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 PDFInfo
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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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- 239000000919 ceramic Substances 0.000 title claims abstract description 99
- 238000005524 ceramic coating Methods 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 96
- 238000005245 sintering Methods 0.000 claims abstract description 39
- 238000005507 spraying Methods 0.000 claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 24
- 229910052575 non-oxide ceramic Inorganic materials 0.000 claims abstract description 22
- 239000011225 non-oxide ceramic Substances 0.000 claims abstract description 22
- 230000007704 transition Effects 0.000 claims abstract description 10
- 238000000151 deposition Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011159 matrix material Substances 0.000 claims description 60
- 239000007921 spray Substances 0.000 claims description 57
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 56
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 38
- 238000000576 coating method Methods 0.000 claims description 35
- 239000011248 coating agent Substances 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 24
- 238000000889 atomisation Methods 0.000 claims description 23
- 239000002994 raw material Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 18
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 16
- 239000002002 slurry Substances 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 239000012159 carrier gas Substances 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 7
- 244000137852 Petrea volubilis Species 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 239000011800 void material Substances 0.000 claims description 6
- 239000004677 Nylon Substances 0.000 claims description 2
- 229920001778 nylon Polymers 0.000 claims description 2
- 239000007791 liquid phase Substances 0.000 abstract description 12
- 239000000758 substrate Substances 0.000 abstract description 9
- 230000003628 erosive effect Effects 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 36
- 229910021426 porous silicon Inorganic materials 0.000 description 20
- 239000000463 material Substances 0.000 description 6
- 238000005229 chemical vapour deposition Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- 238000005336 cracking Methods 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000011224 oxide ceramic Substances 0.000 description 3
- 229910052574 oxide ceramic Inorganic materials 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 230000036961 partial effect Effects 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 230000000274 adsorptive effect Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
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- 230000007797 corrosion Effects 0.000 description 1
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- 230000007423 decrease Effects 0.000 description 1
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Abstract
一种多孔陶瓷表面致密陶瓷涂层的结构及制备方法，其结构为在多孔陶瓷基体表面包括双层结构陶瓷涂层，即致密层以及多孔陶瓷基体和致密层间的过渡层，致密层和过渡层采用在多孔基体表面喷涂沉积非氧化物陶瓷粉体内层和氧化物混合物粉体外层，烧结之后得到；其制备方法为：在多孔陶瓷基体表面喷涂沉积非氧化物粉体内层和氧化物混合物粉体外层，通过高温，外层先形成液相，浸渗到内层中，促进非氧化物粉体烧结，形成致密层：部分液相通过内层浸渗到多孔基体表面，形成过渡层；本发明解决了陶瓷涂层易开裂，分层，以及液相易渗入到多孔基体内部等问题；该结构的陶瓷涂层可明显降低多孔陶瓷基体的吸水率，提高多孔陶瓷基体表面硬度和抗冲蚀能力。
A structure and preparation method of a dense ceramic coating on the surface of a porous ceramic, the structure of which includes a double-layer structure ceramic coating on the surface of a porous ceramic substrate, that is, a dense layer and a transition layer between the porous ceramic substrate and the dense layer, the dense layer and the transition layer The layer is obtained by spraying and depositing the inner layer of non-oxide ceramic powder and the outer layer of oxide mixture powder on the surface of the porous substrate, and then sintering; the preparation method is: spraying and depositing the inner layer of non-oxide powder and the outer layer of oxide mixture on the surface of the porous ceramic substrate The outer layer of the powder, through high temperature, the outer layer first forms a liquid phase and infiltrates into the inner layer to promote the sintering of the non-oxide powder to form a dense layer: part of the liquid phase penetrates through the inner layer to the surface of the porous substrate to form a transition layer The present invention solves the problems that the ceramic coating is easy to crack and delaminate, and the liquid phase easily penetrates into the porous substrate; the ceramic coating of this structure can obviously reduce the water absorption rate of the porous ceramic substrate, and improve the surface hardness and resistance of the porous ceramic substrate. Erosion ability.
Description
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 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 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 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 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 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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