CN103232238A - Preparation method of high-strength electric smelting zirconia ceramic ball - Google Patents
Preparation method of high-strength electric smelting zirconia ceramic ball Download PDFInfo
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Abstract
The invention relates to a preparation method of a high-strength electric smelting zirconia ceramic ball. The preparation method comprises the following steps of: carrying out special superfine grinding on monoclinic type electric smelting zirconia powder with the ZrO2+HfO2 content higher than 99.6%, so that the monoclinic type electric smelting zirconia powder achieves characteristics which are extremely similar to those of a chemical zirconia electrode; and preparing the high-strength ceramic ball with high abrasion performance by adopting the forming processes and sintering processes including spray granulation, cold isostatic forming, sintering, polishing and the like, wherein the density of the high-strength ceramic ball is higher than 6.00g/cm<3>, and the hardness HV of the high-strength ceramic ball exceeds 1250. And therefore, the preparation method can be used for breaking through the technical bottleneck of preparing the high-strength ceramic ball by the electric smelting zirconia, greatly lowering the production cost and enabling the application prospect to be very extensive.
Description
Technical field
The present invention relates to the ceramic technology field, is a kind of preparation method of high strength electric-melting zirconia Ceramic Balls specifically.
Background technology
Excellent specific properties such as the zirconia ceramics ball is high temperature resistant because having, corrosion-resistant, wear resistance is strong, toughness is better, high rigidity, rigidity height, mainly be applied to fields such as grinding medium, bearing, sealing member, be widely used in extra-fine grinding and the dispersion of industry materials such as nonmetalliferous ore, coating, printing ink, paint, dyestuff, titanium dioxide, agricultural chemicals, magneticsubstance, food, medicine, makeup.
The yttrium stable zirconium oxide that the production technology of existing zirconia ceramics ball generally adopts chemical method production to obtain is made raw material, and is expensive, limited the further application of zirconia ceramics ball to a certain extent.Zirconium white is divided into chemical oxidation zirconium and electric-melting zirconia by the difference of production technique.The chemical oxidation zirconium is the explained hereafter that adopts chemical industry for making chlorine and alkali and high-temperature calcination, and product purity height, quality are good, but the technological process of production is longer, need to consume a large amount of acid-base reagents, and production cost is higher; Electric-melting zirconia then is to adopt the physical method of arc melting to produce, and technical process is shorter, and production cost is lower, only is 2/3 of chemical oxidation zirconium generally, but the purity of product and some physicalies are poor slightly.In recent years, along with improving constantly of electric-melting zirconia production technology, all there had been very big change aspects such as the purity of its product, granularity and activity, and electric-melting zirconia is in the structural ceramics field, and especially the application of Ceramic Balls will become a reality.
Utilize zirconium white to prepare Ceramic Balls, present present Research is: be main raw material with the chemical oxidation zirconium, adopt isostatic pressing method, can produce high-intensity Ceramic Balls, but production cost is higher, be difficult to apply on a large scale; Be main raw material with the electric-melting zirconia, though cost is lower, because influences such as oxidated zirconium purity, globule size, granule-morphology, free-running property are difficult to prepare high-intensity zirconia ceramics ball, therefore, restricted the large-scale industrialization application.
Summary of the invention
In order to overcome the defective of above-mentioned prior art, technical problem to be solved by this invention provides a kind of preparation method of high strength electric-melting zirconia Ceramic Balls, overcome the deficiency that electric-melting zirconia exists at aspects such as purity, granularity and activity, adopt rational moulding and sintering process, for the electric-melting zirconia Ceramic Balls for preparing low-cost high-strength provides feasible method.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
A kind of preparation method of high strength electric-melting zirconia Ceramic Balls may further comprise the steps:
Step 1, select ZrO for use
2+ HfO
2Content is ground to mean particle size D 50 with it and reaches below 0.6 micron at the electric-melting zirconia powder of the monocline type more than 99.6%, and D90 reaches below 1.2 microns, and D97 reaches below 1.5 microns;
Step 2, adding stablizer and fully mixing in ground electric-melting zirconia ultrafine powder;
Step 3, the material that mixes is carried out spray granulating and drying;
Step 4, the granulation powder is adopted cold isostatic compaction;
Step 5, with the Ceramic Balls base substrate of forming after burning till, polishing, make high strength electric-melting zirconia Ceramic Balls.
Wherein, in step 2, add the 3mol% yttrium oxide as stablizer, the purity of yttrium oxide is more than 99.9%, and D50 is less than 0.5 micron.
Wherein, in step 4, the granulation powder is adopted cold isostatic compaction under 200～300MPa pressure.
Wherein, also comprise baking step between step 4 and step 5, bake out temperature is 120～150 ℃.
Wherein, in step 5, described Ceramic Balls base substrate burns till according to following sintering curve:
Normal temperature～300 ℃, 0.5～2 ℃/min of temperature rise rate;
300～600 ℃, 1～3 ℃/min of temperature rise rate;
600 ℃ of insulation 2～4h;
600～1100 ℃, 1～3 ℃/min of temperature rise rate;
1100 ℃ of insulation 1～2h;
1100～1650 ℃, 1500～1650 ℃ of top temperatures, 0.5～2 ℃/min of temperature rise rate is incubated 4～8h under the top temperature;
Naturally be cooled to 200 ℃, kiln discharge.
Preparation method provided by the present invention, carry out special extra-fine grinding processing by the electric-melting zirconia powder to monocline type, make it reach the characteristic very similar to the chemical oxidation zirconium, by rational moulding process and firing process, prepared density at 6.00g/cm again
3More than, hardness HV surpasses 1250, and the high-strength ceramic ball with high-wearing feature has been broken through the technical bottleneck that electric-melting zirconia prepares the high-strength ceramic ball, has reduced production cost significantly, and application prospect is very wide.
Embodiment
By describing technology contents of the present invention, structural attitude in detail, realized purpose and effect, give explanation below in conjunction with embodiment is detailed.
Embodiment 1
(1) gets ZrO
2+ HfO
2Content is the electric-melting zirconia powder 94.6kg of 99.6% monocline type, adopt ultra-fine stirring mill that it is ground, by adjusting and control the parameters such as proportioning, rotating speed and liquid-solid ratio of the zirconium oxide bead of grinding machine, its mean particle size D 50 is reached about 0.6 micron, D90 reaches below 1.2 microns, D97 reaches below 1.5 microns, through scanning electron microscope analysis, and the particle almost spherical of electric-melting zirconia ultrafine powder;
(2) in ground electric-melting zirconia ultrafine powder, add the 5.4kg yttrium oxide, the purity of yttrium oxide is more than 99.9%, and D50 adds 100kg water again less than 0.5 micron, add organic alcohols polymkeric substance 1kg, in agitating ball mill, fully be mixed and made into the suspension slip;
(3) the suspension slip is carried out mist projection granulating in centrifugal spray dryer, obtain granularity and be 80～120 microns granulation powder;
(4) the granulation powder is packed into grinding tool, moulding in cold isostatic press, forming pressure is 200MPa;
(5) with the Ceramic Balls base substrate oven dry of forming, bake out temperature is controlled at 120 ℃;
(6) burn till: the Ceramic Balls base substrate is put into sintering oven, burn till according to following sintering curve:
Normal temperature～300 ℃, 1 ℃/min of temperature rise rate;
300～600 ℃, 2 ℃/min of temperature rise rate;
600 ℃ of insulation 3h;
600～1100 ℃, 2 ℃/min of temperature rise rate;
1100 ℃ of insulation 2h;
1100～1500 ℃, 1 ℃/min of temperature rise rate, 1500 ℃ of insulation 8h;
Cool to 200 ℃ with the furnace, kiln discharge obtains sintered body;
(7) sintered body is polished, can obtain density is 6.00g/cm
3High strength electric-melting zirconia Ceramic Balls, record hardness HV and reach 1256.
Embodiment 2
(1) gets ZrO
2+ HfO
2Content is the electric-melting zirconia powder 94.6kg of 99.7% monocline type, adopt ultra-fine stirring mill that it is ground, by adjusting and control the parameters such as proportioning, rotating speed and liquid-solid ratio of the zirconium oxide bead of grinding machine, its mean particle size D 50 is reached about 0.4 micron, D90 reaches below 1 micron, D97 reaches below 1.2 microns, through scanning electron microscope analysis, and the particle almost spherical of electric-melting zirconia ultrafine powder;
(2) in ground electric-melting zirconia ultrafine powder, add the 5.4kg yttrium oxide, the purity of yttrium oxide is more than 99.9%, and D50 adds 100kg water again less than 0.5 micron, add organic alcohols polymkeric substance 1kg, in agitating ball mill, fully be mixed and made into the suspension slip;
(3) the suspension slip is carried out mist projection granulating in centrifugal spray dryer, obtain granularity and be 80～120 microns granulation powder;
(4) the granulation powder is packed into grinding tool, moulding in cold isostatic press, forming pressure is 300MPa;
(5) with the Ceramic Balls base substrate oven dry of forming, bake out temperature is controlled at 150 ℃;
(6) burn till: the Ceramic Balls base substrate is put into sintering oven, burn till according to following sintering curve:
Normal temperature～300 ℃, 1 ℃/min of temperature rise rate;
300～600 ℃, 2 ℃/min of temperature rise rate;
600 ℃ of insulation 4h;
600～1100 ℃, 2 ℃/min of temperature rise rate;
1100 ℃ of insulation 2h;
1100～1650 ℃, 1 ℃/min of temperature rise rate, 1650 ℃ of insulation 8h;
Cool to 200 ℃ with the furnace, kiln discharge obtains sintered body;
(7) sintered body is polished, can obtain density is 6.02g/cm
3High strength electric-melting zirconia Ceramic Balls, record hardness HV and reach 1260.
The above only is embodiments of the invention; be not so limit claim of the present invention; every equivalent structure or equivalent flow process conversion that utilizes description of the present invention to do; or directly or indirectly be used in other relevant technical fields, all in like manner be included in the scope of patent protection of the present invention.
Claims (5)
1. the preparation method of a high strength electric-melting zirconia Ceramic Balls may further comprise the steps:
Step 1, select ZrO for use
2+ HfO
2Content is ground to mean particle size D 50 with it and reaches below 0.6 micron at the electric-melting zirconia powder of the monocline type more than 99.6%, and D90 reaches below 1.2 microns, and D97 reaches below 1.5 microns;
Step 2, adding stablizer and fully mixing in ground electric-melting zirconia ultrafine powder;
Step 3, the material that mixes is carried out spray granulating and drying;
Step 4, the granulation powder is adopted cold isostatic compaction;
Step 5, with the Ceramic Balls base substrate of forming after burning till, polishing, make high strength electric-melting zirconia Ceramic Balls.
2. the preparation method of high strength electric-melting zirconia Ceramic Balls according to claim 1 is characterized in that: in step 2, add the 3mol% yttrium oxide as stablizer, the purity of yttrium oxide is more than 99.9%, and D50 is less than 0.5 micron.
3. the preparation method of high strength electric-melting zirconia Ceramic Balls according to claim 1 is characterized in that: in step 4, the granulation powder is adopted cold isostatic compaction under 200～300MPa pressure.
4. the preparation method of high strength electric-melting zirconia Ceramic Balls according to claim 1 is characterized in that: comprise also that between step 4 and step 5 baking step, bake out temperature are 120～150 ℃.
5. the preparation method of high strength electric-melting zirconia Ceramic Balls according to claim 1, it is characterized in that: in step 5, described Ceramic Balls base substrate burns till according to following sintering curve:
Normal temperature～300 ℃, 0.5～2 ℃/min of temperature rise rate;
300～600 ℃, 1～3 ℃/min of temperature rise rate;
600 ℃ of insulation 2～4h;
600～1100 ℃, 1～3 ℃/min of temperature rise rate;
1100 ℃ of insulation 1～2h;
1100～1650 ℃, 1500～1650 ℃ of top temperatures, 0.5～2 ℃/min of temperature rise rate is incubated 4～8h under the top temperature;
Naturally be cooled to 200 ℃, kiln discharge.
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Cited By (4)
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| CN104528823A (en) * | 2015-01-06 | 2015-04-22 | 武汉拓柏仕科技有限公司 | Zirconia powder, product thereof and preparation method thereof |
| CN105813964A (en) * | 2013-12-17 | 2016-07-27 | 京瓷株式会社 | Fiber guide |
| CN110845245A (en) * | 2019-12-13 | 2020-02-28 | 中钢集团洛阳耐火材料研究院有限公司 | Compact high-purity zirconia refractory product |
| CN111747743A (en) * | 2020-06-12 | 2020-10-09 | 广州凯立达电子股份有限公司 | Spherical piezoelectric ceramic and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104529506B (en) * | 2015-01-16 | 2016-08-17 | 临江北峰硅藻土有限公司 | A kind of preparation method of composite natral porous mineral ceramic fine bead |
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| CN102241510A (en) * | 2010-05-13 | 2011-11-16 | 郑州振中电熔锆业有限公司 | Electric melting method for manufacturing yttria stabilized zirconia |
| US20120175826A1 (en) * | 2008-09-29 | 2012-07-12 | Christos Aneziris | Material composition for producing a fireproof material and the use thereof, and fireproof moulding body and method for the production thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105813964A (en) * | 2013-12-17 | 2016-07-27 | 京瓷株式会社 | Fiber guide |
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| CN110845245B (en) * | 2019-12-13 | 2022-03-01 | 中钢集团洛阳耐火材料研究院有限公司 | Compact high-purity zirconia refractory product |
| CN111747743A (en) * | 2020-06-12 | 2020-10-09 | 广州凯立达电子股份有限公司 | Spherical piezoelectric ceramic and preparation method thereof |
| CN111747743B (en) * | 2020-06-12 | 2022-08-12 | 广州凯立达电子股份有限公司 | Spherical piezoelectric ceramic and preparation method thereof |
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