CN112359336A - Preparation method of high-purity and high-density molybdenum trioxide target - Google Patents
Preparation method of high-purity and high-density molybdenum trioxide target 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, carrying out roasting treatment on ammonium molybdate to obtain high-purity molybdenum trioxide; step 2, filling the high-purity molybdenum trioxide powder obtained in the step 1 into a mold, and carrying out atmosphere protection hot-pressing treatment to obtain a high-density molybdenum trioxide blank; step 3, carrying out 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 supplementation treatment to finally obtain the high-purity molybdenum trioxide target. The preparation method of the high-purity and high-density molybdenum trioxide target can obtain the high-purity and high-density molybdenum trioxide target.
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 is a special phenomenon in which a material reversibly changes between a colored state of low transmittance or a bleached state of high transmittance by injecting or extracting charges (ions or electrons) under the action of an alternating high-low or positive-negative external electric field. Tungsten trioxide is a typical representative of inorganic electrochromic materials, currently identified as WO3The electrochromic device made of functional materials has the problems of over-heavy color, insufficient softness and the like, the application range of the electrochromic device is severely limited, and people are prompted to apply MoO with similar structure3A new exploration is developed. MoO3Is also a cathode electrochromic material, and the color change mechanism thereof is in accordance with WO3Similarly, but with relatively low coloring efficiency, has a color ratio of WO3A softer neutral color and thus for many buildings this is more suitable. In addition, the aim of broadening the spectrum absorption width is achieved by molybdenum-tungsten mixed oxide films. Therefore, molybdenum trioxide is also gradually attracting attention as a new power of electrochromic materials. MoO3The 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 attractive application prospect.
At present, the 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-substrate adhesion, easy control of process parameters and the like, and is widely researched and adopted. And a large number of literatures show that the molybdenum trioxide thin film is realized by a reactive sputtering method. The reactive sputtering method is to perform reaction on Ar + O by using a metal molybdenum target material2The molybdenum oxide film is prepared by reactive sputtering in the atmosphere, and the sputtering process can be controlled by regulating O2Gas flow, sputtering gas pressure, etcAnd (3) parameters are adopted to realize the optimized preparation of the molybdenum trioxide film. Due to the reactive sputtering process O2The proportion of the flow can affect the oxidation degree of Mo in the sputtered film and directly affect the purity of the molybdenum trioxide film, and if MoO is directly adopted3The sputtering of the target material, and the problems can be eliminated from the source. As is known to all, molybdenum trioxide has obvious sublimation phenomenon above 600 ℃, and high-density MoO cannot be obtained by a normal pressure sintering method of the material above 600 DEG C3Although the sublimation phenomenon is inhibited below 600 ℃, the density is not obviously 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 invention adopts the technical scheme that a preparation method of a high-purity and high-density molybdenum trioxide target material is implemented according to the following steps:
step 1, carrying out roasting treatment on ammonium molybdate to obtain high-purity molybdenum trioxide powder;
step 2, filling the high-purity molybdenum trioxide powder obtained in the step 1 into a mold, and carrying out atmosphere protection hot-pressing treatment to obtain a high-density molybdenum trioxide blank;
step 3, carrying out 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 supplementation 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 more of ammonium dimolybdate, ammonium tetramolybdate, ammonium heptamolybdate, ammonium octamolybdate and ammonium dodecamolybdate.
The roasting treatment process in the step 1 is a process of carrying out high-temperature treatment on ammonium molybdate to carry out decomposition reaction to obtain the high-purity molybdenum trioxide, the temperature range of the high-temperature treatment is 300-600 ℃, the atmosphere is air, and the roasting 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 0.5-50 mu m.
The temperature of the atmosphere protection hot-pressing sintering in the step 2 is 400-650 ℃, the pressure is 30-500 MPa, the time is 15-240 min, and the protective 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%.
And 3, carrying out secondary oxygen supplement treatment in the muffle furnace in the air atmosphere, wherein the temperature in the muffle furnace is 400-600 ℃, and the oxygen supplement 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%, and the density is not less than 98.5%.
The invention has the beneficial effects that:
1. according to the invention, the high-purity and high-density molybdenum trioxide target material is prepared by directly combining an atmosphere protection hot pressing method and an air furnace oxygen supplement treatment, and is formed in one step, the pretreatment of ball milling or rough blank pressing and the like on the raw material molybdenum trioxide powder is not needed, the process flow is shortened, the production efficiency is improved, the size and the shape of the molybdenum trioxide target material can be controlled through different hot pressing molds, the method is flexible and convenient, the protective atmosphere is introduced in the hot pressing process, the molybdenum trioxide is prevented from sublimating, and the density of the product can be improved.
2. According to the invention, the secondary oxygen supplement treatment is carried out by adopting the air atmosphere furnace, so that oxygen lost by the molybdenum trioxide in the hot pressing process can be effectively supplemented, and the high purity of the molybdenum trioxide in the final target product is ensured.
3. The molybdenum trioxide target material prepared by the method has high quality purity and density and regular appearance, and is suitable for being used as a precursor for preparing a molybdenum trioxide film by a sputtering deposition method.
4. The method has simple process and low requirement on equipment, and is suitable for large-scale production.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a preparation method of a high-purity and high-density molybdenum trioxide target, which is implemented according to the following steps:
step 1, performing roasting 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 roasting 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 temperature range of the high-temperature treatment is 300-600 ℃, the atmosphere is air, the roasting 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, filling the high-purity molybdenum trioxide powder obtained in the step 1 into a mold, and carrying out atmosphere protection hot-pressing treatment to obtain a high-density molybdenum trioxide blank, wherein the temperature of atmosphere protection hot-pressing sintering is 400-650 ℃, the pressure is 30-500 MPa, the time is 15-240 min, and the protective atmosphere is as follows: inert gases such as argon or nitrogen and the like are used to obtain the high-density molybdenum trioxide blank, and the density of the high-density molybdenum trioxide blank is not less than 98.5%;
step 3, carrying out secondary oxygen supplementation on the high-density molybdenum trioxide blank obtained in the step 2 in an air atmosphere muffle furnace 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 supplementation treatment to finally obtain the high-purity molybdenum trioxide target material, wherein the purity of the finally obtained molybdenum trioxide target material is not less than 99.95%, and the density is not less than 98.5%.
Example 1
A preparation method of a high-purity and high-density molybdenum trioxide target material is specifically implemented according to the following steps:
step 1, carrying out roasting treatment on ammonium dimolybdate at the roasting temperature of 400 ℃ for 60min to obtain high-purity molybdenum trioxide, wherein the mass purity of the high-purity molybdenum trioxide powder is 99.95%, and the average particle size is 30 microns;
step 2, filling the high-purity molybdenum trioxide powder obtained by roasting in the step 1 into a die, and carrying out hot pressing for 240min under the protection of argon atmosphere at the temperature of 400 ℃ and the pressure of 100MPa to obtain a high-density molybdenum trioxide blank;
step 3, carrying out 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 60 min;
and 4, machining and cleaning the blank subjected to the secondary oxygen supplementation treatment to finally obtain the high-purity molybdenum trioxide target.
Through detection, the molybdenum trioxide target material prepared by the embodiment has the mass purity of 99.95% and the density of 98.5%.
Example 2
A preparation method of a high-purity and high-density molybdenum trioxide target material is specifically implemented according to the following steps:
step 1, carrying out roasting treatment on ammonium dimolybdate at the roasting temperature of 600 ℃ for 20min to obtain high-purity molybdenum trioxide, wherein the mass purity of the high-purity molybdenum trioxide powder is 99.95%, and the average particle size is 0.5 mu m;
step 2, filling the high-purity molybdenum trioxide powder obtained by roasting in the step 1 into a die, and carrying out hot pressing for 15min under the protection of argon atmosphere at 650 ℃ and 30MPa to obtain a high-density molybdenum trioxide blank;
step 3, carrying out 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 15 min;
and 4, machining and cleaning the blank subjected to the secondary oxygen supplementation treatment to finally obtain the high-purity molybdenum trioxide target.
Through detection, the molybdenum trioxide target material prepared in the embodiment has the mass purity of 99.98% and the density of 99.1%.
Example 3
A preparation method of a high-purity and high-density molybdenum trioxide target material is specifically implemented according to the following steps:
step 1, carrying out roasting treatment on ammonium dimolybdate at the roasting temperature of 300 ℃ for 120min to obtain high-purity molybdenum trioxide, wherein the mass purity of the high-purity molybdenum trioxide powder is 99.97%, and the average particle size is 50 microns;
step 2, filling the high-purity molybdenum trioxide powder obtained by roasting in the step 1 into a die, and carrying out hot pressing for 15min under the protection of argon atmosphere at 500 ℃ and under the pressure of 500MPa to obtain a high-density molybdenum trioxide blank;
step 3, carrying out 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 120 min;
and 4, machining and cleaning the blank subjected to the secondary oxygen supplementation treatment to finally obtain the high-purity molybdenum trioxide target.
Through detection, the mass purity of the molybdenum trioxide target material prepared by the embodiment is 99.96%, and the density is 99.8%.
Example 4
A preparation method of a high-purity and high-density molybdenum trioxide target material is specifically implemented according to the following steps:
step 1, carrying out roasting treatment on ammonium dimolybdate at the roasting temperature of 500 ℃ for 90min to obtain high-purity molybdenum trioxide, wherein the mass purity of the high-purity molybdenum trioxide powder is 99.95%, and the average particle size is 30 microns;
step 2, filling the high-purity molybdenum trioxide powder obtained by roasting in the step 1 into a die, and carrying out hot pressing for 120min under the protection of argon atmosphere at 500 ℃ and under the pressure of 60MPa to obtain a high-density molybdenum trioxide blank;
step 3, carrying out 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 90 min;
and 4, machining and cleaning the blank subjected to the secondary oxygen supplementation treatment to finally obtain the high-purity molybdenum trioxide target.
Through detection, the molybdenum trioxide target material prepared by the embodiment has the mass purity of 99.95% and the density of 98.6%.
Claims (9)
1. A preparation method of a high-purity and high-density molybdenum trioxide target is characterized by comprising the following steps:
step 1, carrying out roasting treatment on ammonium molybdate to obtain high-purity molybdenum trioxide powder;
step 2, filling the high-purity molybdenum trioxide powder obtained in the step 1 into a mold, and carrying out atmosphere protection hot-pressing treatment to obtain a high-density molybdenum trioxide blank;
step 3, carrying out 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 supplementation treatment to finally obtain the high-purity molybdenum trioxide target.
2. The method for preparing a high-purity and high-density molybdenum trioxide target material according to claim 1, wherein the ammonium molybdate in the step 1 is one or a mixture of ammonium dimolybdate, ammonium tetramolybdate, ammonium heptamolybdate, ammonium octamolybdate and ammonium dodecamolybdate.
3. The method for preparing a high-purity and high-density molybdenum trioxide target material as claimed in claim 1, wherein the roasting treatment process in step 1 is a process of subjecting ammonium molybdate to high temperature treatment for decomposition reaction to obtain high-purity molybdenum trioxide, the temperature range of the high temperature treatment is 300-600 ℃, the atmosphere is air, and the roasting time is 20-120 min.
4. The method for preparing a high-purity and high-density molybdenum trioxide target material according to claim 1, wherein the purity of the high-purity molybdenum trioxide in the step 1 is at least 99.95%, and the average particle size is 0.5 μm to 50 μm.
5. The preparation method of the high-purity high-density molybdenum trioxide target material according to claim 1, wherein the temperature of the atmosphere protection hot-pressing sintering in the step 2 is 400-650 ℃, the pressure is 30-500 MPa, the time is 15-240 min, and the protective atmosphere is: an inert gas.
6. The method for preparing a high-purity and high-density molybdenum trioxide target material according to claim 5, wherein the inert gas is argon or nitrogen.
7. The method for preparing a high-purity and high-density molybdenum trioxide target material according to claim 1, wherein the density of the high-density molybdenum trioxide blank in the step 2 is not less than 98.5%.
8. The preparation method of the high-purity high-density molybdenum trioxide target material according to claim 1, wherein the secondary oxygen supplement treatment is performed in a muffle furnace in an air atmosphere in the step 3, wherein the temperature in the muffle furnace is 400-600 ℃, and the oxygen supplement treatment time is 15-120 min.
9. The method for preparing a high-purity and high-density molybdenum trioxide target material as claimed in claim 1, wherein the purity of the molybdenum trioxide target material finally obtained in the step 4 is not less than 99.95%, and the density is not less than 98.5%.
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| CN114737159A (en) * | 2022-04-14 | 2022-07-12 | 金堆城钼业股份有限公司 | Molybdenum trioxide sputtering target, preparation method and target mold |
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| CN114737159A (en) * | 2022-04-14 | 2022-07-12 | 金堆城钼业股份有限公司 | Molybdenum trioxide sputtering target, preparation method and target mold |
| CN114737159B (en) * | 2022-04-14 | 2024-04-30 | 金堆城钼业股份有限公司 | Molybdenum trioxide sputtering target material, preparation method and target material mold |
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| CN112359336B (en) | 2023-05-26 |
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