CN115637431A - Silicon wafer substrate surface pretreatment method and application thereof - Google Patents
Silicon wafer substrate surface pretreatment method and application thereof Download PDFInfo
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- CN115637431A CN115637431A CN202211334890.0A CN202211334890A CN115637431A CN 115637431 A CN115637431 A CN 115637431A CN 202211334890 A CN202211334890 A CN 202211334890A CN 115637431 A CN115637431 A CN 115637431A
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- 239000000758 substrate Substances 0.000 title claims abstract description 100
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 58
- 239000010703 silicon Substances 0.000 title claims abstract description 58
- 238000002203 pretreatment Methods 0.000 title abstract description 7
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 64
- 239000010432 diamond Substances 0.000 claims abstract description 64
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 21
- 239000000725 suspension Substances 0.000 claims abstract description 18
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 14
- 239000011733 molybdenum Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- 229920002120 photoresistant polymer Polymers 0.000 claims abstract description 13
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- 230000007547 defect Effects 0.000 claims abstract description 9
- 238000000151 deposition Methods 0.000 claims abstract description 8
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 8
- 238000000059 patterning Methods 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 230000010355 oscillation Effects 0.000 claims abstract description 3
- 238000007747 plating Methods 0.000 claims abstract description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 17
- 238000004544 sputter deposition Methods 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 238000005229 chemical vapour deposition Methods 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
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- 235000019441 ethanol Nutrition 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- -1 amyl ethyl Chemical group 0.000 claims 1
- 230000006911 nucleation Effects 0.000 abstract description 10
- 238000010899 nucleation Methods 0.000 abstract description 10
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000007704 transition Effects 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 27
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 7
- 239000000463 material Substances 0.000 description 4
- 239000013077 target material Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
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Abstract
The invention relates to a pretreatment method for the surface of a silicon wafer substrate, which takes a silicon wafer as a substrate and carries out patterning on the surface of the silicon wafer; carrying out magnetron sputtering molybdenum plating treatment on the obtained substrate; carrying out photoresist removing treatment on the obtained substrate; immersing the obtained substrate into a diamond powder suspension for ultrasonic oscillation treatment to form a scratch defect on the surface of the substrate; and cleaning and drying the obtained substrate to obtain the target object. The silicon wafer substrate prepared by the method for pretreating the surface of the silicon wafer substrate is applied to the production of the self-supporting diamond film. The beneficial effects are that: the method comprises the steps of carrying out graphical treatment on the surface of a silicon substrate to form a grid nucleation area with regular arrangement, then depositing a molybdenum transition layer on the surface of the silicon substrate regularly, and forming uniform scratch defects on the surface of a graphical silicon wafer by using diamond powder suspension, so that the density and uniformity of diamond nucleation on the surface of the silicon wafer are improved, and good precondition is provided for the growth of a high-quality diamond thick film.
Description
Technical Field
The invention relates to the field of heteroepitaxial diamond film materials, in particular to a silicon wafer substrate surface pretreatment method and application thereof.
Background
The diamond film has excellent comprehensive performance of good wave permeability from far infrared to ultraviolet, extremely high hardness and thermal conductivity, excellent thermal shock resistance and the like, and becomes an optimal infrared and X-ray window wave-transmitting material, so the CVD diamond thick film has wide application prospect and can be used as one of the optimal materials for optical application.
The research on the growth of the diamond thick film in China has a larger difference compared with the foreign countries, a proper growth substrate is usually needed for the preparation of the CVD diamond thick film, and because the thermal expansion coefficient of the diamond film is small, when the thermal expansion coefficient of a substrate material is larger than that of the diamond, larger thermal stress is generated between the substrate and the diamond to cause cracks generated by the thin film to further influence the performance of the thin film, a monocrystalline silicon wafer is usually used as the substrate.
At present, in the deposition preparation of a diamond film, the surface of a silicon wafer needs to be ground by diamond powder for a long time so as to improve the nucleation rate of the diamond film in the heteroepitaxy process. The distribution, depth, length and the like of grinding scratches on the surface of the silicon wafer influence the growth orientation, surface appearance, structural uniformity, stress and other characteristics of the diamond film to a certain extent.
It is very difficult to obtain uniformly distributed grinding scratches on the surface of the silicon wafer, and when the pretreatment result of the surface of the silicon wafer is not ideal, the diamond film is easy to form uneven structural features along with the increase of the thickness of the diamond film, so that larger stress and cracks are generated, and the substrate is also easy to warp and crack, so that the damage of the diamond film is caused.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a silicon wafer substrate surface pretreatment method and application thereof, so as to overcome the defects in the prior art.
The technical scheme for solving the technical problems is as follows: a silicon wafer substrate surface pretreatment method comprises the following steps:
s100, patterning is carried out on the surface of a silicon wafer serving as a substrate to form a grid nucleation area with regular arrangement;
s200, performing magnetron sputtering molybdenum plating treatment on the substrate obtained in the S100;
s300, carrying out photoresist removing treatment on the substrate obtained in the S200;
s400, immersing the substrate obtained in the step S300 into the diamond powder suspension for ultrasonic oscillation treatment so as to form scratch defects on the surface of the substrate;
and S500, cleaning and drying the substrate obtained in the S400 to obtain the target object.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the silicon wafer used in step S100 is first cleaned and dried, and then patterned.
Further, the cleaning mode is ultrasonic cleaning, and the parameters of the ultrasonic cleaning are set as follows: and (3) ultrasonically cleaning the substrate for 5-10 min by using absolute ethyl alcohol, acetone and deionized water in sequence, and then drying the substrate in a nitrogen atmosphere.
Further, the mask used for patterning in step S100 includes regular patterns with a certain arrangement rule and a regular shape, and the distance between every two adjacent patterns is maintained at more than 30 μm.
Further, the magnetron sputtering process in the step S200 is as follows: the sputtering gas is Ar, the flow rate is controlled to be 15.0mL/min, the sputtering pressure is kept between 0.2Pa and 0.4Pa, the coating time is 15min to 20min, and the thickness of the molybdenum layer to be coated is controlled to be 0.3 +/-0.1 mu m.
Further, the volume fraction of Ar was 99.999%.
Further, the photoresist removing process in step S300 is to dip the substrate into an organic solvent to dissolve the photoresist.
Further, the organic solvent is acetone, ethanol or amyl alcohol.
Furthermore, the average diameter of the diamond micro powder in the diamond powder suspension is 5 +/-3 microns, and the solvent in the diamond powder suspension is ethanol, acetone or amyl alcohol.
Further, in step S500, the cleaning mode is ultrasonic cleaning, and the parameters of the ultrasonic cleaning are set as follows: sequentially and respectively ultrasonically cleaning by using absolute ethyl alcohol, acetone and deionized water, and then drying at the temperature of 40-60 ℃ in the atmosphere of nitrogen.
The beneficial effects of the invention are:
1) The method comprises the steps of forming a grid nucleation area with regular arrangement by carrying out patterning treatment on the surface of a silicon substrate, depositing a molybdenum transition layer on the surface of the silicon substrate regularly, and forming uniform scratch defects on the patterned surface of a silicon wafer by using a diamond powder suspension, so that the density and uniformity of diamond nucleation on the surface of the silicon wafer are improved, and good precondition is provided for the growth of a high-quality diamond thick film;
2) The transition layer molybdenum is regularly and uniformly deposited on the silicon substrate to improve the nucleation rate of uniform nucleation of the diamond film, which can be generally 10 6 -10 7 Increase the nucleation rate to 10 9 -10 10 The internal stress caused by the non-uniformity of the nucleation rate can be effectively avoided;
3) The process flow is simple, the used technology is the mature industrial production flow at present, and the method is suitable for mass industrial production and popularization.
Based on the technical scheme, the invention also provides a target prepared by the silicon wafer substrate surface pretreatment method, which is applied to the production of the self-supporting diamond film.
Adopt above-mentioned further beneficial effect to do: the silicon chip substrate has lower thermal expansion coefficient, reduces the probability of breakage of the diamond film, can reduce the breakage probability of the silicon chip substrate from 50 percent to below 10 percent, solves the problem that the prepared diamond film is easy to generate cracks and fracture due to the non-ideal pretreatment process in the prior art, and increases the yield of the growth of the diamond film.
Further, the production method of the self-supporting diamond film is as follows: putting a silicon wafer substrate into a microwave plasma chemical vapor deposition system, pumping to the air pressure of 0.1pa, introducing 300sccm hydrogen, starting microwaves when the pressure rises to 1kPa, adjusting the power and the pressure to enable the temperature to be 850 ℃ and the pressure to be 13kPa, introducing 6sccm methane, depositing for 120h, and soaking the prepared diamond film in a mixed solution of concentrated nitric acid and hydrofluoric acid to completely dissolve the silicon wafer substrate to obtain the self-supporting diamond film.
Drawings
FIG. 1 is a flow chart of a method for pretreating the surface of a silicon wafer substrate according to the present invention;
FIG. 2 is a flow chart of the pretreatment of the surface of the silicon wafer substrate according to the present invention.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
Example 1
As shown in fig. 1 and fig. 2, a method for pretreating the surface of a silicon wafer substrate comprises the following steps:
s100, selecting a monocrystalline silicon wafer with the diameter of 50mm as a substrate, sequentially carrying out ultrasonic cleaning on the substrate by using acetone, absolute ethyl alcohol and deionized water, then drying the monocrystalline silicon wafer with the diameter of 50mm after ultrasonic cleaning in a nitrogen atmosphere, carrying out graphical treatment on the surface of the obtained substrate by using a mask plate, and forming uniformly distributed graphs on the photoresist deposited on the silicon, wherein the used mask plate comprises regular square patterns arranged in a longitude and latitude mode, the side length of each regular square pattern is 50 micrometers, and the distance between every two adjacent square patterns is 50 micrometers;
s200, placing the substrate obtained in the step S100 into a direct current magnetron sputtering system, wherein the target is metal molybdenum, the distance between the target and the substrate is 80mm, the sputtering gas is Ar (the volume fraction is 99.999%), the flow rate is controlled to be 15.0mL/min, the sputtering pressure is kept at 0.3Pa, when the background vacuum degree of a vacuum chamber reaches 50mPa, sputtering coating is started for 20min, and the thickness of a coated molybdenum layer is 0.2 mu m;
s300, soaking the substrate obtained in the step S200 in acetone to completely remove the photoresist;
s400, putting the substrate obtained in the step S300 into a diamond powder suspension, and performing ultrasonic treatment for 60min to form a scratch defect on the surface of the substrate, wherein the diamond powder suspension is prepared as follows: weighing 5g of diamond micropowder with the average particle size of 5 +/-1.0 mu m, putting the diamond micropowder into a beaker, and gradually dripping 100ml of absolute ethyl alcohol into the beaker to prepare a diamond powder suspension;
s500, carrying out ultrasonic cleaning on the substrate obtained in the step S400 by using acetone, absolute ethyl alcohol and deionized water in sequence for 15min, then putting the substrate into an oven, introducing nitrogen, setting the temperature to be 60 ℃, and drying.
And (2) putting the pretreated silicon wafer substrate into a microwave plasma chemical vapor deposition system, starting a mechanical vacuum pump to ensure that the air pressure is 0.1pa, introducing 300sccm hydrogen, starting microwaves when the pressure is raised to 1kPa, adjusting the power and the pressure to ensure that the temperature is 850 ℃, the pressure is 13kPa, introducing 6sccm methane, depositing for 120h, and soaking the prepared diamond film into a mixed solution of concentrated nitric acid and hydrofluoric acid to completely dissolve the silicon wafer substrate to obtain the self-supporting diamond film.
Example 2
As shown in fig. 1 and fig. 2, a method for pretreating the surface of a silicon wafer substrate comprises the following steps:
s100, selecting a monocrystalline silicon wafer with the diameter of 100mm as a substrate, sequentially carrying out ultrasonic cleaning on the substrate by using acetone, absolute ethyl alcohol and deionized water, then drying the monocrystalline silicon wafer with the diameter of 100mm after ultrasonic cleaning in a nitrogen atmosphere, carrying out graphical treatment on the surface of the obtained substrate by using a mask, and forming uniformly distributed graphs on the photoresist deposited on the silicon, wherein the used mask comprises regular rectangular patterns arranged in a longitude and latitude mode, the long side of each regular rectangular pattern is 50 microns, the short side is 25 microns, and the distance between every two adjacent rectangular patterns is 40 microns;
s200, placing the substrate obtained in the step S100 into a direct current magnetron sputtering system, wherein the target material is metal molybdenum, the distance between the target material and the substrate is 90mm, the sputtering gas is Ar (the volume fraction is 99.999%), the flow rate is controlled to be 15.0mL/min, the sputtering pressure is kept at 0.2Pa, when the background vacuum degree of a vacuum chamber reaches 40mPa, sputtering coating is started for 15min, and the thickness of a coated molybdenum layer is 0.2 mu m;
s300, soaking the substrate obtained in the step S200 in amyl alcohol, and completely removing the photoresist;
s400, placing the substrate obtained in the step S300 into a diamond powder suspension, and carrying out ultrasonic treatment for 50min to form a scratch defect on the surface of the substrate, wherein the diamond powder suspension is prepared as follows: weighing 5g of diamond micropowder with the average particle size of 5 +/-1.0 mu m, putting the diamond micropowder into a beaker, and gradually dripping 100ml of amyl alcohol into the beaker to prepare diamond powder suspension;
s500, carrying out ultrasonic cleaning on the substrate obtained in the step S400 by using acetone, absolute ethyl alcohol and deionized water in sequence for 15min, then putting the substrate into an oven, introducing nitrogen, setting the temperature to be 60 ℃, and drying.
And (2) putting the pretreated silicon wafer substrate into a microwave plasma chemical vapor deposition system, starting a mechanical vacuum pump to ensure that the air pressure is 0.1pa, introducing 300sccm hydrogen, starting microwaves when the pressure is raised to 1kPa, adjusting the power and the pressure to ensure that the temperature is 850 ℃, the pressure is 13kPa, introducing 6sccm methane, depositing for 120h, and soaking the prepared diamond film into a mixed solution of concentrated nitric acid and hydrofluoric acid to completely dissolve the silicon wafer substrate to obtain the self-supporting diamond film.
Example 3
As shown in fig. 1 and fig. 2, a method for pretreating the surface of a silicon wafer substrate comprises the following steps:
s100, selecting a monocrystalline silicon wafer with the diameter of 150mm as a substrate, sequentially carrying out ultrasonic cleaning on the substrate by using acetone, absolute ethyl alcohol and deionized water, then drying the monocrystalline silicon wafer with the diameter of 150mm after ultrasonic cleaning in a nitrogen atmosphere, carrying out patterning treatment on the surface of the obtained substrate by using a mask, and forming uniformly distributed patterns on a photoresist deposited on the silicon, wherein the used mask comprises regular circular patterns arranged in a longitude and latitude mode, the diameter of each regular circular pattern is 50 mu m, and the distance between every two adjacent circular patterns is 50 mu m;
s200, placing the substrate obtained in the step S100 into a direct current magnetron sputtering system, wherein the target material is metal molybdenum, the distance between the target material and the substrate is 100mm, the sputtering gas is Ar (the volume fraction is 99.999%), the flow rate is controlled to be 15.0mL/min, the sputtering pressure is kept at 0.4Pa, when the background vacuum degree of a vacuum chamber reaches 50mPa, sputtering coating is started for 20min, and the thickness of a coated molybdenum layer is 0.3 mu m;
s300, soaking the substrate obtained in the step S200 in acetone to completely remove the photoresist;
s400, putting the substrate obtained in the step S300 into a diamond powder suspension, and performing ultrasonic treatment for 60min to form a scratch defect on the surface of the substrate, wherein the diamond powder suspension is prepared as follows: weighing 5g of diamond micropowder with the average particle size of 5 +/-1.0 mu m, putting the diamond micropowder into a beaker, and gradually dripping 100ml of acetone into the beaker to prepare diamond powder suspension;
s500, carrying out ultrasonic cleaning on the substrate obtained in the step S400 by using acetone, absolute ethyl alcohol and deionized water in sequence for 15min, then putting the substrate into an oven, introducing nitrogen, setting the temperature to be 60 ℃, and drying.
And (2) putting the pretreated silicon wafer substrate into a microwave plasma chemical vapor deposition system, starting a mechanical vacuum pump to ensure that the air pressure is 0.1pa, introducing 300sccm hydrogen, starting microwaves when the pressure is raised to 1kPa, adjusting the power and the pressure to ensure that the temperature is 850 ℃, the pressure is 13kPa, introducing 6sccm methane, depositing for 120h, and soaking the prepared diamond film into a mixed solution of concentrated nitric acid and hydrofluoric acid to completely dissolve the silicon wafer substrate to obtain the self-supporting diamond film.
Although embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are exemplary and not to be construed as limiting the present invention, and that changes, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A method for pretreating the surface of a silicon wafer substrate is characterized by comprising the following steps:
s100, patterning the surface of a silicon wafer serving as a substrate;
s200, performing magnetron sputtering molybdenum plating treatment on the substrate obtained in the S100;
s300, carrying out photoresist removing treatment on the substrate obtained in the S200;
s400, immersing the substrate obtained in the step S300 into the diamond powder suspension for ultrasonic oscillation treatment so as to form scratch defects on the surface of the substrate;
and S500, cleaning and drying the substrate obtained in the S400 to obtain the target object.
2. The method of pretreating the surface of a silicon wafer substrate according to claim 1, wherein: the silicon wafer adopted in the step S100 is firstly cleaned and dried, and then is patterned, wherein the cleaning mode is ultrasonic cleaning, and parameters of the ultrasonic cleaning are set as follows: and (3) ultrasonically cleaning the substrate for 5-10 min by using absolute ethyl alcohol, acetone and deionized water in sequence, and then drying the substrate in a nitrogen atmosphere.
3. The method of pretreating the surface of a silicon wafer substrate according to claim 1, wherein: the mask used for patterning in step S100 includes regular patterns with a certain arrangement rule and a regular shape, and the distance between every two adjacent patterns is maintained at more than 30 μm.
4. The method of pre-treating the surface of a silicon wafer substrate according to claim 1, wherein: the magnetron sputtering process in the step S200 comprises the following steps: the sputtering gas is Ar, the flow rate is controlled to be 15.0mL/min, the sputtering pressure is kept between 0.2Pa and 0.4Pa, the coating time is 15min to 20min, and the thickness of the molybdenum layer to be coated is controlled to be 0.3 +/-0.1 mu m.
5. The method of pretreating the surface of a silicon wafer substrate according to claim 1, wherein: the photoresist removing process in step S300 is to immerse the substrate in an organic solvent to dissolve the photoresist.
6. The method of pre-treating the surface of a silicon wafer substrate according to claim 5, wherein: the organic solvent is acetone, ethanol or amyl alcohol.
7. The method of pretreating the surface of a silicon wafer substrate according to claim 1, wherein: the average diameter of the diamond micro powder in the diamond powder suspension is 5 +/-3 mu m, and the solvent in the diamond powder suspension is ethanol, acetone or amyl ethyl alcohol.
8. The method of pretreating the surface of a silicon wafer substrate according to claim 1, wherein: in the step S500, the cleaning mode is ultrasonic cleaning, and parameters of the ultrasonic cleaning are set as: sequentially and respectively ultrasonically cleaning by using absolute ethyl alcohol, acetone and deionized water, and then drying at the temperature of 40-60 ℃ in the atmosphere of nitrogen.
9. A silicon wafer substrate prepared by the method for pretreating the surface of a silicon wafer substrate according to any one of claims 1 to 8 is used for producing a self-supporting diamond film.
10. Use according to claim 9, characterized in that: the production method of the self-supporting diamond film comprises the following steps:
putting a silicon wafer substrate into a microwave plasma chemical vapor deposition system, pumping to the air pressure of 0.1pa, introducing 300sccm hydrogen, starting microwaves when the pressure rises to 1kPa, adjusting the power and the pressure to enable the temperature to be 850 ℃ and the pressure to be 13kPa, introducing 6sccm methane, depositing for 120h, and soaking the prepared diamond film in a mixed solution of concentrated nitric acid and hydrofluoric acid to completely dissolve the silicon wafer substrate to obtain the self-supporting diamond film.
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