CN103693997A - Structure and preparation method of compact ceramic coating on surface of porous ceramic - Google Patents

Structure and preparation method of compact ceramic coating on surface of porous ceramic Download PDF

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CN103693997A
CN103693997A CN201310608160.XA CN201310608160A CN103693997A CN 103693997 A CN103693997 A CN 103693997A CN 201310608160 A CN201310608160 A CN 201310608160A CN 103693997 A CN103693997 A CN 103693997A
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porous ceramic
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CN103693997B (en
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王红洁
王超
范星宇
牛敏
史忠旗
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Xian Jiaotong University
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Abstract

The invention provides a structure and preparation method of a compact ceramic coating on the surface of a porous ceramic. The structure is that the surface of a porous ceramic matrix comprises a double-layer-structured ceramic coating, i.e., a compact layer and a transition layer between the porous ceramic matrix and the compact layer, and the compact layer and the transition layer are prepared by spraying and depositing a non-oxide ceramic powder inner layer and an oxide mixture powder outer layer on the surface of the porous ceramic matrix and carrying out sintering. The preparation method comprises the following steps: spraying and depositing the non-oxide ceramic powder inner layer and the oxide mixture powder outer layer on the surface of the porous ceramic matrix; allowing the outer layer to form a liquid phase at first through high temperature and to infiltrate into the inner layer so as to promote sintering of non-oxide powder, thereby forming the compact layer; and allowing a part of the liquid phase to infiltrate to the surface of the porous ceramic matrix so as to form the transition layer. According to the invention, problems like easy cracking and laying of the ceramic coating and easy infiltration of the liquid phase into the porous matrix are overcome; the ceramic coating with the structure can substantially reduce water absorption of the porous ceramic matrix and improve surface hardness and anti-ablation capability of the porous ceramic matrix.

Description

A kind of structure and preparation method of porous ceramic surface ceramic of compact coating
Technical field
The invention belongs to the preparing technical field of ceramic coating, be specifically related to a kind of method of preparing ceramic of compact coating in porous ceramic matrix surface.
Background technology
Porous ceramics can be regarded the complex body of pottery and pore as, the advantage that has had both stupalith and vesicular structure, have that density is little, high temperature resistant, corrosion-resistant, anti-thermal shock, thermal expansivity be little, the features such as easy processing, it is a kind of good structure-function integration material, can be used as lagging material, electromagnetic wave transparent material etc.But because it is surperficial and inside is all vesicular structures, and hole is communicated with.In use, be easy to moisture in absorbed air, thereby can increase the thermal conductivity of porous ceramics and the dielectric properties of reduction porous ceramics; In addition, porous ceramic matrix surface is more coarse, has a large amount of pores, has significantly reduced the mechanical property of porous ceramics.Therefore, the application of porous ceramics in some field is limited by very large.
At present, solve the conventional method of problem that above-mentioned porous ceramics exists and have two kinds: a kind of is the stupalith that directly preparation has density gradient.As Boeing has prepared the silicon nitride material with density gradient, the structure of this material is divided into two-layer: low density (0.5～1.8g/cm 3) nitride porous silicon materials be sandwich layer, top layer is highdensity silicon nitride material.Israel develops a kind of low density (1.0～2.2g/cm 3) nitride porous silicon layer and high-density (2.8～3.2g/cm 3) silicon nitride material that silicon nitride layer is composited, this mechanical strength is high, can resistance to 1600 ℃ of high temperature.But this mode is unfavorable for preparing the sample of complicated shape.And a lot of stupaliths are difficult to realize at low temperatures densification sintering.Another kind is at porous ceramic surface, to prepare the fine and close ceramic coating of one deck.The mode of preparation coating is as chemical vapour deposition (CVD), sol-gel method etc.Adopting CVD method is mainly the Si in the densification of porous ceramic surface deposition one deck 3n 4, SiC, B 4c coating.After deposition, the water absorption decreased of porous matrix 95%～99.82%, bending strength has improved 13.6%～24.4%.And adopt CVD legal system for coating, and sedimentation effect is low, and cost is high, and is difficult to deposit at the matrix surface of complicated shape; Sol-gel method is mainly to prepare oxide ceramic coating at porous ceramic surface, but this kind of method efficiency is low, and technological process is loaded down with trivial details, and the interface of coating and matrix is wayward.Therefore the ceramic coating that, adopts above method to prepare porous ceramic surface is difficult for realizing industrial applications.
Slip spraying is a kind of conventional method of preparing ceramic coating.Spray angle is more flexible, can prepare ceramic coating at the matrix surface of complicated shape.And preparation technology is simple, cost is low, and efficiency is high, is convenient to industrial applications.The patent of the number of patent application 201210396094.X of people's applications such as Wang Hongjie adopts the technique of slip spraying at the mono-layer oxidized powder of porous ceramic matrices suitable surface deposition, through oversintering, has prepared fine and close oxide ceramic coating.But this oxide ceramic coating be take glassy phase as main, and its hardness is lower, and the ability of Anti-erosion is poor.Conventionally, adopting slip spraying coating process to prepare non-oxide ceramic coatings is that non-oxide ceramics powder and the oxide powder as sintering aid are mixed, and sprays to afterwards matrix surface.In this method, sintering aid can first form liquid phase in sintering process, thereby realizes the liquid phase sintering of ceramic coating.But can there is very large volumetric shrinkage in sintering process in coating, cause coating and MATRIX CRACKING, layering, and produce the defects such as pore.Meanwhile, because porous matrix has very strong adsorptive power, liquid phase is easy to penetrate into the inside of porous matrix, and coat-thickness is difficult to control.Affect on the one hand the performance of matrix, affect on the other hand the compactness of coating.
Summary of the invention
The shortcoming existing in order to overcome above-mentioned prior art, the present invention proposes a kind of structure and preparation method of porous ceramic matrices suitable surface compact ceramic coating, solve liquid phase and infiltrated the excessively dark problem of porous matrix, can prepare fine and close ceramic coating on high porosity ceramic matrix surface, and this preparation method has simply, flexibly, efficient and be easy to the feature of industrial applications.
For achieving the above object, the present invention adopts following technical scheme to be achieved:
A kind of structure of porous ceramic surface ceramic of compact coating, porous ceramic matrix surface comprises bilayer structure ceramic coating, it is the transition layer between tight zone and porous ceramic matrices suitable and tight zone, described tight zone and transition layer are to adopt at porous matrix surface spraying deposition non-oxide ceramics powder internal layer and oxide mixture powder skin, after oversintering, obtain.
Described non-oxide ceramics powder is α-Si 3n 4powder, β-Si 3n 4powder or γ-Y 2si 2o 7powder.
Described hopcalite powder is Y 2o 3, SiO 2and Al 2o 3mixture, its mass ratio is Y 2o 3: SiO 2: Al 2o 3=(3～4): (3～5): (2～3).
The void content of described porous ceramic matrices suitable is 30～60%.
The preparation method of the structure of porous ceramic surface ceramic of compact coating described above, is characterized in that: comprise the steps:
Step 1, matrix is processed: choose porous ceramic matrices suitable, use 400 orders, 800 orders, it is smooth that 1000 order sand paper are successively ground to matrix surface, then the porous ceramic matrices suitable after grinding is put into distilled water ultrasonic cleaning 20～30min, matrix is put into baking oven after cleaning twice, at 70～80 ℃, dry 10～12h;
Step 2, Pulp preparation: non-oxide ceramics raw material powder and dehydrated alcohol are mixed, its solid content is 10～30%, take silicon nitride ball as abrading-ball, the mixture of non-oxide ceramics raw material powder and dehydrated alcohol and silicon nitride ball are placed in to ball grinder ball milling 8～12h, are prepared into non-oxide ceramics slip; Hopcalite powder and dehydrated alcohol are mixed, its solid content is 20～30%, take silicon nitride ball as abrading-ball, the mixture of oxide raw material powder and dehydrated alcohol and silicon nitride ball are placed in to ball grinder ball milling 12h, be prepared into hopcalite slip;
Step 3, slip spraying: first, the non-oxide ceramics slip preparing is packed in air atomization spray gun, make spray gun perpendicular to specimen surface, ceramic slurry is sprayed on to the surface of porous ceramic matrices suitable, form non-oxide ceramics powder internal layer; Then, the hopcalite slip preparing is packed in air atomization spray gun, make spray gun perpendicular to specimen surface, hopcalite slip is sprayed to the surface of non-oxide ceramics powder layer, form oxide mixture powder outer;
Step 4, dry: the sample for preparing powder layer to be put into baking oven, at 40～50 ℃, dry 8～10h;
Step 5, sample sintering: dried sample is put into and carries out sintering in atmosphere sintering furnace.Sintering temperature is 1400～1800 ℃, and sintering atmosphere is N 2, pressure is 0.15MPa, sintering time is 1h.
Described in step 3, air atomization spray gun use pressurized air is carrier gas, and pressure is 0.5～0.7MPa, and nozzle diameter is 0.5mm, spray distance 100～300mm, spray gun translational speed 20cm/s, spraying number of times 4～8 times.
Sintering described in step 5, detailed process is: 1200 ℃ of following temperature rise rates are 10 ℃/min, and 1200 ℃ above heats up and rate of temperature fall is 2 ℃/min, and 1200～800 ℃ of rate of temperature fall are 5 ℃/min, and 800 ℃ cool to normal temperature below with the furnace.
Described in step 2, the mass ratio of silicon nitride ball and non-oxide ceramics powder and hopcalite powder is 3:1.
Described in step 2, ball grinder is nylon tank.
The inventive method is in porous ceramic matrices suitable surface spraying deposition double-layer ceramic powder layer, it is non-oxidized substance powder internal layer, outer with hopcalite powder, by high temperature, outer oxide thing first forms liquid phase, is infiltrated up in non-oxidized substance powder internal layer, promote non-oxidized substance powder sintering, form tight zone: Partial Liquid Phase is infiltrated up to porous matrix surface by internal layer, form transition layer, thereby obtain bilayer structure; By the infiltration of liquid phase, fill to promote liquid phase sintering and the densification of ceramic coating.This method has not only solved the defects such as coating cracking, layering.Meanwhile, Partial Liquid Phase also can be passed ceramic coating, penetrates in the pore of porous ceramic matrices suitable, forms transition layer.Therefore, final ceramic coating structure is also double-deck, i.e. tight zone and transition layer.Can prepare fine and close ceramic coating on high porosity ceramic matrix surface by this method.And this technique has simply, flexibly, efficient and be easy to the feature of industrial applications.Compared to the prior art, tool of the present invention has the following advantages:
1) preparation method is simple, and cost is low.Compare with sol-gel method without preparing colloidal sol, and follow-up binder removal process, the production cycle significantly shortens; Compare with CVD method, preparation process is without the main equipment of complex and expensive, and production unit is simple, adopt air atomization spray gun spraying to prepare coating on the surface of complicated substrate, and can control coat-thickness by spraying number of times, technique is simple, cost is low, and efficiency is high, is convenient to industrial applications.
2) after coating sintering, be combined well with porous matrix, interface is clear, as shown in Figure 3; Non-oxide ceramics powder internal layer can effectively stop the outer liquid inner infiltration of porous matrix in opposite directions, thereby has reduced the impact of coating on porous ceramic matrices suitable performance.
3) present method has solved coating owing to shrinking, do not mated the coating cracking causing, the problems such as layering in sintering process.The coating even compact obtaining, coat-thickness is 45～200 μ m, can make the water-intake rate of matrix decline 84.4～90.7%, hardness improves 4.4～10.6 times.
Accompanying drawing explanation
Fig. 1 is coating production schematic diagram of the present invention.
Fig. 2 is β-Si 3n 4the surface topography of base ceramic coating.
Fig. 3 is β-Si 3n 4the Cross Section Morphology of base ceramic coating.
Embodiment
Below in conjunction with drawings and the specific embodiments, the present invention is described in further detail.
Embodiment 1:
The present embodiment is to prepare fine and close β-Si at porous silicon nitride ceramic matrix surface 3n 4base ceramic coating, comprises the following steps:
Step 1, matrix is processed: first selecting void content is that 60% porous silicon nitride is matrix, and then selecting order number is that 400 orders, 800 orders, 1000 object sand paper successively carry out fine grinding to porous silicon nitride ceramic matrix; Porous silicon nitride ceramic matrix after fine grinding is put into distilled water and carry out ultrasonic cleaning 30min; The porous silicon nitride ceramic matrix cleaning is put into baking oven and dry 10h, bake out temperature is 70 ℃;
Step 2, Pulp preparation: select β-Si 3n 4powder is ceramics powder raw material, by β-Si 3n 4powder mixes with dehydrated alcohol, and the solid content of its slip is 20%; Take silicon nitride ball as abrading-ball, by β-Si 3n 4the mixture of powder and dehydrated alcohol and silicon nitride ball are placed in ball grinder ball milling 10h, are prepared into β-Si 3n 4ceramic slurry, silicon nitride ball and β-Si 3n 4the mass ratio of powder is 3:1; By Y 2o 3, SiO 2, Al 2o 3raw material powder and dehydrated alcohol mix, Y 2o 3, SiO 2, Al 2o 3ratio be mass ratio: Y 2o 3: SiO 2: Al 2o 3=3:5:2, the solid content of its slip is 20%, take silicon nitride ball as abrading-ball, by Y 2o 3-SiO 2-Al 2o 3the mixture of raw material powder and dehydrated alcohol and silicon nitride ball are placed in ball grinder ball milling 12h, are prepared into Y 2o 3-SiO 2-Al 2o 3oxide compound slip, silicon nitride ball and Y 2o 3-SiO 2-Al 2o 3the mass ratio of raw material powder is 3:1;
Step 3, slip spraying: first, by β-Si 3n 4slip packs in air atomization spray gun, makes spray gun perpendicular to porous silicon nitride matrix surface, by β-Si 3n 4ceramic slurry is sprayed on the surface of porous ceramic matrices suitable, forms β-Si 3n 4ceramic powder layer; It is carrier gas that air atomization spray gun is used pressurized air, and pressure is 0.5-0.7MPa, nozzle diameter 0.5mm, spray distance 200mm, spray gun translational speed 20cm/s, spraying number of times 6 times; Then, by Y 2o 3-SiO 2-Al 2o 3slip packs in air atomization spray gun, makes spray gun perpendicular to specimen surface, by Y 2o 3-SiO 2-Al 2o 3ceramic slurry is sprayed on β-Si 3n 4the surface of ceramic powder layer, forms Y 2o 3-SiO 2-Al 2o 3oxide powder layer; It is carrier gas that air atomization spray gun is used pressurized air, and pressure is 0.5-0.7MPa, nozzle diameter 0.5mm, spray distance 200mm, spray gun translational speed 20cm/s, spraying number of times 6 times;
Step 4, dry: the sample for preparing powder layer to be put into baking oven, at 50 ℃, dry 8h;
Step 5, sample sintering: by dried sample at 0.15MPa pressure N 2under protective atmosphere at 1400 ℃ sintering; sintering time is 1h; concrete intensification and temperature-fall period are: 1200 ℃ of following temperature rise rates are 10 ℃/min; 1200 ℃～1400 ℃ intensifications and rate of temperature fall are 2 ℃/min; 1200～800 ℃ of rate of temperature fall are 5 ℃/min, and 800 ℃ cool to normal temperature below with the furnace.
The present embodiment is prepared β-Si after measured 3n 4after base coating, sample water-intake rate has declined 85.5%, and sample hardness has improved 5.4 times, and has good erosion resistance, and coat-thickness is 150～180 μ m, and between coating and matrix, combination firmly.
Embodiment 2:
The present embodiment is to prepare fine and close Y at porous silicon nitride ceramic matrix surface 2si 2o 7base ceramic coating, comprises the following steps:
Step 1, matrix is processed: first selecting void content is that 50% porous silicon nitride is matrix, and then selecting order number is that 400 orders, 800 orders, 1000 object sand paper successively carry out fine grinding to porous silicon nitride ceramic matrix; Porous silicon nitride ceramic matrix after fine grinding is put into distilled water and carry out ultrasonic cleaning 25min; The porous silicon nitride ceramic matrix cleaning is put into baking oven and dry 10h, bake out temperature is 70 ℃;
Step 2, Pulp preparation: select γ-Y 2si 2o 7powder is ceramics powder raw material, by γ-Y 2si 2o 7powder mixes with dehydrated alcohol, and the solid content of its slip is 30%; Take silicon nitride ball as abrading-ball, by γ-Y 2si 2o 7the mixture of powder and dehydrated alcohol and silicon nitride ball are placed in ball grinder ball milling 12h, are prepared into γ-Y 2si 2o 7ceramic slurry, silicon nitride ball and γ-Y 2si 2o 7the mass ratio of powder is 3:1; By Y 2o 3, SiO 2, Al 2o 3raw material powder and dehydrated alcohol mix, Y 2o 3, SiO 2, Al 2o 3ratio be mass ratio: Y 2o 3: SiO 2: Al 2o 3=3:5:2, the solid content of its slip is 30%.Take silicon nitride ball as abrading-ball, by Y 2o 3-SiO 2-Al 2o 3the mixture of raw material powder and dehydrated alcohol and silicon nitride ball are placed in ball grinder ball milling 12h, are prepared into Y 2o 3-SiO 2-Al 2o 3oxide compound slip, silicon nitride ball and Y 2o 3-SiO 2-Al 2o 3the mass ratio of raw material powder is 3:1;
Step 3, slip spraying: first, by γ-Y 2si 2o 7slip packs in air atomization spray gun, makes spray gun perpendicular to porous silicon nitride matrix surface, by γ-Y 2si 2o 7ceramic slurry is sprayed on the surface of porous ceramic matrices suitable, forms γ-Y 2si 2o 7ceramic powder layer; It is carrier gas that air atomization spray gun is used pressurized air, and pressure is 0.5-0.7MPa, nozzle diameter 0.5mm, spray distance 100mm, spray gun translational speed 20cm/s, spraying number of times 4 times; Then, by Y 2o 3-SiO 2-Al 2o 3slip packs in air atomization spray gun, makes spray gun perpendicular to specimen surface, by Y 2o 3-SiO 2-Al 2o 3ceramic slurry is sprayed on γ-Y 2si 2o 7the surface of ceramic powder layer, forms Y 2o 3-SiO 2-Al 2o 3oxide powder layer; It is carrier gas that air atomization spray gun is used pressurized air, and pressure is 0.5-0.7MPa, nozzle diameter 0.5mm, spray distance 200mm, spray gun translational speed 20cm/s, spraying number of times 4 times;
Step 4, dry: the sample for preparing powder layer to be put into baking oven, at 40 ℃, dry 8h;
Step 5, sample sintering: by dried sample at 0.15MPa pressure N 2under protective atmosphere at 1450 ℃ sintering; sintering time is 1h; concrete intensification and temperature-fall period are: 1200 ℃ of following temperature rise rates are 10 ℃/min; 1200 ℃～1450 ℃ intensifications and rate of temperature fall are 2 ℃/min; 1200～800 ℃ of rate of temperature fall are 5 ℃/min, and 800 ℃ cool to normal temperature below with the furnace.
The present embodiment is prepared Y after measured 2si 2o 7after base coating, sample water-intake rate has declined 89.1%, and sample hardness has improved 4.4 times, and has good erosion resistance, and coat-thickness is 180～200 μ m, and between coating and matrix, combination firmly.
Embodiment 3:
The present embodiment is to prepare high performance β-Si at porous silicon nitride ceramic matrix surface 3n 4base ceramic coating, comprises the following steps:
Step 1, matrix is processed: first selecting void content is that 55.7% porous silicon nitride is matrix, and then selecting order number is that 400 orders, 800 orders, 1000 object sand paper successively carry out fine grinding to porous silicon nitride ceramic matrix; Porous silicon nitride ceramic matrix after fine grinding is put into distilled water and carry out ultrasonic cleaning 30min; The porous silicon nitride ceramic matrix cleaning is put into baking oven and dry 10h, bake out temperature is 70 ℃;
Step 2, Pulp preparation: select α-Si 3n 4powder is ceramics powder raw material, by α-Si 3n 4powder mixes with dehydrated alcohol, and the solid content of its slip is 10%; Take silicon nitride ball as abrading-ball, by α-Si 3n 4the mixture of powder and dehydrated alcohol and silicon nitride ball are placed in ball grinder ball milling 8h, are prepared into α-Si 3n 4ceramic slurry, silicon nitride ball and α-Si 3n 4the mass ratio of powder is 3:1; By Y 2o 3, SiO 2, Al 2o 3raw material powder and dehydrated alcohol mix, Y 2o 3, SiO 2, Al 2o 3ratio be mass ratio: Y 2o 3: SiO 2: Al 2o 3=4:3:3, the solid content of its slip is 20%.Take silicon nitride ball as abrading-ball, by Y 2o 3-SiO 2-Al 2o 3the mixture of raw material powder and dehydrated alcohol and silicon nitride ball are placed in ball grinder ball milling 12h, are prepared into Y 2o 3-SiO 2-Al 2o 3oxide compound slip, silicon nitride ball and Y 2o 3-SiO 2-Al 2o 3the mass ratio of raw material powder is 3:1;
Step 3, slip spraying: first, by α-Si 3n 4slip packs in air atomization spray gun, makes spray gun perpendicular to porous silicon nitride matrix surface, by α-Si 3n 4ceramic slurry is sprayed on the surface of porous ceramic matrices suitable, forms α-Si 3n 4ceramic powder layer; It is carrier gas that air atomization spray gun is used pressurized air, and pressure is 0.5-0.7MPa, nozzle diameter 0.5mm, spray distance 200mm, spray gun translational speed 20cm/s, spraying number of times 8 times; Then, by Y 2o 3-SiO 2-Al 2o 3slip packs in air atomization spray gun, makes spray gun perpendicular to specimen surface, by Y 2o 3-SiO 2-Al 2o 3ceramic slurry is sprayed on α-Si 3n 4the surface of ceramic powder layer, forms Y 2o 3-SiO 2-Al 2o 3oxide powder layer; It is carrier gas that air atomization spray gun is used pressurized air, and pressure is 0.5-0.7MPa, nozzle diameter 0.5mm, spray distance 200mm, spray gun translational speed 20cm/s, spraying number of times 8 times;
Step 4, dry: the sample for preparing powder layer to be put into baking oven, at 40 ℃, dry 10h;
Step 5, sample sintering: by dried sample at 0.15MPa pressure N 2under protective atmosphere at 1800 ℃ sintering; sintering time is 1h; concrete intensification and temperature-fall period are: 1200 ℃ of following temperature rise rates are 10 ℃/min; 1200 ℃～1800 ℃ intensifications and rate of temperature fall are 2 ℃/min; 1200～800 ℃ of rate of temperature fall are 5 ℃/min, and 800 ℃ cool to normal temperature below with the furnace.
After measured, wait axle shape α-Si 3n 4through high temperature sintering, change bar-shaped β-Si completely into 3n 4, formed β-Si 3n 4base coating.The present embodiment is prepared β-Si 3n 4as shown in Figure 2, the cross section of coating as shown in Figure 3 for base coatingsurface.After preparation coating, sample water-intake rate has declined 90.7%, and sample hardness has improved 10.6 times, and has good erosion resistance, and coat-thickness is 45～60 μ m, and between coating and matrix, combination firmly.
Embodiment 4:
The present embodiment is at the fine and close β-Si of porous sialon ceramic matrix surface preparation 3n 4base ceramic coating, comprises the following steps:
Step 1: matrix is processed: first selecting void content is that 30% sialon pottery is matrix, and then selecting order number is that 400 orders, 800 orders, 1000 object sand paper successively carry out fine grinding to porous sialon ceramic matrix; Porous sialon matrix after fine grinding is put into distilled water and carry out ultrasonic cleaning 20min; The porous sialon pottery cleaning is put into baking oven and dry 12h, bake out temperature is 80 ℃;
Step 2, Pulp preparation: select β-Si 3n 4powder is ceramics powder raw material, by β-Si 3n 4powder mixes with dehydrated alcohol, and the solid content of its slip is 20%, take silicon nitride ball as abrading-ball, by β-Si 3n 4the mixture of powder and dehydrated alcohol and silicon nitride ball are placed in ball grinder ball milling 10h, are prepared into β-Si 3n 4ceramic slurry, silicon nitride ball and β-Si 3n 4the mass ratio of powder is 3:1; By Y 2o 3, SiO 2, Al 2o 3raw material powder and dehydrated alcohol mix, Y 2o 3, SiO 2, Al 2o 3ratio be mass ratio: Y 2o 3: SiO 2: Al 2o 3=3:5:2, the solid content of its slip is 20%.Take silicon nitride ball as abrading-ball, by Y 2o 3-SiO 2-Al 2o 3the mixture of raw material powder and dehydrated alcohol and silicon nitride ball are placed in ball grinder ball milling 12h, are prepared into Y 2o 3-SiO 2-Al 2o 3oxide compound slip, silicon nitride ball and Y 2o 3-SiO 2-Al 2o 3the mass ratio of raw material powder is 3:1;
Step 3, slip spraying: first, by β-Si 3n 4slip packs in air atomization spray gun, makes spray gun perpendicular to porous sialon matrix surface, by β-Si 3n 4ceramic slurry is sprayed on the surface of porous sialon matrix, forms β-Si 3n 4ceramic powder layer; It is carrier gas that air atomization spray gun is used pressurized air, and pressure is 0.5-0.7MPa, nozzle diameter 0.5mm, spray distance 300mm, spray gun translational speed 20cm/s, spraying number of times 6 times; Then, by Y 2o 3-SiO 2-Al 2o 3slip packs in air atomization spray gun, makes spray gun perpendicular to specimen surface, by Y 2o 3-SiO 2-Al 2o 3ceramic slurry is sprayed on β-Si 3n 4the surface of ceramic powder layer, forms Y 2o 3-SiO 2-Al 2o 3oxide powder layer; It is carrier gas that air atomization spray gun is used pressurized air, and pressure is 0.5-0.7MPa, nozzle diameter 0.5mm, spray distance 200mm, spray gun translational speed 20cm/s, spraying number of times 6 times;
Step 4, dry: the sample for preparing powder layer to be put into baking oven, at 50 ℃, dry 8h;
Step 5, sample sintering: by dried sample at 0.15MPa pressure N 2under protective atmosphere at 1400 ℃ sintering; sintering time is 1h; concrete intensification and temperature-fall period are: 1200 ℃ of following temperature rise rates are 10 ℃/min; 1200 ℃～1400 ℃ intensifications and rate of temperature fall are 2 ℃/min; 1200～800 ℃ of rate of temperature fall are 5 ℃/min, and 800 ℃ cool to normal temperature below with the furnace.
The present embodiment is prepared β-Si after measured 3n 4after base coating, sample water-intake rate has declined 84.4%, and sample hardness has improved 5 times, and has good erosion resistance, and coat-thickness is 150～180 μ m, and between coating and matrix, combination firmly.

Claims (9)

1. the structure of a porous ceramic surface ceramic of compact coating, porous ceramic matrix surface comprises bilayer structure ceramic coating, it is the transition layer between tight zone and porous ceramic matrices suitable and tight zone, it is characterized in that: described tight zone and transition layer are to adopt at porous matrix surface spraying deposition non-oxide ceramics powder internal layer and oxide mixture powder skin, after oversintering, obtain.
2. the structure of a kind of porous ceramic surface ceramic of compact coating according to claim 1, is characterized in that: described non-oxide ceramics powder is α-Si 3n 4powder, β-Si 3n 4powder or γ-Y 2si 2o 7powder.
3. the structure of a kind of porous ceramic surface ceramic of compact coating according to claim 1, is characterized in that: described hopcalite powder is Y 2o 3, SiO 2and Al 2o 3mixture, its mass ratio is Y 2o 3: SiO 2: Al 2o 3=(3～4): (3～5): (2～3).
4. the structure of a kind of porous ceramic surface ceramic of compact coating according to claim 1, is characterized in that: the void content of described porous ceramic matrices suitable is 30～60%.
5. the preparation method of the structure of the porous ceramic surface ceramic of compact coating described in claim 1 to 4 any one, is characterized in that: comprise the steps:
Step 1, matrix is processed: choose porous ceramic matrices suitable, use 400 orders, 800 orders, it is smooth that 1000 order sand paper are successively ground to matrix surface, then the porous ceramic matrices suitable after grinding is put into distilled water ultrasonic cleaning 20～30min, matrix is put into baking oven after cleaning twice, at 70～80 ℃, dry 10～12h;
Step 2, Pulp preparation: non-oxide ceramics raw material powder and dehydrated alcohol are mixed, its solid content is 10～30%, take silicon nitride ball as abrading-ball, the mixture of non-oxide ceramics raw material powder and dehydrated alcohol and silicon nitride ball are placed in to ball grinder ball milling 8～12h, are prepared into non-oxide ceramics slip; Hopcalite powder and dehydrated alcohol are mixed, its solid content is 20～30%, take silicon nitride ball as abrading-ball, the mixture of oxide raw material powder and dehydrated alcohol and silicon nitride ball are placed in to ball grinder ball milling 12h, be prepared into hopcalite slip;
Step 3, slip spraying: first, the non-oxide ceramics slip preparing is packed in air atomization spray gun, make spray gun perpendicular to specimen surface, ceramic slurry is sprayed on to the surface of porous ceramic matrices suitable, form non-oxide ceramics powder internal layer; Then, the hopcalite slip preparing is packed in air atomization spray gun, make spray gun perpendicular to specimen surface, hopcalite slip is sprayed to the surface of non-oxide ceramics powder layer, form oxide mixture powder outer;
Step 4, dry: the sample for preparing powder layer to be put into baking oven, at 40～50 ℃, dry 8～10h;
Step 5, sample sintering: dried sample is put in atmosphere sintering furnace and carries out sintering, and sintering temperature is 1400～1800 ℃, and sintering atmosphere is N 2, pressure is 0.15MPa, sintering time is 1h.
6. preparation method according to claim 5, is characterized in that: described in step 3, air atomization spray gun use pressurized air is carrier gas, and pressure is 0.5～0.7MPa, nozzle diameter is 0.5mm, spray distance 100～300mm, spray gun translational speed 20cm/s, spraying number of times 4～8 times.
7. preparation method according to claim 5, it is characterized in that: sintering described in step 5, detailed process is: 1200 ℃ of following temperature rise rates are 10 ℃/min, 1200 ℃ above heats up and rate of temperature fall is 2 ℃/min, 1200～800 ℃ of rate of temperature fall are 5 ℃/min, and 800 ℃ cool to normal temperature below with the furnace.
8. preparation method according to claim 5, is characterized in that: described in step 2, the mass ratio of silicon nitride ball and non-oxide ceramics powder and hopcalite powder is 3:1.
9. preparation method according to claim 5, is characterized in that: described in step 2, ball grinder is nylon tank.
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