CN100410427C - Method for preparing material of ZrW1.7Mo0.308 single crystal in minus heat expansion - Google Patents
Method for preparing material of ZrW1.7Mo0.308 single crystal in minus heat expansion Download PDFInfo
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- CN100410427C CN100410427C CNB2006100402005A CN200610040200A CN100410427C CN 100410427 C CN100410427 C CN 100410427C CN B2006100402005 A CNB2006100402005 A CN B2006100402005A CN 200610040200 A CN200610040200 A CN 200610040200A CN 100410427 C CN100410427 C CN 100410427C
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- hydrochloric acid
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Abstract
The present invention relates to a preparation method for ZrW<1.7>Mo<0.3>0<8> single crystals of negative thermal expansion materials, which belongs to the technical field of functional ceramic materials. Zirconyl nitrate, ammonium tungstate and ammonium molybdate are respectively dissolved in deionized water according to the mol ratio of Zr<4+> to W<6+> to Mo<6+>, which is equal to 2 to 1.7 to 0.3, the three kinds of solution is evenly mixed into mixing solution under the condition of continuous stir, concentrated hydrochloric acid solution is added into the mixing solution, the concentrated hydrochloric acid solution is 1/6 to 1/3 of the mixing solution, and the concentrated hydrochloric acid solution and the mixing solution are uniformly stirred at 20 DEG C to 80 DEG C; the mixing solution is sealed at 160 to 200 DEG C and heated for at least nine hours under the hydrothermal condition. After the reaction is finished, the products are repeatedly washed by deionized water and baked at 50 to 80 DEG C to obtain precursors (ZrW<1.7>Mo<0.3>M<7>(OH) <2>(H<2>O) <2>), and the precursors are heated at 500 to 680 DEG C for more than five hours to obtain the final products (ZrW<1.7>Mo<0.3>0<8> single crystals). The present invention has the advantages of simple process, easy operation and industrialization.
Description
Technical field
The invention belongs to the ceramic material technical field, particularly a kind of negative heat expansion compound ZrW
1.7Mo
0.3O
8The preparation method of monocrystalline.
Background technology
ZrW
1.7Mo
0.3O
8Be good negative heat expansion compound, stronger isotropy negative expansion effect is arranged in wide temperature range.This good characteristic both can use this negative thermal expansion material separately, also can be used to prepare matrix material, thus the volume coefficient of accurate control material, and its potential Application Areas has electronics, optics, microelectronics, light communication system and daily life.Traditional hydration precursor thermal decomposition method complex steps needs long generated time; The synthetic sintering temperature of conventional solid phase method is higher, and WO
3And MoO
3Highly volatile is difficult to synthetic single cube of phase ZrW
1.7Mo
0.3O
8Though microwave method, acid vapour hydrolysis precursor method have been simplified preparation flow to a certain extent, have shortened generated time, technology is very harsh.Up to the present, still there is not Hydrothermal Growth ZrW
1.7Mo
0.3O
8The report of monocrystalline.
Summary of the invention
The objective of the invention is to utilize the synthetic fast negative thermal expansion material ZrW of hydrothermal method
1.7Mo
0.3O
8Monocrystalline.
A kind of negative thermal expansion material ZrW
1.7Mo
0.3O
8The preparation method of monocrystalline is characterized in that adopting hydrothermal method to synthesize negative thermal expansion material ZrW
1.7Mo
0.3O
8Monocrystalline.Raw materials usedly be: ZrO (NO
3)
25H
2O (analytical pure), N
5H
37W
6O
24H
2O (chemical pure), N
6H
24Mo
7O
244H
2O (chemical pure), HCl (analytical pure).
Preparation technology is:
(1) Zircosol ZN, ammonium tungstate and ammonium molybdate are pressed Zr
4+: W
6+: Mo
6+Mol ratio is respectively to be dissolved in deionized water at 2: 1.7: 0.3, constantly under the stirring condition three kinds of solution is being mixed, and adds concentrated hydrochloric acid solution to mixed solution, and its volume is that 1/6～1/3,20 ℃～80 ℃ of mixeding liquid volume stir;
(2) mixed solution in 160～200 ℃ of temperature lower seal heating at least 9 hours, after reaction finishes, is used the deionized water repetitive scrubbing under hydrothermal condition, and 50～80 ℃ of oven dry obtain presoma ZrW
1.7Mo
0.3O
7(OH)
2(H
2O)
2
(3) presoma more than 5 hours, is got final product ZrW in 500～680 ℃ of heating
1.7Mo
0.3O
8Monocrystalline.
Hydrothermal temperature is at 170～190 ℃ in the step 2, and hydro-thermal time 15-20h is good.
The invention has the advantages that and utilize hydrothermal method low temperature to synthesize negative thermal expansion material ZrW fast
1.7Mo
0.3O
8Monocrystalline, by control presoma size control ZrW
1.7Mo
0.3O
8The size of monocrystalline, this method program is simple, easy handling and industrialization.
Figure of description
Fig. 1 ZrW
1.7Mo
0.3O
8SEM figure
Embodiment:
Embodiment 1
Zircosol ZN, ammonium tungstate and ammonium molybdate are pressed Zr
4+: W
6+: Mo
6+Mol ratio be 2: 1.7: 0.3 respectively in the deionized water, constantly under the stirring condition three kinds of solution are being mixed, stir after the 3h, add concentrated hydrochloric acid solution to mixed solution, its volume is that 1/6,20 ℃ of mixeding liquid volume stirs 3h.Then, mixed solution changed over to have in the teflon-lined hydrothermal reaction kettle, at 160 ℃ temperature lower seals heating 9h.After reaction finishes, with distilled water repeatedly centrifuge washing to pH value be 7, drip AgNO to the centrifugal upper strata that goes out in the stillness of night
3Solution can not produce white precipitate, proves Cl
-Remove 50 ℃ of oven dry fully.Presoma is got final product ZrW in 500 ℃ of heating 10h in resistance furnace
1.7Mo
0.3O
8Monocrystalline.
Embodiment 2
Zircosol ZN, ammonium tungstate and ammonium molybdate are pressed Zr
4+: W
6+: Mo
6+Mol ratio be 2: 1.7: 0.3 respectively in the deionized water, constantly under the stirring condition three kinds of solution are being mixed, stir after the 3h, add concentrated hydrochloric acid solution to mixed solution, its volume is that 1/4,60 ℃ of mixeding liquid volume stirs 3h.Then, mixed solution changed over to have in the teflon-lined hydrothermal reaction kettle, at 180 ℃ temperature lower seals heating 15h.After reaction finishes, be 7, drip AgNO in the stillness of night to the centrifugal upper strata that goes out with distilled water repetitive scrubbing to pH value
3Solution can not produce white precipitate, 70 ℃ of oven dry.Presoma is got final product ZrW in 570 ℃ of heating 6h in resistance furnace
1.7Mo
0.3O
8Monocrystalline.
Embodiment 3
Zircosol ZN, ammonium tungstate and ammonium molybdate are pressed Zr
4+: W
6+: Mo
6+Mol ratio be 2: 1.7: 0.3 respectively in the deionized water, constantly under the stirring condition three kinds of solution are being mixed, stir after the 3h, add concentrated hydrochloric acid solution to mixed solution, its volume is that 1/3,80 ℃ of mixeding liquid volume stirs 6h.Then, mixed solution changed over to have in the teflon-lined hydrothermal reaction kettle, at 200 ℃ temperature lower seals heating 48h.After reaction finishes, be 7, drip AgNO in the stillness of night to the centrifugal upper strata that goes out with distilled water repetitive scrubbing to pH value
3Solution can not produce white precipitate, 80 ℃ of oven dry.Presoma is got final product ZrW in 680 ℃ of heating 5h in resistance furnace
1.7Mo
0.3O
8Monocrystalline.
Claims (2)
1. negative thermal expansion material ZrW
1.7Mo
0.3O
8The preparation method of monocrystalline is characterized in that:
(1) Zircosol ZN, ammonium tungstate and ammonium molybdate are pressed Zr
4+: W
6+: Mo
6+Mol ratio is respectively to be dissolved in deionized water at 2: 1.7: 0.3, and three kinds of solution stirring are mixed, and adds concentrated hydrochloric acid solution to mixed solution, and its volume is that 1/6～1/3,20 ℃～80 ℃ of mixeding liquid volume stir;
(2) mixed solution in 160～200 ℃ of temperature lower seal heating at least 9 hours, after reaction finishes, is used the deionized water repetitive scrubbing under hydrothermal condition, and 50～80 ℃ of oven dry obtain presoma ZrW
1.7Mo
0.3O
7(OH)
2(H
2O)
2
(3) presoma more than 5 hours, is got final product ZrW in 500～680 ℃ of heating
1.7Mo
0.3O
8Monocrystalline.
2. a kind of negative thermal expansion material ZrW according to claim 1
1.7Mo
0.3O
8The preparation method of monocrystalline is characterized in that: in the step (2) hydrothermal temperature at 170～190 ℃, hydro-thermal time 15-20h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100402005A CN100410427C (en) | 2006-05-11 | 2006-05-11 | Method for preparing material of ZrW1.7Mo0.308 single crystal in minus heat expansion |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100402005A CN100410427C (en) | 2006-05-11 | 2006-05-11 | Method for preparing material of ZrW1.7Mo0.308 single crystal in minus heat expansion |
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| Publication Number | Publication Date |
|---|---|
| CN1873063A CN1873063A (en) | 2006-12-06 |
| CN100410427C true CN100410427C (en) | 2008-08-13 |
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|---|---|---|---|
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9090480B2 (en) * | 2009-08-27 | 2015-07-28 | Jiangsu University | Process for preparing various morphology NTE compound ZrW0.5Mo1.5O8 |
| CN102745747B (en) * | 2011-12-14 | 2014-07-30 | 江苏大学 | Preparation method for rod-like Sc2W3O12 negative thermal expansion material |
| CN103121720B (en) * | 2012-11-28 | 2014-10-29 | 江苏大学 | Bifunctional material and preparation method thereof |
| CN106315679B (en) * | 2016-08-11 | 2017-10-31 | 河南科技大学 | A kind of method for preparing nano zircite doped tungsten oxide |
| CN114716247A (en) * | 2022-03-21 | 2022-07-08 | 合肥精创科技有限公司 | High-density zirconium tungstate solid solution ceramic and preparation method thereof |
-
2006
- 2006-05-11 CN CNB2006100402005A patent/CN100410427C/en not_active Expired - Fee Related
Non-Patent Citations (10)
| Title |
|---|
| Brief communication low temperature synthesisi ofZrW2O8and Mo-substituted ZrW2O8. C.Closmann et al.Journal of solid state chemistry,Vol.139 . 1998 |
| Brief communication low temperature synthesisi ofZrW2O8and Mo-substituted ZrW2O8. C.Closmann et al.Journal of solid state chemistry,Vol.139 . 1998 * |
| NTE化合物－ZrW1.4Mo0.6O8前驱物法合成及四方相的表征. 刘克文.山西师范大学学报（自然科学版），第19卷第2期. 2005 |
| NTE化合物－ZrW1.4Mo0.6O8前驱物法合成及四方相的表征. 刘克文.山西师范大学学报（自然科学版），第19卷第2期. 2005 * |
| The preparation and Crystal structure of a basiczirconiummolybdate and its relationship to ion exchange gels. A.Clearfield et al.J.Inorg.nucl.Chem,Vol.34 . 1972 |
| The preparation and Crystal structure of a basiczirconiummolybdate and its relationship to ion exchange gels. A.Clearfield et al.J.Inorg.nucl.Chem,Vol.34 . 1972 * |
| ZrW2－xMoxO8的合成、表征与热膨胀特性. 白海龙等.昆明理工大学学报（理工版），第29卷第5期. 2004 |
| ZrW2－xMoxO8的合成、表征与热膨胀特性. 白海龙等.昆明理工大学学报（理工版），第29卷第5期. 2004 * |
| 水热法合成负热膨胀材料ZrW2O8. 邢奇凤等.金属学报，第41卷第6期. 2005 |
| 水热法合成负热膨胀材料ZrW2O8. 邢奇凤等.金属学报，第41卷第6期. 2005 * |
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