CN203474661U - Uniform and composite spherical ceramic particle - Google Patents
Uniform and composite spherical ceramic particle Download PDFInfo
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- CN203474661U CN203474661U CN201320537823.9U CN201320537823U CN203474661U CN 203474661 U CN203474661 U CN 203474661U CN 201320537823 U CN201320537823 U CN 201320537823U CN 203474661 U CN203474661 U CN 203474661U
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Abstract
The utility model relates to the technical field of a ceramic matrix powder material, and particularly relates to a uniform and composite spherical ceramic particle. The designed particle is an aggregate of nanoscale and submicron-scale powder with high sphericity. At least two different kinds of inorganic powder are used for preparing the aggregate; the two kinds of powder are connected by sintering or intermolecular force; the local density from the center of a particle body to the outer surface gradually increases or increases in a multistep manner, the highest extent local density exist at the outer surface of the particle body. By adopting the design disclosed by the utility model, the difference between the component of an individual particle and the overall average component of the particles is smaller than 3% within the range that the average particle size is 10-500 microns; the sphericity of over 80% of particles is greater than 0.92; pollution or emission of a toxic gas is free in the overall preparation process. The uniform and composite spherical ceramic particle can be widely applied to frosting treatment on a metal surface, and residual stress removal, strengthening treatment, anti-fatigue treatment and the like of a member surface, as well as fine processing of nanoscale powder, manufacturing of a ceramic coating and the like.
Description
Technical field
The utility model relates to ceramic base powder body material technical field, relates in particular to a kind of evenly compound globular ceramic particle.
Background technology
The preparation of ceramic base powder body material and application research and development thereof are the important composition parts of " advanced manufacturing technology ", be China and in the world each Main Developed Countries determined one of strategic hi-tech of first developing.
The micron order ceramic particle of high sphericity is widely used in a plurality of industrial circles, such as the Wear-resistant Treatment of pottery and surface of plastic products, the abrasionproof of the frosted on metal products surface and destressing, drive disk assembly undermines the fine grinding of thermal protection, particle and pulverulent material etc.
The production of common this micron level spherical particle, is high-pressure air to be purged to the raw material of melting, then collects the particle of being wrapped up in band by the atomization of high-pressure air institute.Then the particulate product of collecting is screened, the step such as shaping, cleaning obtains the finished product.Mainly there is the defect of six aspects in the product of the production of this method: 1) sphericity of formed spherical particle is lower.2) formed spherical particle has wider particle size distribution conventionally, therefore uncontrollable to the productive rate of specific product.Result is exactly that production efficiency is low, cannot carry out product customized.3) this manufacturing process requires the multi-component masses of melting can form stable improving uniformity of melt, therefore be difficult to manufacture, cannot form the composite system of stablizing eutectic.4) while being shaped, need to, by heating material to melting, therefore cannot be applied to more oxidizable material system.5) molten mass, rapidly in process of cooling, cannot accurately be controlled cooling direction, and product exists higher internal stress, affects the mechanical properties such as intensity of product.6) there is by product and the waste gas of a large amount of contaminatives in production process.
Utility model content
The technical problems to be solved in the utility model is: the defect of producing ceramic particle in order to solve the method for applying high voltage air purge atomized molten slip in prior art, the utility model provides a kind of evenly compound globular ceramic particle.
The utility model solves the technical scheme that its technical problem adopts: a kind of evenly compound globular ceramic particle, comprise at least two kinds of inorganic materials, wherein at least one is stupalith, the ball-like structure that described particle degree spherical in shape is greater than 0.9, the agent structure of particle is compound by sintering processing by the powder of the stupalith of nano level and/or submicron order; The center of particle to the local density of outside surface gradually or staged increase, and reach Gao local density at the outside surface of particle.This structure is the technique of using pneumatic granulation and roll being shaped due to us, and not completely crued slip, under the effect of surface tension and capillary force, then through sintering, forms low outer high density distribution in particle.And the particle that traditional molten atomizing produces is not possess this constructional feature.
As preferably, described inorganic materials is pottery and/or the metal fine powder of nano level and/or submicron order, comprises one or more in zirconium white, aluminum oxide, silicon nitride, aluminium nitride, silicon-dioxide, zirconium silicate, norbide, boron nitride, diamond, wolfram varbide and metal.But be not limited only to this.
As preferably, described stupalith is the ceramic of nano level and/or submicron order, comprises one or more in zirconium white, aluminum oxide, silicon nitride, aluminium nitride, silicon-dioxide, zirconium silicate, norbide, boron nitride, diamond and wolfram varbide.But be not limited only to this.
Particle in the composite ceramic particle that the utility model method makes more than 80% has more than 0.92 sphericity.
The difference of the component of individual particles and particle population mean component is less than 3%, has the particle that uniform composite attribute particle population mean component extracts any batch, and this is the average composition of particle in batches.
The volume average particle size of the described particle that the utility model method makes is 10 μ m-500 μ m.
Described particle has relatively loose core, relatively fine and close excessively layer and fine and close outer shell from inside to outside.
A preparation method for even compound globular ceramic particle, the method is prepared the globular ceramic particle that median size is 10 μ m-250 μ m, comprises the steps:
A) grinding distribution: by least two kinds of inorganic micro powders, wherein at least one is ceramic, and water or/and organic solvent and dispersion agent simultaneously or after substep feeds intake, the median size that is blended into micro mist with wet grinding is 0.5 μ m-1 μ m;
B) pneumatic granulation: will in the material obtaining in a), add the mixture of water or water and alcohols to dilute, regulate viscosity 100-2000cPa and the solids content 20-50wt% of slip, make slurry reach atomised jet, carry out the requirement of pneumatic granulation,
C) particle of pneumatic granulation is dried scalping;
D) to c) in the particle that makes carry out sintering;
E) particle after sintering is carried out to ball milling polishing, cleaning;
F) particle to polishing, after cleaning be dried, scalping;
G) particle after scalping is selected to circle, fine screen.
In step b), can also in ± 10% scope, further finely tune viscosity, the solids content of slip, make the pulp particle of atomised jet possess stable aerodynamic diameter, this diameter is the 110-130% of the diameter of the final ceramic particle of preparing;
As preferably, the content of described dispersion agent is 0.01-3wt%(initial content), described dispersion agent comprises one or more in tripoly phosphate sodium STPP, Sodium hexametaphosphate 99, trisodium phosphate, triethyl hexyl phosphoric acid, methyl amyl alcohol, derivatived cellulose, polyacrylamide, guar gum, fatty acid polyglycol ester and LBD-1.But be not limited only to this.
Inorganic micro powder described in aforesaid method is pottery and/or the metal fine powder of nano level and/or submicron order, comprises one or more in zirconium white, aluminum oxide, silicon nitride, aluminium nitride, silicon-dioxide, zirconium silicate, norbide, boron nitride, diamond, wolfram varbide and metal.But be not limited only to this.Described ceramic is the ceramic of nano level and/or submicron order, comprises one or more in zirconium white, aluminum oxide, silicon nitride, aluminium nitride, silicon-dioxide, zirconium silicate, norbide, boron nitride, diamond and wolfram varbide.But be not limited only to this.
A preparation method for even compound globular ceramic particle, the method is prepared the globular ceramic particle that median size is 150 μ m-500 μ m, comprises the steps:
A) grinding distribution: by least two kinds of inorganic micro powders, wherein at least one is ceramic, and water and organic solvent and dispersion agent are simultaneously or after substep feeds intake, the median size that is blended into micro mist with wet grinding is 0.5 μ m-1 μ m;
B) slip in step a) is made to compound uniform granular powder by spray drying device;
C) take out part powder in step b) and put into whipping appts and carry out high speed dispersion shearing, make to grow in powder the composite granule idiosome of 0.05-0.5mm;
D) again idiosome is added in the powder of remainder in described step b) and roll by same sense of rotation, in the process of rolling, impel powder to be evenly coated on idiosome gradually, be grown to the spherical ceramic particles (target grain size is slightly larger than the particle diameter that finally makes particle) of target grain size;
E) to d) in the spherical ceramic particles that generates be dried;
F) to e) in the particle that generates carry out sintering;
G) particle after sintering is carried out to ball milling polishing, cleaning;
H) particle to polishing, after cleaning be dried, scalping;
I) particle after scalping is selected to circle, fine screen.
In aforesaid method, conduct preferably, the content of described dispersion agent is 0.01-3wt%(initial content), described dispersion agent comprises one or more in tripoly phosphate sodium STPP, Sodium hexametaphosphate 99, trisodium phosphate, triethyl hexyl phosphoric acid, methyl amyl alcohol, derivatived cellulose, polyacrylamide, guar gum, fatty acid polyglycol ester and LBD-1.But be not limited only to this.
Described inorganic micro powder is pottery and/or the metal fine powder of nano level and/or submicron order, comprises one or more in zirconium white, aluminum oxide, silicon nitride, aluminium nitride, silicon-dioxide, zirconium silicate, norbide, boron nitride, diamond, wolfram varbide and metal.But be not limited only to this.Described ceramic is the ceramic of nano level and/or submicron order, comprises one or more in zirconium white, aluminum oxide, silicon nitride, aluminium nitride, silicon-dioxide, zirconium silicate, norbide, boron nitride, diamond and wolfram varbide.But be not limited only to this.
The beneficial effects of the utility model are, even compound globular ceramic particle of the present utility model and preparation method thereof, what design is a kind of particle of high sphericity, this particle is the aggregate of nano level and sub-micron powder, at least two kinds of different inorganic powders are used to manufacture this aggregate, between powder, by sintering or Intermolecular Forces, connect.The component of individual particle and particle population mean component difference are less than 3%, have evenly compound characteristic.The production method that purges atomized molten slip with the high-pressure air of main application in current industry is compared, and the spherical ceramic particles product in the utility model has five major technique advantages:
1) spherical products is comprised of nanometer and the sub-micron grain of sintering, compare and have better mechanical property, and sphericity is higher than traditional technology with traditional technology, and average sphericity is 0.92-0.95.
2) raw material of spherical particle can be used nanometer scale ceramics powder, can produce almost the even compound spherical particle of component proportion arbitrarily.
3) because technique is used the temperature range of near room temperature, so spherical particle material of the present utility model can be non-oxide ceramics, metal, metal-ceramic composite, such as diamond, silicon nitride, aluminium nitride, aluminium etc.
4), by adjusting the colloid chemistry character of water base or other solvent slip, the spherical particle size range of generation is adjustable and size-grade distribution is narrow, greatly enhances productivity.
5) full preparation process is pollution-free discharges with toxic gas.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the utility model is further illustrated.
Fig. 1 is the micro-image of the utility model globular ceramic particle;
Fig. 2 is the structural representation of the utility model globular ceramic particle;
Fig. 3 is the utility model process flow sheet;
Fig. 4 is the utility model spray granulation plant schematic diagram.
In figure: 1, particle.
Embodiment
By reference to the accompanying drawings the utility model is described in further detail now.These accompanying drawings are the schematic diagram of simplification, basic structure of the present utility model is only described in a schematic way, so it only show the formation relevant with the utility model.
In Fig. 2, be the globular ceramic particle that the utility model makes, there is from inside to outside relatively loose core 1-1, relatively fine and close excessively layer 1-2, fine and close outer shell 1-3.
In Fig. 3, before grinding distribution and mist projection granulating, can pass through spiral pump feeding.
Fig. 4 comprises connected successively material agitator 10, pressure feed pump 11, atomizing lance 4, drying tower 5, one-level dust-precipitator 6, secondary dust collecting 7, induced draft fan 8 and fly-ash separator 9, secondary dust collecting 7 comprises cyclonic separator and sack cleaner, can select as required, fly-ash separator 9 comprises water bath dust-removing and venturi scrubber, can select as required.Atomizing lance 4 is also connected with well heater 3, well heater 3 is connected with fan 2, and fan 2 is connected with air filter 12.
Zirconium white-5% alumina composite ceramic micron ball.First, the following technical grade zirconia powder of 0.5mm and aluminum oxide powder are made into slip according to 95:5 and water and 0.25% Sodium hexametaphosphate 99, in grinding machine, grind 4-48 hour, be less than 0.8 μ m to D50.The slip of milled regulates concentration and viscosity in transfer batch can, and adding weight ratio is water and the Virahol of 95:5, and making solids content is 35-50%, and viscosity is 200-600cPa.Then with spiral pump, add pneumatic prilling granulator, by atomizing lance to the spherical ceramic particles that ejects target grain size in drying tower.Product after pneumatic granulation removes after a small amount of by product in irregular shape, is dried and high temperature sintering.More typical drying temperature is 200-500 ℃, and sintering temperature is 1300-1550 ℃.Sintered products enters subsequently ball mill and carries out surface finish processing.Particulate product after ball mill polishing, through fine screen, obtains median size 10 μ m, more than 0.95 particle of average spherical degree.Conversion process condition can obtain median size at the particle of 30 μ m and 50 μ m.With the EDS energy spectrum analysis of scanning electronic microscope, the difference of the component of individual particles and particle population mean component is less than 3%.
Its Production Flow Chart equally can be with reference to accompanying drawing 3 (a).
Products obtained therefrom is mainly used in the frosted of metallic surface and processes.
Embodiment 2
Zirconium silicate-25% alumina composite ceramic micron ball.First, the following technical grade zirconium silicate powder of 0.5mm and aluminum oxide powder are made into slip according to 75:25 and water and 0.5% triethyl hexyl phosphoric acid, then with hopper, add grinding machine to grind 4-48h, in grinding machine, be ground to D50 and be less than 1 μ m.The slip of milled regulates concentration and viscosity in transfer batch can, adds water and ethylene glycol that weight ratio is 98:2, makes the concentration 30-40% of general solid materials, and viscosity is 500-700cPa.Then with spiral pump, add pneumatic prilling granulator.Product after pneumatic granulation, after scalping, is dried and high temperature sintering.More typical drying temperature is 200-500 ℃, and sintering temperature is 1100-1200 ℃.Sintered products enters subsequently ball mill and carries out surface finish processing.Particulate product drying after ball mill polishing and scalping, fine screen, obtain median size at 40 μ m, more than 0.95 particle of average spherical degree.With the EDS energy spectrum analysis of scanning electronic microscope, the difference of the component of individual particles and particle population mean component is less than 3%.
Its Production Flow Chart equally can be with reference to accompanying drawing 3 (a).
What products obtained therefrom was mainly used in metal component surface goes unrelieved stress intensive treatment.
Embodiment 3
500 μ m diameter yttria-stabilized zirconia composite titanium oxide ceramic microspheres.First, by the yttrium stable zirconium oxide powder of 1 μ m, the technical grade titanium oxide powder of 2um is made into slip according to 80:20 and water and 0.5% tripoly phosphate sodium STPP, then with hopper, add grinding machine to grind 4-48h, in grinding machine, be ground to D50 and be less than 0.5 μ m, powdery pulp is made to compound uniform powder by spray drying device.Take out part powder and in stirred pot, use high speed dispersor high speed shear, depending on forming the difference of target seed particle size, can suitably spray the aqueous dispersant of 0.1-1% with the formation of help idiosome.Idiosome particle and remaining powder are placed in to specific equipment rolling tablets press.In device rolling process, powder wraps up idiosome gradually, grows high sphericity particle, can obtain target particles particle diameter by controlling growth time 2-12h.Spherical ceramic particles, after scalping, is dried and high temperature sintering.More typical drying temperature is 200-500 ℃, and sintering temperature is 1400-1500 ℃.Sintered products enters subsequently ball mill and carries out surface finish processing.Particulate product drying and fine screen after ball mill polishing, obtain median size at 500 μ m, more than 0.95 particle of average spherical degree.With the EDS energy spectrum analysis of scanning electronic microscope, the difference of the component of individual particles and particle population mean component is less than 3%.
Its Production Flow Chart equally can be with reference to accompanying drawing 3 (b).
Products obtained therefrom is mainly used in the nano level powder of attrition process, such as ceramic ink etc.
Embodiment 4
40 μ m diameter wolfram varbide chromium cobalt mixture microballoons.First, by the tungsten carbide powder of 40 μ m, technical grade chromium and the cobalt of 50 μ m are made into slip according to 86:4:10 and Virahol, be ground to D50 and be less than 0.5 μ m in grinding machine, then with hopper, add grinding machine to grind 4-48h.The slip of milled regulates concentration and viscosity in transfer batch can, adds Virahol and water, and ratio is 95:5, and making general solids content is 20-30%, and viscosity is 500-700cPa.Then with spiral pump, add pneumatic prilling granulator.Product after pneumatic granulation is dried, and more typical drying temperature is 200-500 ℃.Then in nitrogen protection atmosphere, carry out sintering, sintering temperature is 900-1100 ℃.Sintered product, after scalping and fine screen, obtains median size at 40 μ m, more than 0.90 particle of average spherical degree.Product particle is through ICP ultimate analysis, the difference of the component of individual particles and particle population mean component within 1%, or the component that also can say each particle with the feed composition difference of initial proportioning within 1%.
Its Production Flow Chart equally can be with reference to accompanying drawing 3 (a), is that last polished finish is depending on applicable cases.
Products obtained therefrom is mainly used in thermospray wear-resistant metal ceramic coating, such as the contact surface of sliding surface bearing, uses the feed particles of high sphericity high evenness can increase substantially the consistence of coating.
Embodiment 5
The partially stabilized yttrium zirconium white of 0.35-0.45mm complex microsphere.First the zirconia powder of 2 μ m, the aluminum oxide of 5 μ m, yttrium oxide add 0.3% Sodium hexametaphosphate 99 to be made into slurry according to 70%:25%:5% and deionized water, then with hopper, add grinding machine to grind 4-48h, make the slurry that D50 is less than 0.5 μ m.Powdery pulp is made to compound uniform powder by spray drying device.Take out part powder and in stirred pot, use high speed dispersor high speed shear, depending on forming the difference of target seed particle size, can suitably spray the aqueous dispersant of 0.1-1% with the formation of help idiosome.Idiosome and residue powder are placed in to rolling tablets press.In device rolling process, powder evenly wraps up idiosome gradually, grows high sphericity particle, can obtain target particles particle diameter by controlling growth time 4-12h.Spherical ceramic particles, after scalping, is dried and high temperature sintering.More typical drying temperature is 200-500 ℃, and sintering temperature is 1400-1500 ℃.Sintered products enters subsequently ball mill and carries out surface finish processing.Particulate product drying and fine screen after ball mill polishing, obtain median size at 400 μ m, more than 0.95 particle of average spherical degree.
Its Production Flow Chart equally can be with reference to accompanying drawing 3 (b).
Products obtained therefrom is mainly used in the nano level powder of attrition process, is especially applicable to the grinding of high-hardness inorganic powder, such as ceramic ink etc.This product can provide the stronger stress degree of depth for shot-peening simultaneously, reaches better metal strengthening effect.
Embodiment 6
0.25-0.35mm cerium stabilizing zirconium oxide complex microsphere.First the zirconia powder of 2 μ m, the cerium oxide of 2 μ m, 5 μ m aluminum oxide add 0.3% Sodium hexametaphosphate 99 to be made into slurry according to the ratio of 75%:20%:5% and deionized water, then with hopper, add grinding machine to grind 4-48h, make the slurry that D50 is less than 0.5 μ m.Powdery pulp is made to compound uniform powder by spray drying device.Take out part powder and in stirred pot, use high speed dispersor high speed shear, depending on forming the difference of target seed particle size, can suitably spray the aqueous dispersant of 0.1-1% with the formation of help idiosome.Idiosome particle and residue powder are placed in to specific equipment rolling tablets press.In device rolling process, powder evenly wraps up idiosome gradually, grows high sphericity particle, can obtain target particles particle diameter by controlling growth time 2-12h.Spherical ceramic particles, after scalping, is dried and high temperature sintering.More typical drying temperature is 200-500 ℃, and sintering temperature is 1400-1500 ℃.Sintered products enters subsequently ball mill and carries out surface finish processing.Particulate product drying and fine screen after ball mill polishing, obtain median size at 300 μ m, more than 0.95 particle of average spherical degree.
Its Production Flow Chart equally can be with reference to accompanying drawing 3 (b).
Products obtained therefrom can be for the nano level powder of attrition process.As shot peening strengthening material, its high specific gravity, the characteristic of high-modulus is excellent to the antifatigue treatment effect of engine blade, as sand-blast material, can remove high rigidity oxide skin, and without metal residual.
Particle diameter in above embodiment and sphericity are measured and are used optical imagery to draw through computed in software, and reference instrument is Ma Erwen Morphologi G3.
The above-mentioned foundation desirable embodiment of the present utility model of take is enlightenment, and by above-mentioned description, relevant staff can, within not departing from the scope of this utility model technological thought, carry out various change and modification completely.The technical scope of this utility model is not limited to the content on specification sheets, must determine its technical scope according to claim scope.
Claims (4)
1. an even compound globular ceramic particle, it is characterized in that: comprise at least two kinds of inorganic materials, wherein at least one is stupalith, the ball-like structure that described particle (1) degree spherical in shape is greater than 0.9, the agent structure of particle (1) is compound by sintering processing by the powder of the stupalith of nano level and/or submicron order; The center of particle (1) to the local density of outside surface gradually or staged increase, and reach Gao local density at the outside surface of particle (1).
2. the even compound globular ceramic particle described in claim 1, is characterized in that: the particle in described finished product composite ceramic particle more than 80% has more than 0.92 sphericity.
3. the even compound globular ceramic particle as described in any one in claim 1 or 2, is characterized in that: the volume average particle size of described particle (1) is between 10 μ m-500 μ m.
4. even compound globular ceramic particle as described in claim 1, is characterized in that: described particle (1) has relatively loose core (1-1), relatively fine and close excessively layer (1-2) and fine and close outer shell (1-3) from inside to outside.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110935394A (en) * | 2019-11-05 | 2020-03-31 | 南京清大迈特新材料有限公司 | Micro-nano powder fine processing method and device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110935394A (en) * | 2019-11-05 | 2020-03-31 | 南京清大迈特新材料有限公司 | Micro-nano powder fine processing method and device |
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