CN115948718B - High-purity magnesium sputtering target material and preparation method thereof - Google Patents
High-purity magnesium sputtering target material and preparation method thereof Download PDFInfo
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 146
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 146
- 239000011777 magnesium Substances 0.000 title claims abstract description 146
- 238000005477 sputtering target Methods 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000013077 target material Substances 0.000 title abstract description 19
- 238000005096 rolling process Methods 0.000 claims abstract description 95
- 238000010438 heat treatment Methods 0.000 claims abstract description 67
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 238000005097 cold rolling Methods 0.000 claims abstract description 10
- 238000001192 hot extrusion Methods 0.000 claims description 9
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000011282 treatment Methods 0.000 claims description 2
- 230000007547 defect Effects 0.000 abstract description 9
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000007670 refining Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 29
- 239000013078 crystal Substances 0.000 description 12
- 239000002994 raw material Substances 0.000 description 9
- 238000010586 diagram Methods 0.000 description 7
- 238000003754 machining Methods 0.000 description 7
- 238000001953 recrystallisation Methods 0.000 description 7
- 230000002159 abnormal effect Effects 0.000 description 6
- 238000005242 forging Methods 0.000 description 5
- 238000000576 coating method Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 210000001787 dendrite Anatomy 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000265 homogenisation Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- -1 argon ions Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention belongs to the technical field of sputtering targets, and particularly relates to a high-purity magnesium sputtering target and a preparation method thereof. The preparation method of the high-purity magnesium sputtering target material comprises the following steps: after homogenizing heat treatment, rolling the magnesium plate on a cold rolling mill, and controlling the rolling process until the total rolling deformation of the magnesium plate reaches 50% -60%; then heat treatment is carried out for 1 to 3 hours at the temperature of 200 to 300 ℃ and the high-purity magnesium sputtering target is obtained after cooling. The method is beneficial to refining the grain size, improving the tissue uniformity and effectively avoiding the defects of edge cracks, cracks and the like of a magnesium target tissue.
Description
Technical Field
The invention belongs to the technical field of sputtering targets, and particularly relates to a high-purity magnesium sputtering target and a preparation method thereof.
Background
The sputtering coating is that electrons and argon collide under the action of a magnetic field, and ionized argon ions bombard the sputtering target material continuously, so that target material atoms are deposited on the surface of a coating substrate, and the coating process is realized. The quality of the target determines the quality of the coating film, wherein the sputtering target for the semiconductor chip has the highest requirements on the composition, the structure and the performance of the target.
At present, few researches are carried out on a magnesium target for the semiconductor magnetron sputtering, on one hand, as the heating temperature rise and the heat dissipation temperature reduction of magnesium are faster than those of other metals, the temperature in the plastic working process is too fast and uneven, and edge cracks and cracks are easy to occur; magnesium, on the other hand, has a narrower range of hot working temperatures than other metallic materials. Therefore, this presents a certain difficulty in the shaping of the magnesium target.
As disclosed in the prior art CN113846302a, a magnesium target material, a preparation method and use thereof are disclosed, the preparation method comprises the steps of performing a first vacuum heat treatment on a magnesium ingot, performing a first forging under argon atmosphere, performing a second vacuum heat treatment on a cooled magnesium blank, performing a second forging, performing cold rolling for 20-30 times at room temperature on the obtained magnesium blank, and finally performing a third vacuum heat treatment on the magnesium blank, and performing mechanical processing after cooling to obtain the magnesium target material. In the preparation method of the magnesium target, magnesium blanks are rolled for multiple times at room temperature, so that the magnesium blanks are easy to generate edge cracks and cracks, and the yield of materials is reduced.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide the high-purity magnesium sputtering target material and the preparation method thereof, and the high-purity magnesium sputtering target material prepared by the method has the advantages of no internal defects such as edge cracks, cracks and the like, uniform structure, average grain size of less than or equal to 30 mu m and higher yield.
Based on the above purpose, the technical scheme adopted by the invention is as follows:
in a first aspect, the invention provides a method for preparing a high-purity magnesium sputtering target, comprising the following steps:
After homogenizing heat treatment, rolling the magnesium plate on a cold rolling mill, and controlling the rolling process until the total rolling deformation of the magnesium plate reaches 50% -60%; then heat treatment is carried out for 1 to 3 hours at the temperature of 200 to 300 ℃ and the high-purity magnesium sputtering target is obtained after cooling.
The invention provides a preparation method of a high-purity magnesium sputtering target material, which is different from the prior art, by carrying out heat treatment and cold rolling on a magnesium plate, the magnesium plate is rolled at a temperature below magnesium recrystallization temperature and above room temperature, and then is subjected to recrystallization heat treatment, so that the internal structure of the magnesium plate is defect-free, the structure is uniform, the grain size is less than or equal to 30 mu m, the use requirement of the sputtering target material for a semiconductor chip can be met, and the yield is higher.
According to the invention, the magnesium plate subjected to homogenization heat treatment is directly subjected to cold rolling, so that the temperature of the magnesium plate in the rolling process is between the temperature and the recrystallization temperature of the magnesium plate, grains are refined, and abnormal growth of the grains is avoided, so that the target tissue is not uniform; meanwhile, the plasticity of the target material is improved, and the loss of the target material is reduced.
According to the invention, the performance of the target is further optimized by controlling the heat treatment temperature of the rolled magnesium blank, and if the heat treatment temperature is too high, abnormal growth of crystal grains can be caused; if the temperature is too low, complete recrystallization cannot be completed. The heat treatment temperature of the magnesium billet after rolling is preferably 200 to 300 ℃, for example, 200 ℃, 220 ℃, 260 ℃,280 ℃, etc., and the heat treatment time is 1 to 3 hours, for example, 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours, etc., but the heat treatment temperature is not limited to the above-mentioned values, and other values not shown in the above-mentioned value range are equally applicable.
Preferably, the rolling process comprises the steps of:
Controlling rolling parameters until the rolling deformation reaches 15% -20%, and performing first rolling heat treatment on the magnesium plate;
Controlling rolling parameters, rolling the magnesium plate until the total deformation of the magnesium plate reaches 30% -35%, and performing second rolling heat treatment on the magnesium plate;
And controlling rolling parameters, and rolling the magnesium plate until the total deformation reaches 50% -60%.
Preferably, during the rolling process, the rolling deformation of two adjacent times is not more than 20%.
In the rolling process, the deformation between two rolling heat treatments is controlled, and if the deformation is too large, cracks can be generated in the magnesium target rolling process; if the deformation is too small, the grain refinement effect is not obvious. As a preferred solution, the deformation between the two rolling heat treatments cannot exceed 20%. For example, 15%,16%,17%,18%,19%,20% and the like may be used, but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned range are equally applicable.
Preferably, the temperature of the first rolling heat treatment is 200-400 ℃, and the heat treatment time is 10-30 min; the temperature of the second rolling heat treatment is 200-400 ℃, and the heat treatment time is 10-30 min.
In the rolling process, the rolling heat treatment temperature of the magnesium plate needs to be controlled, if the temperature is too high, abnormal growth of crystal grains can be caused, and the effect of grain refinement cannot be achieved; if the temperature is too low, edge cracks and fissures are generated in the magnesium plate rolling process.
As a preferable embodiment, the rolling heat treatment temperature is 200 to 400 ℃, for example, 200 ℃, 250 ℃, 300 ℃, 400 ℃ and the like; the heat treatment time is 10 to 30 minutes, and may be, for example, 10 minutes, 15 minutes, 20 minutes, 25 minutes, 30 minutes, etc., but is not limited to the values listed, and other values not listed in the range are applicable.
Preferably, the rolling parameters include a rolling rate and a reduction per pass, and in the rolling process, the rolling rate is controlled to be 10-30 m/min and the reduction per pass is controlled to be 1-5 mm.
The magnesium plate manufactured by the rolling process has no internal defects, small grain size, better performance and higher yield by controlling the rolling process and process parameters.
Preferably, in the rolling process and the heat treatment process after rolling, the heat treatment is performed after wrapping the magnesium plate with tin paper when the magnesium plate is heat treated.
The invention adopts a mode that tin paper is used for wrapping the magnesium plate in the heat treatment process after the rolling process and the heat treatment process after the rolling process, and aims to reduce the oxidation of the magnesium plate in the heat treatment process. Compared with the existing vacuum heating mode, the method is simpler and easier to operate.
Preferably, the temperature of homogenizing heat treatment of the magnesium board is 300-500 ℃ and the heat treatment time is 1-3 h.
The magnesium plate is refined after hot extrusion, the abnormal growth of the crystal grains can be caused by the excessively high temperature, and defects and stress can not be eliminated due to the excessively low temperature, so that difficulties are caused to subsequent deformation processing.
Preferably, the purity of the magnesium plate is not lower than 4N.
The raw material magnesium plate used in the present invention may have a purity of not less than 4N, for example, 4N3, 4N5, 4N8, 5N, etc., but is not limited to the listed values, and other non-listed values within the range are equally applicable.
Preferably, the magnesium plate is a magnesium plate subjected to a hot extrusion treatment.
The structure of the as-cast magnesium ingot is a coarse dendrite structure, the grain size is between hundreds of micrometers and even millimeters, the grain cannot be refined effectively only by rolling, and the large deformation means such as forging or extrusion is needed.
Preferably, the target material after rolling and heat treatment is cooled in a furnace-mounted cooling mode.
In a second aspect, the present invention provides a high purity magnesium sputter target produced by the above-described production method.
Preferably, the high-purity magnesium sputtering target material prepared by the invention has no defect inside, uniform structure and average grain size less than or equal to 30 mu m.
Compared with the prior art, the invention has the following beneficial effects:
According to the invention, the magnesium plate after hot extrusion is used as a raw material, and is directly cold-rolled in a cold rolling mill without being cooled to room temperature after homogenization heat treatment, so that the temperature of the magnesium plate in the rolling process is between the temperature and the recrystallization temperature of the magnesium plate, grains are refined, abnormal growth of the grains is avoided, the target tissue is not uniform, the plasticity of the target is improved, and the loss of the target is reduced; according to the invention, by controlling the rolling deformation and the rolling temperature, edge cracking and cracks in the magnesium material rolling process are further effectively avoided, and the grain size is further refined. The high-purity magnesium plate target material prepared by the method has the advantages of no defect of internal tissues, uniform tissues, fine grains and grain size less than or equal to 30 mu m, and can meet the use requirement of the sputtering target material for the semiconductor chip. The preparation method has low equipment requirement and simple preparation process flow, and has important significance for realizing the industrialized production of the magnesium target.
Drawings
FIG. 1 is a metallographic structure diagram of a longitudinal section of a magnesium plate raw material;
FIG. 2 is a metallographic view of a longitudinal section of a magnesium target in example 1;
FIG. 3 is a graph of ultrasonic C-scan results of a magnesium target blank;
FIG. 4 is a metallographic view of a longitudinal section of a magnesium target in example 2;
FIG. 5 is a metallographic view of a longitudinal section of a magnesium target in example 3;
FIG. 6 is a metallographic view of a longitudinal section of the magnesium target of comparative example 1;
FIG. 7 is a metallographic view of a longitudinal section of the magnesium target of comparative example 2.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples. It will be appreciated by persons skilled in the art that the specific embodiments described herein are for purposes of illustration only and are not intended to be limiting.
The test methods used in the examples are conventional methods unless otherwise specified; the materials, reagents and the like used, unless otherwise specified, are all commercially available.
Example 1
The embodiment provides a preparation method of a high-purity magnesium sputtering target, which comprises the following steps:
Step 1: the magnesium plate with the purity of 4N6 after hot extrusion is selected as a raw material, the metallographic structure of the longitudinal section is shown in figure 1, and compared with the as-cast coarse dendrite structure of pure magnesium (the grain size is more than 500 mu m), the magnesium plate with the purity of 4N6 after hot extrusion is selected, and the grain is thinned to be less than 300 mu m.
Step 2: and (3) tightly wrapping the magnesium board obtained in the step (1) by using tinfoil, and then preserving heat for 2 hours at the temperature of 350 ℃.
Step 3: and (3) immediately rolling the magnesium plate subjected to the heat treatment in the step (2) on a cold rolling mill. The rolling rate was 30m/min, and the reduction per pass was 1mm. When the rolling deformation reaches 16%, the magnesium plate is kept at 300 ℃ for 10min and then is rolled continuously, and when the rolling deformation reaches 31%, the magnesium plate is kept at 300 ℃ for 10min and then is rolled continuously until the total deformation reaches 55%.
Step 4: and (5) heat treatment of the target blank. And (3) preserving the heat of the target blank obtained in the step (3) at 220 ℃ for 1h, and then cooling the target blank with a furnace.
Step 5: and (5) machining a target finished product. And (5) machining the target blank obtained in the step (4) to a finished product size according to the drawing requirements.
The metallographic structure diagram of the longitudinal section of the magnesium target prepared by the embodiment is shown in fig. 2, the crystal grains are obviously refined, the crystal grains are relatively uniformly distributed, the average crystal grain size is 30 mu m, the ultrasonic C scanning result diagram of the magnesium target blank is shown in fig. 3, and the defects such as edge cracks, cracks and the like in the magnesium target prepared by the method of the invention can be overcome. The magnesium target prepared by the method has the yield up to 93 percent and higher yield.
Example 2
The embodiment provides a preparation method of a high-purity magnesium sputtering target, which comprises the following steps:
Step 1: selecting a magnesium plate raw material with the purity of 4N8 after hot extrusion.
Step 2: and (3) tightly wrapping the magnesium board obtained in the step (1) by using tinfoil, and then preserving heat for 2 hours at the temperature of 350 ℃.
Step 3: and (3) immediately rolling the magnesium plate subjected to the heat treatment in the step (2) on a cold rolling mill. The rolling rate was 20m/min, and the reduction per pass was 1.5mm. When the rolling deformation reaches 15%, the magnesium plate is kept at 300 ℃ for 20min and then is rolled continuously, and when the rolling deformation reaches 33%, the magnesium plate is kept at 300 ℃ for 20min and then is rolled continuously until the total deformation reaches 50%.
Step 4: and (5) heat treatment of the target blank. And (3) preserving the heat of the target blank obtained in the step (3) at 260 ℃ for 1h, and then cooling the target blank with a furnace.
Step 5: and (5) machining a target finished product. And (5) machining the target blank obtained in the step (4) to a finished product size according to the drawing requirements.
The metallographic structure diagram of the longitudinal section of the magnesium target prepared by the example is shown in fig. 4, the crystal grains are obviously refined, the distribution of the crystal grains is relatively uniform, and the average crystal grain size is 28 mu m.
Example 3
The embodiment provides a preparation method of a high-purity magnesium sputtering target, which comprises the following steps:
Step 1: selecting a magnesium plate raw material with the purity of 4N5 after hot extrusion.
Step 2: and (3) tightly wrapping the magnesium board obtained in the step (1) by using tinfoil, and then preserving heat for 2 hours at the temperature of 350 ℃.
Step 3: and (3) immediately rolling the magnesium plate subjected to the heat treatment in the step (2) on a cold rolling mill. The rolling rate was 10m/min, and the reduction per pass was 2mm. When the rolling deformation reaches 15%, the magnesium plate is kept at 300 ℃ for 30min and then is rolled continuously, and when the rolling deformation reaches 34%, the magnesium plate is kept at 300 ℃ for 30min and then is rolled continuously until the total deformation reaches 52%.
Step 4: and (5) heat treatment of the target blank. And (3) preserving the heat of the target blank obtained in the step (3) at 260 ℃ for 1h, and then cooling the target blank with a furnace.
Step 5: and (5) machining a target finished product. And (5) machining the target blank obtained in the step (4) to a finished product size according to the drawing requirements.
The metallographic structure diagram of the longitudinal section of the magnesium target prepared in this example is shown in FIG. 5, the average grain size is refined to 22 μm grains, and the grains are uniformly distributed.
Comparative example 1
This comparative example provides a method for preparing a high purity magnesium sputtering target, which is the same as that of example 3 except that the temperature 260 ℃ of the heat treatment of step (4) is replaced with 180 ℃.
The metallographic structure diagram of the longitudinal section of the magnesium target prepared in this comparative example is shown in fig. 6, and although the crystal grains are refined, part of the crystal grains are still larger, and the crystal grains are unevenly distributed.
Comparative example 2
This comparative example provides a method for preparing a high purity magnesium sputtering target, which is the same as that of example 3 except that the temperature of 260 ℃ of the heat treatment of step (4) is replaced with 350 ℃.
The metallographic structure diagram of the longitudinal section of the magnesium target prepared by this comparative example is shown in fig. 7, some grains are abnormally grown up, the grains are extremely enlarged, and the average grain size is increased.
Comparative example 3
The comparative example provides a preparation method of a magnesium target, comprising the following steps:
(1) Preserving heat of a magnesium ingot with the purity of 4N for 6 hours at 300 ℃ under vacuum, sequentially upsetting and drawing out under argon atmosphere, repeating for 2 times, and cooling to room temperature by adopting water cooling to obtain a first magnesium blank;
(2) The first magnesium blank obtained in the step (1) is subjected to heat preservation for 3 hours at the temperature of 250 ℃ under the vacuum condition, then upsetting and drawing are sequentially carried out under the argon atmosphere, the process is repeated for 2 times, and then water cooling is adopted to cool to the room temperature, so that a second magnesium blank is obtained;
(3) Rolling the second magnesium blank obtained in the step (2) for 20 times at room temperature to obtain a third magnesium blank;
(4) And (3) preserving heat of the third magnesium blank obtained in the step (3) for 2 hours at the temperature of 100 ℃ under vacuum, then cooling to room temperature by adopting water cooling, and obtaining the magnesium target after machining.
Comparative example 4
This comparative example provides a method for preparing a high purity magnesium sputtering target, which is the same as example 3 except that the raw material is replaced with a magnesium ingot having a purity of 4N5 from a magnesium plate raw material having a purity of 4N5 after hot extrusion.
Comparative example 5
This comparative example provides a method for preparing a high purity magnesium sputtering target, which is the same as that of example 3 except that the heat preservation temperature of the magnesium plate in step 3 is adjusted from 300 ℃ to 410 ℃.
Comparative example 6
This comparative example provides a method for preparing a high purity magnesium sputtering target, which is the same as that of example 3 except that the heat preservation temperature of the magnesium plate in step 3 is adjusted from 300 ℃ to 190 ℃.
Comparative example 7
This comparative example provides a method for producing a high-purity magnesium sputtering target, which is the same as in example 3 except that the rolling deformation amounts in step 3 are adjusted from 15%, 34% and 52% to 15%, 40% and 52%, respectively.
Comparative example 8
This comparative example provides a method for producing a high-purity magnesium sputtering target, which is the same as in example 3 except that the rolling deformation amounts in step 3 are adjusted from 15%, 34% and 52% to 15%, 28% and 52%, respectively.
The average grain sizes and the yields of the magnesium targets obtained in examples 1 to 3 and comparative examples 1 to 8, which are the proportions of the magnesium targets having a uniform structure, a grain size of less than 30 μm and no defects in the interior, were measured and counted, and the results are shown in the following table.
In summary, the preparation method of the invention is adopted in examples 1-3, and the magnesium target material with uniform internal structure is obtained by carrying out recrystallization heat treatment after rolling below the recrystallization temperature and above room temperature, and the grain size of the magnesium target material is less than or equal to 30 mu m, so that the process flow is simple, the heat treatment does not need a vacuum environment, and the requirement on equipment is low. Comparative example 1 reduced the temperature of the heat treatment of the target blank, the grains did not completely recrystallize, resulting in an increase in the average grain size; comparative example 2 increased the temperature of the heat treatment of the target blank, resulting in abnormal growth of some grains and deterioration of the uniformity of the grains. The target blank described in comparative example 3 was subjected to 2 times of forging, 1 time of rolling and 3 times of vacuum heat treatment with gradually decreasing temperature, and the grains were refined to 22 to 30. Mu.m. The preparation method is complex in flow, and the possibility of introducing defects is increased through repeated forging, so that the yield is low, but the preparation method only comprises rolling and heat treatment, the heat treatment does not need a vacuum environment, the requirement on equipment is low, industrialization is facilitated, and the yield is relatively high. The raw material selected in comparative example 4 is magnesium ingot which is not hot extruded, and the grain size prepared by the process of the invention is still larger. The comparative example 5 increased the rolling heat treatment temperature, and the grains began to grow again in the course of refinement, resulting in insignificant grain refinement, an average grain size of 56 μm, and uneven grain distribution. Comparative example 6 reduced the heat treatment temperature of rolling, and the temperature of the plate was lowered too rapidly during rolling, and obvious cracks were formed at the edges of the magnesium plate. Comparative example 7 increased the total deformation between the first rolling and the second rolling, and comparative example 8 increased the total deformation between the second rolling and the third rolling, resulting in excessive deformation during rolling and cracking of the magnesium plate edge.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (5)
1. The preparation method of the high-purity magnesium sputtering target is characterized by comprising the following steps of:
After homogenizing heat treatment, rolling the magnesium plate on a cold rolling mill, and controlling the rolling process until the total rolling deformation of the magnesium plate reaches 50% -60%; then heat treatment is carried out for 1 to 3 hours at the temperature of 200 to 300 ℃ and the high-purity magnesium sputtering target is obtained after cooling;
The rolling process comprises the following steps: controlling rolling parameters until the rolling deformation reaches 15% -20%, and performing first rolling heat treatment on the magnesium plate; controlling rolling parameters, rolling the magnesium plate until the total deformation of the magnesium plate reaches 30% -35%, and performing second rolling heat treatment on the magnesium plate; controlling rolling parameters, and rolling the magnesium plate until the total deformation reaches 50% -60%;
in the rolling process, the rolling deformation of two adjacent times is not more than 20%;
the temperature of the first rolling heat treatment is 200-400 ℃, and the heat treatment time is 10-30 min; the temperature of the second rolling heat treatment is 200-400 ℃, and the heat treatment time is 10-30 min;
the temperature of homogenizing heat treatment of the magnesium board is 300-500 ℃, and the heat treatment time is 1-3 hours;
The purity of the magnesium plate is not lower than 4N; the magnesium plate is subjected to hot extrusion treatment.
2. The method for preparing a high purity magnesium sputtering target according to claim 1, wherein the rolling parameters include a rolling rate and a rolling reduction per pass, and in the rolling process, the rolling rate is controlled to be 10-30 m/min, and the rolling reduction per pass is controlled to be 1-5 mm.
3. The method for producing a high purity magnesium sputtering target according to any one of claims 1 to 2, wherein the heat treatment is performed by wrapping a magnesium plate with tin foil and then performing the heat treatment in both the rolling process and the heat treatment process after rolling.
4. A high purity magnesium sputter target, characterized in that said target is produced by the production method according to any one of claims 1-2.
5. The high purity magnesium sputtering target according to claim 4, wherein the high purity magnesium sputtering target is defect-free inside, has a uniform structure, and has an average grain size of 30 μm or less.
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| CN114951333A (en) * | 2022-06-02 | 2022-08-30 | 太原理工大学 | Method for preparing high-performance rare earth magnesium alloy plate by upsetting and rolling |
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| CN1788926A (en) * | 2004-12-17 | 2006-06-21 | 长沙市美克科技开发有限公司 | Sheet rolling and heat treatment technology for magnesium alloy with thickness below millimeter |
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| CN110125201A (en) * | 2019-05-23 | 2019-08-16 | 广东省材料与加工研究所 | A kind of magnesium alloy anode thin plate and preparation method thereof |
| CN114951333A (en) * | 2022-06-02 | 2022-08-30 | 太原理工大学 | Method for preparing high-performance rare earth magnesium alloy plate by upsetting and rolling |
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