CN108203299A - A kind of method that presoma comminution granulation prepares spherical zirconia powder - Google Patents
A kind of method that presoma comminution granulation prepares spherical zirconia powder Download PDFInfo
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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Abstract
The invention discloses a kind of methods that presoma comminution granulation prepares spherical zirconia powder, by being stirred evenly after zirconium ion solution is mixed with ruthenium ion solution, precipitating reagent is made with ammonium hydroxide or ammonium oxalate and forms precipitation, using ceramic membrane separation and filter-pressing method removal solvent, it sizes mixing for acidified dose and carries out mist projection granulating, finally carry out heat treatment and can obtain spherical nanostructure Zirconium powder；The obtained granularity of spherical nanostructure Zirconium powder is 20~90 μm, is made of the tetragonal phase zirconium oxide crystal grain of nanostructured, and crystallite dimension is 10~100nm, and even particle size distribution is controllable.This method is modulated into slurry by hydroxide precursor and is granulated, and finally carries out calcination processing and obtains the uniform-spherical powder of good fluidity, do not need to be dried, azeotropic distillation, plasma spheroidization or secondary clacining etc.；The preparation method of the present invention relatively shortens technological process with the relevant technologies, cost is reduced, suitable for large-scale industrial production.
Description
Technical field
The present invention relates to technical field of ceramic material, are specially related to being suitable for thermal spraying (plasma spraying or flame spray
Apply) etc. techniques prepare the method that the one step comminution granulation of presoma of thermal barrier coating prepares spherical zirconia powder.
Background technology
Nano level zirconia material is because with certain unique performances：It is insulator under room temperature, is then conductor under high temperature,
With sensitivity characteristic and increasing tougheness etc., it is widely used in manufacture structural ceramics (such as row of reactor jacket, aero-engine
Thick stick, cylinder liner etc.), function ceramics (such as gas, temperature, humidity, sonic transducer), piezoelectric ceramics, electronic ceramics (such as capacitance
Device, oscillator, buzzer, adjuster, electric-heating assembly etc.), bioceramic, high-temperature fuel cell, High Temperature Optical component, magnetic fluid
In the high-tech products such as generator electrode.Zirconium oxide is when applied to hot spray process technique, by nanometer aggregate spherical powder grain
Metal surface is sprayed to as slush state, does not melt crystal phase structure, size distribution and the shape of part nano particle among spherolite
State plays decisive role to the compactness of coating and toughness etc..Thus need to be oxidized mobility, the dispersion that zirconium powder body has had
The features such as property.It needs to obtain the coating structure containing nanostructured in spraying process, it is necessary to assure in original spraying powder contain
Nanostructured, and do not occur to grow up completely in spraying process；But simple nano-scale particle quality is too small, momentum is insufficient,
Even if in spraying process, into flame stream, substantial portion of nano-powder cannot be also had by flame entrained by moving flame stream
Stream is blown away, and is in addition easily sintered during spraying, and it is that cannot be used for direct spraying to be stranded this simple nano material.
In the relevant technologies, it is made of by ball milling after yttrium oxide-stabilized zirconium oxide powder, deionized water and dispersant
The slurry being stirred is carried out mist projection granulating, obtains yttria-stabilized zirconia pelletizing by slurry.
But inventor has found, spraying requirement is not achieved in obtained zirconium oxide pelletizing consistency, needs to carry out plasmasphere
Change or secondary clacining process can be only achieved densification.
Invention content
The purpose of the present invention is to provide the method that presoma comminution granulation prepares spherical zirconia powder, this method at present
The prilling process used is compared, and most important feature is to shorten technological process, reduces energy consumption, while remain in spherical powder
The nanostructured in portion, suitable for large-scale industrial production.
To achieve these goals, technical solution used in the embodiment of the present invention is that a kind of presoma comminution granulation prepares ball
The method of shape Zirconium powder, includes the following steps：
1) mixed solution is prepared：Zirconates is dissolved in deionized water, obtains solution A, yttrium salt is dissolved in deionized water, is obtained molten
A, B solution are uniformly mixed to obtain mixed solution by liquid B；
2) sediment is prepared：Obtained mixed solution is instilled dropwise in ammonium hydroxide or ammonium oxalate solution, precipitation is formed, stirs
Ageing obtains sediment after mixing；
3) washing process：By sediment, removal foreign ion obtains presoma object after ceramic membrane, press filtration processing；
4) slurry is granulated：The slurry that obtained presoma object is handled with acidulant, is set using spray drying
Precursor spherical powder is prepared for be granulated；
5) calcination processing：Obtained precursor spherical powder calcination processing is obtained into tetragonal phase structure spherical zircite, and make
Spherical powder is densified to obtain spherical zircite powder.
Preferably, in step (1), the solution A is basic zirconium chloride, acetic acid zirconium or zirconium nitrate solution etc., and zirconium ion is dense
It spends for 0.1mol/L~1.0mol/L, the solution B is yttrium nitrate, yttrium chloride or yttrium sulfate solution etc., and ruthenium ion is a concentration of
0.1mol/L~0.5mol/L, wherein ruthenium ion are 3~5 with zirconium ion molar ratio：100.
Preferably, in step (2), mixing time is 1~2h, digestion time for 12~for 24 hours.
Preferably, in step (4), the acidulant is hydrochloric acid, nitric acid either matching by arbitrary between dilute sulfuric acid or two kinds
Than；The solid content of the slurry is 25%~35%；The mode of the spray drying is centrifugal or two streamings, and the spraying is dry
Dry inlet temperature is 150 DEG C~200 DEG C, and outlet temperature is 80 DEG C~120 DEG C.
Preferably, in step (5), calcination temperature is 600 DEG C~800 DEG C, and soaking time is 1~5h.
Compared with the relevant technologies, the advantageous effect that the technical solution of the embodiment of the present invention offer is brought is：The present invention's
One step comminution granulation of presoma prepares spherical zirconia powder, is directly granulated to obtain spherical zircite forerunner by hydroxide slurry
Body does not need to be dried, azeotropic distillation etc.；The zirconium oxide presoma is subjected to primary calcining densification and can obtain spherical shape
Zirconium powder does not need to carry out plasma spheroidization or secondary clacining；Preparation process is simple, shortens technological process, reduces
Cost, operation convenient to carry out.
Description of the drawings
Fig. 1 is the method flow schematic diagram that the embodiment of the present invention prepares spherical zirconia powder；
Fig. 2 is the XRD spectra of spherical zirconia powder prepared by the embodiment of the present invention two, three；
Fig. 3 is the scanning electron microscope schematic diagram of spherical zirconia powder prepared by the embodiment of the present invention four；
Fig. 4 is the scanning electron microscope schematic diagram of spherical zirconia powder prepared by the embodiment of the present invention five；
Fig. 5 is the scanning electron microscope schematic diagram of spherical zirconia powder prepared by the embodiment of the present invention five.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing to embodiment party of the present invention
Formula is further described.
Embodiment one
With reference to attached drawing 1, an embodiment of the present invention provides a kind of method that presoma comminution granulation prepares spherical zirconia powder,
Include the following steps：
1) mixed solution is prepared：Zirconates is dissolved in deionized water, obtains solution A, yttrium salt is dissolved in deionized water, is obtained molten
A, B solution are uniformly mixed to obtain mixed solution by liquid B；Wherein, solution A be basic zirconium chloride, acetic acid zirconium or zirconium nitrate solution,
Zirconium ion concentration is 0.1mol/L~1.0mol/L；Solution B be yttrium nitrate, yttrium chloride or yttrium sulfate solution, ruthenium ion concentration
For 0.1mol/L~0.5mol/L, wherein ruthenium ion and zirconium ion molar ratio are 3~5：100；
2) sediment is prepared：Obtained mixed solution is instilled dropwise in ammonium hydroxide or ammonium oxalate solution, precipitation is formed, stirs
Ageing obtains sediment after mixing；Wherein, mixing time is 1~2h, digestion time for 12~for 24 hours；It is prepared by coprecipitation method
Hydroxide colloid, at low cost, required equipment is simple, convenient for large-scale industrial production；
3) washing process：By sediment, removal foreign ion obtains presoma object after ceramic membrane, press filtration processing；
4) slurry is granulated：The slurry that obtained presoma object is handled with acidulant, is set using spray drying
Precursor spherical powder is prepared for be granulated；The acidulant is hydrochloric acid, nitric acid is either between dilute sulfuric acid or two kinds
Arbitrary proportioning；The solid content of the slurry is 25%~35%；The mode of the spray drying is centrifugal or two streamings, described
The inlet temperature of spray drying is 150 DEG C~200 DEG C, and outlet temperature is 80 DEG C~120 DEG C；It is directly made by hydroxide slurry
Grain obtains spherical zircite presoma, does not need to be dried, the processes such as azeotropic distillation, shortens technological process；
5) calcination processing：Obtained precursor spherical powder calcination processing is obtained into tetragonal phase structure spherical zircite, and make
Spherical powder is densified to obtain the spherical zircite powder of single cubic phase nano structure.Calcination temperature is 600 DEG C~800 DEG C, and
Heat preservation is 1~5h under corresponding calcination temperature.By once calcining one in directly synthesis zirconium oxide spherical powder, with the relevant technologies
Plasma spheroidization or secondary clacining processing are carried out after secondary granulation again compared to simpler, energy saving.
The spherical zirconia powder obtained using the preparation method of the embodiment of the present invention can directly be satisfied with plasma spray
The hot-spraying techniques demand such as painting, flame-spraying, electric arc spraying can be widely used for preparing various high temperature resistance thermal barrier coatings or anti-height
Temperature, abrasion performance, corrosion-resistant finishes.Applied to industries such as aerospace, gas turbine, ship, automobile, machinery, chemical industry.
Embodiment two
With reference to attached drawing 1, an embodiment of the present invention provides a kind of method that presoma comminution granulation prepares spherical zirconia powder,
Include the following steps：
1) mixed solution is prepared：Zirconates is dissolved in deionized water, obtains solution A, yttrium salt is dissolved in deionized water, is obtained molten
A, B solution are uniformly mixed to obtain mixed solution by liquid B；Wherein, zirconium ion concentration is 0.1mol/L in mixed solution；Ruthenium ion
A concentration of 0.1mol/L；
2) sediment is prepared：Obtained mixed solution is instilled dropwise in ammonium hydroxide or ammonium oxalate solution, precipitation is formed, stirs
Ageing obtains sediment after mixing；Wherein, mixing time 1h, digestion time 12h；
3) washing process：By sediment, removal foreign ion obtains presoma object after ceramic membrane, press filtration processing；
4) slurry is granulated：The slurry that obtained presoma object is handled with acidulant, is set using spray drying
Precursor spherical powder is prepared for be granulated；The solid content of the slurry is 25%；
5) calcination processing：By obtained precursor spherical powder, calcination processing obtains tetragonal phase structure spherical shape oxygen at 800 DEG C
Change zirconium, and spherical powder is made to be densified to obtain the spherical zircite powder of single cubic phase nano structure.
With reference to attached drawing 2, the object of the spherical zirconia powder of preparation is mutually tetragonal phase, and size distribution is 20~70 μm, flowing
Property is 32.25s/50g, apparent density 2.10g/cm3。
Embodiment three
With reference to attached drawing 1, an embodiment of the present invention provides a kind of method that presoma comminution granulation prepares spherical zirconia powder,
Include the following steps：
1) mixed solution is prepared：Zirconates is dissolved in deionized water, obtains solution A, yttrium salt is dissolved in deionized water, is obtained molten
A, B solution are uniformly mixed to obtain mixed solution by liquid B；Wherein, zirconium ion concentration is 1.0mol/L in mixed solution；Ruthenium ion
A concentration of 0.5mol/L；
2) sediment is prepared：Obtained mixed solution is instilled dropwise in ammonium hydroxide or ammonium oxalate solution, precipitation is formed, stirs
Ageing obtains sediment after mixing；Wherein, mixing time 2h, digestion time 18h；
3) washing process：By sediment, removal foreign ion obtains presoma object after ceramic membrane, press filtration processing；
4) slurry is granulated：The slurry that obtained presoma object is handled with acidulant, is set using spray drying
Precursor spherical powder is prepared for be granulated；The solid content of the slurry is 30%；
5) calcination processing：By obtained precursor spherical powder, calcination processing obtains tetragonal phase structure spherical shape oxygen at 700 DEG C
Change zirconium, and spherical powder is made to be densified to obtain the spherical zircite powder of single cubic phase nano structure.
With reference to attached drawing 2, the object of the spherical zirconium Zirconium powder of preparation is mutually tetragonal phase, and size distribution is 30~75 μm, stream
Dynamic property is 35.40s/50g, apparent density 1.91g/cm3。
Example IV
With reference to attached drawing 1, an embodiment of the present invention provides a kind of method that presoma comminution granulation prepares spherical zirconia powder,
Include the following steps：
1) mixed solution is prepared：Zirconates is dissolved in deionized water, obtains solution A, yttrium salt is dissolved in deionized water, is obtained molten
A, B solution are uniformly mixed to obtain mixed solution by liquid B；Wherein, zirconium ion concentration is 0.5mol/L in mixed solution；Ruthenium ion
A concentration of 1.0mol/L；
2) sediment is prepared：Obtained mixed solution is instilled dropwise in ammonium hydroxide or ammonium oxalate solution, precipitation is formed, stirs
Ageing obtains sediment after mixing；Wherein, mixing time 1.5h, digestion time 18h；
3) washing process：By sediment, removal foreign ion obtains presoma object after ceramic membrane, press filtration processing；
4) slurry is granulated：The slurry that obtained presoma object is handled with acidulant, is set using spray drying
Precursor spherical powder is prepared for be granulated；The solid content of the slurry is 30%；
5) calcination processing：By obtained precursor spherical powder, calcination processing obtains tetragonal phase structure spherical shape oxygen at 600 DEG C
Change zirconium, and spherical powder is made to be densified to obtain the spherical zircite powder of single cubic phase nano structure.Remaining is the same as embodiment one.
With reference to attached drawing 3, the object of the spherical zirconium Zirconium powder of preparation is mutually tetragonal phase, and Oxygen potential reaches more than 90%, grain
Degree is distributed as 30~80 μm, mobility 37.52s/50g, apparent density 1.73g/cm3。
Embodiment five
With reference to attached drawing 1, an embodiment of the present invention provides a kind of method that presoma comminution granulation prepares spherical zirconia powder,
Include the following steps：
1) mixed solution is prepared：Zirconates is dissolved in deionized water, obtains solution A, yttrium salt is dissolved in deionized water, is obtained molten
A, B solution are uniformly mixed to obtain mixed solution by liquid B；Wherein, zirconium ion concentration is 0.2mol/L in mixed solution；Ruthenium ion
A concentration of 0.2mol/L；
2) sediment is prepared：Obtained mixed solution is instilled dropwise in ammonium hydroxide or ammonium oxalate solution, precipitation is formed, stirs
Ageing obtains sediment after mixing；Wherein, mixing time 1h, digestion time 12h；
3) washing process：By sediment, removal foreign ion obtains presoma object after ceramic membrane, press filtration processing；
4) slurry is granulated：The slurry that obtained presoma object is handled with acidulant, is set using spray drying
Precursor spherical powder is prepared for be granulated；The solid content of the slurry is 35%；
5) calcination processing：By obtained precursor spherical powder, calcination processing obtains tetragonal phase structure spherical shape oxygen at 700 DEG C
Change zirconium, and spherical powder is made to be densified to obtain the spherical zircite powder of single cubic phase nano structure.Remaining is the same as embodiment one.
With reference to attached drawing 4, the object of the spherical zirconium Zirconium powder of preparation is mutually tetragonal phase, crystallite size is distributed as 10~
100nm, size distribution are 20~70 μm, mobility 36.34s/50g, apparent density 1.80g/cm3。
Embodiment six
With reference to attached drawing 1, an embodiment of the present invention provides a kind of method that presoma comminution granulation prepares spherical zirconia powder,
Include the following steps：
1) mixed solution is prepared：Zirconates is dissolved in deionized water, obtains solution A, yttrium salt is dissolved in deionized water, is obtained molten
A, B solution are uniformly mixed to obtain mixed solution by liquid B；Wherein, zirconium ion concentration is 1.0mol/L in mixed solution；Ruthenium ion
A concentration of 1.0mol/L；
2) sediment is prepared：Obtained mixed solution is instilled dropwise in ammonium hydroxide or ammonium oxalate solution, precipitation is formed, stirs
Ageing obtains sediment after mixing；Wherein, mixing time 2h, digestion time is for 24 hours；
3) washing process：By sediment, removal foreign ion obtains presoma object after ceramic membrane, press filtration processing；
4) slurry is granulated：The slurry that obtained presoma object is handled with acidulant, is set using spray drying
Precursor spherical powder is prepared for be granulated；The solid content of the slurry is 35%；
5) calcination processing：By obtained precursor spherical powder, calcination processing obtains tetragonal phase structure spherical shape oxygen at 800 DEG C
Change zirconium, and spherical powder is made to be densified to obtain the spherical zircite powder of single cubic phase nano structure.Remaining is the same as embodiment one.
With reference to attached drawing 5, the object of the spherical zirconium Zirconium powder of preparation is mutually tetragonal phase, through characterization, spherical zirconium zirconia powder
The crystal grain of body is spherical in shape, and crystallite size is distributed as 10~100nm, and size distribution is 35~90 μm, mobility 30.65s/50g,
Apparent density is 2.06g/cm3。
Herein, the involved nouns of locality such as forward and backward, upper and lower are to be located in figure with parts in attached drawing and zero
Part mutual position defines, only for the purpose of expressing the technical solution clearly and conveniently.It should be appreciated that the noun of locality
Use should not limit the claimed range of the application.
In the absence of conflict, the feature in embodiment and embodiment herein-above set forth can be combined with each other.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of method that presoma comminution granulation prepares spherical zirconia powder, it is characterized in that, by zirconium ion solution and ruthenium ion
It is stirred evenly after solution mixing, making precipitating reagent with ammonium hydroxide or ammonium oxalate forms precipitation, using ceramic membrane separation and filter-pressing method
Solvent is removed, sizes mixing for acidified dose and carries out mist projection granulating, heat treatment is finally carried out and can obtain spherical nanostructure Zirconium powder.
2. the method that a kind of presoma comminution granulation according to claim 1 prepares spherical zirconia powder, it is characterized in that, tool
Body includes the following steps：
1) mixed solution is prepared：Zirconates is dissolved in deionized water, obtains solution A, yttrium salt is dissolved in deionized water, obtains solution B,
A, B solution are uniformly mixed to obtain mixed solution；
2) sediment is prepared：Obtained mixed solution is instilled dropwise in ammonium hydroxide or ammonium oxalate solution, precipitation is formed, after stirring
Ageing obtains sediment；
3) washing process：By sediment, removal foreign ion obtains presoma object after ceramic membrane, press filtration processing；
4) slurry is granulated：The slurry that obtained presoma object is handled with acidulant, using spray drying device into
Row is granulated and precursor spherical powder is prepared；
5) calcination processing：Obtained precursor spherical powder calcination processing is obtained into tetragonal phase structure spherical zircite, and make spherical shape
Powder is densified to obtain spherical zircite powder.
3. the method that a kind of presoma comminution granulation according to claim 2 prepares spherical zirconia powder, it is characterized in that, step
Suddenly in (1), the solution A be basic zirconium chloride, acetic acid zirconium or zirconium nitrate solution, zirconium ion concentration for 0.1mol/L~
1.0mol/L, the solution B for yttrium nitrate, yttrium chloride or yttrium sulfate solution etc., a concentration of 0.1mol/L of ruthenium ion~
0.5mol/L, wherein ruthenium ion are 3~5 with zirconium ion molar ratio：100.
4. the method that a kind of presoma comminution granulation according to claim 2 prepares spherical zirconia powder, it is characterized in that, step
Suddenly in (2), mixing time is 1~2h, digestion time for 12~for 24 hours.
5. the method that a kind of presoma comminution granulation according to claim 2 prepares spherical zirconia powder, it is characterized in that, step
Suddenly in (4), the acidulant is hydrochloric acid, the nitric acid either arbitrary proportioning between dilute sulfuric acid or two kinds；Consolidating for the slurry contains
Amount is 25%~35%；The mode of the spray drying is centrifugal or two streamings, and the inlet temperature of the spray drying is 150
DEG C~200 DEG C, outlet temperature is 80 DEG C~120 DEG C.
6. the method that a kind of presoma comminution granulation according to claim 2 prepares spherical zirconia powder, it is characterized in that, step
Suddenly in (5), calcination temperature is 600 DEG C~800 DEG C, and soaking time is 1~5h.
7. according to the method that a kind of presoma comminution granulation of claim 1~6 any one of them prepares spherical zirconia powder,
It is characterized in that：In step (5), obtained spherical zirconia powder is tetragonal phase grain structure, and crystallite dimension is 10~100nm,
The granularity of spherical powder is 20~90 μm, and powder fluidity is 30~40s/50g, and consistency is 1.6~2.1g/cm3。
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| CN110451956A (en) * | 2019-09-12 | 2019-11-15 | 广东东方锆业科技股份有限公司 | A kind of method that citrate method prepares compound zirconia predecessor |
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| CN110835263A (en) * | 2019-10-31 | 2020-02-25 | 中国船舶重工集团公司第七二五研究所 | Method for preparing zirconia ceramic microspheres |
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| CN113403567A (en) * | 2021-06-25 | 2021-09-17 | 西安热工研究院有限公司 | Nano yttrium oxide stabilized zirconia thermal barrier coating and preparation method thereof |
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| CN114015963A (en) * | 2021-11-09 | 2022-02-08 | 内蒙古工业大学 | Low-thermal-conductivity thermal barrier coating with vertical crack structure and preparation method thereof |
| CN114105212A (en) * | 2021-11-12 | 2022-03-01 | 中国恩菲工程技术有限公司 | Spherical iron oxide and preparation method and application thereof |
| CN116102350A (en) * | 2022-12-27 | 2023-05-12 | 中铝广西有色稀土开发有限公司 | Preparation method of spherical composite zirconia powder |
| CN116425542A (en) * | 2023-03-02 | 2023-07-14 | 河南工程学院 | Method for preparing rare earth tantalate powder for spraying by adopting solid-phase ball milling method |
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| CN110350225B (en) * | 2019-07-05 | 2022-07-19 | 湖南稀土金属材料研究院 | Scandium-zirconium ceramic electrolyte sheet and preparation method thereof |
| CN110467460B (en) * | 2019-09-12 | 2022-03-11 | 广东东方锆业科技股份有限公司 | Method for preparing composite zirconium oxide precursor by oxalate method |
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