CN101723683A - Preparation method of yttrium oxide-stabilized zirconium oxide powder with hollow spherical nanostructure - Google Patents
Preparation method of yttrium oxide-stabilized zirconium oxide powder with hollow spherical nanostructure Download PDFInfo
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Abstract
The invention provides a preparation method of yttrium oxide-stabilized zirconium oxide powder with hollow a spherical nanostructure, belonging to the technical field of material preparation. The method comprises the steps of: taking noncrystal yttrium oxide-stabilized zirconium oxide powder with an amorphous phase structure as raw materials; heating with over-distance plasma flame; collecting by means of water cooling; and drying with low temperature to prepare the yttrium oxide-stabilized zirconium oxide powder with the hollow spherical nanostructure. The prepared powder has the characteristics of low fill density and high fluidity, and the like, and the microstructure is the nanocrystalline hollow spherical nanostructure, therefore, the powder is particularly suitable for a plasma spraying technology to prepare a high-temperature abrasion-resistant good-sealing coating, has simple technological process and high technology content, and can be produced in batch. Meanwhile, the powder material also can be used for the other spraying technologies (such as a hypersonic flame spraying technology and a detonation spraying technology) to prepare an oxygen sensor coating, an oxygen separation membrane, a fuel battery coating, and the like, and can be used for the fields of aerospace, precise instrument, petroleum and electron, etc.
Description
Technical field
The invention belongs to technical field of material, particularly a kind of preparation method of hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder.
Background technology
The yttria-stabilized zirconia ceramic powder material has excellent comprehensive performances such as high temperature under the lower thermal conductivity, high thermal expansion coefficient, 1400 ℃ is stable, anticorrosive mutually, is broad research, the heat barrier coat material that generally adopts now.Because stablizer Y in the zirconium white of stabilized with yttrium oxide
3+Valence mumber and Zr
4+Valence mumber do not wait, for keeping the crystalline electric neutrality thereby at ZrO
2In produced the oxygen room.High-temperature fuel cell solid electrolyte coating and high-temperature fuel cell electrode coating, oxygen sensitive sensor ionogen and the oxygen sensitive sensor electrode coating of using this performance preparation have had comparatively deep research and application.
But problems such as the yttria-stabilized zirconia structure coating of conventional preparation exists, and fragility is serious, coating and the low abradability difference of high base strength.Development in science and technology requires the equipment work temperature to promote significantly, caused the continuous lifting of work package to the coating performance requirement, the all urgent proposition of the bottleneck that the development of the working end of aerospace field and internal combustion turbine runs into needs a kind of new function thermal barrier coating: long service at high temperature, directly form significantly temperature drop at work matrix and working end, to obtain better effect of heat insulation, guarantee matrix works better under lower temperature; Can seal up high-temperature fuel gas again, obtain maximum hydrodynamic force, during work with can abrasive form consumption, thereby guarantee the service life of work package, increase work efficiency.For reaching this requirement, a lot of more deep researchs have been carried out.After traditional yttria-stabilized zirconia ceramic powder plasma spraying, the porosity of preparation coating is generally 2～10%.But and the coating that possesses characteristics such as high rate of closed hole, porous nickel distribute, pore dimension is little heat-proof quality and wear hardness will improve high temperature simultaneously and be on active service the time, to be the intersection point of thermal barrier coating of future generation and high-temperature abrasive coat system development, also be the key point that solves two type coating system development bottlenecks.At present, the method for coat system that can realize the coating porosity constructional feature of the heat insulation abradable seal requirement of new type high temperature has: three kinds of liquid zirconium salt solution injected plasma sprayings, hollow sphere yttrium oxide-stabilized zirconium oxide powder plasma spraying, amorphous yttrium oxide-stabilized zirconium oxide powder plasma spraying.
It is a kind of that people such as Padture etc., Cheng Xudong mentions in its patent and the document published is that raw material passes through the ceramic coating to a kind of porosity height of the final preparation of the transformation of thermal plasma spraying equipment feeding part, even pore distribution with the liquid phase.But, adopt this method to have numerous defectives such as sedimentation effect is low, anchoring strength of coating is little, coat-thickness is little.Simultaneously, this method need be transformed equipment, and scrap build has high input, and is difficult for realizing.
Sulzer metco company, General Electric company have mentioned and have adopted novel hollow zirconia ceramics powder to carry out plasma spraying, and coating has soft, the porous of coating matter, and void content is greatly about 25%～30% constructional feature.But the powder size of this method preparation is bigger, also have bigger hole, and macrovoid tends to cause generation of defects.
The novel amorphous yttria-stabilized zirconia ceramic spherical powdered material of employings such as Lin Feng is that raw material prepares a kind of special composite structure that novel high-performance ceramic coating system has nano particle and the common composition of honeycomb-like network by atmospheric plasma spraying.
At present, still less than research and patent report about hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method of hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder, it is characterized in that, the preparation method is:
(1) the amorphous yttrium oxide-stabilized zirconium oxide powder of preparation amorphous phase structure,
1. according to the weight ratio Yttrium trichloride: zirconium oxychloride=1: 10～get Yttrium trichloride, zirconium oxychloride at 1: 40 is added to the water Yttrium trichloride and zirconium oxychloride, fully dissolving and thorough mixing;
2. add concentration evenly and rapidly and be 20～60% ammoniacal liquor and make two kinds of salt co-precipitation, obtain having the yttria-stabilized zirconia of crystal water, ageing 1～12h obtains gel;
3. gel and water or alcohol are carried out thorough mixing according to mass ratio at 1: 1, in mixed solution, add dispersion agent and binding agent, dispersion agent adopts ethylene glycol, add-on is to account for 0.5～5% of slurry weight percentage composition, binding agent adopts polyvinyl alcohol, and add-on is to account for 0.5～5% of slurry weight percentage composition;
4. ball milling 40～80min, ultrasonic dispersing 0～3h is made into slurry behind the ball milling;
5. the slurry with preparation carries out spraying drying, obtains the amorphous yttrium oxide-stabilized zirconium oxide powder of amorphous phase structure;
(2) the amorphous yttrium oxide-stabilized zirconium oxide powder of amorphous phase structure is put into the plasma powder feeder, carry out the plasma flame heating, powder feeding rate is 15～100g/min, powder feeding air pressure is 4～10L/min, operating voltage is 55～80V, the plasma body working current is 500～650A, the heated length of plasma flame is 150～250mm, plasma body master gas is argon gas and nitrogen or wherein a kind of, the auxilliary gas of plasma body is hydrogen, the pressure of water cycle cooling spray gun is 1.5～1.8MPa, and the air cooling distance that powder particle is complete is 2～4.5m;
(3) powder water-cooled in stainless steel vessel is collected, and the powder of plasma heating collides mutually with the water molecules that is in 10～40 ℃, wetting, rapid condensation 0.5～3min;
(4) condensed powder is dried down at 50～150 ℃, obtain hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder.
The phase structure of described hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder be cube with the mixed phase of amorphous phase or cube with the mixed phase of monocline phase.
Beneficial effect of the present invention is:
The present invention can prepare the nanocrystalline hollow sphere ceramic powder material of 3～15% Yttrium oxide doping zirconium oxides, the hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder of preparation has characteristics such as low-apparent-density, high workability, microtexture is nanocrystalline hollow sphere structure, be particularly suitable for plasma spraying prepared high-temperature abradable seal coating, and this technical process is simple, equipment and technology content height can be produced in batches.Simultaneously, this powdered material also can be used for other spraying coating process (as hypersonic flame spraying, detonation flame spraying technology) preparation oxygen sensor coating, oxygen separation membrane, fuel cell coating etc., is applied to fields such as aerospace, precision instrument, oil, electronics.
Description of drawings
Fig. 1 is the hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder crystalline phase microphotograph of embodiment 1 preparation;
Fig. 2 is the hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder scanning electron microscope pattern photo of embodiment 1 preparation;
Fig. 3 is the hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder X-ray diffraction analysis collection of illustrative plates of embodiment 1 preparation.
Embodiment
The invention will be further described below in conjunction with embodiment and accompanying drawing:
Embodiment 1
A kind of preparation method of hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder:
(1) the amorphous yttrium oxide-stabilized zirconium oxide powder of preparation amorphous phase structure,
1. according to the weight ratio Yttrium trichloride: zirconium oxychloride=get Yttrium trichloride, zirconium oxychloride at 1: 11 is added to the water Yttrium trichloride and zirconium oxychloride, fully dissolving and thorough mixing;
2. add concentration evenly and rapidly and be 40% ammoniacal liquor and make two kinds of salt co-precipitation, obtain having the yttria-stabilized zirconia of crystal water, ageing 5h obtains gel;
3. gel and water are carried out thorough mixing according to mass ratio at 1: 1, add dispersion agent and binding agent in mixed solution, dispersion agent adopts ethylene glycol, and add-on is to account for 3% of slurry weight percentage composition, binding agent adopts polyvinyl alcohol, and add-on is to account for 3% of slurry weight percentage composition;
4. ball milling 60min, ultrasonic dispersing 2h is made into slurry behind the ball milling;
5. the slurry with preparation carries out spraying drying, obtains the amorphous yttrium oxide-stabilized zirconium oxide powder of amorphous phase structure;
(2) the amorphous yttrium oxide-stabilized zirconium oxide powder of amorphous phase structure is put into the plasma powder feeder, carry out the plasma flame heating, powder feeding rate is 30g/min, and powder feeding air pressure is 6L/min, and operating voltage is 75V, the plasma body working current is 600A, the heated length of plasma flame is 150mm, and plasma body master gas is argon gas, and the auxilliary gas of plasma body is hydrogen, the pressure of water cycle cooling spray gun is 1.5MPa, and the air cooling distance that powder particle is complete is 3m;
(3) powder water-cooled in stainless steel vessel is collected, and the powder of plasma heating collides mutually with the water molecules that is in 15 ℃, wetting, rapid condensation 1.5min;
(4) condensed powder is dried down at 130 ℃, obtain hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder.
The phase structure of the hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder of preparing for cube with the mixed phase of amorphous phase, hollow structure is even, average grain size 160nm is the hollow nano spherical ceramic powdered material of 8% Yttrium oxide doping zirconium oxide.
Fig. 1 is the hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder crystalline phase microphotograph of embodiment 1 preparation, hollow structure by the metallographicobservation powder is even, Fig. 2 is the hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder scanning electron microscope pattern photo of embodiment 1 preparation, the surface topography of observing powder by photo is subsphaeroidal, and Fig. 3 is the hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder X-ray diffraction analysis collection of illustrative plates of embodiment 1 preparation.Obtain zirconic phase composition by analysis and be mainly a cube phase.
The loose density and the flowability that adopt international detection method to measure powder are: loose density 1.9g/cm
3, velocity of flow 32s/50g.
Embodiment 2
A kind of preparation method of hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder:
(1) the amorphous yttrium oxide-stabilized zirconium oxide powder of preparation amorphous phase structure,
1. according to the weight ratio Yttrium trichloride: zirconium oxychloride=get Yttrium trichloride, zirconium oxychloride at 1: 11 is added to the water Yttrium trichloride and zirconium oxychloride, fully dissolving and thorough mixing;
2. add concentration evenly and rapidly and be 30% ammoniacal liquor and make two kinds of salt co-precipitation, obtain having the yttria-stabilized zirconia of crystal water, ageing 4h obtains gel;
3. gel and alcohol are carried out thorough mixing according to mass ratio at 1: 1, add dispersion agent and binding agent in mixed solution, dispersion agent adopts ethylene glycol, and add-on is to account for 2% of slurry weight percentage composition, binding agent adopts polyvinyl alcohol, and add-on is to account for 4% of slurry weight percentage composition;
4. ball milling 50min, ultrasonic dispersing 3h is made into slurry behind the ball milling;
5. the slurry with preparation carries out spraying drying, obtains the amorphous yttrium oxide-stabilized zirconium oxide powder of amorphous phase structure;
(2) the amorphous yttrium oxide-stabilized zirconium oxide powder of amorphous phase structure is put into the plasma powder feeder, carry out the plasma flame heating, powder feeding rate is 45g/min, and powder feeding air pressure is 6L/min, and operating voltage is 70V, the plasma body working current is 580A, the heated length of plasma flame is 200mm, and plasma body master gas is argon gas, and the auxilliary gas of plasma body is hydrogen, the pressure of water cycle cooling spray gun is 1.6MPa, and the air cooling distance that powder particle is complete is 2.5m;
(3) powder water-cooled in stainless steel vessel is collected, and the powder of plasma heating collides mutually with the water molecules that is in 18 ℃, wetting, rapid condensation 2min;
(4) condensed powder is dried down at 120 ℃, obtain hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder.
The phase structure of the hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder of preparing for cube with the mixed phase of amorphous phase, hollow structure is even, average grain size 135nm is the hollow nano spherical ceramic powdered material of 8% Yttrium oxide doping zirconium oxide.
The loose density and the flowability that adopt international detection method to measure powder are: loose density 2.2g/cm
3, velocity of flow 30s/50g.
Embodiment 3
A kind of preparation method of hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder:
(1) the amorphous yttrium oxide-stabilized zirconium oxide powder of preparation amorphous phase structure,
1. according to the weight ratio Yttrium trichloride: zirconium oxychloride=get Yttrium trichloride, zirconium oxychloride at 1: 11 is added to the water Yttrium trichloride and zirconium oxychloride, fully dissolving and thorough mixing;
2. add concentration evenly and rapidly and be 50% ammoniacal liquor and make two kinds of salt co-precipitation, obtain having the yttria-stabilized zirconia of crystal water, ageing 4h obtains gel;
3. gel and water are carried out thorough mixing according to mass ratio at 1: 1, add dispersion agent and binding agent in mixed solution, dispersion agent adopts ethylene glycol, and add-on is to account for 4% of slurry weight percentage composition, binding agent adopts polyvinyl alcohol, and add-on is to account for 2% of slurry weight percentage composition;
4. ball milling 40min, ultrasonic dispersing 2.5h is made into slurry behind the ball milling;
5. the slurry with preparation carries out spraying drying, obtains the amorphous yttrium oxide-stabilized zirconium oxide powder of amorphous phase structure;
(2) the amorphous yttrium oxide-stabilized zirconium oxide powder of amorphous phase structure is put into the plasma powder feeder, carry out the plasma flame heating, powder feeding rate is 35g/min, and powder feeding air pressure is 6L/min, and operating voltage is 78V, the plasma body working current is 650A, the heated length of plasma flame is 250mm, and plasma body master gas is argon gas, and the auxilliary gas of plasma body is hydrogen, the pressure of water cycle cooling spray gun is 1.8MPa, and the air cooling distance that powder particle is complete is 4m;
(3) powder water-cooled in stainless steel vessel is collected, and the powder of plasma heating collides mutually with the water molecules that is in 20 ℃, wetting, rapid condensation 3min;
(4) condensed powder is dried down at 110 ℃, obtain hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder.
The phase structure of the hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder of preparing for cube with monocline mixed phase mutually, hollow structure is even, average grain size 178nm is the hollow nano spherical ceramic powdered material of 8% Yttrium oxide doping zirconium oxide.
The loose density and the flowability that adopt international detection method to measure powder are: loose density 2.0g/cm
3, velocity of flow 35s/50g.
Claims (2)
1. the preparation method of a hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder is characterized in that, the preparation method is:
(1) the amorphous yttrium oxide-stabilized zirconium oxide powder of preparation amorphous phase structure,
1. according to the weight ratio Yttrium trichloride: zirconium oxychloride=1: 10～get Yttrium trichloride, zirconium oxychloride at 1: 40 is added to the water Yttrium trichloride and zirconium oxychloride, fully dissolving and thorough mixing;
2. add concentration evenly and rapidly and be 20～60% ammoniacal liquor and make two kinds of salt co-precipitation, obtain having the yttria-stabilized zirconia of crystal water, ageing 1～12h obtains gel;
3. gel and water or alcohol are carried out thorough mixing according to mass ratio at 1: 1, in mixed solution, add dispersion agent and binding agent, dispersion agent adopts ethylene glycol, add-on is to account for 0.5～5% of slurry weight percentage composition, binding agent adopts polyvinyl alcohol, and add-on is to account for 0.5～5% of slurry weight percentage composition;
4. ball milling 40～80min, ultrasonic dispersing 0～3h is made into slurry behind the ball milling;
5. the slurry with preparation carries out spraying drying, obtains the amorphous yttrium oxide-stabilized zirconium oxide powder of amorphous phase structure;
(2) the amorphous yttrium oxide-stabilized zirconium oxide powder of amorphous phase structure is put into the plasma powder feeder, carry out the plasma flame heating, powder feeding rate is 15～100g/min, powder feeding air pressure is 4～10L/min, operating voltage is 55～80V, the plasma body working current is 500～650A, the heated length of plasma flame is 150～250mm, plasma body master gas is argon gas and nitrogen or wherein a kind of, the auxilliary gas of plasma body is hydrogen, the pressure of water cycle cooling spray gun is 1.5～1.8MPa, and the air cooling distance that powder particle is complete is 2～4.5m;
(3) powder water-cooled in stainless steel vessel is collected, and the powder of plasma heating collides mutually with the water molecules that is in 10～40 ℃, wetting, rapid condensation 0.5～3min;
(4) condensed powder is dried down at 50～150 ℃, obtain hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder.
2. the preparation method of a kind of hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder according to claim 1, it is characterized in that, the phase structure of described hollow sphere nanostructure yttrium oxide-stabilized zirconium oxide powder be cube with the mixed phase of amorphous phase or cube with the mixed phase of monocline phase.
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| CN102145913A (en) * | 2011-04-21 | 2011-08-10 | 北京矿冶研究总院 | Preparation method of nano spherical yttrium oxide powder for thermal spraying |
| CN102296263A (en) * | 2010-06-25 | 2011-12-28 | 中国科学院微电子研究所 | Modification treatment method for inner surface of plasma etching process chamber |
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| CN107915484A (en) * | 2017-12-12 | 2018-04-17 | 苏州炻原新材料科技有限公司 | A kind of preparation method of shell structure Zirconium oxide powder used for hot spraying |
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| ATE405686T1 (en) * | 2005-06-16 | 2008-09-15 | Sulzer Metco Us Inc | ALUMINUM OXIDE DOPED WEARABLE CERAMIC MATERIAL |
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| CN102863254A (en) * | 2011-07-08 | 2013-01-09 | 黄世鲜 | Nano-particle material and preparation method thereof |
| CN102863254B (en) * | 2011-07-08 | 2014-08-20 | 黄世鲜 | Nano-particle material and preparation method thereof |
| CN104492266A (en) * | 2014-12-26 | 2015-04-08 | 合肥创想能源环境科技有限公司 | Multi-channel tubular ceramic membrane element |
| CN105720250A (en) * | 2016-02-21 | 2016-06-29 | 钟玲珑 | Preparation method of graphene/zirconium dioxide hollow sphere/sulfur composite material |
| CN107740031A (en) * | 2017-12-12 | 2018-02-27 | 苏州炻原新材料科技有限公司 | A kind of shell structure Zirconium oxide powder used for hot spraying |
| CN107915484A (en) * | 2017-12-12 | 2018-04-17 | 苏州炻原新材料科技有限公司 | A kind of preparation method of shell structure Zirconium oxide powder used for hot spraying |
| CN107915484B (en) * | 2017-12-12 | 2020-12-01 | 苏州炻原新材料科技有限公司 | Preparation method of thin-shell-structure zirconium oxide powder for thermal spraying |
| CN111217605A (en) * | 2019-12-30 | 2020-06-02 | 西安航天复合材料研究所 | Method and device for preparing large-particle-size thin-wall hollow sphere zirconia powder |
| CN111217606A (en) * | 2020-02-24 | 2020-06-02 | 东莞市永笃纳米科技有限公司 | Zirconia micro-bead nano material and preparation method thereof |
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Address after: 100088, 2, Xinjie street, Beijing Co-patentee after: Youyan Powder New Materials Co.,Ltd. Patentee after: GENERAL Research Institute FOR NONFERROUS METALS Address before: 100088, 2, Xinjie street, Beijing Co-patentee before: GRIPM ADVANCED MATERIALS Co.,Ltd. Patentee before: General Research Institute for Nonferrous Metals |
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Effective date of registration: 20190809 Address after: 101407 Beijing city Huairou District Yanqi Yanqi Economic Development Zone South four Street No. 12 Patentee after: Youyan Powder New Materials Co.,Ltd. Address before: 100088, 2, Xinjie street, Beijing Co-patentee before: Youyan Powder New Materials Co.,Ltd. Patentee before: General Research Institute for Nonferrous Metals |