CN115595539A - Zinc-magnesium target material and preparation method thereof - Google Patents
Zinc-magnesium target material and preparation method thereof Download PDFInfo
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- PGTXKIZLOWULDJ-UHFFFAOYSA-N [Mg].[Zn] Chemical compound [Mg].[Zn] PGTXKIZLOWULDJ-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 239000013077 target material Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000005096 rolling process Methods 0.000 claims abstract description 50
- 230000006698 induction Effects 0.000 claims abstract description 35
- 229910000861 Mg alloy Inorganic materials 0.000 claims abstract description 34
- 239000000956 alloy Substances 0.000 claims abstract description 34
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 25
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000004321 preservation Methods 0.000 claims abstract description 22
- 238000001816 cooling Methods 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 16
- 239000011777 magnesium Substances 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 16
- 239000011701 zinc Substances 0.000 claims abstract description 16
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000012545 processing Methods 0.000 claims abstract description 13
- 238000005266 casting Methods 0.000 claims abstract description 12
- 230000001681 protective effect Effects 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 40
- 229910052786 argon Inorganic materials 0.000 claims description 20
- 229910003363 ZnMgO Inorganic materials 0.000 claims description 7
- 238000005086 pumping Methods 0.000 claims 1
- 239000010409 thin film Substances 0.000 claims 1
- 238000005204 segregation Methods 0.000 abstract description 5
- 239000000047 product Substances 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 16
- 230000007547 defect Effects 0.000 description 11
- 238000007599 discharging Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 238000005336 cracking Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000013386 optimize process Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000009489 vacuum treatment Methods 0.000 description 1
Classifications
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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
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1828—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof the active layers comprising only AIIBVI compounds, e.g. CdS, ZnS, CdTe
- H01L31/1832—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof the active layers comprising only AIIBVI compounds, e.g. CdS, ZnS, CdTe comprising ternary compounds, e.g. Hg Cd Te
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Abstract
The invention discloses a zinc-magnesium target material and a preparation method thereof, and belongs to the technical field of target material preparation. The preparation method of the zinc-magnesium target material comprises the following steps: uniformly mixing a zinc source and a magnesium source, placing the mixture into a vacuum induction furnace for vacuumizing treatment, and introducing protective atmosphere until the pressure in the furnace is 2-10 Pa; starting a vacuum induction furnace at the speed of 20-30 ℃/min for magnetic induction heating to 520-560 ℃, preserving heat for 20-35 min, then cooling to 430-450 ℃, and continuing preserving heat for 3-5 h; casting the mixture obtained after heat preservation into a mold and cooling to obtain a zinc-magnesium alloy material; preheating a zinc-magnesium alloy material to 300-320 ℃, rolling, and processing the shape and the size of the obtained blank target to obtain the zinc-magnesium target material. According to the method, zinc and magnesium are rapidly fused by magnetic induction high-temperature heating, then the temperature is reduced and the temperature is kept, so that material loss and component segregation are avoided, and finally the target obtained by preheating and rolling is defect-free in the interior, high in component uniformity and capable of achieving a relative density of more than 99.5%.
Description
Technical Field
The invention relates to the technical field of target preparation, in particular to a zinc-magnesium target and a preparation method thereof.
Background
In the solar cell, the ZnMgO film not only has the characteristics of a TCO film, but also has larger forbidden bandwidth, higher visible light transmittance and structural stability than a ZnO film, an AZO film and the like. Meanwhile, the ZnMgO film is green and nontoxic, has rich sources and wide development space.
The prior process method for preparing the ZnMgO film mostly takes ZnMgO powder as a raw material to directly prepare the ZnMgO film or takes a zinc-magnesium target material to sputter in an oxygen atmosphere. However, the target products prepared by the existing methods have certain defects, so that the uniformity of the components is poor, and the relative density always does not reach the ideal degree.
Disclosure of Invention
Based on the defects in the prior art, the invention aims to provide a preparation method of a zinc-magnesium target, the method is characterized in that zinc and magnesium are rapidly fused by magnetic induction heating treatment, then material loss and component segregation caused by zinc vapor pressure are avoided by multi-section temperature zone treatment, and finally the target obtained by rolling is free of defects in the interior, high in component uniformity and capable of achieving a relative density of more than 99.5%.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a zinc-magnesium target material comprises the following steps:
(1) Uniformly mixing a zinc source and a magnesium source, putting the mixture into a vacuum induction furnace for vacuumizing treatment, and introducing protective atmosphere until the pressure in the furnace is 2-10 Pa;
(2) Starting a vacuum induction furnace at the speed of 20-30 ℃/min for magnetic induction heating to 520-560 ℃, preserving heat for 20-35 min, then cooling to 430-450 ℃, and continuing preserving heat for 3-5 h;
(3) Casting the mixed material obtained in the step (2) after heat preservation into a mould for cooling to obtain a zinc-magnesium alloy material;
(4) Preheating a zinc-magnesium alloy material to 300-320 ℃, rolling, and processing the shape and the size of the obtained blank target to obtain the zinc-magnesium target material.
According to the preparation method of the zinc-magnesium target material, the raw material zinc and the raw material magnesium are quickly and uniformly mixed by heating to a high degree through magnetic induction heating, the component uniformity of a product is guaranteed, then the product is quickly cooled to a lower temperature region for two-stage heat preservation, the material loss and component segregation caused by the zinc vapor pressure can be avoided, the product is cast to a mold and finally rolled in a preheating process, the internal defects of the finally prepared zinc-magnesium target material can be eliminated, the target material appearance is good, the phenomena of cracking and the like can not occur, the relative density is high, and the quality of the finished product is good.
Preferably, the mass ratio of the zinc source to the magnesium source in the step (1) is (90-99.9): (0.1-10).
According to actual needs and a proper range of a processing temperature rise interval, the uniformity of the set conditions during the preparation of the zinc-magnesium target material can be effectively controlled when the adding proportion of the zinc source and the magnesium source is in the range, and the uniform quality of products in batches is guaranteed.
Preferably, the step of performing vacuum treatment in step (1) is: vacuumizing the vacuum induction furnace until the pressure in the furnace is lower than 3 x 10 -3 Pa, then injecting protective atmosphere until the pressure in the furnace is changed to normal pressure, and vacuumizing until the pressure in the furnace is lower than 3X 10 - 2 Pa。
More preferably, the protective atmosphere is argon.
Preferably, the rolling times in the step (4) are 8-10 times, and the thickness of each rolling is 0.1-0.3 mm.
When the zinc-magnesium alloy material is heated to 300-320 ℃, the workability is obviously improved, and after the zinc-magnesium alloy material is rolled for multiple times by adopting thinner rolling thickness, the internal defect degree in the obtained blank target can be effectively reduced, so that the density of the product is obviously improved, and meanwhile, the undesirable phenomena of cracking and the like caused by overhigh rolling degree can be avoided.
The invention also aims to provide the zinc-magnesium target material prepared by the preparation method of the zinc-magnesium target material.
The zinc-magnesium target material prepared by the preparation method can realize the relative density of 99.7 percent at most under the optimized process, has high component uniformity, does not have a defect structure in the interior, does not crack in the appearance and the like, and has high relative quality.
The invention further aims to provide application of the zinc-magnesium target material in preparation of ZnMgO films for solar cells.
The invention has the beneficial effects that the invention provides the preparation method of the zinc-magnesium target material, the method firstly heats the zinc and the magnesium to a higher temperature by magnetic induction heating treatment to rapidly fuse the zinc and the magnesium, then reduces the temperature to a specific temperature to carry out heat preservation treatment to avoid material loss and component segregation caused by zinc vapor pressure, and finally, the target material obtained by a special preheating rolling process has no defect in the interior, high component uniformity and relative density of more than 99.5 percent.
Detailed Description
In order to better illustrate the objects, technical solutions and advantages of the present invention, the present invention will be further described below with reference to specific examples/comparative examples, which are intended to be a detailed understanding of the contents of the present invention, but are not intended to be limiting. All other embodiments obtained by a person skilled in the art without making any inventive step are within the scope of protection of the present invention. Unless otherwise stated, the experimental reagents, raw materials and instruments designed in the practice and comparative examples of the present invention are common reagents, raw materials and instruments.
Example 1
One embodiment of the zinc-magnesium target material and the preparation method thereof comprises the following steps:
(1) Uniformly mixing zinc powder and magnesium powder according to a mass ratio of 90 -3 Pa, then injecting argon until the pressure in the furnace is changed to normal pressure, and vacuumizing until the pressure in the furnace is lower than 3X 10 -2 Pa, finally introducing argon until the pressure in the furnace is 10Pa;
(2) Starting a vacuum induction furnace at the speed of 30 ℃/min for magnetic induction heating to 560 ℃, preserving heat for 20min, then cooling to 450 ℃, and continuously preserving heat for 3h;
(3) Casting the mixed material obtained in the step (2) after heat preservation into a mould, cooling to the temperature lower than 40 ℃, and discharging to obtain a zinc-magnesium alloy material;
(4) Preheating the zinc-magnesium alloy material to 310 ℃, then putting the zinc-magnesium alloy material into a rolling machine for rolling, wherein the rolling thickness is 0.2mm each time, rolling for 10 times back and forth, and processing the obtained blank target according to the shape and size requirements to obtain the zinc-magnesium target material.
Example 2
One embodiment of the zinc-magnesium target material and the preparation method thereof comprises the following steps:
(1) Uniformly mixing zinc powder and magnesium powder according to a mass ratio of 99.9 to 0.1, placing the mixture into a vacuum induction furnace, and vacuumizing the vacuum induction furnace until the pressure in the furnace is lower than 3 multiplied by 10 -3 Pa, then injecting argon until the pressure in the furnace is changed to normal pressure, and vacuumizing until the pressure in the furnace is lower than 3X 10 -2 Pa, finally introducing argon until the pressure in the furnace is 10Pa;
(2) Starting a vacuum induction furnace at the speed of 25 ℃/min for magnetic induction heating to 530 ℃, preserving heat for 25min, then cooling to 430 ℃, and continuing preserving heat for 4h;
(3) Casting the mixed material obtained in the step (2) after heat preservation into a mould, cooling to the temperature lower than 40 ℃, and discharging to obtain a zinc-magnesium alloy material;
(4) Preheating the zinc-magnesium alloy material to 300 ℃, then putting the zinc-magnesium alloy material into a rolling machine for rolling, wherein the rolling thickness is 0.3mm each time, rolling for 8 times back and forth, and processing the obtained blank target according to the shape and size requirements to obtain the zinc-magnesium target.
Example 3
One embodiment of the zinc-magnesium target material and the preparation method thereof comprises the following steps:
(1) Uniformly mixing zinc powder and magnesium powder according to a mass ratio of 94 -3 Pa, then injecting argon until the pressure in the furnace is changed to normal pressure, and vacuumizing until the pressure in the furnace is lower than 3X 10 -2 Pa, finally introducing argon until the pressure in the furnace is 10Pa;
(2) Starting a vacuum induction furnace at the speed of 25 ℃/min for magnetic induction heating to 520 ℃, keeping the temperature for 25min, then cooling to 440 ℃, and keeping the temperature for 4h;
(3) Casting the mixed material obtained in the step (2) after heat preservation into a mould, cooling to the temperature lower than 40 ℃, and discharging to obtain a zinc-magnesium alloy material;
(4) Preheating the zinc-magnesium alloy material to 320 ℃, then putting the zinc-magnesium alloy material into a rolling machine for rolling, wherein the rolling thickness is 0.2mm each time, rolling for 9 times back and forth, and processing the obtained blank target according to the shape and size requirements to obtain the zinc-magnesium target material.
Comparative example 1
A preparation method of a zinc-magnesium target material comprises the following steps:
(1) Uniformly mixing zinc powder and magnesium powder according to a mass ratio of 90 -3 Pa, then injecting argon until the pressure in the furnace is changed to normal pressure, and vacuumizing until the pressure in the furnace is lower than 3X 10 -2 Pa, finally introducing argon until the pressure in the furnace is 10Pa;
(2) Starting a vacuum induction furnace at the speed of 30 ℃/min, carrying out magnetic induction heating to 450 ℃, and continuously preserving heat for 3h;
(3) Casting the mixed material obtained after heat preservation in the step (2) into a mould, cooling to the temperature lower than 40 ℃, and discharging to obtain a zinc-magnesium alloy material;
(4) Preheating the zinc-magnesium alloy material to 310 ℃, then putting the zinc-magnesium alloy material into a rolling machine for rolling, wherein the rolling thickness is 0.2mm each time, rolling for 10 times back and forth, and processing the obtained blank target according to the shape and size requirements to obtain the zinc-magnesium target material.
Comparative example 2
A preparation method of a zinc-magnesium target material comprises the following steps:
(1) Uniformly mixing zinc powder and magnesium powder according to a mass ratio of 90 -3 Pa, then injecting argon until the pressure in the furnace is changed to normal pressure, and vacuumizing until the pressure in the furnace is lower than 3X 10 -2 Pa, finally introducing argon until the pressure in the furnace is 10Pa;
(2) Starting a vacuum induction furnace at the speed of 30 ℃/min, carrying out magnetic induction heating to 560 ℃, and carrying out heat preservation for 20min;
(3) Casting the mixed material obtained in the step (2) after heat preservation into a mould, cooling to the temperature lower than 40 ℃, and discharging to obtain a zinc-magnesium alloy material;
(4) Preheating a zinc-magnesium alloy material to 310 ℃, putting the zinc-magnesium alloy material into a rolling machine for rolling, wherein the rolling thickness is 0.2mm each time, rolling for 10 times back and forth, and processing the obtained blank target according to the shape and size requirements to obtain the zinc-magnesium target material.
Comparative example 3
A preparation method of a zinc-magnesium target material comprises the following steps:
(1) Uniformly mixing zinc powder and magnesium powder according to a mass ratio of 90 -3 Pa, then injecting argon until the pressure in the furnace is changed to normal pressure, and vacuumizing until the pressure in the furnace is lower than 3X 10 -2 Pa, finally introducing argon until the pressure in the furnace is 10Pa;
(2) Starting a vacuum induction furnace at the speed of 30 ℃/min for magnetic induction heating to 560 ℃, preserving heat for 20min, then cooling to 450 ℃, and continuing preserving heat for 3h;
(3) Casting the mixed material obtained after heat preservation in the step (2) into a mould, cooling to the temperature lower than 40 ℃, and discharging to obtain a zinc-magnesium alloy material;
(4) And directly putting the zinc-magnesium alloy material into a rolling machine for rolling, wherein the rolling thickness is 0.2mm each time, rolling for 10 times back and forth, and processing the obtained blank target according to the shape and size requirements to obtain the zinc-magnesium target material.
Comparative example 4
A preparation method of a zinc-magnesium target material comprises the following steps:
(1) Uniformly mixing zinc powder and magnesium powder according to a mass ratio of 90 -3 Pa, then injecting argon until the pressure in the furnace is changed to normal pressure, and vacuumizing until the pressure in the furnace is lower than 3X 10 -2 Pa, finally introducing argon until the pressure in the furnace is 10Pa;
(2) Starting a vacuum induction furnace at the speed of 30 ℃/min for magnetic induction heating to 560 ℃ and preserving heat for 3h +20min;
(3) Casting the mixed material obtained after heat preservation in the step (2) into a mould, cooling to the temperature lower than 40 ℃, and discharging to obtain a zinc-magnesium alloy material;
(4) Preheating a zinc-magnesium alloy material to 310 ℃, putting the zinc-magnesium alloy material into a rolling machine for rolling, wherein the rolling thickness is 0.2mm each time, rolling for 10 times back and forth, and processing the obtained blank target according to the shape and size requirements to obtain the zinc-magnesium target material.
Comparative example 5
(1) Uniformly mixing zinc powder and magnesium powder according to a mass ratio of 90 -3 Pa, then injecting argon until the pressure in the furnace is changed to normal pressure, and vacuumizing until the pressure in the furnace is lower than 3X 10 -2 Pa, finally introducing argon until the pressure in the furnace is 10Pa;
(2) Starting a vacuum induction furnace at the speed of 30 ℃/min for magnetic induction heating to 450 ℃, and preserving heat for 3h +20min;
(3) Casting the mixed material obtained in the step (2) after heat preservation into a mould, cooling to the temperature lower than 40 ℃, and discharging to obtain a zinc-magnesium alloy material;
(4) Preheating the zinc-magnesium alloy material to 310 ℃, then putting the zinc-magnesium alloy material into a rolling machine for rolling, wherein the rolling thickness is 0.2mm each time, rolling for 10 times back and forth, and processing the obtained blank target according to the shape and size requirements to obtain the zinc-magnesium target material.
Comparative example 6
(1) Uniformly mixing zinc powder and magnesium powder according to a mass ratio of 90 -3 Pa, then injecting argon until the pressure in the furnace is changed to normal pressure, and vacuumizing until the pressure in the furnace is lower than 3X 10 -2 Pa, finally introducing argon until the pressure in the furnace is 10Pa;
(2) Starting a vacuum induction furnace at the speed of 30 ℃/min for magnetic induction heating to 560 ℃, preserving heat for 20min, then cooling to 480 ℃, and continuing preserving heat for 2h;
(3) Casting the mixed material obtained in the step (2) after heat preservation into a mould, cooling to the temperature lower than 40 ℃, and discharging to obtain a zinc-magnesium alloy material;
(4) Preheating a zinc-magnesium alloy material to 310 ℃, putting the zinc-magnesium alloy material into a rolling machine for rolling, wherein the rolling thickness is 0.2mm each time, rolling for 10 times back and forth, and processing the obtained blank target according to the shape and size requirements to obtain the zinc-magnesium target material.
Effect example 1
In order to verify the performance superiority of the product prepared by the preparation method of the zinc-magnesium target material, the internal defect test, the component uniformity test and the relative density test of the products of each embodiment and comparative example are carried out, wherein the internal defect test is directly confirmed by adopting ultrasonic scanning C-Scan; the method mainly comprises the steps of taking points at the head, the middle and the tail of the prepared zinc-magnesium target material to test the magnesium content by an elemental analysis method, and taking an average value; the relative density is directly tested by adopting a traditional Archimedes method; if the target material is cracked or has no complete morphology, the test is not performed. The test results are shown in table 1.
TABLE 1
As can be seen from Table 1, the zinc-magnesium target material prepared by the preparation method of the zinc-magnesium target material has high relative density, no obvious defect inside, high component uniformity and expected doping amount of magnesium in each part. In contrast, the process of comparative example 1 lacks the high-temperature zinc-magnesium fusion step, and the magnesium element is not uniformly distributed although the prepared product has higher relative density; compared with the product in the comparative example 2, because the temperature is not reduced and the two-stage heat preservation treatment process is carried out, the product has material loss and component segregation, the inner part has small hole defects, and the relative density of the target material is lower and is only 99 percent; the product of comparative example 3 is not subjected to preheating treatment during rolling, and has poor processability, so that cracking phenomenon occurs after rolling, and the use requirement cannot be met; the products of comparative example 4 and comparative example 5 are not subjected to two-stage heat preservation treatment, and although the products are subjected to heat preservation for the same time, the component uniformity of the products cannot reach the expected degree easily, and meanwhile, the relative density of the products of comparative example 5 is insufficient; the product of comparative example 6 undergoes a second heat preservation treatment in the preparation process, but the time is short, the equivalent density of the product is high, but the uniformity of the components is insufficient; in addition, the inventor finds that if the high-temperature section heat preservation is carried out for a long time in the two-section heat preservation process, zinc and magnesium in the raw materials volatilize to different degrees, the proportion of zinc and magnesium in the final product deviates from the expectation, and therefore the two-section heat preservation treatment needs to be carried out for a specific time.
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 to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (6)
1. The preparation method of the zinc-magnesium target is characterized by comprising the following steps:
(1) Uniformly mixing a zinc source and a magnesium source, putting the mixture into a vacuum induction furnace for vacuumizing treatment, and introducing protective atmosphere until the pressure in the furnace is 2-10 Pa;
(2) Starting a vacuum induction furnace at the speed of 20-30 ℃/min for magnetic induction heating to 520-560 ℃, preserving heat for 20-35 min, then cooling to 430-450 ℃, and continuously preserving heat for 3-5 h;
(3) Casting the mixed material obtained after heat preservation in the step (2) into a mould, and cooling to obtain a zinc-magnesium alloy material;
(4) Preheating the zinc-magnesium alloy material to 300-320 ℃, rolling, and processing the shape and the size of the obtained blank target to obtain the zinc-magnesium target material.
2. The method for preparing the zinc-magnesium target material according to claim 1, wherein the mass ratio of the zinc source to the magnesium source in the step (1) is (90-99.9): (0.1-10).
3. The method for preparing the zinc-magnesium target material according to claim 1, wherein the step of performing vacuum pumping in the step (1) comprises the following steps: vacuumizing the vacuum induction furnace until the pressure in the furnace is lower than 3 x 10 -3 Pa, then injecting protective atmosphere until the pressure in the furnace is changed to normal pressure, and vacuumizing until the pressure in the furnace is lower than 3X 10 -2 Pa; preferably, the protective atmosphere is argon.
4. The method for preparing the zinc-magnesium target material according to claim 1, wherein the rolling in the step (4) is performed for 8 to 10 times, and the thickness of each rolling is 0.1 to 0.3mm.
5. The zinc-magnesium target material prepared by the preparation method of the zinc-magnesium target material according to any one of claims 1 to 4.
6. The use of the zinc-magnesium target material of claim 5 in the preparation of a ZnMgO thin film for a solar cell.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211125573.8A CN115595539A (en) | 2022-09-15 | 2022-09-15 | Zinc-magnesium target material and preparation method thereof |
Applications Claiming Priority (1)
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