CN113666717A - Conductive TeOXRotary target material and preparation method thereof - Google Patents
Conductive TeOXRotary target material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a conductive TeOXThe preparation method of the rotary target comprises the following steps: (1) mixing Te powder and TeO2Uniformly mixing the powder to obtain a mixture; (2) spraying a release agent on a graphite die, then coating a layer of boron nitride powder, then loading the mixture obtained in the step (1) into the graphite die for hot pressing, cooling and discharging to obtain TeOXThe target is rotated. The invention also provides TeO prepared by the preparation methodXThe target is rotated. TeO2Reacts with a mold release agent having reducibility at high temperature, and thus the present inventionA layer of boron nitride powder is coated on the contact surface of the release agent and the powder. The target material prepared by the method has the relative density of more than 90 percent, the purity of more than 5N 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 conductive TeOXA rotary target material and a preparation method thereof.
Background
Tellurium oxide (TeO)X) Has good acousto-optic performance, chemical stability, mechanical durability and dielectric constant, and has wide application in active optical devices such as deflectors, modulators, tunable optical filters, ray detectors, gas sensors and the likeAnd (4) foreground. Reported that TeO2The refractive index of the base glass is SiO2100 times higher, indicating its potential application in nonlinear optics technology. But the existing TeOXThe film being essentially formed by thermal evaporation or by tellurium target material and O2Prepared by reactive sputtering. Which typically results in TeOXThe uniformity of the film composition was insufficient. And pure TeO2The target material has poor conductivity, which is not beneficial to subsequent sputtering coating.
In view of the above, the present invention is to provide a TeO with low resistivity, high purity and high densityXA preparation method of a rotary target.
Disclosure of Invention
In order to achieve the purpose, the invention adopts the technical scheme that: conductive TeOXThe preparation method of the rotary target comprises the following steps:
(1) mixing Te powder and TeO2Uniformly mixing the powder to obtain a mixture;
(2) spraying a release agent on a graphite die, then coating a layer of boron nitride powder, then loading the mixture obtained in the step (1) into the graphite die for hot pressing, cooling and discharging to obtain TeOXThe target is rotated.
According to the invention, a layer of boron nitride powder is coated on the contact surface of the release agent and the powder, so that good sliding property between the material powder and the internal mold can be ensured, and TeO can be effectively avoided2And a problem of reaction with a mold release agent having reducibility at high temperature.
As a further improvement of the invention, in the step (1), Te powder and TeO2The mass ratio of the powder is 5-15% to 85-95%. X is more than or equal to 1.64 and less than or equal to 1.88.
As a further improvement of the invention, Te powder and TeO2The particle size of the powder was-325 mesh, and the purity was 5N.
As a further improvement of the invention, in the step (1), the mixing operation is ball milling and mixing in a ball milling tank.
As a further improvement of the present invention, in the step (2), before hot pressing, the method further comprises the following steps: and putting the graphite mold filled with the materials into a hot pressing furnace.
As a further improvement of the invention, in the step (2), the hot pressing process comprises the steps of firstly vacuumizing the furnace body until the absolute vacuum degree is lower than 5Pa, then heating to 300-400 ℃, preserving heat for 40-60 min, continuously heating to 660-680 ℃, preserving heat for 30-50 min, then starting pressurizing, and continuously preserving heat for 50-60 min after the pressure reaches 18-25 MPa.
As a further improvement of the invention, the temperature rising rate of the temperature rising to 300-400 ℃ is 4-6 ℃/min, the temperature rising rate of the temperature rising to 660-680 ℃ is 5-10 ℃/min, and the time of pressurizing to 18-25 MPa is 30-50 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 mixing TeO obtained in the step (2)XAnd rotating the target material to perform machining, grinding and polishing treatment.
Simultaneously provides a conductive TeOXThe rotary target material adopts the TeOXThe preparation method of the rotary target material is obtained.
Compared with the prior art, the invention has the beneficial effects that: the tellurium powder and the tellurium dioxide powder are used as raw materials to manufacture the target material, which can reduce the resistivity of the target material while ensuring that the target material can reach 5N purity (without introducing other impurity elements), and is beneficial to sputtering and coating of the target material. A layer of boron nitride powder is smeared on the contact surface of the release agent and the powder, so that good sliding property between the material powder and the internal mold can be ensured, and TeO can be effectively avoided2And a problem of reaction with a mold release agent having reducibility at high temperature. The target material prepared by the method has the relative density of more than 90 percent, the purity of more than 5N and the resistivity of less than 2000 omega cm.
Drawings
FIG. 1 shows the relative densities and resistivities of targets prepared in 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 conductive TeOXThe preparation method of the rotary target comprises the following steps:
(1) mixing Te powder and TeO2Uniformly mixing the powder to obtain a mixture;
(2) spraying a release agent on a graphite die, then coating a layer of boron nitride powder, then loading the mixture obtained in the step (1) into the graphite die for hot pressing, cooling and discharging to obtain TeOXThe target is rotated.
In certain embodiments of the present invention, in step (1), Te powder and TeO2The mass ratio of the powder is 5-15% to 85-95%. The Te powder accounts for too little mass, which can cause the resistivity of the synthesized target material to be too large and can not meet the sputtering requirement; too much mass proportion of Te powder can cause the thermal expansion coefficient of the target material to be increased, and extrusion cracking during hot pressing can be caused.
In certain embodiments of the invention, Te powder and TeO2The particle size of the powder was-325 mesh, and the purity was 5N.
As a further improvement of the invention, in the step (1), the mixing operation is ball milling and mixing in a ball milling tank.
As a further improvement of the present invention, in the step (2), before hot pressing, the method further comprises the following steps: and putting the graphite mold filled with the materials into a hot pressing furnace.
As a further improvement of the invention, in the step (2), the hot pressing process comprises the steps of firstly vacuumizing the furnace body until the absolute vacuum degree is lower than 5Pa, then heating to 300-400 ℃, preserving heat for 40-60 min, continuously heating to 660-680 ℃, preserving heat for 30-50 min, then starting pressurizing, and continuously preserving heat for 50-60 min after the pressure reaches 18-25 MPa.
As a further improvement of the invention, the temperature rising rate of the temperature rising to 300-400 ℃ is 4-6 ℃/min, the temperature rising rate of the temperature rising to 660-680 ℃ is 5-10 ℃/min, and the time of pressurizing to 18-25 MPa is 30-50 min. Because the bending strength of the TeOx material is very low (9.549MPa), if the pressure is too fast or too high, the hot-pressing crack of the target material can be caused; if the pressing is too slow, the hot pressing time is long, and time and labor are wasted.
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 mixing TeO obtained in the step (2)XAnd rotating the target material to perform machining, grinding and polishing treatment.
Simultaneously provides a conductive TeOXThe rotary target material adopts the TeOXThe preparation method of the rotary target material is obtained.
Example 1.
Conductive TeOXThe preparation method of the rotary target comprises the following steps:
(1) mixing-325 mesh Te powder and-325 mesh TeO2And (3) filling the powder into a ball milling tank according to the mass ratio of 5% to 95%, and uniformly mixing to obtain a mixture.
(2) Spraying a release agent on a graphite mold, then coating a layer of boron nitride powder, then loading the mixture obtained in the step (1) into the graphite mold, then placing the graphite mold into a hot pressing furnace, vacuumizing the furnace body until the absolute vacuum degree is lower than 5Pa, then heating to 300 ℃ at the heating rate of 4 ℃/min, preserving heat for 40min, continuously heating to 660 ℃ at the heating rate of 5 ℃/min, preserving heat for 30min, then starting pressurizing, pressurizing for 30min, continuing preserving heat for 50min after the pressure reaches 18MPa, finally starting pressure relief when the temperature is reduced to be lower than 300 ℃ along with the furnace, discharging after the temperature is reduced to room temperature, and obtaining TeOXThe target is rotated.
(3) Machining, grinding and polishing the target material obtained in the step (2) to obtain TeO with different sizes and shapesXThe target is rotated.
TeO prepared in this exampleXThe target density is tested by adopting a drainage method and the resistivity is tested by adopting a four-probe resistivity tester by rotating the target, and the test result is shown in figure 1.
TeO prepared in this exampleXRotateThe target material has high relative density and good conductivity, the resistivity is 1882 omega-cm, and the relative density reaches 90.5%.
Example 2.
Conductive TeOXThe preparation method of the rotary target comprises the following steps:
(1) mixing-325 mesh Te powder and-325 mesh TeO2And (3) filling the powder into a ball milling tank according to the mass ratio of 10% to 90%, and uniformly mixing to obtain a mixture.
(2) Spraying a release agent on a graphite mold, then coating a layer of boron nitride powder, then loading the mixture obtained in the step (1) into the graphite mold, then placing the graphite mold into a hot pressing furnace, vacuumizing the furnace body until the absolute vacuum degree is lower than 5Pa, then heating to 350 ℃ at the heating rate of 5 ℃/min, preserving heat for 50min, continuously heating to 670 ℃ at the heating rate of 8 ℃/min, preserving heat for 40min, then starting pressurizing, pressurizing for 40min, continuing preserving heat for 55min after the pressure reaches 22MPa, finally starting pressure relief when the temperature is reduced to be lower than 300 ℃ along with the furnace, discharging after the temperature is reduced to room temperature, and obtaining TeOXThe target is rotated.
(3) Machining, grinding and polishing the target material obtained in the step (2) to obtain TeO with different sizes and shapesXThe target is rotated.
TeO prepared in this exampleXThe target density is tested by adopting a drainage method and the resistivity is tested by adopting a four-probe resistivity tester by rotating the target, and the test result is shown in figure 1.
TeO prepared in this exampleXThe rotary target material has high relative density and good conductivity, the resistivity of the rotary target material is 1551 omega cm, and the relative density reaches 91.4%.
Example 3.
Conductive TeOXThe preparation method of the rotary target comprises the following steps:
(1) mixing-325 mesh Te powder and-325 mesh TeO2And (3) filling the powder into a ball milling tank according to the mass ratio of 15% to 85%, and uniformly mixing to obtain a mixture.
(2) Spraying a release agent on the graphite mould, then coating a layer of boron nitride powder, and obtaining the product in the step (1)Putting the mixture into a graphite mold, putting the graphite mold into a hot-pressing furnace, vacuumizing the furnace body until the absolute vacuum degree is lower than 5Pa, heating to 400 ℃ at the heating rate of 6 ℃/min, keeping the temperature for 60min, continuously heating to 680 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 50min, pressurizing for 50min, keeping the temperature for 60min after the pressure reaches 25MPa, finally starting pressure relief when the temperature is reduced to be lower than 300 ℃ along with the furnace, cooling to room temperature, discharging, and obtaining TeOXThe target is rotated.
(3) Machining, grinding and polishing the target material obtained in the step (2) to obtain TeO with different sizes and shapesXThe target is rotated.
TeO prepared in this exampleXThe target density is tested by adopting a drainage method and the resistivity is tested by adopting a four-probe resistivity tester by rotating the target, and the test result is shown in figure 1.
TeO prepared in this exampleXThe rotary target material has high relative density and good conductivity, the resistivity is 1306 omega-cm, the relative density reaches 93.5%, and the purity is 5N.
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 (10)
1. Conductive TeOXThe preparation method of the rotary target is characterized by comprising the following steps:
(1) mixing Te powder and TeO2Uniformly mixing the powder to obtain a mixture;
(2) spraying a release agent on a graphite die, then coating a layer of boron nitride powder, then loading the mixture obtained in the step (1) into the graphite die for hot pressing, cooling and discharging to obtain TeOXThe target is rotated.
2. The method according to claim 1, wherein in the step (1), Te powder and TeO2The mass ratio of the powder is 5-15% to 85-95%.
3. The method of claim 1, wherein Te powder and TeO2The particle size of the powder was-325 mesh, and the purity was 5N.
4. The method of claim 1, wherein in the step (1), the mixing operation is ball milling and mixing in a ball milling tank.
5. The method according to claim 1, wherein the step (2) further comprises the following steps before the hot pressing: and putting the graphite mold filled with the materials into a hot pressing furnace.
6. The preparation method according to claim 1, wherein in the step (2), the hot pressing process comprises the steps of vacuumizing the furnace body to an absolute vacuum degree of less than 5Pa, heating to 300-400 ℃, keeping the temperature for 40-60 min, continuously heating to 660-680 ℃, keeping the temperature for 30-50 min, starting pressurizing, and keeping the temperature for 50-60 min after the pressure reaches 18-25 MPa.
7. The method according to claim 6, wherein the temperature raising rate is 4 to 6 ℃/min when the temperature is raised to 300 to 400 ℃, the temperature raising rate is 5 to 10 ℃/min when the temperature is raised to 660 to 680 ℃, and the time for pressurizing to 18 to 25MPa is 30 to 50 min.
8. The preparation method according to claim 1, wherein in the step (2), the temperature reduction and tapping operation is to start pressure relief when the temperature of the furnace is reduced to less than 300 ℃, and to tap the furnace after the temperature is reduced to room temperature.
9. The method according to claim 1, further comprising a step (3) of reacting the TeO obtained in the step (2)XRotary targetThe material is subjected to machining, grinding and polishing.
10. Conductive TeOXA rotary target, characterized in that it uses TeO according to any of claims 1 to 9XThe preparation method of the rotary target material is obtained.
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| JPS6134743A (en) * | 1984-07-26 | 1986-02-19 | Matsushita Electric Ind Co Ltd | Manufacture of photoelectromagnetic recording medium |
| JPS61122951A (en) * | 1984-11-19 | 1986-06-10 | Matsushita Electric Ind Co Ltd | Coating method of recording medium for optical recording disk |
| JPS6256352A (en) * | 1985-09-06 | 1987-03-12 | 東ソー株式会社 | Sputtering target for optical recording and manufacture |
| CN104694889A (en) * | 2013-12-10 | 2015-06-10 | 北京有色金属研究总院 | Preparation method of CdTe sputtering target material |
| CN104362248A (en) * | 2014-10-10 | 2015-02-18 | 浙江理工大学 | Method for preparing high-seebeck-coefficient tellurium/tellurium oxide nanocomposite with solvothermal |
| CN109550960A (en) * | 2018-11-06 | 2019-04-02 | 金堆城钼业股份有限公司 | A method of preventing HIP sintering part and jacket adhesion |
| CN110127633A (en) * | 2019-06-25 | 2019-08-16 | 先导薄膜材料（广东）有限公司 | A kind of cadmium telluride target and preparation method thereof |
| CN111020334A (en) * | 2020-01-08 | 2020-04-17 | 郑州航空工业管理学院 | Preparation method of high-densification tungsten-copper refractory alloy |
| CN111304476A (en) * | 2020-02-29 | 2020-06-19 | 郑州航空工业管理学院 | Preparation method of fine-grain powder superalloy for inhibiting formation of original grain boundary |
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