CN115679282A - Preparation method of titanium-silicon target material - Google Patents
Preparation method of titanium-silicon target material Download PDFInfo
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- CN115679282A CN115679282A CN202211359968.4A CN202211359968A CN115679282A CN 115679282 A CN115679282 A CN 115679282A CN 202211359968 A CN202211359968 A CN 202211359968A CN 115679282 A CN115679282 A CN 115679282A
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- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000013077 target material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 78
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 30
- 239000010439 graphite Substances 0.000 claims abstract description 30
- 238000005245 sintering Methods 0.000 claims abstract description 30
- 238000000498 ball milling Methods 0.000 claims abstract description 29
- 239000010936 titanium Substances 0.000 claims abstract description 22
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 15
- 238000007731 hot pressing Methods 0.000 claims abstract description 13
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 9
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- 238000007873 sieving Methods 0.000 claims abstract description 4
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- 238000011049 filling Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 8
- 238000011068 loading method Methods 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
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- 229910008482 TiSiN Inorganic materials 0.000 description 2
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Abstract
The invention discloses a preparation method of a titanium-silicon target material, relates to the field of semiconductor processing, and aims to solve the problem that the existing preparation method of the titanium-silicon target material is easy to have defects, and the technical scheme is as follows: a, selecting Ti powder and Si powder as raw materials, introducing TiH 2 Powder; b, mixing 60-90 parts by mass of Si powder, 10-35 parts by mass of Ti powder and 1-10 parts by mass of TiH 2 Adding the powder into a planetary ball-milling vacuum tank, and vacuumizing the tank body to be below 500 Pa; c, sieving the ball-milled powder by a 40-100-mesh sieve, and putting the powder into a titanium tank for vacuum sintering pretreatment; d, putting the mixture into a hot-pressing graphite mold; e, placing the graphite mold under a pressure head of a vacuum hot-pressing furnace, and sintering; and F, after sintering, reducing the temperature to room temperature along with the furnace, taking out the die for demolding, and carrying out various machining on the titanium-silicon blank target material to meet the requirements of the required product. One of the inventionThe preparation method of the titanium-silicon target can obtain a product with uniform microstructure, small grain size and easy cold processing.
Description
Technical Field
The invention relates to the field of semiconductor processing, in particular to a preparation method of a titanium-silicon target material.
Background
The Physical Vapor Deposition (PVD) technique is a technique of realizing the migration of a material by using physical processes such as thermal evaporation, glow discharge, arc discharge, etc. under a vacuum condition, and depositing and forming a coating on the surface of a specific part; including vacuum evaporation coating, sputter coating, and ion coating. Chemical Vapor Deposition (CVD) is also widely used as a type of coating process, but overall, PVD has a lower process temperature, a shorter production cycle, and no contamination compared to CVD. And the PVD coating surface has the advantages of better metallic luster, thin film layer, high hardness, stable chemical property, small friction coefficient and the like. It is becoming rapidly widespread in the fields of machinery, electronics, semiconductors, optics, aviation, traffic, etc.
With the development of hard coating materials, the development of TiCN and TiAlN from the original TiN and TiC becomes a main research direction on how to improve the wear resistance and the application temperature of the coating. And nitrogen is introduced during the TiSi target sputtering to form a TiSiN hard coating, so that a special nano composite structure of amorphous Si3N4 wrapped TiN is formed, and the hardness and the oxidation resistance of the coating are obviously improved. The service temperature can reach 1100 ℃, the mechanical wear resistance, the abrasion resistance of the wear-resistant material and the application temperature of the film layer are greatly improved compared with TiCN, tiAlN and the like, and a more excellent high-temperature wear-resistant oxidation-resistant film material is provided for industries such as automobiles, tools and dies and the like. High-speed dry cutting becomes the main development direction of future cutters, and the high-speed dry cutting attracts attention as a new generation of cutter coating material, and the demand of the target material for cutter coating is increasingly expanded.
One of the key technologies for preparing the TiSiN hard film layer by magnetron sputtering is to provide a high-quality titanium silicon target material. The titanium-silicon alloy belongs to intermetallic compounds, the titanium-silicon target material prepared by the existing smelting method has the defects of alloy brittleness, component segregation and the like, the silicon addition amount is generally not more than 15% of the weight, the cast ingot with the silicon addition amount of more than 15% is easy to crack, the component segregation and the brittle crack are easy to generate with the silicon addition amount of less than 15%, and meanwhile, the titanium-silicon target material is difficult to prepare by a fusion casting method due to poor alloy ductility. In terms of the preparation method, the hot isostatic pressing process is a method for obtaining a high-quality product better for the titanium silicon target material, and an alloy sputtering target material with excellent comprehensive performance is easy to obtain. However, when the hot isostatic pressing is used for directly pressing the powder, the deformation amount in the pressing process is large, so that high requirements are provided for the sheath material, and the preparation cost is greatly increased; if the blank is pressed, the working procedure is increased, and the production process is complicated. SPS sintering is a rapid sintering technology, products can be densified within a short time, the grain size is controllable, but the rapidly sintered products often have strong brittleness, the processing difficulty is increased, machining is needed after heat treatment, and due to the fact that the sintering time is too short, free Si phases exist in alloy target materials, and the magnetron sputtering is not facilitated.
Therefore, a new solution is needed to solve this problem.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for preparing a titanium-silicon target material, which adopts a vacuum hot pressing method to prepare the titanium-silicon target material and is easy to obtain the titanium-silicon target material with uniform microstructure, small grain size and easy cold processing.
The technical purpose of the invention is realized by the following technical scheme: a preparation method of a titanium-silicon target material comprises the following steps:
a, selecting Ti powder and Si powder as raw materials, and introducing TiH according to atomic ratio 2 A powder;
b, mixing 60-90 parts by mass of Si powder, 10-35 parts by mass of Ti powder and 1-10 parts by mass of TiH 2 Adding the powder into a planetary ball-milling vacuum tank, and vacuumizing the tank body to be below 500 Pa;
c, sieving the ball-milled powder by a 40-100-mesh sieve, and putting the powder into a titanium tank for vacuum sintering pretreatment;
d, calculating the required weight of the pre-sintered powder according to the size of the product, and then filling the pre-sintered powder into a hot-pressing graphite die;
e, placing the graphite mold under a pressure head of a vacuum hot-pressing furnace, prepressing the mold at 0.5-5 MPa, and setting sintering parameters for sintering;
f, after sintering, reducing the temperature to room temperature along with the furnace, taking out the die for demolding operation, and carrying out various machining on the titanium-silicon blank target material until the required product requirement is met
The invention is further configured to: the purity of the Si powder is more than or equal to 3N, D =5-20 μm; the purity of the Ti powder is more than or equal to 3N, D =25-60 μm; the TiH 2 The purity of the powder is more than or equal to 3N, D =1-10 μm.
The invention is further configured to: in the step B, ball milling parameters comprise ball-material ratio of 3: 1-10: 1, ball milling rotation speed of 150r/min-400r/min, ball milling time of 6-12h and loading capacity of 1/3-2/3 of the volume of the ball milling tank.
The invention is further configured to: the grinding balls are high-hardness zirconium balls, the grinding balls are prepared balls with the sizes of phi 3mm, phi 6mm and phi 10mm, the ratio of the grinding balls to the large, medium and small balls is 3-5: 2-4, and the selected tank body is a vacuum tank with polytetrafluoroethylene/polyurethane lining.
The invention is further configured to: in the step D, filling graphite paper at the bottom and around the inside of the mold during mold filling, adding the powder into the graphite cavity in several times, leveling the powder when adding one layer, and then placing the graphite paper, wherein the graphite mold and the graphite paper are uniformly sprayed with a high-temperature resistant mold release agent.
The invention is further configured to: in step E, the sintering parameters include: firstly, the furnace body is vacuumized to 10 DEG -2 Heating to 450-650 ℃ at a speed of 3-8 ℃/min and keeping the temperature for 1-4 h below Pa; then heating to 800-1000 ℃ at the speed of 3-8 ℃/min, and preserving the heat for 0.5-4 h; finally, heating to 1200-1400 ℃ at the speed of 2-5 ℃/min; boosting the pressure to 10-35 MPa, and keeping the temperature for 1-6 h; after the heat preservation is finished, the temperature is reduced to 800-1000 ℃ at the speed of 2-5 ℃/min.
The invention is further configured to: in step C, the presintering temperature is 550-750 ℃, the presintering time is 1-3h, and the presintering vacuum degree is 10 -2 pa。
In summary, the invention has at least the following beneficial effects:
(1) the introduction of the titanium source adopts two kinds of powder, namely titanium powder and titanium hydride powder, the titanium hydride powder generates hydrogen after pyrolysis and generates titanium powder in situ, and the generation of the hydrogen can reduce the titanium powder with oxidized surface and purify the powder.
(2) And the high-speed planetary ball mill is adopted, and ball milling parameters and medium selection are optimized to crush and disperse the powder, so that the powder with finer particle size and more uniform dispersion is obtained.
(3) Vacuum hot pressing is adopted for sintering, and the high-quality titanium-silicon sputtering target material with high density, uniform microstructure and controllable phase composition is successfully prepared through reasonable process parameter setting.
(4) Reasonable raw material selection and vacuum hot pressing are adopted to successfully prepare the titanium-silicon sputtering target material which has low oxygen content, uniform microstructure, fine crystal grains, high density and easy processing.
Drawings
FIG. 1 is a flow chart of a preparation method of the present invention;
FIG. 2 is a schematic view of the mold filling;
fig. 3 is a diagram of a product object of the present invention.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
The invention provides a preparation method of a titanium-silicon target material, which is shown in figure 1:
a, selecting Ti powder and Si powder as raw materials, and introducing a proper amount of TiH according to atomic ratio 2 And (3) powder. The selective advantage of the system is that TiH 2 The powder will generate H after pyrolysis 2 The Ti powder particles oxidized on the surface can be reduced and the function of purifying the powder can be achieved. The sintered product has the advantages of high density, uniform microstructure, fine crystal grains, low oxygen content, easy processing and the like.
B, mixing 60-90 parts by mass of Si powder (the purity is more than or equal to 3N, D50=5-20 μm), 10-35 parts by mass of Ti powder (the purity is more than or equal to 3N, D50=25-60 μm) and 1-10 parts by mass of TiH 2 Adding powder (the purity is more than or equal to 3N, D =1-10 μm) into a planetary ball milling vacuum tank, and vacuumizing the tank body to be less than 500 Pa. Ball milling parameters, ball material ratio of 3: 1-10: 1, ball milling rotation speed of 150r/min-400r/min, ball milling time of 6-12h and loading capacity of 1/3-2/3 of the volume of the ball milling tank. The grinding balls are high-hardness zirconium balls, the grinding balls are prepared balls with the sizes of phi 3mm, phi 6mm and phi 10mm, the ratio of the grinding balls to the large, medium and small balls is 3-5: 2-4, and the selected tank body is a vacuum tank with polytetrafluoroethylene/polyurethane lining.
And C, sieving the ball-milled powder by a 40-100-mesh sieve, and putting the powder into a titanium tank for vacuum sintering pretreatment, wherein the presintering temperature is 550-750 ℃, the presintering time is 1-3h, and the presintering vacuum degree is 10-2Pa. The powder after presintering has the advantages of low gas content, clean particle surface, high activity and the like, and is more beneficial to sintering.
And D, calculating the required weight of the pre-sintered powder according to the size of the product, then loading the pre-sintered powder into a hot-pressing graphite mold, filling graphite paper at the bottom and around the inside of the mold during mold loading, adding the powder into a graphite cavity in a grading manner, flattening the powder by adding one layer of powder, then placing the graphite paper, and uniformly spraying a high-temperature-resistant release agent on the graphite mold and the graphite paper, wherein the structure is shown in figure 2.
And E, placing the graphite mold under a pressure head of the vacuum hot-pressing furnace, pre-pressing the mold for 0.5-5 MPa, and setting sintering parameters. Firstly, the furnace body is vacuumized to 10 degrees -2 Heating to 450-650 ℃ at a speed of 3-8 ℃/min and keeping the temperature for 1-4 h below Pa; then heating to 800-1000 ℃ at the speed of 3-8 ℃/min, and preserving heat for 0.5-4 h; finally, heating to 1200-1400 ℃ at the speed of 2-5 ℃/min; boosting the pressure to 10-35 MPa, and keeping the temperature for 1-6 h; after the heat preservation is finished, cooling to 800-1000 ℃ at the speed of 2-5 ℃/min;
and F, after sintering, reducing the temperature to room temperature along with the furnace, taking out the die for demolding, and performing various machining on the titanium-silicon blank target material until the required product requirement is met, as shown in figure 3.
The following is illustrated in detail by specific examples and comparative examples:
example 1
85 parts by mass of Si powder (the purity is more than or equal to 3N, D50=10 μm), 10 parts by mass of Ti powder (the purity is more than or equal to 3N, D50=45 μm) and 5 parts by mass of TiH 2 Powder (purity is more than or equal to 3N, D =2 μm) is added into a vacuum ball milling tank and is vacuumized to 200Pa. The ball milling parameter is that the ball material ratio is 5: 1, the ball milling rotating speed is 250r/min, the ball milling time is 8h, and the loading capacity is 1/2 of the volume of the ball milling tank. The ratio of the large, medium and small sizes of phi 3mm, phi 6mm and phi 10mm is 3: 4: 3. The average particle size of the powder after ball milling is about 5 μm.
The pellets were screened out using a 100 mesh screen and the powder was placed in a titanium can for vacuum pre-firing.
When in vacuum presintering, the hearth is firstly vacuumized to the vacuum degree of 10-2Pa, then the temperature is raised to 600 ℃ at the heating rate of 10 ℃/min, and the hearth is cooled to the room temperature along with the furnace after being kept warm for 2 h.
Calculating the required weight of the pre-sintered powder according to the size of a product, then loading the powder into a hot-pressing graphite die, filling graphite paper at the bottom and around the inside of the die, adding the powder into a graphite cavity in a grading manner, leveling the powder when adding one layer, then filling the graphite paper, and uniformly spraying a high-temperature-resistant die agent on the graphite die and the graphite paper.
And placing the graphite mold under a pressure head of a vacuum hot-pressing furnace, prepressing the mold for 5MPa, and setting sintering parameters. Firstly, the furnace body is vacuumized to 10 degrees -2 Heating to 600 ℃ at the speed of 8 ℃/min and keeping the temperature for 2 hours below Pa; then raising the temperature to 1000 ℃ at a speed of 5 ℃/min, and keeping the temperature for ih; heating to 1300 deg.C at a rate of 5 deg.C/min, pressurizing to 15MPa, and maintaining for 1.5h; after the heat preservation is finished, removing the pressure, and cooling to 900 ℃ at the speed of 5 ℃/min; and then, after the temperature is reduced to room temperature along with the furnace, taking out the die for demoulding operation, and carrying out various machining on the titanium-silicon blank target material to meet the requirements of the required product.
Example 2
Example 2 is essentially the same as example 1 except that: the powder ratio is 70 parts by mass of Si powder (the purity is more than or equal to 3N, D =5 μm), 20 parts by mass of Ti powder (the purity is more than or equal to 3N, D =25 μm) and 10 parts by mass of TiH 2 Powder (purity ≥ 3N, D50=2 μm)
Example 3
Example 3 is essentially the same as example 1, except that: the powder ratio is 65 parts of Si powder (the purity is more than or equal to 3N, D50=5 μm), 25 parts of Ti powder (the purity is more than or equal to 3N, D50=25 μm) and 10 parts of TiH 2 Powder (purity ≥ 3N, D =2 μm)
Example 4
Example 4 is essentially the same as example 1, except that: the heat preservation time for sintering at 1400 ℃ is 1h.
Example 5
Example 5 is essentially the same as example 1, except that: the sintering temperature was 1250 ℃ and the pressing pressure was 25MPa.
Comparative example
Comparative example 1
Comparative example 1 is substantially the same as example 1 except that: the powder ratio is 85 parts of Si powder (the purity is more than or equal to 3N, D50=10 μm) and 15 parts of Ti powder (the purity is more than or equal to 3N, D50=45 μm).
Comparative example 2
85 parts by mass of Si powder (purity is not less than 3N, D50=10 μm), 10 parts by mass of Ti powder (purity is not less than 3N, D50=45 μm), and 5 parts by mass of TiH 2 Powder (purity is more than or equal to 3N, D =2 μm) is added into a vacuum ball milling tank and is vacuumized to 200Pa. The ball milling parameter is that the ball material ratio is 5: 1, the ball milling rotating speed is 250r/min, the ball milling time is 8h, and the loading capacity is 1/2 of the volume of the ball milling tank. The ratio of the large, medium and small sizes of phi 3mm, phi 6mm and phi 10mm is 3: 4: 3. The average particle size of the powder after ball milling is about 5 μm.
And carrying out spray granulation treatment on the uniformly mixed composite powder. Selecting PVA as a binder, adding PVA with the powder weight of 1% into deionized water, fully dissolving, adding the powder into the solution, and continuously stirring in the adding process to form uniform suspension with the solid content of 40%; and then polyethylene glycol in an amount of 0.5% by weight of the powder and polyether-modified silicon in an amount of 0.2% by weight of the powder are added. And (4) fully mixing the suspension, and then carrying out spray granulation, wherein the feeding mode is peristaltic pump feeding. The granulation parameters are as follows: the temperature of the air inlet is set to 280 ℃, the temperature of the air outlet is set to 100 ℃, and the rotating speed of a centrifugal disc is 8500r/min; the obtained granulated powder had a particle size of 200 mesh, a water content of 1.2%, a bulk density of 2.27g/cm3 and a flowability of 35s.
And (3) carrying out cold press molding on the granulated powder, wherein the molding pressure is 150MPa, and the pressure maintaining time is 5min, so that a biscuit with certain strength is obtained.
Carrying out vacuum pressureless sintering on the biscuit subjected to cold press molding, and vacuumizing a furnace body to 10 DEG -2 pa, heating to 600 ℃ at the speed of 8 ℃/min and keeping the temperature for 2 hours; then raising the temperature to 1000 ℃ at a speed of 5 ℃/min, and preserving the temperature for 1h; heating to 1300 ℃ at the speed of 5 ℃/min, and preserving heat for 1.5h; after the heat preservation is finished, removing the pressure, and cooling to 900 ℃ at the speed of 5 ℃/min; then the temperature is reduced to room temperature along with the furnace to obtain a blank.
Comparative examples 3 to 4
Comparative examples 3 to 4 were the same as example 1 except that the sintering temperatures were 1100 ℃ and 1450 ℃.
Comparative examples 5 to 6
Comparative examples 5 to 6 were substantially the same as example 1 except that the pressing pressures were 5MPa and 10MPa.
Comparative example 7
Comparative example 7 is the same as example 1 except that SPS sintering was carried out. The sintering equipment is pre-vacuumized to below 10 < -2 > Pa. Firstly, heating to 800 ℃ at a heating rate of 150 ℃/min, and keeping the temperature for 5min; and then heating to 1300 ℃ at the heating rate of 200 ℃/min, preserving the heat for 10min to obtain a titanium-silicon blank target material, and machining to obtain the product.
The above examples and comparative examples were subjected to performance tests, and the test results were as follows:
| density/% | Average grain size/. Mu.m | Oxygen content/PPM | Degree of alloying/% | |
| Example 1 | 99.7 | 68 | 239 | 100 |
| Example 2 | 99.5 | 71 | 262 | 100 |
| Example 3 | 99.6 | 66 | 247 | 100 |
| Example 4 | 99.8 | 74 | 272 | 100 |
| Example 5 | 99.6 | 56 | 254 | 100 |
| Comparative example 1 | 99.4 | 64 | 608 | 100 |
| Comparative example 2 | 95.1 | 70 | 361 | 94 |
| Comparative example 3 | 97.8 | 47 | 244 | 87 |
| Comparative example 4 | 99.8 | 163 | 261 | 100 |
| Comparative example 5 | 97.1 | 77 | 270 | 100 |
| Comparative example 6 | 98.5 | 73 | 266 | 100 |
| Comparative example 7 | 99.2 | 36 | 225 | 71 |
As can be seen from the above examples and comparative examples, the titanium-silicon alloy target material prepared by the preparation method provided by the invention has the advantages of low oxygen content, high density, fine grain size, high alloying degree and the like, and is suitable for sputter coating of various cutters and dies.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.
Claims (7)
1. The preparation method of the titanium-silicon target is characterized by comprising the following steps:
a, selecting Ti powder and Si powder as raw materials, and introducing TiH according to atomic ratio 2 Powder;
b, mixing 60-90 parts by mass of Si powder, 10-35 parts by mass of Ti powder and 1-10 parts by mass of TiH 2 Adding the powder into a planetary ball-milling vacuum tank, and vacuumizing the tank body to be below 500 Pa;
c, sieving the ball-milled powder by a 40-100-mesh sieve, and putting the powder into a titanium tank for vacuum sintering pretreatment;
d, calculating the required weight of the pre-sintered powder according to the size of the product, and then filling the pre-sintered powder into a hot-pressing graphite die;
e, placing the graphite mold under a pressure head of a vacuum hot-pressing furnace, prepressing the mold at 0.5-5 MPa, and setting sintering parameters for sintering;
and F, after sintering, reducing the temperature to room temperature along with the furnace, taking out the die for demolding, and carrying out various machining on the titanium-silicon blank target material to meet the requirements of the required product.
2. The method for preparing a titanium-silicon target material according to claim 1, wherein the method comprises the following steps: the purity of the Si powder is more than or equal to 3N, D =5-20 μm; the purity of the Ti powder is more than or equal to 3N, D =25-60 μm; the TiH 2 The purity of the powder is more than or equal to 3N, D =1-10 μm.
3. The method for preparing a titanium-silicon target material according to claim 1, wherein the method comprises the following steps: in the step B, ball milling parameters comprise ball-material ratio of 3: 1-10: 1, ball milling rotation speed of 150r/min-400r/min, ball milling time of 6-12h and loading capacity of 1/3-2/3 of the volume of the ball milling tank.
4. The method for preparing the titanium-silicon target material according to claim 3, wherein the method comprises the following steps: the selected grinding balls are high-hardness zirconium balls, and the grinding balls are prepared balls with three sizes of phi 3mm, phi 6mm and phi 10mm, and the ratio of the big size to the small size is 3-5: 2-4.
5. The method for preparing a titanium-silicon target material according to claim 1, wherein the method comprises the following steps: in the step D, filling graphite paper at the bottom and around the inside of the mold during mold filling, adding the powder into the graphite cavity in several times, leveling the powder when adding one layer, and then placing the graphite paper, wherein the graphite mold and the graphite paper are uniformly sprayed with a high-temperature resistant mold release agent.
6. The method for preparing a titanium-silicon target material according to claim 1, wherein the method comprises the following steps: in step E, the sintering parameters include: firstly, the furnace body is vacuumized to 10 degrees -2 Heating to 450-650 ℃ at a speed of 3-8 ℃/min and keeping the temperature for 1-4 h below Pa; then heating to 800-1000 ℃ at the speed of 3-8 ℃/min, and preserving heat for 0.5-4 h; finally, heating to 1200-1400 ℃ at the speed of 2-5 ℃/min; boosting the pressure to 10-35 MPa, and keeping the temperature for 1-6 h; after the heat preservation is finished, the temperature is reduced to 800-1000 ℃ at the speed of 2-5 ℃/min.
7. The method for preparing a titanium-silicon target material according to claim 1, wherein the method comprises the following steps: in step C, the pre-sintering temperature is 550-750 ℃, the pre-sintering time is 1-3h, and the pre-sintering vacuum degree is 10 -2 Pa。
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| CN116655372A (en) * | 2023-06-25 | 2023-08-29 | 深圳众诚达应用材料股份有限公司 | Tin oxide-based target material and preparation method thereof |
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