CN112195446B - Arsenic-doped manganous oxide target material and preparation method thereof - Google Patents
Arsenic-doped manganous oxide target material and preparation method thereof Download PDFInfo
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- CN112195446B CN112195446B CN202010953109.2A CN202010953109A CN112195446B CN 112195446 B CN112195446 B CN 112195446B CN 202010953109 A CN202010953109 A CN 202010953109A CN 112195446 B CN112195446 B CN 112195446B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/12—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on oxides
Abstract
The invention relates toAnd a preparation method of the arsenic-doped manganous oxide target material, which comprises the following steps: (1) Mixing AsMn powder and Mn 2 O 3 Uniformly mixing the powder to obtain a mixture; (2) And (2) putting the mixture obtained in the step (1) into a sheath, putting the sheath into a hot isostatic pressing furnace for sintering, and then cooling and discharging the sheath to obtain the arsenic-doped manganese sesquioxide target material. The invention also provides the arsenic-doped manganous oxide target material prepared by the preparation method. The preparation method provided by the invention has the advantages of low cost and simple operation, and the obtained target has the relative density of more than 95% and the resistivity of less than 2000 omega-cm.
Description
Technical Field
The invention relates to the field of sputtering target material preparation, in particular to an arsenic-doped manganese oxide target material and a preparation method thereof.
Background
Hot isostatic pressing is an advanced sintering process. The product is placed in a closed container, the product is applied with equal pressure and high temperature, and the product is sintered and densified under the action of high temperature and high pressure.
Manganese sesquioxide (Mn) 2 O 3 ) Is a pure black crystal belonging to amphoteric oxide. And as an important functional material oxide, mn 2 O 3 The method has wide application in the fields of electrochemistry, catalysis, adsorption, magnetic materials, chemical sensors and the like. Mn 2 O 3 The conductive coating has excellent physical and chemical properties, but is non-conductive and not beneficial to coating, and the conductivity of the conductive coating is usually improved by doping. At present, the preparation of manganese sesquioxide target materials is rarely reported.
In view of the foregoing, it is an object of the present invention to provide a method for preparing an arsenic-doped manganese oxide target by hot isostatic pressing sintering.
Disclosure of Invention
The invention aims to provide an arsenic-doped manganous oxide target material and a preparation method thereof. The preparation method adopts a hot isostatic pressing sintering method, the uniformly mixed mixture is put into a sheath, the sheath is put into a hot isostatic pressing furnace for sintering, and the arsenic-doped manganese sesquioxide target material can be obtained after cooling and discharging. The preparation method provided by the invention has the advantages of low cost and simple operation, and the obtained target has the relative density of more than 95% and the resistivity of less than 2000 omega-cm.
In order to achieve the purpose, the invention adopts the technical scheme that: an arsenic-doped manganese oxide target material and a preparation method thereof are disclosed, wherein the preparation method comprises the following steps:
(1) Mixing AsMn powder and Mn 2 O 3 Uniformly mixing the powder to obtain a mixture;
(2) And (2) putting the mixture obtained in the step (1) into a sheath, putting the sheath into a hot isostatic pressing furnace for sintering, and then cooling and discharging the sheath to obtain the arsenic-doped manganese sesquioxide target material.
As a further improvement of the invention, in the step (1), asMn powder and Mn 2 O 3 The mass ratio of the powder is 3-5% and 95-97%.
As a further improvement of the invention, the particle size of the AsMn powder is-70 mesh; mn 2 O 3 The particle size of the powder was-100 mesh.
As a further improvement of the invention, in the step (1), the mixing operation is to load the mixture into a mixer for mixing.
As a further improvement of the invention, the step (2) further comprises the following steps after the sheath is installed: and vacuumizing, welding and sealing the sheath.
As a further improvement of the invention, in the step (2), the sintering process comprises the steps of firstly vacuumizing the furnace body until the absolute vacuum degree is lower than 10Pa, then heating to 600-650 ℃, keeping the temperature for 30min, then starting pressurizing, keeping the temperature for 30-50 min after the pressure reaches 75-80 MPa, finally heating to 750-800 ℃, and keeping the temperature for 60-70min.
As a further improvement of the invention, the heating rate of heating to 600-650 ℃ is 6-8 ℃/min, and the heating rate of heating to 750-800 ℃ is 2-3 ℃/min.
As a further improvement of the invention, in the step (2), the temperature reduction and discharge operation is to start pressure relief when the temperature of the furnace is reduced to less than 300 ℃, and discharge the furnace after the temperature is reduced to room temperature.
As a further improvement of the invention, the method also comprises a step (3) of carrying out mechanical processing, grinding and polishing treatment on the arsenic-doped manganous oxide target material obtained in the step (2).
Meanwhile, the arsenic-doped manganous oxide target is prepared by the preparation method of the arsenic-doped manganous oxide target.
Compared with the prior art, the invention has the beneficial effects that: the doping of the arsenic element greatly reduces the resistance of the manganese sesquioxide target material. The arsenic-doped manganous oxide target prepared by the method has the relative density of more than 95 percent and the resistivity of less than 2000 omega cm.
Drawings
Fig. 1 shows the resistivity and relative density of the targets of examples 1, 2 and 3 of the present invention.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
The invention provides a preparation method of an arsenic-doped manganous oxide target material, which comprises the following steps:
(1) Mixing AsMn powder and Mn 2 O 3 Uniformly mixing the powder to obtain a mixture;
(2) And (2) putting the mixture obtained in the step (1) into a sheath, putting the sheath into a hot isostatic pressing furnace for sintering, and then cooling and discharging the sheath to obtain the arsenic-doped manganese sesquioxide target material.
In certain embodiments of the invention, in step (1), asMn powder and Mn are 2 O 3 The mass ratio of the powder is 3-5% to 95-97%. The AsMn powder accounts for too little mass, so that the resistivity of the synthesized target material is too high, and the sputtering requirement cannot be met; too much AsMn powder mass fraction results in Mn 2 O 3 Conversion to Mn 3 O 4 Or MnO, because of Mn 2 O 3 Will deoxidize a little at high temperature and canAs is oxidized to a higher valence state, if the content of As is too large, mn will be generated 2 O 3 A large number of phase changes.
In certain embodiments of the invention, the AsMn powder has a particle size of-70 mesh; mn 2 O 3 The particle size of the powder was-100 mesh. AsMn powder and Mn 2 O 3 Too coarse a powder particle size results in a lower density of the target material obtained by hot isostatic pressing sintering.
As a further improvement of the invention, in the step (1), the mixing operation is to load the mixture into a mixer for mixing.
As a further improvement of the invention, the step (2) further comprises the following steps after the sheath is installed: and vacuumizing, welding and sealing the sheath.
As a further improvement of the invention, in the step (2), the sintering process comprises the steps of firstly vacuumizing the furnace body until the absolute vacuum degree is lower than 10Pa, then heating to 600-650 ℃, keeping the temperature for 30min, then starting pressurizing, keeping the temperature for 30-50 min after the pressure reaches 75-80 MPa, finally heating to 750-800 ℃, and keeping the temperature for 60-70min.
As a further improvement of the invention, the heating rate of heating to 600-650 ℃ is 6-8 ℃/min, and the heating rate of heating to 750-800 ℃ is 2-3 ℃/min.
As a further improvement of the invention, in the step (2), the temperature reduction and discharge operation is to start pressure relief when the temperature of the furnace is reduced to less than 300 ℃, and discharge the furnace after the temperature is reduced to room temperature.
As a further improvement of the invention, the method also comprises a step (3) of carrying out mechanical processing, grinding and polishing treatment on the arsenic-doped manganese oxide target material obtained in the step (2).
Meanwhile, the arsenic-doped manganous oxide target is prepared by the preparation method of the arsenic-doped manganous oxide target.
Example 1.
A preparation method of an arsenic-doped manganous oxide target material comprises the following steps:
(1) Mixing AsMn powder of-70 mesh and Mn of-100 mesh 2 O 3 The powder is filled into a mixer according to the mass ratio of 3 percent to 97 percentAnd (4) uniformly mixing to obtain a mixture.
(2) Putting the mixture obtained in the step (1) into a sheath, then carrying out vacuum-pumping welding sealing on the sheath, putting the sheath into a hot isostatic pressing furnace, vacuumizing the furnace body until the absolute vacuum degree is 10Pa lower, then heating to 600 ℃ at the heating rate of 8 ℃/min, carrying out heat preservation for 30min, then starting pressurization, and continuing to carry out heat preservation for 40min after the pressure reaches 75 MPa; and then heating to 750 ℃ at a speed of 3 ℃/min, preserving heat for 65min, finally, reducing the temperature along with the furnace to less than 300 ℃, relieving pressure, cooling to room temperature, and discharging to obtain the arsenic-doped manganese sesquioxide target material.
(3) And (3) carrying out mechanical processing, grinding and polishing treatment on the arsenic-doped manganous oxide target material obtained in the step (2).
The arsenic-doped manganese sesquioxide target material prepared in the embodiment is subjected to target material density test by adopting a drainage method, and the resistivity test by using a four-probe resistivity tester, wherein the test result is shown in figure 1.
The arsenic-doped manganese trioxide target prepared by the embodiment has excellent performance, the resistivity is 1560 omega cm, and the relative density reaches 95.5%.
Example 2.
A preparation method of an arsenic-doped manganous oxide target material comprises the following steps:
(1) Mixing AsMn powder of-70 mesh and Mn of-100 mesh 2 O 3 And (3) filling the powder with the mass ratio of 4% to 96% into a mixer, and uniformly mixing to obtain a mixture.
(2) Putting the mixture obtained in the step (1) into a sheath, then carrying out vacuum-pumping welding sealing on the sheath, putting the sheath into a hot isostatic pressing furnace, vacuumizing the furnace body until the absolute vacuum degree is 10Pa lower, then heating to 620 ℃ at the heating rate of 7 ℃/min, preserving heat for 30min, then starting pressurizing, and continuing preserving heat for 50min after the pressure reaches 78 MPa; and then heating to 800 ℃ at a speed of 2 ℃/min, preserving heat for 60min, finally, reducing the temperature along with the furnace to less than 300 ℃, relieving pressure, cooling to room temperature, and discharging to obtain the arsenic-doped manganese sesquioxide target material.
(3) And (3) carrying out mechanical processing, grinding and polishing treatment on the arsenic-doped manganese oxide target material obtained in the step (2).
The arsenic-doped manganese sesquioxide target material prepared in the embodiment is tested for target material density by adopting a drainage method, and a four-probe resistivity tester is used for testing resistivity, wherein the test results are shown in figure 1.
The arsenic-doped manganese trioxide target prepared by the embodiment has excellent performance, the resistivity is 1340 omega cm, and the relative density reaches 95.2%.
Example 3.
A preparation method of an arsenic-doped manganous oxide target material comprises the following steps:
(1) Mixing AsMn powder of-70 mesh and Mn of-100 mesh 2 O 3 And (3) filling the powder into a mixer according to the mass ratio of 5% to 95%, and uniformly mixing to obtain a mixture.
(2) Putting the mixture obtained in the step (1) into a sheath, then carrying out vacuum-pumping welding sealing on the sheath, putting the sheath into a hot isostatic pressing furnace, vacuumizing the furnace body until the absolute vacuum degree is 10Pa lower, then heating to 650 ℃ at the heating rate of 6 ℃/min, preserving heat for 30min, then starting pressurizing, and continuing preserving heat for 30min after the pressure reaches 80 MPa; and then heating to 780 ℃ at the speed of 2.5 ℃/min, preserving heat for 65min, finally, beginning pressure relief when the temperature is reduced to less than 300 ℃ along with the furnace, and discharging the material after the temperature is reduced to room temperature to obtain the arsenic-doped manganese sesquioxide target material.
(3) And (3) carrying out mechanical processing, grinding and polishing treatment on the arsenic-doped manganous oxide target material obtained in the step (2).
The arsenic-doped manganese sesquioxide target material prepared in the embodiment is tested for target material density by adopting a drainage method, and a four-probe resistivity tester is used for testing resistivity, wherein the test results are shown in figure 1.
The arsenic-doped manganous oxide target prepared by the embodiment has excellent performance, the resistivity of the arsenic-doped manganous oxide target is 1290 omega-cm, and the relative density reaches 95.9%.
Compared with the prior art, the invention has the beneficial effects that: the doping of the arsenic element greatly reduces the resistance of the manganese sesquioxide target material. The arsenic-doped manganous oxide target prepared by the method has the relative density of more than 95 percent and the resistivity of less than 2000 omega cm.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (4)
1. The arsenic-doped manganous oxide target material and the preparation method thereof are characterized by comprising the following steps:
(1) Mixing AsMn powder and Mn 2 O 3 Uniformly mixing the powder to obtain a mixture;
(2) Putting the mixture obtained in the step (1) into a sheath, putting the sheath into a hot isostatic pressing furnace for sintering, and then cooling and discharging the sheath to obtain the arsenic-doped manganese sesquioxide target material;
in the step (1), asMn powder and Mn 2 O 3 The mass ratio of the powder is 3-5 percent to 95-97 percent;
the particle size of the AsMn powder is-70 meshes; mn 2 O 3 The particle size of the powder is-100 meshes;
in the step (1), the mixing operation is to put the mixture into a mixer for mixing;
in the step (2), the sintering process comprises the steps of firstly vacuumizing the furnace body until the absolute vacuum degree is lower than 10Pa, then heating to 600-650 ℃, preserving heat for 30min, then starting pressurizing, continuing preserving heat for 30 min-50 min after the pressure reaches 75-80 MPa, finally heating to 750-800 ℃, and preserving heat for 60-70min;
the heating rate of heating to 600-650 ℃ is 6-8 ℃/min, and the heating rate of heating to 750-800 ℃ is 2-3 ℃/min;
in the step (2), the cooling and discharging operation is that the pressure is released when the temperature of the furnace is reduced to less than 300 ℃, and the furnace is discharged after the temperature is reduced to the room temperature;
the relative density of the prepared arsenic-doped manganous oxide target material is more than 95 percent, and the resistivity is less than 2000 omega cm.
2. The method of claim 1, wherein the step (2) further comprises the following steps after the step of filling the capsule: and vacuumizing, welding and sealing the sheath.
3. The method according to claim 1, further comprising a step (3) of subjecting the arsenic-doped manganese sesquioxide target obtained in the step (2) to machining, grinding, and polishing.
4. An arsenic-doped manganous oxide target, which is characterized by being prepared by the preparation method of the arsenic-doped manganous oxide target according to any one of claims 1 to 3.
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