CN112359336B - Preparation method of high-purity and high-density molybdenum trioxide target material - Google Patents
Preparation method of high-purity and high-density molybdenum trioxide target material Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-purity and high-density molybdenum trioxide target, which is implemented according to the following steps: step 1, performing baking treatment on ammonium molybdate to obtain high-purity molybdenum trioxide; step 2, loading the high-purity molybdenum trioxide powder obtained in the step 1 into a die, and performing atmosphere protection hot-pressing treatment to obtain a high-density molybdenum trioxide blank; step 3, performing secondary oxygen supplementation on the high-density molybdenum trioxide blank obtained in the step 2 in an air atmosphere muffle furnace; and 4, machining and cleaning the blank subjected to the secondary oxygen supplementing treatment to finally obtain the high-purity molybdenum trioxide target. The preparation method of the high-purity and high-density molybdenum trioxide target material can obtain the high-purity and high-density molybdenum trioxide target material.
Description
Technical Field
The invention belongs to the technical field of target preparation methods, and relates to a preparation method of a high-purity and high-density molybdenum trioxide target.
Background
Electrochromic refers to a special phenomenon that a material is reversibly changed between a low-transmittance colored state or a high-transmittance bleached state by injecting or extracting electric charges (ions or electrons) under the action of alternating high-low or positive-negative external electric fields. Tungsten trioxide is a typical representation of organic electrochromic materials, currently in WO 3 The electrochromic device which is a functional material has the problems of over-heavy color, insufficient softness and the like, severely limits the application range of the electrochromic device and promotes people to MoO with similar structure 3 New heuristics have been developed. MoO (MoO) 3 Is also a cathode electrochromic material, the color change mechanism of which is similar to that of WO 3 Similarly, but with a relatively low coloring efficiency, having a color ratio of WO 3 A more subtle neutral color and thus for many buildings this subtle neutral color is more suitable. In addition, the purpose of widening the spectral absorption width is achieved by a molybdenum-tungsten mixed oxide film. Molybdenum trioxide is therefore also increasingly attracting attention as a new strength of electrochromic materials. MoO (MoO) 3 The method can also be used in the fields of erasable optical storage devices, flat panel displays, chemical sensors, laser printing and the like, and has very attractive application prospects.
The current preparation method of the molybdenum trioxide film mainly comprises the following steps: sputtering, vacuum evaporation, sol-gel, chemical vapor deposition, and the like. The magnetron sputtering method has the advantages of stable performance, high deposition rate, low substrate temperature rise, good film uniformity, strong film base adhesion, easy control of technological parameters and the like, and is widely researched and adopted. While a great deal of literature shows that molybdenum trioxide films are all realized by reactive sputtering. The reactive sputtering method is to use metal molybdenum target material in Ar+O 2 Preparing a molybdenum oxide film by reactive sputtering in atmosphere, wherein the sputtering process can be realized by regulating and controlling O 2 And the optimized preparation of the molybdenum trioxide film is realized by the parameters of air flow, sputtering air pressure and the like. Due to the reactive sputtering process O 2 The ratio of the flow rate can influence the oxidation degree of the Mo of the sputtering film, directly influence the purity of the molybdenum trioxide film, and if MoO is directly adopted 3 Such problems can be eliminated from the source by sputtering the target. It is known that molybdenum trioxide has obvious sublimation phenomenon at above 600 ℃, and the material can not obtain high-density MoO by a normal pressure sintering method at above 600 DEG C 3 While at 600 ℃ or below, sublimation is inhibited, but the density is not significantly improved.
Disclosure of Invention
The invention aims to provide a preparation method of a high-purity and high-density molybdenum trioxide target material, which can obtain the high-purity and high-density molybdenum trioxide target material.
The technical scheme adopted by the invention is that the preparation method of the high-purity and high-density molybdenum trioxide target material is implemented according to the following steps:
step 1, performing baking treatment on ammonium molybdate to obtain high-purity molybdenum trioxide powder;
step 2, loading the high-purity molybdenum trioxide powder obtained in the step 1 into a die, and performing atmosphere protection hot-pressing treatment to obtain a high-density molybdenum trioxide blank;
step 3, performing secondary oxygen supplementation on the high-density molybdenum trioxide blank obtained in the step 2 in an air atmosphere muffle furnace;
and 4, machining and cleaning the blank subjected to the secondary oxygen supplementing treatment to finally obtain the high-purity molybdenum trioxide target.
The present invention is also characterized in that,
the ammonium molybdate in the step 1 is one or a mixture of several of ammonium dimolybdate, ammonium tetramolybdate, ammonium heptamolybdate, ammonium octamolybdate and ammonium dodecamolybdate.
The baking treatment process in the step 1 is a process of carrying out high-temperature treatment on ammonium molybdate to generate decomposition reaction to obtain high-purity molybdenum trioxide, wherein the high-temperature treatment temperature is 300-600 ℃, the atmosphere is air, and the baking time is 20-120 min.
The purity of the high-purity molybdenum trioxide in the step 1 is at least 99.95 percent, and the average grain diameter is 0.5 mu m to 50 mu m.
The atmosphere protection hot-pressing sintering temperature in the step 2 is 400-650 ℃, the pressure is 30-500 MPa, the time is 15-240 min, and the protection atmosphere is as follows: an inert gas.
The inert gas is argon or nitrogen.
The density of the high-density molybdenum trioxide blank in the step 2 is not less than 98.5 percent.
And (3) performing secondary oxygen supplementing treatment in an air atmosphere muffle furnace, wherein the temperature in the muffle furnace is 400-600 ℃, and the oxygen supplementing treatment time is 15-120 min.
The purity of the molybdenum trioxide target material finally obtained in the step 4 is not less than 99.95 percent, and the density is not less than 98.5 percent.
The beneficial effects of the invention are as follows:
1. according to the invention, the high-purity high-density molybdenum trioxide target material is prepared by directly combining an atmosphere protection hot-pressing method with air furnace oxygen supplementing treatment, and is formed at one time, the pretreatment such as ball milling or rough blank pressing is not required to be carried out on raw material molybdenum trioxide powder, so that the process flow is shortened, the production efficiency is improved, the size and shape of the molybdenum trioxide target material can be controlled through different hot-pressing dies, the method is flexible and convenient, the protection atmosphere is introduced in the hot-pressing process to prevent the molybdenum trioxide from sublimating, and the product density can be improved.
2. The invention adopts the air atmosphere furnace to carry out secondary oxygen supplementing treatment, and can effectively supplement oxygen lost by molybdenum trioxide in the hot pressing process, thereby ensuring the high purity of the molybdenum trioxide in the final target product.
3. The molybdenum trioxide target prepared by the method has high quality, purity and density, regular shape and suitability for being used as a precursor for preparing the molybdenum trioxide film by a sputtering deposition method.
4. The invention has simple process, low requirement on equipment and suitability for large-scale production.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention discloses a preparation method of a high-purity and high-density molybdenum trioxide target, which is implemented according to the following steps:
step 1, performing baking treatment on ammonium molybdate to obtain high-purity molybdenum trioxide powder, wherein the ammonium molybdate is one or a mixture of more of ammonium dimolybdate, ammonium tetramolybdate, ammonium heptamolybdate, ammonium octamolybdate and ammonium dodecamolybdate, the baking treatment process is a process of performing high-temperature treatment on the ammonium molybdate to perform decomposition reaction to obtain the high-purity molybdenum trioxide, the high-temperature treatment temperature range is 300-600 ℃, the atmosphere is air, the baking time is 20-120 min, the purity of the obtained high-purity molybdenum trioxide is at least 99.95%, and the average particle size is 0.5-50 mu m;
step 2, loading the high-purity molybdenum trioxide powder obtained in the step 1 into a die, and performing atmosphere protection hot-pressing treatment to obtain a high-density molybdenum trioxide blank, wherein the atmosphere protection hot-pressing sintering temperature is 400-650 ℃, the pressure is 30-500 MPa, the time is 15-240 min, and the protection atmosphere is as follows: the density of the obtained high-density molybdenum trioxide blank is not less than 98.5 percent by inert gases such as argon or nitrogen;
step 3, performing secondary oxygen supplementation on the high-density molybdenum trioxide blank obtained in the step 2 in an air atmosphere muffle furnace, so as to ensure the oxygen content and purity of the molybdenum trioxide blank, wherein the temperature in the muffle furnace is 400-600 ℃, and the oxygen supplementation treatment time is 15-120 min;
and 4, machining and cleaning the blank subjected to the secondary oxygen supplementing treatment to finally obtain the high-purity molybdenum trioxide target, wherein the purity of the finally obtained molybdenum trioxide target is not less than 99.95%, and the density of the finally obtained molybdenum trioxide target is not less than 98.5%.
Example 1
The preparation method of the high-purity and high-density molybdenum trioxide target material is implemented according to the following steps:
step 1, performing baking treatment on ammonium dimolybdate, wherein the baking temperature is 400 ℃, the baking time is 60min, and the high-purity molybdenum trioxide powder with the mass purity of 99.95% and the average particle diameter of 30 μm is obtained;
step 2, loading the high-purity molybdenum trioxide powder obtained by the baking in the step 1 into a die, and carrying out argon atmosphere protection hot pressing for 240min at 400 ℃ and 100MPa to obtain a high-density molybdenum trioxide blank;
step 3, performing secondary oxygen supplementation on the high-density molybdenum trioxide blank obtained in the step 2 in an air atmosphere muffle furnace, wherein the treatment temperature is 500 ℃, and the treatment time is 60min;
and 4, machining and cleaning the blank subjected to the secondary oxygen supplementing treatment to finally obtain the high-purity molybdenum trioxide target.
The detection shows that the mass purity of the molybdenum trioxide target material prepared by the embodiment is 99.95%, and the compactness is 98.5%.
Example 2
The preparation method of the high-purity and high-density molybdenum trioxide target material is implemented according to the following steps:
step 1, performing baking treatment on ammonium dimolybdate, wherein the baking temperature is 600 ℃, the baking time is 20min, and the high-purity molybdenum trioxide powder with the mass purity of 99.95% and the average particle diameter of 0.5 μm is obtained;
step 2, loading the high-purity molybdenum trioxide powder obtained by the baking in the step 1 into a die, and carrying out argon atmosphere protection hot pressing for 15min at 650 ℃ and under the pressure of 30MPa to obtain a high-density molybdenum trioxide blank;
step 3, performing secondary oxygen supplementation on the high-density molybdenum trioxide blank obtained in the step 2 in an air atmosphere muffle furnace, wherein the treatment temperature is 600 ℃, and the treatment time is 15min;
and 4, machining and cleaning the blank subjected to the secondary oxygen supplementing treatment to finally obtain the high-purity molybdenum trioxide target.
The detection shows that the mass purity of the molybdenum trioxide target material prepared by the embodiment is 99.98%, and the compactness is 99.1%.
Example 3
The preparation method of the high-purity and high-density molybdenum trioxide target material is implemented according to the following steps:
step 1, performing baking treatment on ammonium dimolybdate, wherein the baking temperature is 300 ℃, the baking time is 120min, and the high-purity molybdenum trioxide powder with the mass purity of 99.97% and the average particle diameter of 50 μm is obtained;
step 2, loading the high-purity molybdenum trioxide powder obtained by the baking in the step 1 into a die, and carrying out argon atmosphere protection hot pressing for 15min at 500 ℃ and under the pressure of 500MPa to obtain a high-density molybdenum trioxide blank;
step 3, performing secondary oxygen supplementation on the high-density molybdenum trioxide blank obtained in the step 2 in an air atmosphere muffle furnace, wherein the treatment temperature is 400 ℃, and the treatment time is 120min;
and 4, machining and cleaning the blank subjected to the secondary oxygen supplementing treatment to finally obtain the high-purity molybdenum trioxide target.
The detection shows that the mass purity of the molybdenum trioxide target material prepared by the embodiment is 99.96%, and the compactness is 99.8%.
Example 4
The preparation method of the high-purity and high-density molybdenum trioxide target material is implemented according to the following steps:
step 1, performing baking treatment on ammonium dimolybdate, wherein the baking temperature is 500 ℃, the baking time is 90min, and the high-purity molybdenum trioxide powder with the mass purity of 99.95% and the average particle diameter of 30 μm is obtained;
step 2, loading the high-purity molybdenum trioxide powder obtained by the baking in the step 1 into a die, and carrying out argon atmosphere protection hot pressing for 120min at 500 ℃ and under the pressure of 60MPa to obtain a high-density molybdenum trioxide blank;
step 3, performing secondary oxygen supplementation on the high-density molybdenum trioxide blank obtained in the step 2 in an air atmosphere muffle furnace, wherein the treatment temperature is 580 ℃, and the treatment time is 90min;
and 4, machining and cleaning the blank subjected to the secondary oxygen supplementing treatment to finally obtain the high-purity molybdenum trioxide target.
The detection shows that the mass purity of the molybdenum trioxide target material prepared by the embodiment is 99.95%, and the compactness is 98.6%.
Claims (7)
1. The preparation method of the high-purity and high-density molybdenum trioxide target is characterized by comprising the following steps of:
step 1, performing baking treatment on ammonium molybdate to obtain high-purity molybdenum trioxide powder;
step 2, loading the high-purity molybdenum trioxide powder obtained in the step 1 into a die, and performing atmosphere protection hot-pressing treatment to obtain a high-density molybdenum trioxide blank;
step 3, performing secondary oxygen supplementation on the high-density molybdenum trioxide blank obtained in the step 2 in an air atmosphere muffle furnace;
step 4, machining and cleaning the blank subjected to the secondary oxygen supplementing treatment to finally obtain a high-purity molybdenum trioxide target;
the atmosphere protection hot-pressing sintering temperature in the step 2 is 400-650 ℃, the pressure is 30-500 MPa, the time is 15-240 min, and the protection atmosphere is: an inert gas;
and (3) performing secondary oxygen supplementing treatment in an air atmosphere muffle furnace, wherein the temperature in the muffle furnace is 400-600 ℃, and the oxygen supplementing treatment time is 15-120 min.
2. The method for preparing a high-purity and high-density molybdenum trioxide target according to claim 1, characterized in that the ammonium molybdate in the step 1 is one or a mixture of several of ammonium dimolybdate, ammonium tetramolybdate, ammonium heptamolybdate, ammonium octamolybdate and ammonium dodecamolybdate.
3. The method for preparing the high-purity and high-density molybdenum trioxide target according to claim 1, characterized in that the baking treatment process in the step 1 is a process of carrying out high-temperature treatment on ammonium molybdate to generate decomposition reaction, so as to obtain the high-purity molybdenum trioxide, wherein the temperature range of the high-temperature treatment is 300-600 ℃, the atmosphere is air, and the baking time is 20-120 min.
4. The method for preparing a high-purity and high-density molybdenum trioxide target according to claim 1, characterized in that the high-purity molybdenum trioxide in step 1 has a purity of at least 99.95% and an average particle diameter of 0.5 μm to 50 μm.
5. The method for preparing a high purity, high density molybdenum trioxide target according to claim 1, characterized in that the inert gas is argon or nitrogen.
6. The method for preparing a high-purity and high-density molybdenum trioxide target according to claim 1, characterized in that the density of the high-density molybdenum trioxide blank in the step 2 is not less than 98.5%.
7. The method for preparing a high-purity and high-density molybdenum trioxide target according to claim 1, characterized in that the purity of the finally obtained molybdenum trioxide target in the step 4 is not less than 99.95% and the density is not less than 98.5%.
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| CN102126757A (en) * | 2010-01-19 | 2011-07-20 | 中国环境科学研究院 | Method for pollution-free production of molybdenum oxide |
| CN104060223A (en) * | 2013-03-21 | 2014-09-24 | 海洋王照明科技股份有限公司 | Conductive thin film, preparation method and application thereof |
| CN103194624A (en) * | 2013-04-18 | 2013-07-10 | 金堆城钼业股份有限公司 | Method for preparing high-purity molybdenum trioxide |
| CN105329945A (en) * | 2015-12-04 | 2016-02-17 | 湖北中澳纳米材料技术有限公司 | Device and method for preparing high-purity and high-dissolvability molybdenum trioxide with industrial molybdic acid |
| CN111527234A (en) * | 2017-10-06 | 2020-08-11 | 普兰西股份有限公司 | Target material for depositing molybdenum oxide layer |
| CN107746080A (en) * | 2017-11-16 | 2018-03-02 | 金堆城钼业股份有限公司 | A kind of preparation method of molybdenum disulfide target |
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