CN101993248A - Additive for sintering yttrium-stabilized zirconia at low temperature - Google Patents
Additive for sintering yttrium-stabilized zirconia at low temperature Download PDFInfo
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- CN101993248A CN101993248A CN2009100561452A CN200910056145A CN101993248A CN 101993248 A CN101993248 A CN 101993248A CN 2009100561452 A CN2009100561452 A CN 2009100561452A CN 200910056145 A CN200910056145 A CN 200910056145A CN 101993248 A CN101993248 A CN 101993248A
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Abstract
The invention relates to a component of an additive for sintering yttrium-stabilized zirconia at low temperature and an adding method, belonging to the technical field of special ceramics. Because the dispersion distribution of NiO or CuO in zirconia powder is difficult to realize by adding the NiO or CuO into 3Y-TZP in a ball-milling way, and the additive with single component has limited improvement effect on the sintering performance of yttrium-stabilized zirconia, the additive with a plurality of components is adopted; the additive comprises the following components in percentage by weight: 1 percent of titanium dioxide, 0.3-3 percent of strontium oxide and 0.3-3 percent of barium oxide; and the addition is 0.2-2 percent of zirconium oxychloride. The adding way of the additive comprises the following steps of: firstly, dissolving the additive with hydrochloric acid or nitric acid; then adding the additive into a zirconium-yttrium mixed solution; and stirring the materials at 50-70 DEG C to obtain a uniform zirconium-yttrium mixed solution. In the invention, small amount of the additive is added into zirconia, which achieves quite obvious effects of reducing the sintering temperature of the zirconia and improving the microstructure and the mechanical performance.
Description
Technical field
The present invention relates to the preparation method in a kind of micron and submicron technology field, specifically is a kind of preparation method of yttrium stable zirconium oxide powder of suitable easy fired.
Background technology
Because the solid state sintering temperature of yttrium stable zirconium oxide (3Y-TZP) is higher, is generally 1500-1650 ℃, the energy consumption that higher sintering temperature is produced zirconia ceramics is higher, and under higher sintering temperature, the easy secondary of zirconium white crystal grain is grown up, and forms burning.Usually add additive at Zirconium powder and reduce zirconic sintering temperature, improve its microstructure, improve its mechanical property.
Find through literature search prior art, people such as Chen Han are at " Rare Metals Materials and engineering " (Vol.36, Suppl.1,2007) deliver the research paper that is entitled as " NiO is to the influence of 3Y-TZP ceramic material property ", studied of the influence of small amount of N iO (0.25-1mol%) additive 3Y-TZP stupalith sintering and mechanical property.People such as Liu Yang are at " Chinese pottery " (Vol.44, No.4,2008) deliver the research paper that is entitled as " nanometer CuO is to the influence of 3Y-PSZ stupalith sintering and mechanical property ", studied of the influence of trace (0.7-0.15mol%) CuO additive 3Y-TZP stupalith sintering and mechanical property.
Above method of modifying all is in ball milling NiO or CuO to be joined among the 3Y-TZP, because the NiO or the CuO that add, even nanoscale, but because secondary agglomeration, the size of its second particle also can reach micron order or submicron order, is difficult to realize that its disperse in Zirconium powder distributes.
Summary of the invention
The objective of the invention is at the shortcomings and deficiencies that exist in the prior art, propose a kind of composition of easy fired yttrium stable zirconium oxide additive and add technology.The composition of additive is titanium dioxide, strontium oxide, barytic mixture, and three's weight ratio is 1: 0.3-3: 0.3-3, add-on is the 0.2-2% of zirconium oxychloride weight.The adding mode of this additive is: at first with hydrochloric acid or nitric acid additive is dissolved, join then in the zirconium yttrium mixing solutions.The amount of the additive that the present invention need add in zirconium white seldom to reducing zirconic sintering temperature, is improved its microstructure, and the effect that improves its mechanical property is very obvious.
The present invention is achieved by the following technical solutions, and concrete steps are as follows:
The first step, the preparation of solution.
Zirconates is solubility salts such as zirconium oxychloride, stablizer adds with the soluble salt such as the forms such as Yttrium trichloride, Yttrium trinitrate of yttrium oxide, the weight ratio of zirconium oxychloride, yttrium oxide, pure water is 100: 2: 100, the amount of yttrium oxide is converted into the amount of Yttrium trichloride or Yttrium trinitrate etc., above-mentioned material is mixed.
Precipitation agent is ammoniacal liquor, bicarbonate of ammonia, urea etc., and weight percent concentration is 3-10%.
In second step, add additive
Additive is titanium dioxide, strontium oxide, barytic mixture, and the weight ratio of three kinds of components is 1: 0.3-3: 0.3-3, add-on is the 0.2-2% of zirconium oxychloride.At first additive is dissolved, join then in the zirconium yttrium mixing solutions, above-mentioned material was stirred 1 hour the zirconium yttrium mixing solutions that obtains mixing at 50-70 ℃ down with hydrochloric acid or nitric acid.
The 3rd step, co-precipitation
Zirconium yttrium mixing solutions and precipitation agent are dripped simultaneously, and temperature of reaction is 60-80 ℃, and the pH value of reaction soln is 9-10, after dropwising, continues to stir 1 hour, makes material reaction complete.
In the 4th step, filter and washing
Adopt plate and frame to filter and carry out solid-liquid separation, throw out is washed with pure water, repeated multiple times, when checking scrub raffinate with the silver nitrate solution of 1M white depositions does not appear and till.
The 5th step, oven dry
The throw out of washes clean is dried down at 200-250 ℃.
The 6th step, corase grind
Adopt crusher that dried material is roughly ground the order to 50-100.
The 7th step, calcining
With the material saggar of packing into after the corase grind, calcining temperature is 600-1050 ℃, is incubated 2-5 hour.
The 8th step, ball milling
Adopt stirring ball mill will calcine good material and be milled to 0.5-1.0 μ m.
The 9th step, granulation
Adopt sponging granulator to obtain the spherical agglomerates of 30-100 μ m.
The tenth step, dry-pressing
Dry-pressing formed under the pressure of 200-300MPa.
The tenth step, sintering
1350-1500 ℃ of sinter molding, the density of the yttrium stable zirconium oxide pottery that obtains is 6.00-6.05cm with dry-pressing formed green compact
3/ g.
Description of drawings
Fig. 1 is the inventive method schema;
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1:
The weight ratio of zirconium oxychloride, Yttrium trichloride, pure water is 100: 13: 100, prepares zirconium yttrium mixing solutions down at 70 ℃, and precipitation agent employing weight percent concentration is 8% weak ammonia.
With weight ratio is 1: 0.3: 0.3 titanium dioxide, strontium oxide, barium oxide additive preparation, and the add-on of additive is 0.2% of a zirconium oxychloride.Additive with 10% diluted hydrochloric acid dissolution, is added zirconium yttrium mixing solutions, above-mentioned material was stirred 1 hour down at 70 ℃, obtain limpid zirconium yttrium mixing solutions.
Zirconium yttrium mixing solutions and precipitation agent are dripped simultaneously, and temperature of reaction is 80 ℃, and the pH value of reaction soln is 9, after dropwising, continues to stir 1 hour, makes material reaction complete.
Adopt plate and frame to filter and carry out solid-liquid separation, throw out is washed with pure water, when checking scrub raffinate with the silver nitrate solution of 1M white depositions does not appear and till.
Throw out oven dry, corase grind, calcining, ball milling, granulation are obtained yttrium stable zirconium oxide granulation powder.
Yttrium stable zirconium oxide granulation powder is dry-pressing formed under the pressure of 200MPa, the density 6.00cm of the yttrium stable zirconium oxide pottery that obtains in 1500 ℃ of sintering
3/ g.
Embodiment 2:
The weight ratio of zirconium oxychloride, Yttrium trichloride, pure water is 100: 13: 100, prepares zirconium yttrium mixing solutions down at 70 ℃, and precipitation agent employing weight percent concentration is 8% weak ammonia.
With weight ratio is 1: 1: 1 titanium dioxide, strontium oxide, barium oxide additive preparation, and the add-on of additive is 1% of a zirconium oxychloride.Additive with 10% diluted hydrochloric acid dissolution, is added zirconium yttrium mixing solutions, above-mentioned material was stirred 1 hour down at 70 ℃, obtain limpid zirconium yttrium mixing solutions.
Zirconium yttrium mixing solutions and precipitation agent are dripped simultaneously, and temperature of reaction is 80 ℃, and the pH value of reaction soln is 9, after dropwising, continues to stir 1 hour, makes material reaction complete.
Adopt plate and frame to filter and carry out solid-liquid separation, throw out is washed with pure water, when checking scrub raffinate with the silver nitrate solution of 1M white depositions does not appear and till.
Throw out oven dry, corase grind, calcining, ball milling, granulation are obtained yttrium stable zirconium oxide granulation powder.
Yttrium stable zirconium oxide granulation powder is dry-pressing formed under the pressure of 200MPa, the density 6.05cm of the yttrium stable zirconium oxide pottery that obtains in 1450 ℃ of sintering
3/ g.
Embodiment 3:
The weight ratio of zirconium oxychloride, Yttrium trichloride, pure water is 100: 13: 100, prepares zirconium yttrium mixing solutions down at 70 ℃, and precipitation agent employing weight percent concentration is 8% weak ammonia.
With weight ratio is 1: 3: 3 titanium dioxide, strontium oxide, barium oxide additive preparation, and the add-on of additive is 2% of a zirconium oxychloride.Additive with 10% diluted hydrochloric acid dissolution, is added zirconium yttrium mixing solutions, above-mentioned material was stirred 1 hour down at 70 ℃, obtain limpid zirconium yttrium mixing solutions.
Zirconium yttrium mixing solutions and precipitation agent are dripped simultaneously, and temperature of reaction is 80 ℃, and the pH value of reaction soln is 9, after dropwising, continues to stir 1 hour, makes material reaction complete.
Adopt plate and frame to filter and carry out solid-liquid separation, throw out is washed with pure water, when checking scrub raffinate with the silver nitrate solution of 1M white depositions does not appear and till.
Throw out oven dry, corase grind, calcining, ball milling, granulation are obtained yttrium stable zirconium oxide granulation powder.
Yttrium stable zirconium oxide granulation powder is dry-pressing formed under the pressure of 200MPa, the density 6.01cm of the yttrium stable zirconium oxide pottery that obtains in 1350 ℃ of sintering
3/ g.
Claims (1)
1. the composition of an easy fired yttrium stable zirconium oxide additive and adding method is characterized in that:
1, additive is titanium dioxide, strontium oxide, barytic mixture, and the weight ratio of component is 1: 0.3-3: 0.3-3, add-on is the 0.2-2% of zirconium oxychloride weight.
2, the adding mode of additive is: at first with hydrochloric acid or nitric acid additive is dissolved, join then in the zirconium yttrium mixing solutions, above-mentioned material was stirred 1 hour the mixing solutions that obtains mixing at 50-70 ℃ down.
3, the sintering temperature that adds the yttrium stable zirconium oxide of additive is 1350-1500 ℃.
4, the sintered density that adds the yttrium stable zirconium oxide of additive reaches 6.00-6.05cm
3/ g.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016091062A1 (en) * | 2014-12-08 | 2016-06-16 | 比亚迪股份有限公司 | Ceramic and manufacturing method thereof |
| CN106316392A (en) * | 2016-08-30 | 2017-01-11 | 全南晶鑫环保材料有限公司 | Environment-friendly technology for preparing yttrium-zirconium powder with semi-solid state method |
| CN107473737A (en) * | 2017-08-09 | 2017-12-15 | 三祥新材股份有限公司 | Combined oxidation zirconium powder for SOFC and preparation method thereof |
| CN109336618A (en) * | 2018-11-05 | 2019-02-15 | 浙江金琨锆业有限公司 | A kind of method of efficient preparation high dispersive zirconia ceramics powder |
| CN112851343A (en) * | 2021-01-20 | 2021-05-28 | 陈彩霞 | Antibacterial wear-resistant ceramic and preparation method thereof |
| CN114621005A (en) * | 2020-12-14 | 2022-06-14 | 万华化学(四川)有限公司 | Nano complex phase color zirconia ceramic and preparation method and application thereof |
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2009
- 2009-08-10 CN CN2009100561452A patent/CN101993248A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016091062A1 (en) * | 2014-12-08 | 2016-06-16 | 比亚迪股份有限公司 | Ceramic and manufacturing method thereof |
| US10106465B2 (en) | 2014-12-08 | 2018-10-23 | Byd Company Limited | Ceramic and preparation method therefor |
| CN106316392A (en) * | 2016-08-30 | 2017-01-11 | 全南晶鑫环保材料有限公司 | Environment-friendly technology for preparing yttrium-zirconium powder with semi-solid state method |
| CN106316392B (en) * | 2016-08-30 | 2019-04-12 | 全南晶鑫环保材料有限公司 | A kind of technique that environmentally protective semisolid method prepares yttrium zirconium powder body |
| CN107473737A (en) * | 2017-08-09 | 2017-12-15 | 三祥新材股份有限公司 | Combined oxidation zirconium powder for SOFC and preparation method thereof |
| CN109336618A (en) * | 2018-11-05 | 2019-02-15 | 浙江金琨锆业有限公司 | A kind of method of efficient preparation high dispersive zirconia ceramics powder |
| CN114621005A (en) * | 2020-12-14 | 2022-06-14 | 万华化学(四川)有限公司 | Nano complex phase color zirconia ceramic and preparation method and application thereof |
| CN112851343A (en) * | 2021-01-20 | 2021-05-28 | 陈彩霞 | Antibacterial wear-resistant ceramic and preparation method thereof |
| CN112851343B (en) * | 2021-01-20 | 2021-11-30 | 广东恒盛佳陶瓷有限公司 | Antibacterial wear-resistant ceramic and preparation method thereof |
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Application publication date: 20110330 |