CN102190331A - Novel method for preparing zirconium tungstate powder - Google Patents
Novel method for preparing zirconium tungstate powder Download PDFInfo
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- CN102190331A CN102190331A CN2010101294998A CN201010129499A CN102190331A CN 102190331 A CN102190331 A CN 102190331A CN 2010101294998 A CN2010101294998 A CN 2010101294998A CN 201010129499 A CN201010129499 A CN 201010129499A CN 102190331 A CN102190331 A CN 102190331A
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Abstract
The invention relates to a novel method for preparing zirconium tungstate powder, which is characterized by comprising the following process steps of: weighing in a stoichiometric ratio of ZrO2 to WO3 of 1:2, putting the ZrO2 and WO3 into a resin ball mill, adding absolute ethanol serving as a solvent, performing ball milling in a ball mill for 8 hours, standing for sedimentation, removing an upper-layer clear solvent, drying in an oven, putting powder into a quartz crucible, heating at 600DEG C for 4 hours, taking out, and cooling in the air; grinding for 40 minutes; regulating the temperature to be 800DEG C, heating for 8 hours, cooling together with a furnace, taking out, and grinding for 40 minutes; heating at 900DEG C for 12 hours, cooling together with a furnace, taking out, and grinding for 40 minutes; and putting ZrO2 and WO3 mixed powder into a mold with the diameter of 60mm, pressing under the pressure of 125MPa into a round sheet, and keeping the temperature of 1,220DEG C for 3 hours. Compared with the prior art, the novel method has the advantages that: the grain size is 0.5-1mu m, the purity is high, and the average coefficient of linear expansion is -5.33*10<-6>/K in a section of 20-700DEG C.
Description
Technical field
The present invention relates to a kind of making method of novel wolframic acid zirconium powder body.
Background technology
At present, ZrW
2O
8The making method of powder is following several: the oxide compound direct synthesis technique, and with ZrO
2And WO
3Be blended in ball milling 24h in the planetary ball mill by suitable proportion, the platinum mandarin orange pot that places sealing is more than 1200 ℃ of sintering 48h, and quenching obtains ZrW then
2O
8Powder, solid phase method sintering temperature height, required time is long, and because WO
3High volatility, that obtain usually is ZrW
2O
8And WO
3Mixture.Therefore, with the synthetic single ZrW of solid phase method
2O
8Very difficult.Combustion synthesis method, combustion synthesis method synthesizes ZrW
2O
8, speed of response is than very fast, but product is impure, and in reaction process, discharge deleterious oxynitride, cause environmental pollution, be not suitable for industrial application.Low temperature synthesis method, low temperature synthesis method are meant that low temperature synthesizes ZrW
2O
8Sol-gel method, though this method has been avoided high temperature sintering, its complex steps, processing condition harshness, and its generated time is long, also is not suitable for big batch production.Wet-chemical is in conjunction with the microwave calcination synthesis method, and wet chemistry method is in conjunction with the synthetic ZrW of microwave calcination process
2O
8, shortened the reaction times, but only reduced the temperature of building-up reactions to a certain extent.
Summary of the invention
Be to overcome the deficiencies in the prior art order of the present invention, provide a kind of and can reduce the high temperature section soaking time, obtain the making method of purer wolframic acid zirconium powder body.
For achieving the above object, design a kind of making method of novel wolframic acid zirconium powder body, it is characterized in that described processing step is: with ZrO
2And WO
3Be raw material, press ZrO
2: WO
3=1: 2 stoichiometric ratio weighing.With ZrO
2And WO
3Put into the resin ball grinder, add dehydrated alcohol as solvent, ball milling is 8 hours in ball mill.Staticly settle, go to put into baking oven after the clear solvent of upper strata and dry, take out and grind to form powdery.Powder is placed in the quartz crucible, takes out behind 600 ℃ of heating 4h, place air to lower the temperature; Grind 40min; Temperature adjustment to 800 ℃ heating 8h takes out behind the furnace cooling and grinds 40min; Then, take out behind the furnace cooling and grind 40min at 900 ℃ of heating 12h; In the mould of diameter 60mm, put into ZrO
2And WO
3Mixed powder, be pressed into thin rounded flakes with the pressure of 125MPa, at 1220 ℃ of insulation 3h, quenching obtains corresponding product.
The present invention compared with prior art adopts the solid state chemistry method of fractional steps to synthesize high purity negative expansion ZrW
2O
8Powder, particle diameter be between 0.5～1 μ m, the purity height, and on 20 ℃-700 ℃ interval, average coefficient of linear expansion is-5.33 * 10
-6/ K.
Description of drawings
The present invention is further described below in conjunction with drawings and Examples.
Fig. 1 is a process flow sheet of the present invention.
Appointment Fig. 1 is a Figure of abstract.
Embodiment
The present invention will be further described in conjunction with the accompanying drawings, and the manufacturing technology of this device is very clearly concerning this professional people.
Processing step is: with ZrO
2And WO
3Be raw material, press ZrO
2: WO
3=1: 2 stoichiometric ratio weighing.With ZrO
2And WO
3Put into the resin ball grinder, add dehydrated alcohol as solvent, ball milling is 8 hours in ball mill.Staticly settle, go to put into baking oven after the clear solvent of upper strata and dry, take out and grind to form powdery.Powder is placed in the quartz crucible, takes out behind 600 ℃ of heating 4h, place air to lower the temperature; Grind 40min; Temperature adjustment to 800 ℃ heating 8h takes out behind the furnace cooling and grinds 40min; Then, take out behind the furnace cooling and grind 40min at 900 ℃ of heating 12h; In the mould of diameter 60mm, put into ZrO
2And WO
3Mixed powder, be pressed into thin rounded flakes with the pressure of 125MPa, at 1220 ℃ of insulation 3h, quenching obtains corresponding product.
The ZrW that makes by manufacture craft of the present invention
2O
8, size is even, and is functional.Below be the ZrW that our company produces
2O
8The pattern of sample and performance test:
Adopt the ZrW of scanning electron microscope (SEM) to making by the solid state chemistry method of fractional steps
2O
8Powder carries out granularity and surperficial figure and features is measured.The ZrW of solid phase method of fractional steps preparation
2O
8The powder granule size is even, tiny, size 1～0.5 μ m.We get ZrW
2O
8Sample carries out X-ray diffraction and measures, surveying instrument adopts Japanese D/max2500PC fully automatic powder X-ray diffractometer of science, source of radiation adopt CuKa (λ=0.15418nm), with the continuous sweep of 5 ° of (2 θ)/min speed, the ZrW that the substep solid state chemistry method of fractional steps is obtained 1220 ℃ of insulations
2O
8Powder carries out XRD analysis, and the result coincide with No.50-1868 card figure shown in figure *, and not assorted peak, shows that the powder of the solid state chemistry method of fractional steps preparation of adopting our company's independent research is pure ZrW
2O
8
The wolframic acid zirconium powder end that the present invention produces has the negative expansion performance, not only can use separately, and can be widely used in all kinds of matrix materials, in order to improve the volume coefficient of material.Mainly this wolframic acid zirconium powder end is applied in the preparation of Resins, epoxy/wolframic acid zirconium packaged material at present.In addition, this all right optics in wolframic acid zirconium powder end, system, the various fields such as application of temperature correlation equipment.
Claims (1)
1. the making method of a novel wolframic acid zirconium powder body is characterized in that described processing step is: with ZrO
2And WO
3Be raw material, press ZrO
2: WO
3=1: 2 stoichiometric ratio weighing is with ZrO
2And WO
3Put into the resin ball grinder, add dehydrated alcohol as solvent, ball milling is 8 hours in ball mill, staticly settle, go to put into baking oven after the clear solvent of upper strata and dry, take out and grind to form powdery, powder is placed in the quartz crucible, takes out behind 600 ℃ of heating 4h, place air to lower the temperature; Grind 40min; Temperature adjustment to 800 ℃ heating 8h takes out behind the furnace cooling and grinds 40min; Then, take out behind the furnace cooling and grind 40min at 900 ℃ of heating 12h; In the mould of diameter 60mm, put into ZrO
2And WO
3Mixed powder, be pressed into thin rounded flakes with the pressure of 125MPa, at 1220 ℃ of insulation 3h, quenching obtains corresponding product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101294998A CN102190331A (en) | 2010-03-19 | 2010-03-19 | Novel method for preparing zirconium tungstate powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101294998A CN102190331A (en) | 2010-03-19 | 2010-03-19 | Novel method for preparing zirconium tungstate powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102190331A true CN102190331A (en) | 2011-09-21 |
Family
ID=44599330
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010101294998A Pending CN102190331A (en) | 2010-03-19 | 2010-03-19 | Novel method for preparing zirconium tungstate powder |
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|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104495939A (en) * | 2014-11-26 | 2015-04-08 | 上海交通大学 | Hydrothermal synthesis method of nano-scale zirconium tungstate hollow spheres |
| CN105110377A (en) * | 2015-08-05 | 2015-12-02 | 哈尔滨工业大学 | Method for using solid phase reaction sintering method to prepare negative thermal expansion material of zirconium tungstate |
| RU2639244C1 (en) * | 2016-11-25 | 2017-12-20 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский государственный университет" (ТГУ) | Method of producing zirconium tungstate powder |
| CN112299846A (en) * | 2020-11-16 | 2021-02-02 | 郑州大学 | Negative thermal expansion ceramic Ta2W2O11And solid phase sintering synthesis method thereof |
| CN114031118A (en) * | 2021-12-20 | 2022-02-11 | 哈尔滨工业大学 | Preparation method of high-purity alpha-zirconium tungstate |
-
2010
- 2010-03-19 CN CN2010101294998A patent/CN102190331A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104495939A (en) * | 2014-11-26 | 2015-04-08 | 上海交通大学 | Hydrothermal synthesis method of nano-scale zirconium tungstate hollow spheres |
| CN104495939B (en) * | 2014-11-26 | 2016-07-06 | 上海交通大学 | The hydrothermal synthesis method of nanoscale tungsten wire array hollow ball |
| CN105110377A (en) * | 2015-08-05 | 2015-12-02 | 哈尔滨工业大学 | Method for using solid phase reaction sintering method to prepare negative thermal expansion material of zirconium tungstate |
| RU2639244C1 (en) * | 2016-11-25 | 2017-12-20 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский государственный университет" (ТГУ) | Method of producing zirconium tungstate powder |
| CN112299846A (en) * | 2020-11-16 | 2021-02-02 | 郑州大学 | Negative thermal expansion ceramic Ta2W2O11And solid phase sintering synthesis method thereof |
| CN114031118A (en) * | 2021-12-20 | 2022-02-11 | 哈尔滨工业大学 | Preparation method of high-purity alpha-zirconium tungstate |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20110921 |