CN107266051A - A kind of preparation method of alumina zirconia ceramic material - Google Patents

A kind of preparation method of alumina zirconia ceramic material Download PDF

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CN107266051A
CN107266051A CN201710675727.3A CN201710675727A CN107266051A CN 107266051 A CN107266051 A CN 107266051A CN 201710675727 A CN201710675727 A CN 201710675727A CN 107266051 A CN107266051 A CN 107266051A
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zirconium
powder
preparation
alumina zirconia
alurnina
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黄�俊
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Zhangjiagang New Material Technology Development Co Ltd
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Zhangjiagang New Material Technology Development Co Ltd
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    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract

The invention discloses a kind of preparation method of alumina zirconia ceramic material, comprise the following steps:(1) alumina zirconia suspension is prepared:Deionized water, dispersant are added into alumina powder and Zirconium powder, is well mixed, uses ammoniacal liquor to adjust pH for 8~10,30~60min of magnetic agitation, ultrasonic disperse handles 10~15min, obtains alumina zirconia suspension;(2) sintering aid MgO is added into above-mentioned alumina zirconia suspension, with 80~200rpm rotating speed 90~150min of ball milling mixing, alumina zirconia slurry is obtained;(3) above-mentioned alumina zirconia slurry is filtered by vacuum, dried under the conditions of 80~100 DEG C, ground, sieving obtains alumina zirconia powder;(4) above-mentioned alumina zirconia powder is loaded into graphite jig, row sinters 2~5h in sintering furnace under 1450~1600 DEG C of temperature conditionss, and is incubated 1~2 hour under the conditions of 500~800 DEG C, cooling obtains alumina zirconia ceramics.Ceramic bending strength and fracture toughness produced by the present invention are high.

Description

A kind of preparation method of alurnina-zirconia ceramics material
Technical field
The present invention relates to field of material technology, more particularly to a kind of preparation method of alurnina-zirconia ceramics material.
Background technology
Al2O3Composite ceramics is most commonly used one kind of purposes in structural ceramics, and it has fusing point height, high mechanical strength, hard Degree is high, chemical stability is good, density is small, light weight, it is cheap the features such as, but the fracture toughness of this material is very low, It significantly limit the use of the ceramic material.Utilize ZrO2Transformation toughening Al2O3Ceramics have preferable effect, the phase transformation Journey absorbs energy along with the change of volume and shape, reduces crack tip stress concentration, prevents or delay Crack Extension, from And improve Al2O3The fracture toughness of composite ceramics.
The performance of the composite ceramics except with ZrO2Crystal formation has outside the Pass, also has its grain graininess, particle uniformity relevant.Receive The toughening mechanism such as the crack deflection of rice diphase ceramic material and crackle bending, can make with reference to traditional transformation toughening reinforcement mechanism It is standby go out high performance nanocomposite ceramic material.In recent years, micro-nano ZrO2Powder, which is prepared and homogenized, progressively turns into research Hot issue.
Nanometer ZrO2Raw powder's production technology typically has Physical and chemical method, and nanometer ZrO is prepared at present2The method of powder Chemical method mainly is used, such as:Coprecipitation, sol-gel process and hydrothermal synthesis method etc., this method are usually produced to a high, reality Test step more complicated, and use more chemical reagent.Physics prepares method, and such as sputtering method is easy to operate, but is difficult to obtain uniform Composite, ZrO2Easily reunite, influence mechanical performance.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of preparation method of alurnina-zirconia ceramics material, its energy Enough solve problems of the prior art.
The content of the invention
It is an object of the invention to provide a kind of preparation method of alurnina-zirconia ceramics material, to overcome existing skill Deficiency in art.
To achieve the above object, the present invention provides following technical scheme:
A kind of preparation method of alurnina-zirconia ceramics material, comprises the following steps:
(1) aluminium oxide-zirconium oxide suspension is prepared:Deionized water is added into alumina powder and Zirconium powder, is divided Powder, is well mixed, and uses ammoniacal liquor to adjust pH for 8~10,30~60min of magnetic agitation, ultrasonic disperse handles 10~15min, Obtain aluminium oxide-zirconium oxide suspension;
(2) sintering aid MgO is added into above-mentioned aluminium oxide-zirconium oxide suspension, with 80~200rpm rotating speed ball milling 90~150min is mixed, aluminium oxide-zirconium oxide slurry is obtained;
(3) above-mentioned aluminium oxide-zirconium oxide slurry is filtered by vacuum, dried under the conditions of 80~100 DEG C, ground, sieved, obtained Aluminium oxide-zirconium oxide powder;
(4) above-mentioned aluminium oxide-zirconium oxide powder is loaded into graphite jig, in sintering under 1450~1600 DEG C of temperature conditionss 2~5h of row sintering in stove, and 1~2 hour is incubated under the conditions of 500~800 DEG C, cooling obtains alurnina-zirconia ceramics.
It is preferred that, in step (1), the preparation method of the alumina powder includes:Aluminum salt solution is passed through into spray atomization Spray in the ammonium bicarbonate soln under stirring, and added after surfactant polyethylene reaction afterwards, through precipitating, being aged, Filtering, washing, microwave drying, calcining obtain alumina powder.
It is preferred that, in step (1), the preparation method of the Zirconium powder includes:First add in the aqueous solution containing zirconates Enter alcohol, alkaline precipitating agent is added after being well mixed, obtain hydroxide precipitation;By hydroxide precipitation through filtering, washing, use Dry, calcine in distilling apparatus after azeotropic distillation method dehydration, obtain Zirconium powder.
It is preferred that, in step (1), the dispersant is ammonium polymethacrylate.
It is preferred that, the one kind of the aluminium salt in aluminium chloride, aluminum nitrate, aluminum sulfate.
It is preferred that, the one kind of the zirconates in zirconium oxychloride, zirconium sulfate, zirconium carbonate acyl.
Compared with prior art, the advantage of the invention is that:In the present invention, preparation technology is simple, and aluminum oxide can be uniform Ground is dispersed in zirconium oxide, by the bending strength of alurnina-zirconia ceramics material made from the method in the present invention and disconnected Split toughness high.
Embodiment
The present invention is described further by the following example:According to following embodiments, the present invention may be better understood. However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described by embodiment are only used In the explanation present invention, without should be also without limitation on the present invention described in detail in claims.
The present invention discloses a kind of preparation method of alurnina-zirconia ceramics material, comprises the following steps:
(1) aluminium oxide-zirconium oxide suspension is prepared:Deionized water is added into alumina powder and Zirconium powder, is divided Powder, is well mixed, and uses ammoniacal liquor to adjust pH for 8~10,30~60min of magnetic agitation, ultrasonic disperse handles 10~15min, Obtain aluminium oxide-zirconium oxide suspension;
(2) sintering aid MgO is added into above-mentioned aluminium oxide-zirconium oxide suspension, with 80~200rpm rotating speed ball milling 90~150min is mixed, aluminium oxide-zirconium oxide slurry is obtained;
(3) above-mentioned aluminium oxide-zirconium oxide slurry is filtered by vacuum, dried under the conditions of 80~100 DEG C, ground, sieved, obtained Aluminium oxide-zirconium oxide powder;
(4) above-mentioned aluminium oxide-zirconium oxide powder is loaded into graphite jig, in sintering under 1450~1600 DEG C of temperature conditionss 2~5h of row sintering in stove, and 1~2 hour is incubated under the conditions of 500~800 DEG C, cooling obtains alurnina-zirconia ceramics.
In above-mentioned steps (1), the dispersant is ammonium polymethacrylate.
In one embodiment, the preparation method of the alumina powder includes:By aluminum salt solution by being sprayed after spray atomization In ammonium bicarbonate soln under to stirring, and add after surfactant polyethylene reaction, through precipitating, being aged, filter, Washing, microwave drying, calcining obtains alumina powder.
Wherein, the one kind of the aluminium salt in aluminium chloride, aluminum nitrate, aluminum sulfate.
In one embodiment, the preparation method of the Zirconium powder includes:Alcohol is first added in the aqueous solution containing zirconates, Alkaline precipitating agent is added after well mixed, hydroxide precipitation is obtained;By hydroxide precipitation through filtering, washing, using azeotropic Dry, calcine in distilling apparatus after way of distillation dehydration, obtain Zirconium powder.
Wherein, the one kind of the zirconates in zirconium oxychloride, zirconium sulfate, zirconium carbonate acyl.
Embodiment
1st, alumina powder is prepared
By liquor alumini chloridi by being sprayed to after spray atomization in the ammonium bicarbonate soln under stirring, and add surface work Property the reaction of agent polyethylene glycol after, through precipitation, ageing, filtering, washing, microwave drying, calcining obtains alumina powder.
2nd, Zirconium powder is prepared
Alcohol is first added in the aqueous solution of sulfur acid zirconium, alkaline precipitating agent is added after being well mixed, hydroxide is obtained and sinks Form sediment;By hydroxide precipitation through filtering, washing, dry, calcine in distilling apparatus after being dehydrated using azeotropic distillation method, obtain oxygen Change zirconium powder body.
3rd, alurnina-zirconia ceramics material is prepared
Deionized water, ammonium polymethacrylate are added into above-mentioned alumina powder and above-mentioned Zirconium powder, mixing is equal It is even, use ammoniacal liquor to adjust pH for 9, magnetic agitation 40min, ultrasonic disperse processing 10min obtain aluminium oxide-zirconium oxide suspension;
Sintering aid MgO is added into above-mentioned aluminium oxide-zirconium oxide suspension, with 150rpm rotating speed ball milling mixing 120min, obtains aluminium oxide-zirconium oxide slurry;
Above-mentioned aluminium oxide-zirconium oxide slurry is filtered by vacuum, dried under the conditions of 80 DEG C, is ground, sieving, acquisition aluminum oxide- Zirconium oxide powder;
Above-mentioned aluminium oxide-zirconium oxide powder is loaded into graphite jig, row burns in sintering furnace under 1550 DEG C of temperature conditionss 3h is tied, and 1.5 hours are incubated under the conditions of 500~800 DEG C, cooling obtains alurnina-zirconia ceramics.
In the present invention, bending strength test is carried out using three-point bending fracture method to obtained alurnina-zirconia ceramics, Fracture toughness test, mechanical property result are carried out using SENB three-point bending fracture method:Bending strength is 389MPa, is broken Toughness is split for 5.68MPam1/2
Finally, in addition it is also necessary to explanation, term " comprising ", "comprising" or its any other variant are intended to non-exclusive Property include so that process, method, article or equipment including a series of key elements not only include those key elements, and Also include other key elements for being not expressly set out, or also include for this process, method, article or equipment inherently Key element.

Claims (6)

1. a kind of preparation method of alurnina-zirconia ceramics material, it is characterised in that comprise the following steps:
(1) aluminium oxide-zirconium oxide suspension is prepared:Deionized water, dispersant are added into alumina powder and Zirconium powder, It is well mixed, use ammoniacal liquor to adjust pH for 8~10,30~60min of magnetic agitation, ultrasonic disperse handles 10~15min, obtains oxygen Change aluminium-zirconia nanosuspensions;
(2) sintering aid MgO is added into above-mentioned aluminium oxide-zirconium oxide suspension, with 80~200rpm rotating speed ball milling mixing 90~150min, obtains aluminium oxide-zirconium oxide slurry;
(3) above-mentioned aluminium oxide-zirconium oxide slurry is filtered by vacuum, dried under the conditions of 80~100 DEG C, ground, sieving is aoxidized Aluminium-zirconium oxide powder;
(4) above-mentioned aluminium oxide-zirconium oxide powder is loaded into graphite jig, under 1450~1600 DEG C of temperature conditionss in sintering furnace Row 2~5h of sintering, and 1~2 hour is incubated under the conditions of 500~800 DEG C, cooling obtains alurnina-zirconia ceramics.
2. the preparation method of alurnina-zirconia ceramics material according to claim 1, it is characterised in that step (1) In, the preparation method of the alumina powder includes:By aluminum salt solution by spraying to the carbonic acid under stirring after spray atomization In hydrogen ammonium salt solution, and add after surfactant polyethylene reaction, through precipitation, ageing, filtering, washing, microwave drying is forged Burn, obtain alumina powder.
3. the preparation method of alurnina-zirconia ceramics material according to claim 1, it is characterised in that step (1) In, the preparation method of the Zirconium powder includes:Alcohol is first added in the aqueous solution containing zirconates, alkalescence is added after being well mixed Precipitating reagent, obtains hydroxide precipitation;By hydroxide precipitation through filtering, washing, in distillation after being dehydrated using azeotropic distillation method Dry, calcine in device, obtain Zirconium powder.
4. the preparation method of alurnina-zirconia ceramics material according to claim 1, it is characterised in that step (1) In, the dispersant is ammonium polymethacrylate.
5. the preparation method of alurnina-zirconia ceramics material according to claim 2, it is characterised in that the aluminium salt One kind in aluminium chloride, aluminum nitrate, aluminum sulfate.
6. the preparation method of alurnina-zirconia ceramics material according to claim 3, it is characterised in that the zirconates One kind in zirconium oxychloride, zirconium sulfate, zirconium carbonate acyl.
CN201710675727.3A 2017-08-09 2017-08-09 A kind of preparation method of alumina zirconia ceramic material Withdrawn CN107266051A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108726998A (en) * 2018-06-21 2018-11-02 温州医科大学附属口腔医院 A kind of preparation method of Zirconia reinforced alumina dentistry osmotic ceramic
CN108975933A (en) * 2018-09-18 2018-12-11 广东蓝狮医疗科技有限公司 Wear-resistant aluminium oxide-zirconium oxide composite ceramics of a kind of graphite enhancing and preparation method thereof
CN110961570A (en) * 2019-12-31 2020-04-07 三祥新材股份有限公司 Preparation method of zirconium oxide composite spray coating for metal mold casting
CN112521161A (en) * 2020-12-15 2021-03-19 无锡特科精细陶瓷有限公司 Gel injection molding method of aluminum oxide-zirconium dioxide complex phase ceramic
CN113511914A (en) * 2021-06-29 2021-10-19 冠立科技扬州有限公司 In-situ solidification colloidal forming method of high-performance aluminum oxide-based composite ceramic
CN114773055A (en) * 2022-05-24 2022-07-22 内蒙古海特华材科技有限公司 Preparation method of zirconia ceramic capable of efficiently absorbing power frequency electromagnetic field

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JPS5833187B2 (en) * 1977-07-28 1983-07-18 住友電気工業株式会社 Manufacturing method of ceramic materials for tools
JPS60103077A (en) * 1983-11-02 1985-06-07 ティーディーケイ株式会社 Friction resistant ceramic material
CN101665360A (en) * 2009-10-19 2010-03-10 中国海洋大学 Microwave curing process for ceramic material gel casting
CN105272224A (en) * 2015-10-21 2016-01-27 上海大学 Preparation method of Al2O3 doped Mg-PSZ (magnesia partially stabilized zirconia) ceramic
CN106892660A (en) * 2017-01-16 2017-06-27 广东百工新材料科技有限公司 A kind of ceramic mobile phone bonnet and preparation method thereof

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Publication number Priority date Publication date Assignee Title
JPS5833187B2 (en) * 1977-07-28 1983-07-18 住友電気工業株式会社 Manufacturing method of ceramic materials for tools
JPS60103077A (en) * 1983-11-02 1985-06-07 ティーディーケイ株式会社 Friction resistant ceramic material
CN101665360A (en) * 2009-10-19 2010-03-10 中国海洋大学 Microwave curing process for ceramic material gel casting
CN105272224A (en) * 2015-10-21 2016-01-27 上海大学 Preparation method of Al2O3 doped Mg-PSZ (magnesia partially stabilized zirconia) ceramic
CN106892660A (en) * 2017-01-16 2017-06-27 广东百工新材料科技有限公司 A kind of ceramic mobile phone bonnet and preparation method thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108726998A (en) * 2018-06-21 2018-11-02 温州医科大学附属口腔医院 A kind of preparation method of Zirconia reinforced alumina dentistry osmotic ceramic
CN108975933A (en) * 2018-09-18 2018-12-11 广东蓝狮医疗科技有限公司 Wear-resistant aluminium oxide-zirconium oxide composite ceramics of a kind of graphite enhancing and preparation method thereof
CN110961570A (en) * 2019-12-31 2020-04-07 三祥新材股份有限公司 Preparation method of zirconium oxide composite spray coating for metal mold casting
CN110961570B (en) * 2019-12-31 2021-05-25 三祥新材股份有限公司 Preparation method of zirconium oxide composite spray coating for metal mold casting
CN112521161A (en) * 2020-12-15 2021-03-19 无锡特科精细陶瓷有限公司 Gel injection molding method of aluminum oxide-zirconium dioxide complex phase ceramic
CN113511914A (en) * 2021-06-29 2021-10-19 冠立科技扬州有限公司 In-situ solidification colloidal forming method of high-performance aluminum oxide-based composite ceramic
CN114773055A (en) * 2022-05-24 2022-07-22 内蒙古海特华材科技有限公司 Preparation method of zirconia ceramic capable of efficiently absorbing power frequency electromagnetic field

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Application publication date: 20171020