 60min that vibrates in the ultrasonic wave container of 500W under 2000r/min, filter after the vibration, the distilled water wash precipitation is placed in the loft drier at 100 ℃ of dry 90min for 5 times;
1.4 the speed muller with 10000r/min obtains powder to dried throw out grinding 3h, powder after grinding is mixed with the mass ratio of dehydrated alcohol by 1: 10, and the lithium fluoride of the quality 6% of adding grinding back powder, mechanical stirring 30min is placed on the 20min that vibrates in the ultrasonic wave container under 2000r/min; Dry 60min in the baking oven that is placed on 60 ℃ is finished in vibration;
1.5 dried powder is moved into corundum crucible and places High Temperature Furnaces Heating Apparatus, rise to 1200 ℃ with 6 ℃/min after insulation 4h cool to room temperature with the furnace, take out crucible, promptly get Y 4Si 3O 12Powder;
2.Y 2Si 2O 7Synthesizing of superfine powder
2.1 according to Y: Si=2: 3 mol ratio is got the yttrium nitrate aqueous solution of 2.5mol/L and the sodium silicate aqueous solution of 3.75mol/L is mixed in the same container, and mechanical stirring 30min is placed on the 60min that vibrates in the ultrasonic wave container of 500W under 2000r/min;
2.2 the concentration of getting in 2.1 0.5 times be the aqueous sodium hydroxide solution of the yttrium nitrate aqueous solution of 1.25mol/L and 3.75mol/L by 1: 3 mixed in molar ratio in same container, mechanical stirring 30min is placed on the 60min that vibrates in the ultrasonic wave container of 500W under 2000r/min;
2.3 will have sedimentary liquid mixing in same container after above-mentioned 2.1 and 2.2 vibrations, mechanical stirring 90min is placed on the 60min that vibrates in the ultrasonic wave container of 500W under 2000r/min, filter after the vibration, the distilled water wash precipitation is placed in the loft drier at 100 ℃ of dry 90min for 5 times;
2.4 the speed muller with 10000r/min obtains powder to dried throw out grinding 3h, powder after grinding is mixed with the mass ratio of dehydrated alcohol by 1: 10, and the lithium fluoride of the quality 6% of adding grinding back powder, mechanical stirring 30min is placed on the 20min that vibrates in the ultrasonic wave container under 2000r/min; Dry 60min in the baking oven that is placed on 60 ℃ is finished in vibration;
2.5 dried powder is moved into corundum crucible and places High Temperature Furnaces Heating Apparatus, cool to room temperature with the furnace behind the insulation 4h after rising to 1200 ℃ with 6 ℃/min, take out crucible, promptly get Y 2Si 2O 7Powder;
3.Y 2SiO 5Synthesizing of superfine powder
3.1 according to Y: Si=2: 3 mol ratio is got the yttrium nitrate aqueous solution of 1.25mol/L and the sodium silicate aqueous solution of 1.87mol/L is mixed in the same container, and mechanical stirring 30min is placed on the 60min that vibrates in the ultrasonic wave container of 500W under 2000r/min;
3.2 the concentration of getting in 3.1 2 times be the aqueous sodium hydroxide solution of the yttrium nitrate aqueous solution of 2.5mol/L and 7.5mol/L by 1: 3 mixed in molar ratio in same container, mechanical stirring 30min is placed on the 60min that vibrates in the ultrasonic wave container of 500W under 2000r/min;
3.3 will have sedimentary liquid mixing in same container after above-mentioned 3.1 and 3.2 vibrations, mechanical stirring 90min is placed on the 60min that vibrates in the ultrasonic wave container of 500W under 2000r/min, filter after the vibration, the distilled water wash precipitation is placed in the loft drier at 100 ℃ of dry 90min for 5 times;
3.4 the speed muller with 5000～10000r/min obtains powder to dried throw out grinding 3h, powder after grinding is mixed with the mass ratio of dehydrated alcohol by 1: 10, and the lithium fluoride of the quality 6% of adding grinding back powder, mechanical stirring 30min is placed on the 20min that vibrates in the ultrasonic wave container under 2000r/min; Dry 60min in the baking oven that is placed on 60 ℃ is finished in vibration;
3.5 dried powder is moved into corundum crucible and places High Temperature Furnaces Heating Apparatus, cool to room temperature with the furnace behind the insulation 4h after rising to 1200 ℃ with 6 ℃/min, take out crucible, promptly get Y 2SiO 5Powder;
Step 2: water heat electrophoresis deposition prepares gradient iridium silicate coating layer
1.Y 4Si 3O 12The preparation of coating
1.1 according to Y 4Si 3O 12The ratio formulated suspension of powder: Virahol=5g: 100ml; Under 2000r/min, behind the mechanical stirring 12h, in this suspension, introduce iodine, place the ultrasonic wave container 60min that under 500W power, vibrates, continue to stir behind the 36h suspension stand-by by the suspension of 2g: 100ml;
1.2 with Y 4Si 3O 12Suspension join in the water heating kettle that has electrode, with conducting base (C/C, SiC, titanium or metal alloy) is negative electrode, the control hydrothermal temperature is that 200 ℃, deposition voltage are that 300V, depositing time are that 60min carries out water heat electrophoresis deposition, and deposition is finished and treated to take out sample after water heating kettle is cooled to room temperature;
1.3 promptly finish matrix Y after sample being placed 80 ℃ the dry 60min of loft drier 4Si 3O 12The preparation of coating;
2.Y 4Si 3O 12/ Y 2Si 2O 7The preparation of gradient cladding
2.1 according to Y 2Si 2O 7The ratio formulated suspension of powder: Virahol=5g: 100ml; Under 2000r/min, behind the mechanical stirring 12h, in this suspension, introduce iodine, place the ultrasonic wave container 60min that under 500W power, vibrates, continue to stir behind the 36h suspension stand-by by the suspension of 2g: 100ml;
2.2 with Y 2Si 2O 7Suspension join in the water heating kettle that has electrode, and to deposit Y 4Si 3O 12The coating style be negative electrode, the control hydrothermal temperature is that 200 ℃, deposition voltage are that 300V, depositing time are that 60min carries out water heat electrophoresis deposition, deposition is finished and is treated to take out sample after water heating kettle is cooled to room temperature;
2.3 promptly finish Y after sample being placed 80 ℃ the dry 60min of loft drier 4Si 3O 12/ Y 2Si 2O 7The preparation of coating;
3.Y 4Si 3O 12/ Y 2Si 2O 7/ Y 2SiO 5The preparation of gradient cladding
3.1 according to Y 2SiO 5The ratio formulated suspension of powder: Virahol=5g: 100ml; Under 2000r/min, behind the mechanical stirring 12h, in this suspension, introduce iodine, place the ultrasonic wave container 60min that under 500W power, vibrates, continue to stir behind the 36h suspension stand-by by the suspension of 2g: 100ml;
3.2 with Y 2SiO 5Suspension join in the water heating kettle that has electrode, and to deposit Y 4Si 3O 12/ Y 2Si 2O 7The coating style is a negative electrode, and the control hydrothermal temperature is that 200 ℃, deposition voltage are that 300V, depositing time are that 60min carries out water heat electrophoresis deposition, and deposition is finished and treated to take out sample after water heating kettle is cooled to room temperature;
3.3 after sample being placed 80 ℃ the dry 60min of loft drier, finally can obtain Y 4Si 3O 12/ Y 2Si 2O 7/ Y 2SiO 5The coating of gradient.
Embodiment 3
Step 1: yttrium silicate superfine powder synthetic
1, Y 4Si 3O 12Synthesizing of superfine powder
1.1 according to Y: Si=2: 3 mol ratio is mixed in the yttrium nitrate aqueous solution of 1.25mol/L and the sodium silicate aqueous solution of 1.87mol/L in the same container; Mechanical stirring 20min is placed on the 40min that vibrates in the ultrasonic wave container of 300W under 1500r/min;
1.2 get with 1.1 in the concentration of same amount be the aqueous sodium hydroxide solution of the yttrium nitrate aqueous solution of 1.25mol/L and 3.75mol/L by 1: 3 mixed in molar ratio in same container, mechanical stirring 20min is placed on the 40min that vibrates in the ultrasonic wave container of 300W under 1500r/min;
1.3 will have sedimentary liquid mixing in same container after above-mentioned 1.1 and 1.2 vibrations, mechanical stirring 50min is placed on the 30min that vibrates in the ultrasonic wave container of 300W under 1500r/min, filter after the vibration, the distilled water wash precipitation is placed in the loft drier at 80 ℃ of dry 60min for 4 times;
1.4 the speed muller with 8000r/min obtains powder to dried throw out grinding 2h, powder after grinding is mixed with the mass ratio of dehydrated alcohol by 1: 10, and the lithium fluoride of the quality 4% of adding grinding back powder, mechanical stirring 20min is placed on the 15min that vibrates in the ultrasonic wave container under 1500r/min; Dry 40min in the baking oven that is placed on 50 ℃ is finished in vibration;
1.5 dried powder is moved into corundum crucible and places High Temperature Furnaces Heating Apparatus, rise to 1000 ℃ with 4 ℃/min after insulation 2h cool to room temperature with the furnace, take out crucible, promptly get Y 4Si 3O 12Powder;
2.Y 2Si 2O 7Synthesizing of superfine powder
2.1 according to Y: Si=2: 3 mol ratio is got the yttrium nitrate aqueous solution of 2.5mol/L and the sodium silicate aqueous solution of 3.75mol/L is mixed in the same container, and mechanical stirring 20min is placed on the 30min that vibrates in the ultrasonic wave container of 300W under 1500r/min;
2.2 the concentration of getting in 2.1 0.5 times be the aqueous sodium hydroxide solution of the yttrium nitrate aqueous solution of 1.25mol/L and 3.75mol/L by 1: 3 mixed in molar ratio in same container, mechanical stirring 20min is placed on the 30min that vibrates in the ultrasonic wave container of 300W under 1500r/min;
2.3 will have sedimentary liquid mixing in same container after above-mentioned 2.1 and 2.2 vibrations, mechanical stirring 50min is placed on the 30min that vibrates in the ultrasonic wave container of 300W under 1500r/min, filter after the vibration, the distilled water wash precipitation is placed in the loft drier at 80 ℃ of dry 60min for 4 times;
2.4 the speed muller with 8000r/min obtains powder to dried throw out grinding 2h, powder after grinding is mixed with the mass ratio of dehydrated alcohol by 1: 10, and the lithium fluoride of the quality 4% of adding grinding back powder, mechanical stirring 20min is placed on the 15min that vibrates in the ultrasonic wave container under 1500r/min; Dry 40min in the baking oven that is placed on 50 ℃ is finished in vibration;
2.5 dried powder is moved into corundum crucible and places High Temperature Furnaces Heating Apparatus, cool to room temperature with the furnace behind the insulation 2h after rising to 1000 ℃ with 4 ℃/min, take out crucible, promptly get Y 2Si 2O 7Powder;
3.Y 2SiO 5Synthesizing of superfine powder
3.1 according to Y: Si=2: 3 mol ratio is got the yttrium nitrate aqueous solution of 1.25mol/L and the sodium silicate aqueous solution of 1.87mol/L is mixed in the same container, and mechanical stirring 20min is placed on the 30min that vibrates in the ultrasonic wave container of 300W under 1500r/min;
3.2 the concentration of getting in 3.1 2 times be the aqueous sodium hydroxide solution of the yttrium nitrate aqueous solution of 2.5mol/L and 7.5mol/L by 1: 3 mixed in molar ratio in same container, mechanical stirring 20min is placed on the 40min that vibrates in the ultrasonic wave container of 300W under 1500r/min;
3.3 will have sedimentary liquid mixing in same container after above-mentioned 3.1 and 3.2 vibrations, mechanical stirring 50min is placed on the 40min that vibrates in the ultrasonic wave container of 300W under 1500r/min, filter after the vibration, the distilled water wash precipitation is placed in the loft drier at 80 ℃ of dry 60min for 4 times;
3.4 the speed muller with 8000r/min obtains powder to dried throw out grinding 2h, powder after grinding is mixed with the mass ratio of dehydrated alcohol by 1: 10, and the lithium fluoride of the quality 4% of adding grinding back powder, mechanical stirring 20min is placed on the 15min that vibrates in the ultrasonic wave container under 1500r/min; Dry 40min in the baking oven that is placed on 50 ℃ is finished in vibration;
3.5 dried powder is moved into corundum crucible and places High Temperature Furnaces Heating Apparatus, cool to room temperature with the furnace behind the insulation 2h after rising to 1000 ℃ with 4 ℃/min, take out crucible, promptly get Y 2SiO 5Powder;
Step 2: water heat electrophoresis deposition prepares gradient iridium silicate coating layer
1.Y 4Si 3O 12The preparation of coating
1.1 according to Y 4Si 3O 12The ratio formulated suspension of powder: Virahol=3g: 100ml; Under 1500r/min, behind the mechanical stirring 9h, in this suspension, introduce iodine, place the ultrasonic wave container 40min that under 300W power, vibrates, continue to stir behind the 28h suspension stand-by by the suspension of 1g: 100ml;
1.2 with Y 4Si 3O 12Suspension join in the water heating kettle that has electrode, with conducting base (C/C, SiC, titanium or metal alloy) is negative electrode, the control hydrothermal temperature is that 150 ℃, deposition voltage are that 200V, depositing time are that 30min carries out water heat electrophoresis deposition, and deposition is finished and treated to take out sample after water heating kettle is cooled to room temperature;
1.3 promptly finish matrix Y after sample being placed 65 ℃ the dry 45min of loft drier 4Si 3O 12The preparation of coating;
2.Y 4Si 3O 12/ Y 2Si 2O 7The preparation of gradient cladding
2.1 according to Y 2Si 2O 7The ratio formulated suspension of powder: Virahol=3g: 100ml; Under 1500r/min, behind the mechanical stirring 9h, in this suspension, introduce iodine, place the ultrasonic wave container 40min that under 300W power, vibrates, continue to stir behind the 28h suspension stand-by by the suspension of 1g: 100ml;
2.2 with Y 2Si 2O 7Suspension join in the water heating kettle that has electrode, and to deposit Y 4Si 3O 12The coating style be negative electrode, the control hydrothermal temperature is that 150 ℃, deposition voltage are that 200V, depositing time are that 30min carries out water heat electrophoresis deposition, deposition is finished and is treated to take out sample after water heating kettle is cooled to room temperature;
2.3 promptly finish Y after sample being placed 65 ℃ the dry 45min of loft drier 4Si 3O 12/ Y 2Si 2O 7The preparation of coating;
3.Y 4Si 3O 12/ Y 2Si 2O 7/ Y 2SiO 5The preparation of gradient cladding
3.1 according to Y 2SiO 5The ratio formulated suspension of powder: Virahol=3g: 100ml; Under 1500r/min, behind the mechanical stirring 9h, in this suspension, introduce iodine, place the ultrasonic wave container 40min that under 300W power, vibrates, continue to stir behind the 28h suspension stand-by by the suspension of 1g: 100ml;
3.2 with Y 2SiO 5Suspension join in the water heating kettle that has electrode, and to deposit Y 4Si 3O 12/ Y 2Si 2O 7The coating style is a negative electrode, and the control hydrothermal temperature is that 150 ℃, deposition voltage are that 200V, depositing time are that 30min carries out water heat electrophoresis deposition, and deposition is finished and treated to take out sample after water heating kettle is cooled to room temperature;
3.3 after sample being placed 70 ℃ the dry 45min of loft drier, finally can obtain Y 4Si 3O 12/ Y 2Si 2O 7/ Y 2SiO 5The coating of gradient.
The specific physical chemical environment of the present invention under hydrothermal condition can be accelerated the mass transfer velocity in the solution, low and coating preparation of preparation temperature does not need subsequent crystallization heat treatment, avoided to a certain extent in the later stage heat treatment process, may causing curl, defective such as grain coarsening; It is simple that electrophoretic deposition method prepares coating operation, and the utilization rate of raw materials height especially can obtain the coating of uniformity on complex surfaces and porous matrix.

Claims (3)

1, a kind of water heat electrophoresis deposition method of gradient iridium silicate coating layer is characterized in that:
1) Y 4Si 3O 12The preparation of coating
1.1 according to Y 4Si 3O 12Powder: the ratio formulated suspension of Virahol=0.5～5g: 100ml; Under 1000～2000r/min, behind mechanical stirring 6～12h, in this suspension, introduce iodine, place the ultrasonic wave container 15～60min that under 100～500W power, vibrates, continue to stir behind 24～36h suspension stand-by by the suspension of 0.5～2g: 100ml;
1.2 with Y 4Si 3O 12Suspension join in the water heating kettle that has electrode, with the conducting base is negative electrode, the control hydrothermal temperature is that 80～200 ℃, deposition voltage are that 50～300V, depositing time are that 5～60min carries out water heat electrophoresis deposition, and deposition is finished and treated to take out sample after water heating kettle is cooled to room temperature;
1.3 promptly finish matrix Y after sample being placed 50～80 ℃ the dry 30～60min of loft drier 4Si 3O 12The preparation of coating;
2) Y 4Si 3O 12/ Y 2Si 2O 7The preparation of gradient cladding
2.1 according to Y 2Si 2O 7Powder: the ratio formulated suspension of Virahol=0.5～5g: 100ml; Under 1000～2000r/min, behind mechanical stirring 6～12h, in this suspension, introduce iodine, place the ultrasonic wave container 15～60min that under 100～500W power, vibrates, continue to stir behind 24～36h suspension stand-by by the suspension of 0.5～2g: 100ml;
2.2 with Y 2Si 2O 7Suspension join in the water heating kettle that has electrode, and to deposit Y 4Si 3O 12The coating sample be negative electrode, the control hydrothermal temperature is that 80～200 ℃, deposition voltage are that 50～300V, depositing time are that 5～60min carries out water heat electrophoresis deposition, deposition is finished and is treated to take out sample after water heating kettle is cooled to room temperature;
2.3 promptly finish Y after sample being placed 50～80 ℃ the dry 30～60min of loft drier 4Si 3O 12/ Y 2Si 2O 7The preparation of coating;
3) Y 4Si 3O 12/ Y 2Si 2O 7/ Y 2SiO 5The preparation of gradient cladding
3.1 according to Y 2SiO 5Powder: the ratio formulated suspension of Virahol=0.5～5g: 100ml; Under 1000～2000r/min, behind mechanical stirring 6～12h, in this suspension, introduce iodine, place the ultrasonic wave container 15～60min that under 100～500W power, vibrates, continue to stir behind 24～36h suspension stand-by by the suspension of 0.5～2g: 100ml;
3.2 with Y 2SiO 5Suspension join in the water heating kettle that has electrode, and to deposit Y 4Si 3O 12/ Y 2Si 2O 7The coating sample is a negative electrode, and the control hydrothermal temperature is that 80～200 ℃, deposition voltage are that 50～300V, depositing time are that 5～60min carries out water heat electrophoresis deposition, and deposition is finished and treated to take out sample after water heating kettle is cooled to room temperature;
3.3 after sample being placed 50～80 ℃ the dry 30～60min of loft drier, finally can obtain Y 4Si 3O 12/ Y 2Si 2O 7/ Y 2SiO 5The coating of gradient.
2, the water heat electrophoresis deposition method of gradient iridium silicate coating layer according to claim 1 is characterized in that: said conducting base is C/C, SiC, titanium or metal alloy.
3, the water heat electrophoresis deposition method of gradient iridium silicate coating layer according to claim 1 is characterized in that: said Y 4Si 3O 12Powder is synthetic by following technology
1) according to Y: Si=2: 3 mol ratio is mixed in the yttrium nitrate aqueous solution of 1.25mol/L and the sodium silicate aqueous solution of 1.87mol/L in the same container; Mechanical stirring 10～30min is placed on the 10～60min that vibrates in the ultrasonic wave container of ultrasonic power 0＜P≤500W under 1000～2000r/min;
2) get with 1) in the concentration of same amount be the aqueous sodium hydroxide solution of the yttrium nitrate aqueous solution of 1.25mol/L and 3.75mol/L by 1: 3 mixed in molar ratio in same container, mechanical stirring 10～30min is placed on the 10～60min that vibrates in the ultrasonic wave container of ultrasonic power 0＜P≤500W under 1000～2000r/min;
3) with above-mentioned 1) and 2) vibration after have sedimentary liquid mixing in same container, mechanical stirring 10～90min is placed on the 10～60min that vibrates in the ultrasonic wave container of ultrasonic power 0＜P≤500W under 1000～2000r/min, filter after the vibration, the distilled water wash precipitation is placed in the loft drier at 50～100 ℃ of drying 30～90min for 3～5 times;
4) speed muller with 5000～10000r/min obtains powder to dried throw out grinding 1～3h, powder after grinding is mixed with the mass ratio of dehydrated alcohol by 1: 10, and the lithium fluoride of the quality 2～6% of adding grinding back powder, mechanical stirring 10～30min is placed on the 10～20min that vibrates in the ultrasonic wave container under 1000～2000r/min; Dry 30～60min in the baking oven that is placed on 40～60 ℃ is finished in vibration;
5) dried powder is moved into corundum crucible and places High Temperature Furnaces Heating Apparatus, be incubated 1～4h after rising to 800～1200 ℃ with 2～6 ℃/min to cool to room temperature with the furnace, take out crucible, promptly get Y 4Si 3O 12Powder.
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