CN103232238B - 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 ceramic technology field, is a kind of preparation method of high strength electric-melting zirconia Ceramic Balls specifically.
Background technology
The excellent specific properties such as 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 the fields such as grinding medium, bearing, sealing member, be widely used in extra-fine grinding and the dispersion of the industry materials such as nonmetalliferous ore, coating, ink, paint, dyestuff, titanium dioxide, agricultural chemicals, magneticsubstance, food, medicine, makeup.
The production technology of existing zirconia ceramics ball generally adopts chemical method to produce the yttrium stable zirconium oxide obtaining and makes raw material, expensive, has limited to a certain extent the further application of zirconia ceramics ball.Zirconium white, by the difference of production technique, is divided into chemical oxidation zirconium and electric-melting zirconia.Chemical oxidation zirconium is the explained hereafter that adopts chemical industry for making chlorine and alkali and high-temperature calcination, and product purity is high, quality 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 is to adopt the physical method of arc melting to produce, and technical process is shorter, and production cost is lower, is generally only 2/3 of chemical oxidation zirconium, but the purity of product and some physicalies are slightly poor.In recent years, along with improving constantly of electric-melting zirconia production technology, all there had been very large change the aspects such as the purity of its product, granularity and activity, and electric-melting zirconia is in structural ceramics field, and especially the application of Ceramic Balls will become a reality.
Utilize zirconium white to prepare Ceramic Balls, current present Research is: take chemical oxidation zirconium as main raw material, adopt isostatic pressing method, can produce high-intensity Ceramic Balls, but production cost is higher, be difficult to apply on a large scale; Take electric-melting zirconia as main raw material, although cost is lower, due to impacts such as oxidated zirconium purity, globule size, granule-morphology, free-running properties, be difficult to prepare high-intensity zirconia ceramics ball, therefore, restricted large-scale industrialization application.
Summary of the invention
In order to overcome the defect of above-mentioned prior art, technical problem to be solved by this invention is to provide 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 preparing the electric-melting zirconia Ceramic Balls of low-cost high-strength, provide feasible method.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
A preparation method for high strength electric-melting zirconia Ceramic Balls, comprises the following steps:
Step 1, select ZrO
2+ HfO
2content, at the electric-melting zirconia powder of more than 99.6% monocline type, is ground to mean particle size D 50 and is reached below 0.6 micron, and D90 reaches below 1.2 microns, and D97 reaches below 1.5 microns;
Step 2, in ground electric-melting zirconia ultrafine powder, add stablizer and fully mix;
Step 3, the material mixing is carried out to spray granulating and drying;
Step 4, pelletizing is adopted to cold isostatic compaction;
Step 5, by the Ceramic Balls base substrate of forming through burning till, after polishing, make high strength electric-melting zirconia Ceramic Balls.
Wherein, in step 2, add 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, pelletizing is adopted to 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 top temperature;
Naturally be cooled to 200 ℃, kiln discharge.
Preparation method provided by the present invention, by the electric-melting zirconia powder to monocline type, carry out special extra-fine grinding processing, make it reach the characteristic very similar to chemical oxidation zirconium, then by rational moulding process and firing process, prepared density at 6.00g/cm
3above, hardness HV surpasses 1250, have the high-strength ceramic ball of high-wearing feature, has broken through the technical bottleneck that electric-melting zirconia is prepared high-strength ceramic ball, has significantly reduced production cost, and application prospect is very wide.
Embodiment
By describing technology contents of the present invention, structural attitude in detail, being realized object and effect, below in conjunction with embodiment, be explained in detail.
Embodiment 1
(1) get ZrO
2+ HfO
2content is the electric-melting zirconia powder 94.6kg of 99.6% monocline type, adopt Superfine Stirred Mill to grind, by adjusting and control the parameters such as proportioning, rotating speed and liquid-solid ratio of the zirconium oxide bead of grinding machine, make its mean particle size D 50 reach 0.6 micron of left and right, 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 5.4kg yttrium oxide, the purity of yttrium oxide is more than 99.9%, and D50 is less than 0.5 micron, then adds 100kg water, add organic alcohols polymkeric substance 1kg, in agitating ball mill, be fully mixed and made into suspension slip;
(3) suspension slip is carried out in centrifugal spray dryer to mist projection granulating, obtain granularity and be the pelletizing of 80～120 microns;
(4) pack pelletizing into grinding tool, moulding in cold isostatic press, forming pressure is 200MPa;
(5) the Ceramic Balls base substrate of forming is dried, bake out temperature is controlled at 120 ℃;
(6) burn till: Ceramic Balls base substrate is put into sintering oven, according to following sintering curve, burn till:
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 carried out to polishing, can obtain density is 6.00g/cm
3high strength electric-melting zirconia Ceramic Balls, record hardness HV and reach 1256.
Embodiment 2
(1) get ZrO
2+ HfO
2content is the electric-melting zirconia powder 94.6kg of 99.7% monocline type, adopt Superfine Stirred Mill to grind, by adjusting and control the parameters such as proportioning, rotating speed and liquid-solid ratio of the zirconium oxide bead of grinding machine, make its mean particle size D 50 reach 0.4 micron of left and right, 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 5.4kg yttrium oxide, the purity of yttrium oxide is more than 99.9%, and D50 is less than 0.5 micron, then adds 100kg water, add organic alcohols polymkeric substance 1kg, in agitating ball mill, be fully mixed and made into suspension slip;
(3) suspension slip is carried out in centrifugal spray dryer to mist projection granulating, obtain granularity and be the pelletizing of 80～120 microns;
(4) pack pelletizing into grinding tool, moulding in cold isostatic press, forming pressure is 300MPa;
(5) the Ceramic Balls base substrate of forming is dried, bake out temperature is controlled at 150 ℃;
(6) burn till: Ceramic Balls base substrate is put into sintering oven, according to following sintering curve, burn till:
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 carried out to polishing, can obtain density is 6.02g/cm
3high strength electric-melting zirconia Ceramic Balls, record hardness HV and reach 1260.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes description of the present invention to do; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (4)
1. a preparation method for high strength electric-melting zirconia Ceramic Balls, comprises the following steps:
Step 1, select ZrO
2+ HfO
2content, at the electric-melting zirconia powder of more than 99.6% monocline type, is ground to mean particle size D 50 and is reached below 0.6 micron, and D90 reaches below 1.2 microns, and D97 reaches below 1.5 microns;
Step 2, in ground electric-melting zirconia ultrafine powder, add stablizer and fully mix;
Step 3, the material mixing is carried out to spray granulating and drying;
Step 4, pelletizing is adopted to cold isostatic compaction;
Step 5, by the Ceramic Balls base substrate of forming through burning till, after polishing, make high strength electric-melting zirconia Ceramic Balls, 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 top temperature;
Naturally be cooled to 200 ℃, kiln discharge.
2. the preparation method of high strength electric-melting zirconia Ceramic Balls according to claim 1, is characterized in that: in step 2, add 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, pelletizing is adopted to 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: between step 4 and step 5, also comprise that baking step, bake out temperature are 120～150 ℃.
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| CN104529506A (en) * | 2015-01-16 | 2015-04-22 | 临江北峰硅藻土有限公司 | Preparation method of compound natural porous mineral ceramic microbeads |
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| JP6290927B2 (en) * | 2013-12-17 | 2018-03-07 | 京セラ株式会社 | Fiber guide |
| CN104528823B (en) * | 2015-01-06 | 2018-03-23 | 武汉拓柏仕科技有限公司 | A kind of Zirconium powder, its product and preparation method |
| 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 |
| 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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| CN101209926A (en) * | 2007-12-22 | 2008-07-02 | 淄博华创精细陶瓷有限公司 | Method for preparing low cost zirconium oxide ceramic grinding medium |
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| EP2168935A1 (en) * | 2008-09-29 | 2010-03-31 | Siemens Aktiengesellschaft | Material compound for producing a fire-retardant material and its application and fire-retardant moulding body and method for its manufacture |
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| JP2006508011A (en) * | 2002-11-22 | 2006-03-09 | サン−ゴバン セラミックス アンド プラスティクス，インコーポレイティド | Zirconia reinforced alumina ESD protective ceramic composition, component and method for forming the same |
| CN101209926A (en) * | 2007-12-22 | 2008-07-02 | 淄博华创精细陶瓷有限公司 | Method for preparing low cost zirconium oxide ceramic grinding medium |
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