CN114560700B - Non-doped conductive zinc telluride target and preparation method thereof - Google Patents
Non-doped conductive zinc telluride target and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of sputtering target preparation, and discloses a non-doped conductive zinc telluride target and a preparation method thereof. The preparation method comprises the following steps: uniformly mixing zinc telluride powder, tellurium powder and zinc powder, wherein the weight percentage of the zinc telluride powder is 70-90%, and the molar ratio of the tellurium powder to the zinc powder is 1:1; putting the obtained mixed powder into a tube furnace, and heating to 300-350 ℃ under inert atmosphere for pre-sintering; and (2) putting the pre-sintered powder into a mold, then putting the mold into a vacuum hot-pressing furnace, heating to 500-550 ℃ for vacuum hot-pressing treatment, cooling the treated material along with the furnace, discharging the cooled material out of the furnace to obtain a blank target material, and then carrying out post-processing treatment on the blank target material to obtain a non-doped conductive zinc telluride target finished product. The preparation method of the invention has no other element doping, can realize good uniformity under the condition of relatively low hot pressing temperature and pressure, and the obtained zinc telluride target has high relative density and good conductivity.
Description
Technical Field
The invention belongs to the technical field of sputtering target preparation, and particularly relates to a non-doped conductive zinc telluride target and a preparation method thereof.
Background
Zinc telluride is a II-VI compound with a chemical formula of ZnTe, and is increasingly applied in the fields of photoluminescence and electroluminescent devices, solar cells, infrared detectors, thermal imaging technologies and the like. The cadmium telluride thin film solar cell is widely applied at present. With the requirements on carbon peak reaching and carbon neutralization of the environment, the thin-film solar cell is rapidly developed, and the requirements on zinc telluride are higher and higher.
At present, the zinc telluride film is mainly formed by magnetron sputtering, the target material is required to have certain conductivity in the magnetron sputtering preparation process, but the conductivity of the pure zinc telluride target material is poorer, and the conductivity of the pure zinc telluride target material is usually improved by doping copper, silver and other substances with good conductivity. However, the conductivity is increased, and the contents of copper, silver and the like are also increased, so that the film is influenced to a certain extent.
Patent CN 113121232A discloses a preparation method of a conductive zinc telluride target, which comprises the following steps: uniformly mixing zinc telluride powder and cuprous telluride powder, and then carrying out hot-pressing sintering to obtain a conductive zinc telluride target; wherein in the hot-pressing sintering process, the pressure is increased to 45-70 MPa at 500-900 ℃, and then the temperature and pressure are maintained. The invention enables the obtained zinc telluride target to have very good conductivity by doping cuprous telluride in the zinc telluride. However, the method introduces copper element into the target material, which has certain influence on the film; in order to realize good uniformity and improve the relative density of the target material, the temperature and the pressure of the hot-pressing sintering are relatively high.
Patent CN 113402276A discloses a preparation method of a zinc telluride doped planar target, which comprises the following steps: s1) mixing materials: mixing zinc telluride powder, zinc simple substance powder and tellurium simple substance powder to obtain a mixed material; s2) sintering: heating and sintering the mixed material to obtain a sintered material; s3) ball milling: performing ball milling on the sintering material to obtain a ball-milled material; s4) prepressing: prepressing the ball-milled material to obtain a molded blank body; s5) hot pressing: and carrying out vacuum hot-pressing sintering on the formed blank to obtain the zinc telluride zinc-doped planar target. The zinc and tellurium are doped in the zinc telluride, so that the conductivity of the original zinc telluride target can be improved, the purity and the density of the prepared target are higher, and the sputtering conductivity of the target can be improved. However, the method introduces zinc element and excessive tellurium element into the target material, and has free zinc and tellurium, which have certain influence on the film; in addition, in order to realize good uniformity, multiple steps of multi-stage sintering, ball milling treatment and the like are required, and the process is relatively complex.
Patent CN 107805788A discloses a preparation method of a zinc telluride target, which comprises the following steps: s1, grinding to prepare powder: grinding the zinc telluride alloy with the purity of 4.5N or above by using a ball mill and sieving by using a screen to obtain powder with the particle size of 10-200 micrometers; s2, prepressing: putting the powder into a graphite die, prepressing and forming into a blank; s3, blank preparation: loading the blank into a sheath, then carrying out vacuum-pumping sealing on the sheath, and then moving the sheath into a furnace body of a sintering furnace; vacuumizing the furnace body until the absolute vacuum degree is lower than 5Pa, then heating to 400-550 ℃ at the heating rate of 5-10 ℃/min, and preserving heat for 1-2 hours without pressurizing; heating at a heating rate of 10-20 ℃/min, starting continuous pressurization, starting heat preservation and pressure maintaining when the temperature rises to 700-850 ℃ and the pressure reaches 30-70 MPa, closing a heating power supply of the sintering furnace to start cooling after the heat preservation and pressure maintaining for 2-4 hours, and gradually and slowly releasing pressure to normal pressure when the temperature of the furnace body is reduced to 600 ℃; after the furnace body is completely cooled to room temperature, taking out the sheath from the furnace body, and stripping the sheath to obtain a zinc telluride target blank; s4, blank post-processing treatment: and (3) machining and electromachining the zinc telluride target blank, and then polishing, cleaning and drying to obtain the zinc telluride target. Intrinsic zinc telluride, however, is not conductive and its hot pressing temperature and pressure are relatively high in order to achieve high relative density. Therefore, it is significant how to obtain a non-doped conductive zinc telluride target and obtain a high relative density zinc telluride target at a relatively low temperature and pressure.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention mainly aims to provide a preparation method of a non-doped conductive zinc telluride target. The preparation method of the invention has no other element doping, can realize good uniformity under the condition of relatively low hot pressing temperature and pressure, and the obtained zinc telluride target has high relative density and good conductivity.
The invention also aims to provide the non-doped conductive zinc telluride target prepared by the method.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a non-doped conductive zinc telluride target comprises the following preparation steps:
(1) Mixing ingredients: uniformly mixing zinc telluride powder, tellurium powder and zinc powder, wherein the weight percentage of the zinc telluride powder is 70-90%, and the molar ratio of the tellurium powder to the zinc powder is 1:1;
(2) Pre-sintering: putting the mixed powder in the step (1) into a tube furnace, and heating to 300-350 ℃ in an inert atmosphere for pre-sintering;
(3) Hot pressing: putting the powder pre-sintered in the step (2) into a mould, then putting the mould into a vacuum hot-pressing furnace, and heating to 500-550 ℃ for vacuum hot-pressing treatment;
(4) Discharging and post-processing: and (4) cooling the material treated in the step (3) along with the furnace, discharging the material out of the furnace to obtain a blank target material, and then performing post-processing treatment on the blank target material to obtain a non-doped conductive zinc telluride target material finished product.
Further, the purity of the zinc telluride powder, the tellurium powder and the zinc powder in the step (1) is not lower than 5N.
Further, the particle size of the zinc telluride powder in the step (1) is less than 150 μm, and the particle sizes of the tellurium powder and the zinc powder are less than 45 μm.
Further, the heating rate in the step (2) is 10-15 ℃/min.
Further, the time of the pre-sintering in the step (2) is 20-30 min.
Further, the temperature rise rate in the step (3) is 5-10 ℃/min.
Further, the vacuum degree of the vacuum hot pressing treatment in the step (3) is less than 5Pa, and the hot pressing pressure is 30-45 Mpa.
Further, the time of the vacuum hot-pressing treatment in the step (3) is 60-100 min.
Further, the post-processing treatment in the step (4) comprises the following steps: and CNC machining the surface of the target.
The non-doped conductive zinc telluride target is prepared by the method.
Furthermore, the relative density of the non-doped conductive zinc telluride target is more than 96%, and the resistivity is less than 1500 omega cm.
Compared with the prior art, the invention has the beneficial effects that:
(1) The preparation method is simple, has low requirements on equipment and is low in preparation cost.
(2) The conductive zinc telluride target material obtained by the invention has no doping of other elements and has no influence on the prepared zinc telluride film.
(3) According to the invention, the tellurium powder and the zinc powder which are in a theoretical ratio are added, so that the target after hot pressing has conductivity under the condition of no other element doping, and the technical problem that the undoped zinc telluride target is non-conductive is solved.
(4) The undoped zinc telluride target can be prepared under the conditions of relatively low hot pressing temperature and pressure, and the obtained zinc telluride target has high relative density and good conductivity.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
(1) Mixing ingredients: high-purity 5N zinc telluride powder, 5N tellurium powder and 5N zinc powder are selected, wherein the particle size of the zinc telluride powder is less than 150 microns, and the particle size of the tellurium powder and the particle size of the zinc powder are less than 45 microns. Uniformly mixing zinc telluride powder, tellurium powder and zinc powder, wherein the weight percentage of the zinc telluride powder is 90%, and the molar ratio of the tellurium powder to the zinc powder is 1:1.
(2) Pre-sintering: and putting the powder into a tubular furnace in an inert gas atmosphere for heating and presintering, wherein the heating rate is 15 ℃/min, the presintering temperature is 300 ℃, and the presintering time is 30 minutes.
(3) Hot pressing: and (3) putting the pre-sintered powder into a mold, and then putting the mold into a vacuum hot pressing furnace for vacuum hot pressing, wherein the heating rate is 5 ℃/min, the hot pressing temperature is 520 ℃, the pressure is 35Mpa, the heat preservation and pressure maintaining time is 100min, and the vacuum degree is less than 5Pa.
(4) Discharging from the furnace and post-processing: and (4) cooling along with the furnace, discharging to obtain a blank target material, and processing the surface of the target material through CNC to obtain the pure conductive zinc telluride target material.
Example 2
(1) Mixing ingredients: high-purity 5N zinc telluride powder, 5N tellurium powder and 5N zinc powder are selected, wherein the particle size of the zinc telluride powder is less than 150 microns, and the particle size of the tellurium powder and the particle size of the zinc powder are less than 45 microns. Uniformly mixing zinc telluride powder, tellurium powder and zinc powder, wherein the weight percentage of the zinc telluride powder is 80%, and the molar ratio of the tellurium powder to the zinc powder is 1:1.
(2) Pre-sintering: and putting the powder into a tubular furnace in an inert gas atmosphere for heating and presintering, wherein the heating rate is 12 ℃/min, the presintering temperature is 350 ℃, and the presintering time is 25 minutes.
(3) Hot pressing: and (3) putting the pre-sintered powder into a mold, and then putting the mold into a vacuum hot pressing furnace for vacuum hot pressing, wherein the heating rate is 10 ℃/min, the hot pressing temperature is 500 ℃, the pressure is 45Mpa, the heat preservation and pressure maintaining time is 60min, and the vacuum degree is less than 5Pa.
(4) Discharging and post-processing: and (4) cooling along with the furnace, discharging to obtain a blank target material, and processing the surface of the target material through CNC to obtain the pure conductive zinc telluride target material.
Example 3
(1) Mixing ingredients: high-purity 5N zinc telluride powder, 5N tellurium powder and 5N zinc powder are selected, wherein the particle size of the zinc telluride powder is less than 150 microns, and the particle size of the tellurium powder and the particle size of the zinc powder are less than 45 microns. And uniformly mixing zinc telluride powder, tellurium powder and zinc powder, wherein the weight percentage of the zinc telluride powder is 70%, and the molar ratio of the tellurium powder to the zinc powder is 1:1.
(2) Pre-sintering: and putting the powder into a tubular furnace in an inert gas atmosphere for heating and presintering, wherein the heating rate is 10 ℃/min, the presintering temperature is 320 ℃, and the presintering time is 20 minutes.
(3) Hot pressing: and (3) putting the pre-sintered powder into a mold, and then putting the mold into a vacuum hot-pressing furnace for vacuum hot-pressing, wherein the heating rate is 8 ℃/min, the hot-pressing temperature is 550 ℃, the pressure is 40Mpa, the heat-preservation and pressure-maintaining time is 70min, and the vacuum degree is less than 5Pa.
(4) Discharging and post-processing: and (4) cooling along with the furnace, discharging to obtain a blank target material, and processing the surface of the target material through CNC to obtain the pure conductive zinc telluride target material.
Comparative example 1
Compared with the embodiment 3, the preparation method of the invention has the advantages that the tellurium powder and the zinc powder are not added, 100 percent of zinc telluride powder is adopted, and the other preparation processes are the same.
Comparative example 2
Compared with the embodiment 3, the weight of the zinc telluride powder is reduced to 60%, and the rest preparation processes are the same.
The zinc telluride targets obtained in the above examples and comparative examples were subjected to a relative density test (the density of the target was measured by a drainage method and the relative density was calculated) and a resistivity test (the resistivity was measured by a four-probe resistivity tester), and the test results are shown in table 1.
TABLE 1
The results in table 1 show that the target material prepared from pure zinc telluride powder has no conductivity, the target material after hot pressing has conductivity by adding tellurium powder and zinc powder in a theoretical ratio under the condition of no doping of other elements, and the conductivity is good when the weight percentage of the zinc telluride powder is 70-90%, and the resistivity is less than 1500 omega cm. The undoped zinc telluride target material can be prepared under the conditions of relatively low hot pressing temperature (500-550 ℃) and pressure (30-45 Mpa), and the obtained zinc telluride target material has high relative density which is more than 96 percent. And the relative density of the target material is obviously reduced due to the fact that the weight proportion of the zinc telluride powder is too high or too low.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (8)
1. A preparation method of a non-doped conductive zinc telluride target is characterized by comprising the following preparation steps:
(1) Mixing ingredients: uniformly mixing zinc telluride powder, tellurium powder and zinc powder, wherein the weight percentage of the zinc telluride powder is 70% -90%, and the molar ratio of the tellurium powder to the zinc powder is 1:1;
(2) Pre-sintering: putting the mixed powder in the step (1) into a tube furnace, and heating to 300-350 ℃ in an inert atmosphere for pre-sintering;
(3) Hot pressing: filling the powder pre-sintered in the step (2) into a mold, then putting the mold into a vacuum hot pressing furnace, and heating to 500-550 ℃ for vacuum hot pressing treatment;
(4) Discharging and post-processing: cooling the material treated in the step (3) along with the furnace, discharging the material out of the furnace to obtain a blank target material, and performing post-processing treatment on the blank target material to obtain a non-doped conductive zinc telluride target finished product;
the vacuum degree of the vacuum hot pressing treatment in the step (3) is less than 5Pa, the hot pressing pressure is 30 to 45Mpa, and the vacuum hot pressing treatment time is 60 to 100min;
the relative density of the non-doped conductive zinc telluride target is more than 96%, and the resistivity is less than 1500 omega cm.
2. The preparation method of the non-doped conductive zinc telluride target as claimed in claim 1, wherein the purity of the zinc telluride powder, the tellurium powder and the zinc powder in the step (1) is not less than 5N.
3. The method for preparing the undoped conductive zinc telluride target material as claimed in claim 1, wherein the particle size of the zinc telluride powder in the step (1) is less than 150 μm, and the particle sizes of the tellurium powder and the zinc powder are less than 45 μm.
4. The method for preparing the undoped conductive zinc telluride target as claimed in claim 1, wherein the heating rate in the step (2) is 10 to 15 ℃/min.
5. The method for preparing the undoped conductive zinc telluride target material as claimed in claim 1, wherein the pre-sintering time in the step (2) is 20 to 30min.
6. The method for preparing the undoped conductive zinc telluride target as claimed in claim 1, wherein the temperature rise rate in the step (3) is 5 to 10 ℃/min.
7. The method for preparing the undoped conductive zinc telluride target as claimed in claim 1, wherein the post-processing step in the step (4) is: and CNC machining the surface of the target.
8. A non-doped conductive zinc telluride target prepared by the method of any one of claims 1~7.
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| CN115417452B (en) * | 2022-10-19 | 2024-05-14 | 铜仁学院 | Method for producing zinc arsenide by improved fusion synthesis method |
Citations (5)
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