CN116313747A - Surface treatment method of semiconductor polycrystalline silicon material - Google Patents
Surface treatment method of semiconductor polycrystalline silicon material Download PDFInfo
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- CN116313747A CN116313747A CN202310297836.1A CN202310297836A CN116313747A CN 116313747 A CN116313747 A CN 116313747A CN 202310297836 A CN202310297836 A CN 202310297836A CN 116313747 A CN116313747 A CN 116313747A
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000004065 semiconductor Substances 0.000 title claims abstract description 27
- 238000004381 surface treatment Methods 0.000 title claims abstract description 20
- 239000002210 silicon-based material Substances 0.000 title claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 89
- 238000004140 cleaning Methods 0.000 claims abstract description 89
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 82
- 238000005498 polishing Methods 0.000 claims abstract description 47
- 239000000463 material Substances 0.000 claims abstract description 44
- 238000000227 grinding Methods 0.000 claims abstract description 42
- 229920005591 polysilicon Polymers 0.000 claims abstract description 36
- 238000003754 machining Methods 0.000 claims abstract description 9
- 239000012459 cleaning agent Substances 0.000 claims description 121
- 238000001035 drying Methods 0.000 claims description 67
- 239000008367 deionised water Substances 0.000 claims description 61
- 229910021641 deionized water Inorganic materials 0.000 claims description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 61
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 45
- 238000005406 washing Methods 0.000 claims description 39
- 238000005554 pickling Methods 0.000 claims description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
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- 125000000896 monocarboxylic acid group Chemical group 0.000 claims description 16
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- 235000012239 silicon dioxide Nutrition 0.000 claims description 10
- 229910001018 Cast iron Inorganic materials 0.000 claims description 5
- 229910000831 Steel Inorganic materials 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
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- 230000000694 effects Effects 0.000 abstract description 26
- 239000013078 crystal Substances 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 5
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000174 gluconic acid Substances 0.000 description 2
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- 229910052751 metal Inorganic materials 0.000 description 2
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- 238000012545 processing Methods 0.000 description 2
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- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
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- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02002—Preparing wafers
- H01L21/02005—Preparing bulk and homogeneous wafers
- H01L21/02008—Multistep processes
- H01L21/0201—Specific process step
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02002—Preparing wafers
- H01L21/02005—Preparing bulk and homogeneous wafers
- H01L21/02008—Multistep processes
- H01L21/0201—Specific process step
- H01L21/02013—Grinding, lapping
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02002—Preparing wafers
- H01L21/02005—Preparing bulk and homogeneous wafers
- H01L21/02008—Multistep processes
- H01L21/0201—Specific process step
- H01L21/02024—Mirror polishing
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
- H01L21/02052—Wet cleaning only
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02082—Cleaning product to be cleaned
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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
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
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Abstract
The invention relates to a surface treatment method of a semiconductor polycrystalline silicon material, which comprises the steps of machining, ultrasonic cleaning, primary acid cleaning, ultrasonic cleaning, grinding, ultrasonic cleaning, secondary acid cleaning, ultrasonic cleaning, CMP polishing, ultrasonic cleaning and the like. The invention can achieve perfect mirror effect after polishing, and the grain boundary and the grain position have no obvious layering sense. The requirements on the area and the density of crystal grains on the surface of the raw material are not strict. The invention can eliminate layering sense between grain boundary and grain position for the raw materials of semiconductor polysilicon materials with different grain densities, and the finished product effect can meet the mirror effect of market demand, thereby saving production cost and having strong practicability.
Description
Technical Field
The invention relates to a surface treatment method of a semiconductor polycrystalline silicon material, and belongs to the technical field of semiconductor polycrystalline silicon material processing.
Background
Polycrystalline silicon is a form of elemental silicon. When the melted elemental silicon solidifies under supercooling conditions, the silicon atoms are arranged in the form of diamond lattices into a plurality of crystal nuclei, and if the crystal nuclei grow into crystal grains with different crystal face orientations, the crystal grains combine to crystallize into polycrystalline silicon.
The manufacturers for manufacturing the polysilicon material at present finally lead to different areas of crystal grains (figure 1) on the surface of the material due to different crystal pulling processes, and further lead to different acid-resistant corrosivity of the crystal grains and the crystal boundaries due to different material densities. After the polycrystalline silicon material is subjected to ultrasonic cleaning, the surface is corroded by utilizing a mixed solution of hydrofluoric acid and nitric acid, and finally after ultrasonic cleaning and CMP mechanochemical polishing, different layering effects can appear on the mirror surfaces of different materials at grain boundaries (grain boundaries) (figure 2), the grain boundary positions are lower than the grain positions, and the worse-compactness material layering is more obvious.
The grain sizes of polysilicon materials manufactured by different manufacturers are shown in fig. 3 and 4, and the grain sizes are obviously different from the diagrams; the grain boundary of the small-grain polysilicon material processed by the conventional process is very small or insignificant (see fig. 6), and the grain boundary surface of the large-grain polysilicon material processed by the conventional process is very significant (see fig. 5).
The general conventional process at present is as follows:
machining, ultrasonic cleaning, fine grinding, ultrasonic cleaning, acid washing, ultrasonic cleaning, CMP polishing and ultrasonic cleaning.
Based on this, the present invention has been proposed.
Disclosure of Invention
The invention provides a surface treatment method of a semiconductor polysilicon material, which aims at the defects existing in the prior art, and comprises the following main processes:
machining, ultrasonic cleaning, primary acid cleaning, ultrasonic cleaning, grinding, ultrasonic cleaning, secondary acid cleaning, ultrasonic cleaning, CMP polishing and ultrasonic cleaning.
The specific technical scheme is as follows:
a surface treatment method of a semiconductor polysilicon material comprises the following steps:
firstly, machining a semiconductor polycrystalline silicon material to obtain a primary blank; all the shapes are processed by adopting a machine tool according to the drawing of the product, and the size meets the drawing requirement.
Step two, performing ultrasonic cleaning on the surface of the primary blank, firstly cleaning with an alkaline cleaning agent, then rinsing with deionized water, and finally drying to obtain the primary blank subjected to ultrasonic cleaning;
and the surface of the machine tool is cleaned by the pollutants such as greasy dirt, metal impurities and the like, and the ultrasonic cleaning in the second step is adopted, so that the cleaning effect is good.
Step three, pickling the primary blank subjected to primary ultrasonic cleaning by adopting mixed strong acid to obtain a primary pickled primary blank; in the step, mixed strong acid is adopted to clean the surface, so that the brightness and the flatness of the surface can be improved, and the pickling effect is mainly to pretreat structures (including inner and outer diameters, hole structures and the like) except for upper and lower planes. And (3) the product is kept to shake up and down in the pickling process, and is quickly rinsed by deionized water after the pickling is finished, and the product is kept to be thrown up and down each time, wherein the time of the upward and downward throwing is 30-60 s.
Step four, performing ultrasonic cleaning on the primary blank subjected to acid cleaning, firstly cleaning by using an alkaline cleaning agent, then rinsing by using deionized water, and finally drying to obtain a secondary ultrasonic cleaned primary blank; acid residues can be remained on the surface of the product after acid washing, and ultrasonic cleaning is needed to neutralize the surface residual acid.
Step five, grinding the primary blank subjected to the secondary ultrasonic cleaning to obtain a blank; the invention discovers that the method for removing the saw marks and the surface damaged layers by grinding is best through multiple experiments, and can effectively improve the warping degree, the flatness and the parallelism of the polysilicon, thereby achieving a process of fine grinding treatment before polishing.
Step six, performing ultrasonic cleaning on the surface of the blank, firstly cleaning with an alkaline cleaning agent, then rinsing with deionized water, and finally drying to obtain the blank subjected to three ultrasonic cleaning; the surface of the suspension agent, metal impurities, abrasive and other pollutants remained after the grinding process is required to be cleaned by ultrasonic waves.
Step seven, pickling the blank subjected to ultrasonic cleaning for the third time by adopting fine pickling acid to obtain a blank subjected to secondary pickling; the secondary acid washing is to further strengthen and remove impurities such as surface abrasive materials by using the fine washing acid, and the proportion and the type of the fine washing acid greatly influence layering after final polishing due to the difference of corrosion resistance of grain boundaries and grains. In the invention, the surface treatment effect can be improved by adding acetic acid into the fine washing acid and adjusting and optimizing the acid liquor proportion.
Step eight, performing ultrasonic cleaning on the blank subjected to secondary pickling, firstly cleaning by using an alkaline cleaning agent, then rinsing by using deionized water, and finally drying to obtain the blank subjected to three ultrasonic cleaning; after the cleaning by the fine cleaning acid, the acid stain can be remained on the surface of the product, and the ultrasonic cleaning is needed to neutralize the surface acid.
And step nine, performing double-sided mirror polishing on the blank subjected to ultrasonic cleaning for three times to obtain a polished blank.
And step ten, performing ultrasonic cleaning on the polished blank, cleaning with an alkaline cleaning agent, rinsing with deionized water, and finally drying to obtain a finished product. The polishing surface has residual polishing liquid and needs ultrasonic cleaning.
As an improvement of the technical scheme, in the second step, the alkaline cleaning agent is potassium hydroxide or sodium hydroxide solution with the mass fraction of 5-10%, the temperature is 50-60 ℃ when the alkaline cleaning agent is adopted for cleaning, the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 80 kHz;
rinsing with deionized water for at least three times at 50-60 ℃, rinsing for 2min at 40kHz ultrasonic frequency, and rinsing for 2min at 80kHz ultrasonic frequency;
the temperature is 100 ℃ during drying, and the drying time is 10-30 min;
as an improvement of the technical scheme, in the fourth step, the alkaline cleaning agent is potassium hydroxide or sodium hydroxide solution with the mass fraction of 5-10%, the temperature is 50-60 ℃ when the alkaline cleaning agent is adopted for cleaning, the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 80 kHz;
rinsing with deionized water for at least three times at 50-60 ℃, rinsing for 2min at 40kHz ultrasonic frequency, and rinsing for 2min at 80kHz ultrasonic frequency;
the temperature is 100 ℃ and the drying time is 10-30 min.
As an improvement of the technical scheme, in the third step, the mixed strong acid contains HF and HNO 3 The mass fraction of HF in the mixed strong acid is 5-8%, HNO in the mixed strong acid 3 The mass fraction of (2) is 50-60%; the pickling time is 30-60 s, and the steel is put into deionized water for rinsing at least 2 times after the pickling is completed.
As an improvement of the technical scheme, in the fifth step, the removal amount of grinding is 50-60 mu m, a double-sided grinding machine is adopted by grinding equipment, cast iron is adopted by a grinding disc, 1000-1500 meshes of alumina is adopted by grinding materials, and the grinding time is 30-60 min.
As an improvement of the technical proposal, in the seventh step, the fine washing acid contains HF and HNO 3 、CH 3 The mass fraction of HF in the refined acid is 1-2%, HNO in the refined acid 3 The mass fraction of (2) is 10-20%, and the CH in the fine washing acid 3 The mass fraction of COOH is 1-5%, the pickling time is 30-60 s, the pickling is completed, the pickling is carried out in deionized water for at least 2 times, and the up-and-down polishing time of the product is required to be kept at 30-60 s in the pickling process.
As an improvement of the technical proposal, in the seventh step, HF and HNO in the acid are finely washed 3 、CH 3 The mass ratio of COOH was 3:30:5.CH (CH) 3 The excessive and the insufficient COOH content can affect the grain boundary of the mirror surface after final polishing, and can be observed by naked eyes.
As an improvement of the technical scheme, in the step nine, the polishing equipment adopts a CMP mechanochemical double-sided polisher, the polishing solution adopts a silicon dioxide polishing solution, the mass fraction of silicon dioxide in the polishing solution is 1% -3%, and the polishing time is 1-2 h.
As an improvement of the technical scheme, in the step six, the alkaline cleaning agent is potassium hydroxide or sodium hydroxide solution with the mass fraction of 5-10%, the temperature is 50-60 ℃ when the alkaline cleaning agent is adopted for cleaning, the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 80 kHz;
rinsing with deionized water for at least three times at 50-60 ℃, rinsing for 2min at 40kHz ultrasonic frequency, and rinsing for 2min at 80kHz ultrasonic frequency;
the temperature is 100 ℃ and the drying time is 10-30 min.
As an improvement of the technical scheme, in the step eight, the alkaline cleaning agent is potassium hydroxide or sodium hydroxide solution with the mass fraction of 5-10%, the temperature is 50-60 ℃ when the alkaline cleaning agent is adopted for cleaning, the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 80 kHz;
rinsing with deionized water for at least three times at 50-60 ℃, rinsing for 2min at 40kHz ultrasonic frequency, and rinsing for 2min at 80kHz ultrasonic frequency;
the temperature is 100 ℃ and the drying time is 10-30 min.
As an improvement of the technical scheme, in the step ten, the alkaline cleaning agent is potassium hydroxide or sodium hydroxide solution with the mass fraction of 5-10%, the temperature is 50-60 ℃ when the alkaline cleaning agent is adopted for cleaning, the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 80 kHz;
rinsing with deionized water for at least three times at 50-60 ℃, rinsing for 2min at 40kHz ultrasonic frequency, and rinsing for 2min at 80kHz ultrasonic frequency;
the temperature is 100 ℃ and the drying time is 10-30 min.
In the invention, no matter any procedure (such as machining, primary acid washing, grinding, secondary acid washing and CMP polishing) is adopted in the preamble, the same ultrasonic cleaning process can be adopted, and the process parameters, alkaline cleaning agents, two ultrasonic waves with different frequencies and the like can be cleaned. Particularly, in the ultrasonic cleaning process, the rinsing is respectively carried out at the ultrasonic frequency of 40kHz and the ultrasonic frequency of 80kHz, and the effect is better than the rinsing is carried out at the ultrasonic frequency of 80kHz alone.
In the invention, taking the step ten as an example, multiple experiments show that the semiconductor polysilicon material is rinsed under the ultrasonic frequency of 20kHz independently, the probability of generating corrosion holes is more than 10 percent (for example, the probability of generating cracks is more than 2 times when the test is performed for 20 times), the probability of generating cracks is more than 5 per mill, and the crack length is even more than 3cm. Rinsing is carried out under the ultrasonic frequency of 30kHz, the semiconductor polysilicon material has the probability of generating corrosive cavities of more than 3 percent, has the probability of generating cracks of more than 1 per mill, and the crack length is not more than 1cm. Rinsing is carried out under ultrasonic frequency of 40kHz and 80kHz, and no corrosion cavity and crack are found in the semiconductor polysilicon material. Cleaning can be performed only under the ultrasonic frequency of 40kHz, and the cleaning time is usually more than 16 minutes; the cleaning can be performed only at an ultrasonic frequency of 80kHz, and the cleaning time is usually more than 20 minutes.
In addition, in step seven, if the CH in the acid is to be washed 3 COOH is replaced by gluconic acid or citric acid, and the cleaning effect is inferior to that of the present invention, and the layering between the grain boundary and the grain position cannot be eliminated.
The invention has the beneficial effects that:
1. by adopting the method, the invention can achieve a perfect mirror effect after polishing, and the grain boundary and the grain position have no obvious layering sense.
2. The invention has no strict requirement on the area and the density of crystal grains on the surface of the raw material. By adopting the invention, the layering sense between the grain boundary and the grain position can be eliminated by adopting the raw materials of the semiconductor polysilicon material with different grain densities in the actual production and treatment, the finished product effect can meet the mirror effect of market demands, and the production cost is greatly saved.
3. The treatment step of the invention generally does not require additional introduction of new equipment by the producer, nor does it require separate time to re-train the operator with new equipment process training. The production requirements can be met through the step flow after arrangement adjustment and parameter optimization, so the invention has higher practicability.
Drawings
FIG. 1 is a schematic diagram of a surface grain, grain boundary of a conventional polysilicon material;
FIG. 2 is a diagram of an enlarged grain boundary position;
FIG. 3 is a surface physical view of a large grain polysilicon material;
FIG. 4 is a surface physical view of a small grain polysilicon material;
FIG. 5 is a graph of the surface effect of a large grain polysilicon material processed by conventional techniques;
FIG. 6 is a graph of the surface effect of a small grain polysilicon material processed by a conventional process;
FIG. 7 is a graph showing the surface effect of the polysilicon material after the surface treatment method of example 1;
FIG. 8 is a graph showing the surface effect of a processed polysilicon material corresponding to the formulation of the fine cleaning acid of formulation 1;
FIG. 9 is a graph showing the surface effect of a processed polysilicon material corresponding to the formulation of the fine cleaning acid of formulation 2;
FIG. 10 is a graph showing the surface effect of a processed polysilicon material corresponding to the formulation of the fine cleaning acid of formulation 3;
FIG. 11 is a graph showing the surface effect of a processed polysilicon material corresponding to the formulation of the fine cleaning acid of formulation 4;
FIG. 12 is a graph showing the surface effect of a polysilicon material after the surface treatment method of test example 1;
fig. 13 is a graph showing the surface effect of the polysilicon material after the surface treatment method of test example 2 was used.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
1) And machining the semiconductor polycrystalline silicon material to obtain a primary blank.
2) Ultrasonic cleaning is carried out on the surface of the primary blank, firstly alkaline cleaning agent is used for cleaning, then deionized water is used for rinsing, and finally drying is carried out, so that the primary blank after ultrasonic cleaning is obtained; the alkaline cleaning agent is 7.5% potassium hydroxide solution by mass, the temperature is 55+ -2deg.C, the alkaline cleaning agent is cleaned for 5min at 40kHz ultrasonic frequency, and the alkaline cleaning agent is cleaned for 5min at 80kHz ultrasonic frequency. Rinsing with deionized water at 55+ -2deg.C for 2min at 40kHz ultrasonic frequency and for 2min at 80kHz ultrasonic frequency for at least three times. The temperature during drying is 100 ℃, and the drying time is 20min.
3) Pickling the primary blank subjected to primary ultrasonic cleaning by adopting mixed strong acid to obtain a primary pickled primary blank; the mixed strong acid contains HF and HNO 3 The mass fraction of HF in the mixed strong acid is 6.5%, HNO in the mixed strong acid 3 Is 55% by mass; the pickling time is 40s, and the steel is rinsed at least 2 times in deionized water after pickling.
4) Ultrasonic cleaning is carried out on the primary blank after primary acid cleaning, firstly alkaline cleaning agent is used for cleaning, then deionized water is used for rinsing, and finally drying is carried out, so that a secondary ultrasonic cleaned primary blank is obtained; the alkaline cleaning agent is 7.5% potassium hydroxide solution by mass, the temperature is 55+ -2deg.C, the alkaline cleaning agent is cleaned for 5min at 40kHz ultrasonic frequency, and the alkaline cleaning agent is cleaned for 5min at 80kHz ultrasonic frequency. Rinsing with deionized water at 55+ -2deg.C for 2min at 40kHz ultrasonic frequency and for 2min at 80kHz ultrasonic frequency for at least three times. The temperature during drying is 100 ℃, and the drying time is 20min.
5) Grinding the primary blank subjected to the secondary ultrasonic cleaning to obtain a blank; the removal amount of grinding is 50-60 mu m, a double-sided grinding machine is adopted by grinding equipment, cast iron is adopted by a grinding disc, 1200 meshes of alumina is adopted by grinding materials, and the grinding time is 40min.
6) Performing ultrasonic cleaning on the surface of the blank, firstly cleaning with an alkaline cleaning agent, then rinsing with deionized water, and finally drying to obtain the blank subjected to three ultrasonic cleaning; the alkaline cleaning agent is 7.5% potassium hydroxide solution by mass, the temperature is 55+ -2deg.C, the alkaline cleaning agent is cleaned for 5min at 40kHz ultrasonic frequency, and the alkaline cleaning agent is cleaned for 5min at 80kHz ultrasonic frequency. Rinsing with deionized water at 55+ -2deg.C for 2min at 40kHz ultrasonic frequency and for 2min at 80kHz ultrasonic frequency for at least three times. The temperature during drying is 100 ℃, and the drying time is 20min.
7) Carrying out acid washing on the blank subjected to the ultrasonic cleaning for the third time by adopting fine washing acid to obtain a blank subjected to the secondary acid washing; the fine washing acid contains HF and HNO 3 、CH 3 COOH, the mass fraction of HF in the fine washing acid is 1.5%, HNO in the fine washing acid 3 Is 15% by mass of CH in the fine washing acid 3 The mass fraction of COOH is 2.5%, the pickling time is 40s, and the washing is carried out for at least 2 times in deionized water.
8) Ultrasonic cleaning is carried out on the blank subjected to secondary acid cleaning, firstly alkaline cleaning agent is used for cleaning, then deionized water is used for rinsing, and finally drying is carried out, so that the blank subjected to three times of ultrasonic cleaning is obtained; the alkaline cleaning agent is 7.5% potassium hydroxide solution by mass, the temperature is 55+ -2deg.C, the alkaline cleaning agent is cleaned for 5min at 40kHz ultrasonic frequency, and the alkaline cleaning agent is cleaned for 5min at 80kHz ultrasonic frequency. Rinsing with deionized water at 55+ -2deg.C for 2min at 40kHz ultrasonic frequency and for 2min at 80kHz ultrasonic frequency for at least three times. The temperature during drying is 100 ℃, and the drying time is 20min.
9) Performing double-sided mirror polishing on the blank subjected to ultrasonic cleaning for three times to obtain a polished blank; the polishing equipment adopts a CMP mechanochemical double-sided polishing machine, the polishing solution adopts a silicon dioxide polishing solution, the mass fraction of silicon dioxide in the polishing solution is 2%, and the polishing time is 1.5h.
10 And (3) performing ultrasonic cleaning on the polished blank, firstly cleaning with an alkaline cleaning agent, then rinsing with deionized water, and finally drying to obtain a finished product. The alkaline cleaning agent is 7.5% potassium hydroxide solution by mass, the temperature is 55+ -2deg.C, the alkaline cleaning agent is cleaned for 5min at 40kHz ultrasonic frequency, and the alkaline cleaning agent is cleaned for 5min at 80kHz ultrasonic frequency. Rinsing with deionized water at 55+ -2deg.C for 2min at 40kHz ultrasonic frequency and for 2min at 80kHz ultrasonic frequency for at least three times. The temperature during drying is 100 ℃, and the drying time is 20min.
The final product obtained in this example can achieve a very perfect mirror effect without significant layering of grain boundaries and grain locations, as shown in fig. 7.
Example 2
1) And machining the semiconductor polycrystalline silicon material to obtain a primary blank.
2) Ultrasonic cleaning is carried out on the surface of the primary blank, firstly alkaline cleaning agent is used for cleaning, then deionized water is used for rinsing, and finally drying is carried out, so that the primary blank after ultrasonic cleaning is obtained; the alkaline cleaning agent is 10% potassium hydroxide solution by mass, the temperature is 60+/-2 ℃ when the alkaline cleaning agent is used for cleaning, the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 80 kHz. Rinsing with deionized water at 60+ -2deg.C for 2min at 40kHz ultrasonic frequency and for 2min at 80kHz ultrasonic frequency for at least three times. The temperature during drying is 100 ℃, and the drying time is 10min.
3) Pickling the primary blank subjected to primary ultrasonic cleaning by adopting mixed strong acid to obtain a primary pickled primary blank; the mixed strong acid contains HF and HNO 3 The mass fraction of HF in the mixed strong acid is 8%, and HNO in the mixed strong acid 3 Is 50% by mass; the pickling time is 30s, and the steel is rinsed at least 2 times in deionized water after pickling.
4) Ultrasonic cleaning is carried out on the primary blank after primary acid cleaning, firstly alkaline cleaning agent is used for cleaning, then deionized water is used for rinsing, and finally drying is carried out, so that a secondary ultrasonic cleaned primary blank is obtained; the alkaline cleaning agent is 10% potassium hydroxide solution by mass, the temperature is 60+/-2 ℃ when the alkaline cleaning agent is used for cleaning, the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 80 kHz. Rinsing with deionized water at 60+ -2deg.C for 2min at 40kHz ultrasonic frequency and for 2min at 80kHz ultrasonic frequency for at least three times. The temperature during drying is 100 ℃, and the drying time is 20min.
5) Grinding the primary blank subjected to the secondary ultrasonic cleaning to obtain a blank; the removal amount of grinding is 50-60 mu m, a double-sided grinding machine is adopted by grinding equipment, cast iron is adopted by a grinding disc, 1500-mesh alumina is adopted by grinding materials, and the grinding time is 30min.
6) Performing ultrasonic cleaning on the surface of the blank, firstly cleaning with an alkaline cleaning agent, then rinsing with deionized water, and finally drying to obtain the blank subjected to three ultrasonic cleaning; the alkaline cleaning agent is 10% potassium hydroxide solution by mass, the temperature is 60+/-2 ℃ when the alkaline cleaning agent is used for cleaning, the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 80 kHz. Rinsing with deionized water at 60+ -2deg.C for 2min at 40kHz ultrasonic frequency and for 2min at 80kHz ultrasonic frequency for at least three times. The temperature during drying is 100 ℃, and the drying time is 20min.
7) Carrying out acid washing on the blank subjected to the ultrasonic cleaning for the third time by adopting fine washing acid to obtain a blank subjected to the secondary acid washing; the fine washing acid contains HF and HNO 3 、CH 3 COOH, the mass fraction of HF in the fine washing acid is 2%, HNO in the fine washing acid 3 Is 10% by mass of CH in the fine washing acid 3 The mass fraction of COOH is 1%, the pickling time is 60s, and the washing is finished and then the washing is carried out in deionized water for at least 2 times.
8) Ultrasonic cleaning is carried out on the blank subjected to secondary acid cleaning, firstly alkaline cleaning agent is used for cleaning, then deionized water is used for rinsing, and finally drying is carried out, so that the blank subjected to three times of ultrasonic cleaning is obtained; the alkaline cleaning agent is 10% potassium hydroxide solution by mass, the temperature is 60+/-2 ℃ when the alkaline cleaning agent is used for cleaning, the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 80 kHz. Rinsing with deionized water at 60+ -2deg.C for 2min at 40kHz ultrasonic frequency and for 2min at 80kHz ultrasonic frequency for at least three times. The temperature during drying is 100 ℃, and the drying time is 20min.
9) Performing double-sided mirror polishing on the blank subjected to ultrasonic cleaning for three times to obtain a polished blank; the polishing equipment adopts a CMP mechanochemical double-sided polishing machine, the polishing solution adopts a silicon dioxide polishing solution, the mass fraction of silicon dioxide in the polishing solution is 3%, and the polishing time is 1h.
10 And (3) performing ultrasonic cleaning on the polished blank, firstly cleaning with an alkaline cleaning agent, then rinsing with deionized water, and finally drying to obtain a finished product. The alkaline cleaning agent is 10% potassium hydroxide solution by mass, the temperature is 60+/-2 ℃ when the alkaline cleaning agent is used for cleaning, the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 80 kHz. Rinsing with deionized water at 60+ -2deg.C for 2min at 40kHz ultrasonic frequency and for 2min at 80kHz ultrasonic frequency for at least three times. The temperature during drying is 100 ℃, and the drying time is 20min.
Example 3
1) And machining the semiconductor polycrystalline silicon material to obtain a primary blank.
2) Ultrasonic cleaning is carried out on the surface of the primary blank, firstly alkaline cleaning agent is used for cleaning, then deionized water is used for rinsing, and finally drying is carried out, so that the primary blank after ultrasonic cleaning is obtained; the alkaline cleaning agent is potassium hydroxide solution with the mass fraction of 5%, the temperature is 50+/-2 ℃ when the alkaline cleaning agent is used for cleaning, the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 80 kHz. Rinsing with deionized water at 50+ -2deg.C for 2min at 40kHz ultrasonic frequency and for 2min at 80kHz ultrasonic frequency for at least three times. The temperature during drying is 100 ℃, and the drying time is 30min.
3) Pickling the primary blank subjected to primary ultrasonic cleaning by adopting mixed strong acid to obtain a primary pickled primary blank; the mixed strong acid contains HF and HNO 3 The mass fraction of HF in the mixed strong acid is 5%, and HNO in the mixed strong acid 3 Is 60% by mass; the pickling time is 60s, and the steel is rinsed at least 2 times in deionized water after pickling.
4) Ultrasonic cleaning is carried out on the primary blank after primary acid cleaning, firstly alkaline cleaning agent is used for cleaning, then deionized water is used for rinsing, and finally drying is carried out, so that a secondary ultrasonic cleaned primary blank is obtained; the alkaline cleaning agent is potassium hydroxide solution with the mass fraction of 5%, the temperature is 50+/-2 ℃ when the alkaline cleaning agent is used for cleaning, the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 80 kHz. Rinsing with deionized water at 50+ -2deg.C for 2min at 40kHz ultrasonic frequency and for 2min at 80kHz ultrasonic frequency for at least three times. The temperature during drying is 100 ℃, and the drying time is 30min.
5) Grinding the primary blank subjected to the secondary ultrasonic cleaning to obtain a blank; the removal amount of grinding is 50-60 mu m, a double-sided grinding machine is adopted by grinding equipment, cast iron is adopted by a grinding disc, 1000-mesh alumina is adopted by grinding materials, and the grinding time is 60min.
6) Performing ultrasonic cleaning on the surface of the blank, firstly cleaning with an alkaline cleaning agent, then rinsing with deionized water, and finally drying to obtain the blank subjected to three ultrasonic cleaning; the alkaline cleaning agent is potassium hydroxide solution with the mass fraction of 5%, the temperature is 50+/-2 ℃ when the alkaline cleaning agent is used for cleaning, the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 80 kHz. Rinsing with deionized water at 50+ -2deg.C for 2min at 40kHz ultrasonic frequency and for 2min at 80kHz ultrasonic frequency for at least three times. The temperature during drying is 100 ℃, and the drying time is 20min.
7) Carrying out acid washing on the blank subjected to the ultrasonic cleaning for the third time by adopting fine washing acid to obtain a blank subjected to the secondary acid washing; the fine washing acid contains HF and HNO 3 、CH 3 COOH, the mass fraction of HF in the fine washing acid is 1%, HNO in the fine washing acid 3 Is 20% by mass of CH in the fine washing acid 3 The mass fraction of COOH is 5%, the pickling time is 30s, and the washing is finished and then the washing is carried out in deionized water for at least 2 times.
8) Ultrasonic cleaning is carried out on the blank subjected to secondary acid cleaning, firstly alkaline cleaning agent is used for cleaning, then deionized water is used for rinsing, and finally drying is carried out, so that the blank subjected to three times of ultrasonic cleaning is obtained; the alkaline cleaning agent is potassium hydroxide solution with the mass fraction of 5%, the temperature is 50+/-2 ℃ when the alkaline cleaning agent is used for cleaning, the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 80 kHz. Rinsing with deionized water at 50+ -2deg.C for 2min at 40kHz ultrasonic frequency and for 2min at 80kHz ultrasonic frequency for at least three times. The temperature during drying is 100 ℃, and the drying time is 20min.
9) Performing double-sided mirror polishing on the blank subjected to ultrasonic cleaning for three times to obtain a polished blank; the polishing equipment adopts a CMP mechanochemical double-sided polishing machine, the polishing solution adopts a silicon dioxide polishing solution, the mass fraction of silicon dioxide in the polishing solution is 1%, and the polishing time is 2h.
10 And (3) performing ultrasonic cleaning on the polished blank, firstly cleaning with an alkaline cleaning agent, then rinsing with deionized water, and finally drying to obtain a finished product. The alkaline cleaning agent is potassium hydroxide solution with the mass fraction of 5%, the temperature is 50+/-2 ℃ when the alkaline cleaning agent is used for cleaning, the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is used for cleaning for 5min at the ultrasonic frequency of 80 kHz. Rinsing with deionized water at 50+ -2deg.C for 2min at 40kHz ultrasonic frequency and for 2min at 80kHz ultrasonic frequency for at least three times. The temperature during drying is 100 ℃, and the drying time is 20min.
Example 4
For CH contained in the fine washing acid in example 1 3 The ratio of COOH is changed, the rest conditions are unchanged, and the surface effect of the processed final polysilicon material is shown in table 1:
TABLE 1
| HF concentration/% | HNO 3 Concentration/% | CH 3 COOH concentration/% | Surface effect map after processing | |
| Formulation 1 | 1.5 | 15 | 0.1 | See FIG. 8 |
| Formulation 2 | 1.5 | 15 | 1 | See FIG. 9 |
| Formulation 3 | 1.5 | 15 | 5 | See FIG. 10 |
| Formulation 4 | 1.5 | 15 | 10 | See FIG. 11 |
And (3) verifying: HF and HNO 3 Under the condition of unchanged concentration, the concentration of acetic acid is the best at the concentration of 1-5 percent, and the grain boundary on the surface of the mirror surface is hardly seen after final polishing.
Test example 1
In this example, compared with example 1, only CH in the acid was washed 3 COOH is replaced by gluconic acid, the rest conditions are unchanged, and the surface effect of the processed final polysilicon material is shown in fig. 12.
Test example 2
In this example, compared with example 1, only CH in the acid was washed 3 The COOH is replaced by citric acid, the rest conditions are unchanged, and the surface effect of the processed final polysilicon material is shown in fig. 13.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (10)
1. The surface treatment method of the semiconductor polycrystalline silicon material is characterized by comprising the following steps of:
firstly, machining a semiconductor polycrystalline silicon material to obtain a primary blank;
step two, performing ultrasonic cleaning on the surface of the primary blank, firstly cleaning with an alkaline cleaning agent, then rinsing with deionized water, and finally drying to obtain the primary blank subjected to ultrasonic cleaning;
step three, pickling the primary blank subjected to primary ultrasonic cleaning by adopting mixed strong acid to obtain a primary pickled primary blank;
step four, performing ultrasonic cleaning on the primary blank subjected to acid cleaning, firstly cleaning by using an alkaline cleaning agent, then rinsing by using deionized water, and finally drying to obtain a secondary ultrasonic cleaned primary blank;
step five, grinding the primary blank subjected to the secondary ultrasonic cleaning to obtain a blank;
step six, performing ultrasonic cleaning on the surface of the blank, firstly cleaning with an alkaline cleaning agent, then rinsing with deionized water, and finally drying to obtain the blank subjected to three ultrasonic cleaning;
step seven, pickling the blank subjected to ultrasonic cleaning for the third time by adopting fine pickling acid to obtain a blank subjected to secondary pickling;
step eight, performing ultrasonic cleaning on the blank subjected to secondary pickling, firstly cleaning by using an alkaline cleaning agent, then rinsing by using deionized water, and finally drying to obtain the blank subjected to three ultrasonic cleaning;
step nine, performing double-sided mirror polishing on the blank subjected to ultrasonic cleaning for three times to obtain a polished blank;
and step ten, performing ultrasonic cleaning on the polished blank, cleaning with an alkaline cleaning agent, rinsing with deionized water, and finally drying to obtain a finished product.
2. The method for surface treatment of a semiconductor polysilicon material according to claim 1, wherein: in the second step, the alkaline cleaning agent is potassium hydroxide or sodium hydroxide solution with the mass fraction of 5-10%, the temperature is 50-60 ℃ when the alkaline cleaning agent is adopted for cleaning, the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 80 kHz;
rinsing with deionized water for at least three times at 50-60 ℃, rinsing for 2min at 40kHz ultrasonic frequency, and rinsing for 2min at 80kHz ultrasonic frequency;
the temperature is 100 ℃ during drying, and the drying time is 10-30 min;
and/or the number of the groups of groups,
in the fourth step, the alkaline cleaning agent is potassium hydroxide or sodium hydroxide solution with the mass fraction of 5-10%, the temperature is 50-60 ℃ when the alkaline cleaning agent is adopted for cleaning, the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 80 kHz;
rinsing with deionized water for at least three times at 50-60 ℃, rinsing for 2min at 40kHz ultrasonic frequency, and rinsing for 2min at 80kHz ultrasonic frequency;
the temperature is 100 ℃ and the drying time is 10-30 min.
3. The method for surface treatment of a semiconductor polysilicon material according to claim 1, wherein: in step three, the mixed strong acid contains HF and HNO 3 The mass fraction of HF in the mixed strong acid is 5-8%, HNO in the mixed strong acid 3 The mass fraction of (2) is 50-60%; the pickling time is 30-60 s, and the steel is put into deionized water for rinsing at least 2 times after the pickling is completed.
4. The method for surface treatment of a semiconductor polysilicon material according to claim 1, wherein: in the fifth step, the removal amount of grinding is 50-60 mu m, a double-sided grinding machine is adopted as grinding equipment, cast iron is adopted as grinding disc, 1000-1500 meshes of alumina is adopted as grinding material, and the grinding time is 30-60 min.
5. The method for surface treatment of a semiconductor polysilicon material according to claim 1, wherein: in the seventh step, the fine washing acid contains HF and HNO 3 、CH 3 The mass fraction of HF in the refined acid is 1-2%, HNO in the refined acid 3 The mass fraction of (2) is 10-20%, and the CH in the fine washing acid 3 The mass fraction of COOH is 1-5%, the pickling time is 30-60 s, and the pickling is finished and then the solution is put into deionized water for rinsing at least 2 times.
6. The method for surface treatment of a semiconductor polysilicon material according to claim 5, wherein: in step seven, HF, HNO in the acid is washed finely 3 、CH 3 The mass ratio of COOH was 3:30:5.
7. The method for surface treatment of a semiconductor polysilicon material according to claim 1, wherein: in the step nine, the polishing equipment adopts a CMP mechanochemical double-sided polisher, the polishing solution adopts silicon dioxide polishing solution, the mass fraction of silicon dioxide in the polishing solution is 1% -3%, and the polishing time is 1-2 h.
8. The method for surface treatment of a semiconductor polysilicon material according to claim 1, wherein: in the step six, the alkaline cleaning agent is potassium hydroxide or sodium hydroxide solution with the mass fraction of 5-10%, the temperature is 50-60 ℃ when the alkaline cleaning agent is adopted for cleaning, the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 80 kHz;
rinsing with deionized water for at least three times at 50-60 ℃, rinsing for 2min at 40kHz ultrasonic frequency, and rinsing for 2min at 80kHz ultrasonic frequency;
the temperature is 100 ℃ and the drying time is 10-30 min.
9. The method for surface treatment of a semiconductor polysilicon material according to claim 1, wherein: in the step eight, the alkaline cleaning agent is potassium hydroxide or sodium hydroxide solution with the mass fraction of 5-10%, the temperature is 50-60 ℃ when the alkaline cleaning agent is adopted for cleaning, the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 80 kHz;
rinsing with deionized water for at least three times at 50-60 ℃, rinsing for 2min at 40kHz ultrasonic frequency, and rinsing for 2min at 80kHz ultrasonic frequency;
the temperature is 100 ℃ and the drying time is 10-30 min.
10. The method for surface treatment of a semiconductor polysilicon material according to claim 1, wherein: in the step ten, the alkaline cleaning agent is potassium hydroxide or sodium hydroxide solution with the mass fraction of 5-10%, the temperature is 50-60 ℃ when the alkaline cleaning agent is adopted for cleaning, the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 40kHz, and the alkaline cleaning agent is cleaned for 5min at the ultrasonic frequency of 80 kHz;
rinsing with deionized water for at least three times at 50-60 ℃, rinsing for 2min at 40kHz ultrasonic frequency, and rinsing for 2min at 80kHz ultrasonic frequency;
the temperature is 100 ℃ and the drying time is 10-30 min.
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