CN115948718A - 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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- CN115948718A CN115948718A CN202211631294.9A CN202211631294A CN115948718A CN 115948718 A CN115948718 A CN 115948718A CN 202211631294 A CN202211631294 A CN 202211631294A CN 115948718 A CN115948718 A CN 115948718A
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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 carrying out homogenization heat treatment on the magnesium plate, 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-treating for 1-3 h at 200-300 ℃, and cooling to obtain the high-purity magnesium sputtering target material. The magnesium plate after the homogenization heat treatment is directly put into a cold rolling mill for cold rolling without being cooled to room temperature, the rolling process parameters are controlled, and the rolled target blank is cooled after heat preservation treatment at a proper temperature to prepare the magnesium target.
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 a process that electrons collide with argon under the action of a magnetic field, ionized argon ions continuously bombard a sputtering target material, and target material atoms are deposited on the surface of a coating substrate, so that the coating is realized. The quality of the target determines the quality of the coating, 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, the research on the magnesium target for the semiconductor magnetron sputtering is very little, and on one hand, because the heating temperature rise and the heat dissipation temperature reduction of magnesium are faster than those of other metals, the temperature is reduced too fast and unevenly in the plastic processing process, and edge cracks and cracks are easy to occur; on the other hand, magnesium has a narrow hot working temperature range compared with other metal materials. Therefore, this causes a certain difficulty in the working and forming of the magnesium target material.
For example, CN113846302A in the prior art discloses a magnesium target material and a preparation method and use thereof, the preparation method comprises performing first vacuum heat treatment on a magnesium ingot, then performing first forging in an argon atmosphere, performing second vacuum heat treatment on a cooled magnesium blank, then performing second forging, performing cold rolling on the obtained magnesium blank at room temperature for 20-30 times, finally performing 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, the magnesium blank is rolled for multiple times at room temperature, so that edge cracks and cracks are easily generated on the magnesium blank, and the yield of the material is reduced.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a high-purity magnesium sputtering target material and a preparation method thereof, 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 less than or equal to 30 mu m and high 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, which comprises the following steps:
after carrying out homogenization heat treatment on the magnesium plate, 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-treating for 1-3 h at 200-300 ℃, and cooling to obtain the high-purity magnesium sputtering target material.
The invention provides a preparation method of a high-purity magnesium sputtering target material different from the prior art, which is characterized in that a magnesium plate is subjected to heat treatment and cold rolling to be rolled at the temperature below the magnesium recrystallization temperature and above the room temperature, and then is subjected to recrystallization heat treatment, so that the internal structure of the magnesium plate is free of defects, 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 high.
According to the invention, the magnesium plate after the homogenization heat treatment is directly subjected to cold rolling, so that the temperature of the magnesium plate in the rolling process is between room temperature and the recrystallization temperature of the magnesium plate, crystal grains are refined, and abnormal growth of the crystal grains is avoided, and the target material structure is not uniform; meanwhile, the plasticity of the target material is improved, and the loss of the target material is reduced.
The performance of the target material is further optimized by controlling the heat treatment temperature of the rolled magnesium blank, and if the heat treatment temperature is too high, grains grow abnormally; if the temperature is too low, complete recrystallization cannot be accomplished. Preferably, the heat treatment temperature of the rolled magnesium billet is 200 to 300 ℃, for example 200 ℃, 220 ℃, 260 ℃,280 ℃ and the like, and the heat treatment time is 1 to 3 hours, for example 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours and the like, but the heat treatment time is not limited to the above numerical values, and other numerical values not listed in the numerical value range are also applicable.
Preferably, the rolling process comprises the steps of:
controlling rolling parameters until the rolling deformation reaches 15% -20%, and carrying out primary rolling heat treatment on the magnesium plate;
controlling rolling parameters, rolling the magnesium plate until the total deformation reaches 30% -35%, and carrying out secondary rolling heat treatment on the magnesium plate;
controlling rolling parameters, and rolling the magnesium plate until the total deformation reaches 50% -60%.
Preferably, the rolling deformation of two adjacent rolling processes does not exceed 20 percent.
In the rolling process, the deformation between two rolling heat treatments needs to be controlled, and if the deformation is too large, cracks appear in the rolling process of the magnesium target; if the deformation amount is too small, the effect of grain refinement is not significant. Preferably, the deformation between two rolling heat treatments is not more than 20%. For example, the content may be 15%,16%,17%,18%,19%,20%, etc., but the content is not limited to the specific values, and other values not specified in the range of the specific values are also 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.
The rolling heat treatment temperature of the magnesium plate needs to be controlled in the rolling process, if the temperature is too high, grains grow abnormally, and the effect of grain refinement cannot be achieved; if the temperature is too low, edge cracks and cracks can occur 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 ℃ or the like; the heat treatment time is 10 to 30min, and may be, for example, 10min, 15min, 20min, 25min, 30min, etc., but the heat treatment time is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the rolling parameters comprise rolling speed and rolling reduction per pass, in the rolling process, the rolling speed is controlled to be 10-30 m/min, and the rolling reduction per pass is 1-5 mm.
By controlling the rolling process and process parameters, the magnesium plate prepared by the rolling process has no internal defects, small crystal grain size, excellent performance and high yield.
Preferably, in the rolling process and the heat treatment process after rolling, the magnesium plate is wrapped by tinfoil and then subjected to heat treatment.
The invention adopts the mode that tinfoil wraps the magnesium plate in the rolling process and the heat treatment process after rolling, 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 for homogenizing heat treatment of the magnesium plate is 300-500 ℃ and the heat treatment time is 1-3 h.
The crystal grains of the magnesium plate are refined after hot extrusion, the crystal grains grow abnormally due to overhigh temperature, and the defects and the stress cannot be eliminated due to overlow temperature, so that the subsequent deformation processing is difficult, therefore, the homogenization heat treatment is carried out on the magnesium plate at 300-500 ℃ to eliminate the extrusion defects and the stress, and the subsequent processing deformation is facilitated.
Preferably, the purity of the magnesium plate is not less than 4N.
The purity of the raw material magnesium plate used in the present invention is not less than 4N, and may be, for example, 4N3, 4N5, 4N8, 5N, etc., but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
Preferably, the magnesium board is a magnesium board subjected to a hot extrusion process.
The structure of the as-cast magnesium ingot is a coarse dendritic crystal structure, the grain size is hundreds of microns or even millimeters, the grain size is very uneven, the grain can not be effectively refined by only rolling, and large deformation means such as forging or extrusion are needed.
Preferably, the rolled and heat-treated target material is cooled, and the preferred cooling mode is furnace cooling.
In a second aspect, the invention provides a pure magnesium sputtering target material prepared by the preparation 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:
the magnesium plate after hot extrusion is taken as a raw material, and is directly put into a cold rolling mill for cold rolling without being cooled to room temperature after being subjected to homogenization heat treatment, so that the temperature of the magnesium plate in the rolling process is between room temperature and the recrystallization temperature of the magnesium plate, crystal grains are refined, abnormal growth of the crystal grains is avoided, the target material tissue is not uniform, the plasticity of the target material is improved, and the loss of the target material is reduced; the invention further effectively avoids edge cracks and cracks in the rolling process of the magnesium material by controlling the rolling deformation and the rolling temperature, and further refines the grain size. The high-purity magnesium plate target material prepared by the method has the advantages of no defect in internal structure, uniform structure, fine crystal grains and grain size of 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 disclosed by the invention has low requirements on equipment, is simple in preparation process flow, and has important significance in realizing industrial production of the magnesium target material.
Drawings
FIG. 1 is a metallographic structure diagram of a longitudinal section of a magnesium plate raw material;
FIG. 2 is a metallographic structure diagram of a longitudinal section of a magnesium target in example 1;
FIG. 3 is a graph of the results of ultrasonic C-scan of a magnesium target blank;
FIG. 4 is a metallographic structure diagram of a longitudinal section of a magnesium target in example 2;
FIG. 5 is a metallographic structure diagram of a longitudinal section of a magnesium target in example 3;
FIG. 6 is a metallographic structure diagram of a longitudinal section of a magnesium target in comparative example 1;
FIG. 7 is a metallographic structure diagram of a longitudinal section of the magnesium target in comparative example 2.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the following examples. It should be understood by those skilled in the art that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The test methods used in the examples are all conventional methods unless otherwise specified; the materials, reagents and the like used are commercially available unless otherwise specified.
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 after hot extrusion with the purity of 4N6 is selected as a raw material, the metallographic structure of the longitudinal section of the magnesium plate is shown in figure 1, and compared with the as-cast coarse dendritic crystal structure (the grain size is more than 500 mu m) of pure magnesium, the grain of the magnesium plate after hot extrusion selected by the invention is refined to be less than 300 mu m.
Step 2: and (3) tightly wrapping the magnesium board obtained in the step (1) with tinfoil, and then keeping the temperature at 350 ℃ for 2h.
And 3, 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 speed is 30m/min, and the reduction per pass is 1mm. And when the rolling deformation reaches 16%, keeping the temperature of the magnesium plate at 300 ℃ for 10min, and then continuing rolling, and when the rolling deformation reaches 31%, keeping the temperature of the magnesium plate at 300 ℃ for 10min, and then continuing rolling until the total deformation reaches 55%.
And 4, step 4: and (4) carrying out heat treatment on the target blank. And (4) preserving the heat of the target blank obtained in the step (3) at 220 ℃ for 1h, and then cooling the target blank along with the furnace.
And 5: and (4) machining the target finished product. And (4) machining the target blank obtained in the step (4) to the size of a finished product 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 distribution of the crystal grains is relatively uniform, the average crystal grain size is 30 micrometers, and the ultrasonic C scanning result diagram of the magnesium target blank is shown in fig. 3, so that the magnesium target prepared by the method has no defects such as edge cracks, cracks and the like. The yield of the magnesium target prepared by the method of the invention is up to 93 percent, and the yield is high.
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) with tinfoil, and then keeping the temperature at 350 ℃ for 2h.
And step 3: and (3) immediately rolling the magnesium plate subjected to heat treatment in the step (2) on a cold rolling mill. The rolling speed is 20m/min, and the reduction per pass is 1.5mm. And when the rolling deformation reaches 15%, keeping the temperature of the magnesium plate at 300 ℃ for 20min, and then continuing rolling, and when the rolling deformation reaches 33%, keeping the temperature of the magnesium plate at 300 ℃ for 20min, and then continuing rolling until the total deformation reaches 50%.
And 4, step 4: and (4) carrying out heat treatment on the target blank. And (4) preserving the temperature of the target blank obtained in the step (3) at 260 ℃ for 1h, and then cooling the target blank along with the furnace.
And 5: and (4) machining the target finished product. And (4) machining the target blank obtained in the step (4) to the size of a finished product according to the drawing requirements.
The metallographic structure of the longitudinal section of the magnesium target prepared in this example is shown in fig. 4, and the grains are significantly refined, the grain distribution is relatively uniform, and the average grain size is 28 μm.
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) with tinfoil, and then keeping the temperature at 350 ℃ for 2h.
And 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 speed is 10m/min, and the reduction per pass is 2mm. And when the rolling deformation reaches 15%, keeping the temperature of the magnesium plate at 300 ℃ for 30min, and then continuing rolling, and when the rolling deformation reaches 34%, keeping the temperature of the magnesium plate at 300 ℃ for 30min, and then continuing rolling until the total deformation reaches 52%.
And 4, step 4: and (4) carrying out heat treatment on the target blank. And (4) preserving the temperature of the target blank obtained in the step (3) at 260 ℃ for 1h, and then cooling the target blank along with the furnace.
And 5: and (4) machining the target finished product. And (4) machining the target blank obtained in the step (4) to the size of a finished product according to the drawing requirements.
The metallographic structure of the longitudinal section of the magnesium target produced in this example is shown in fig. 5, and the average grain size is reduced to 22 μm, and the grains are uniformly distributed.
Comparative example 1
This comparative example provides a method of manufacturing a high purity magnesium sputtering target, which is the same as that of example 3 except that the temperature of the heat treatment in step (4) was changed from 260 ℃ to 180 ℃.
The metallographic structure of the longitudinal section of the magnesium target produced by the comparative example is shown in fig. 6, and although the crystal grains were refined, some of the crystal grains were still large, and the crystal grains were unevenly distributed.
Comparative example 2
The present comparative example provides a method for preparing a high purity magnesium sputtering target, which is the same as in example 3 except that the temperature of the heat treatment in step (4) was changed from 260 ℃ to 350 ℃.
The metallographic structure of the longitudinal section of the magnesium target produced by this comparative example is shown in fig. 7, in which some grains grow abnormally, the grain size increases extremely poorly, and the average grain size increases.
Comparative example 3
The comparative example provides a preparation method of a magnesium target, comprising the following steps:
(1) Preserving the heat of a magnesium ingot with the purity of 4N for 6 hours at 300 ℃ under a vacuum condition, then sequentially upsetting and drawing out under an argon atmosphere, repeating for 2 times, and cooling to room temperature by adopting water cooling to obtain a first magnesium blank;
(2) Preserving the heat of the first magnesium blank obtained in the step (1) for 3 hours at 250 ℃ under a vacuum condition, then sequentially carrying out upsetting and drawing out under an argon atmosphere, repeating the upsetting and drawing out for 2 times, and then cooling to room temperature by adopting water cooling to obtain a second magnesium blank;
(3) Rolling the second magnesium blank obtained in the step (2) at room temperature for 20 times to obtain a third magnesium blank;
(4) And (4) preserving the heat of the third magnesium blank obtained in the step (3) for 2 hours at the temperature of 100 ℃ under the vacuum condition, cooling to room temperature by adopting water cooling, and machining to obtain the magnesium target.
Comparative example 4
The comparative example provides a preparation method of a high-purity magnesium sputtering target, which is the same as that in example 3 except that a magnesium plate raw material with the purity of 4N5 after hot extrusion is replaced by a magnesium ingot with the purity of 4N 5.
Comparative example 5
The comparative example provides a preparation method of a high-purity magnesium sputtering target, which is the same as that in the example 3 except that the heat preservation temperature of the magnesium plate in the step 3 is adjusted from 300 ℃ to 410 ℃.
Comparative example 6
The comparative example provides a preparation method of a high-purity magnesium sputtering target, which is the same as that in the example 3 except that the heat preservation temperature of the magnesium plate in the 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 were 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 were adjusted from 15%, 34%, and 52% to 15%, 28%, and 52%, respectively.
The average grain size and the yield of the magnesium targets obtained in examples 1 to 3 and comparative examples 1 to 8 were measured and counted, wherein the yield is the ratio of the magnesium target having a uniform structure, a grain size of less than 30 μm, and no internal defects in the assembly, and the results are shown in the following table.
To sum up, in the embodiments 1 to 3, by using the preparation method of the present invention, the magnesium target material with a uniform internal structure is obtained by performing recrystallization heat treatment after rolling at a temperature lower than the recrystallization temperature and higher than the room temperature, and the grain size of the magnesium target material is less than or equal to 30 μm. Comparative example 1 the temperature of the heat treatment of the target blank was reduced and the grains did not complete recrystallization, resulting in an increase in 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 poor uniformity of the grains. The target blank described in comparative example 3 was subjected to 2 forging, 1 rolling and 3 vacuum heat treatments with gradually decreasing temperature to refine the grains to 22-30 μm. The preparation method has a complex flow, and the possibility of introducing defects is increased through multiple times of forging, so that the yield is low. The raw material selected in comparative example 4 is a magnesium ingot which is not subjected to hot extrusion, and the grain size obtained by the process of the invention is still larger. Comparative example 5 increased the rolling heat treatment temperature and the grains started to grow again during the refinement process, resulting in insignificant grain refinement, an average grain size of 56 μm and uneven grain distribution. The comparative example 6 reduces the rolling heat treatment temperature, the temperature of the plate is reduced too fast in the rolling process, and obvious cracks appear on the edge of the magnesium plate. The comparative example 7 increases the total deformation between the first rolling and the second rolling, and the comparative example 8 increases the total deformation between the second rolling and the third rolling, so that the deformation is too large in the rolling process, and cracks also appear on the edge of the magnesium plate.
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. The preparation method of the high-purity magnesium sputtering target is characterized by comprising the following steps of:
after carrying out homogenization heat treatment on the magnesium plate, 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-treating for 1-3 h at 200-300 ℃, and cooling to obtain the high-purity magnesium sputtering target material.
2. The method for preparing the high-purity magnesium sputtering target material according to claim 1, wherein the rolling process comprises the following steps:
controlling rolling parameters until the rolling deformation reaches 15% -20%, and carrying out primary rolling heat treatment on the magnesium plate;
controlling rolling parameters, rolling the magnesium plate until the total deformation reaches 30% -35%, and carrying out secondary rolling heat treatment on the magnesium plate;
controlling rolling parameters, and rolling the magnesium plate until the total deformation reaches 50% -60%.
3. The method for preparing the high-purity magnesium sputtering target according to claim 2, wherein the rolling deformation amount of two adjacent rolling processes is not more than 20%.
4. The method for preparing the high-purity magnesium sputtering target material according to claim 2, wherein the temperature of the first rolling heat treatment is 200 to 400 ℃, and the heat treatment time is 10 to 30min; the temperature of the second rolling heat treatment is 200-400 ℃, and the heat treatment time is 10-30 min.
5. The method for preparing the high-purity magnesium sputtering target material according to claim 2, wherein the rolling parameters comprise 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.
6. The method for preparing the high-purity magnesium sputtering target material according to any one of claims 1 to 5, wherein in the rolling process and the post-rolling heat treatment process, the magnesium plate is subjected to heat treatment after being wrapped with tinfoil.
7. The method for preparing the high-purity magnesium sputtering target material according to claim 1, wherein the temperature for homogenizing the magnesium plate is 300-500 ℃ and the heat treatment time is 1-3 h.
8. The method for preparing a high-purity magnesium sputtering target according to claim 1, wherein the purity of the magnesium plate is not less than 4N; the magnesium board is subjected to hot extrusion treatment.
9. A high-purity magnesium sputtering target material, which is prepared by the preparation method of any one of claims 1 to 5, 7 and 8.
10. The high purity magnesium sputtering target according to claim 9, 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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