CN113213736A - Processing method for prolonging service life of quartz product for LPCVD (low pressure chemical vapor deposition) process - Google Patents
Processing method for prolonging service life of quartz product for LPCVD (low pressure chemical vapor deposition) process Download PDFInfo
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- 239000010453 quartz Substances 0.000 title claims abstract description 153
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 153
- 238000000034 method Methods 0.000 title claims abstract description 49
- 238000004518 low pressure chemical vapour deposition Methods 0.000 title claims abstract description 32
- 238000003672 processing method Methods 0.000 title claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 25
- 239000000126 substance Substances 0.000 claims abstract description 22
- 238000003486 chemical etching Methods 0.000 claims abstract description 19
- 238000005488 sandblasting Methods 0.000 claims abstract description 18
- 238000000137 annealing Methods 0.000 claims abstract description 14
- 238000005498 polishing Methods 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 18
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 230000002378 acidificating effect Effects 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000012459 cleaning agent Substances 0.000 claims description 12
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 12
- 239000011043 treated quartz Substances 0.000 claims description 10
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 6
- 235000019253 formic acid Nutrition 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 230000000873 masking effect Effects 0.000 claims description 4
- 239000002390 adhesive tape Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 150000003377 silicon compounds Chemical class 0.000 abstract description 6
- 238000004381 surface treatment Methods 0.000 abstract description 2
- 239000013618 particulate matter Substances 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 15
- 229910052710 silicon Inorganic materials 0.000 description 15
- 239000010703 silicon Substances 0.000 description 15
- 235000012431 wafers Nutrition 0.000 description 15
- 239000002245 particle Substances 0.000 description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- 238000005530 etching Methods 0.000 description 6
- 238000000151 deposition Methods 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000004576 sand Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 238000012993 chemical processing Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B29/00—Reheating glass products for softening or fusing their surfaces; Fire-polishing; Fusing of margins
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/001—General methods for coating; Devices therefor
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
- C03C23/0075—Cleaning of glass
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling compositions
- C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
- C09K13/08—Etching, surface-brightening or pickling compositions containing an inorganic acid containing a fluorine compound
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention belongs to the technical field of surface treatment of quartz parts for the photovoltaic industry, and particularly relates to a processing method for prolonging the service life of the surface of a quartz product for an LPCVD (low pressure chemical vapor deposition) process. The method comprises the steps of fire polishing, annealing, shielding, sand blasting, shielding object removing, first cleaning, acid chemical solution preparation, chemical etching, second cleaning and the like. The quartz product prepared by the LPCVD process has uniform hilly surfaces, improves the adhesiveness of the silicon compound to the quartz product, does not cause the stripping of the silicon compound deposited on the quartz product, reduces particle pollution, prolongs the service life of the quartz product, and meets the requirements of the photovoltaic industry.
Description
Technical Field
The invention belongs to the technical field of surface treatment of quartz parts for the photovoltaic industry, and particularly relates to a processing method for prolonging the service life of the surface of a quartz product for an LPCVD (low pressure chemical vapor deposition) process.
Background
In integrated circuit processes, LPCVD furnaces are often used to perform chemical vapor deposition processes to produce PN junctions required by the photovoltaic industry. Quartz products (tubes, muffle tubes, boats, doors, trays, etc.) are often used in LPCVD processes because of their superior properties of high temperature resistance, low thermal expansion coefficient, excellent light transmission, good electrical insulation, corrosion resistance, etc.
Most of the known quartz products are made of quartz after fire polishing, as shown in fig. 1, a cross-sectional view of the quartz surface processed by fire polishing is shown, fire polishing is to directly heat the quartz surface by flame (oxyhydrogen flame), and the surface is melted without deformation to form a transparent state, however, as a long-term LPCVD process is performed, a silicon compound layer is deposited on the quartz tube surface, when the silicon compound layer is accumulated to a certain thickness, since the quartz tube surface after fire polishing is smooth, the adhesion is not enough, and the silicon compound layer is easily deposited on the thicker part deposited on the top of the quartz tube, or on the turning part of the quartz tube surface, cracks are generated or a block of particles are formed, when the particles are peeled off, the silicon wafer is contaminated, the yield of the silicon wafer is greatly reduced, and more seriously, because the silicon compound layer is adhered to the peripheral wall of the quartz tube, the quartz tube is broken due to the fact that the temperature is increased and decreased violently, the thermal expansion coefficient and the internal stress are different, and the quartz tube is scrapped in advance.
The surface modification of quartz tubes is known as sand blasting. The sand blasting carries diamond grinding sand grains to impact the surface of the quartz by utilizing high-speed airflow, so that the quartz generates a hill-shaped surface, and the hill-shaped surface formed on the quartz surface after sand blasting can be used for adsorbing and keeping the attachment of deposits. FIG. 2 shows a cross-sectional view of a grit blasted quartz surface. However, the shape of the quartz product used in the photovoltaic industry is complex, some surfaces cannot be directly contacted by sand grains in the sand blasting process, so that the force, the wind speed and the distance of sand blasting are difficult to control, and the inner wall surface of the quartz product is inconsistent with the initial hill shape, so that the hill shape on the sand blasting surface is uneven, and the hill-shaped peak is too sharp, so that the deposition layer is easy to break and peel at the peak, thereby forming particles and influencing the yield of silicon wafers.
As shown in FIG. 3, a cross-sectional view of a quartz surface is chemically processed, and the quartz surface is etched by chemical processing, and an acidic chemical solution is formed by mixing hydrofluoric acid, ammonium fluoride and acetic acid in a certain ratio, so that the quartz surface is in a hill shape and can be used for adsorbing and keeping deposits attached. However, the inner wall surface of the quartz product is not consistent with the initial hilly shape, which causes uneven hilly shape of the surface after chemical etching, and part of hilly parts are too smooth, so that the deposition layer is easy to peel off at the smooth part, and the yield of the silicon wafer is affected.
In the known LPCVD process in the photovoltaic industry, it is generally required that the thickness and quality of the film growth on the surfaces of all silicon wafers in the same LPCVD furnace are kept as consistent as possible, that is, the process gas on the surfaces of the silicon wafers is uniformly distributed in the LPCVD furnace, and then if there are more silicon wafers placed in the LPCVD furnace, the length of the gas inlet pipe for the process gas in the opposite LPCVD furnace is required to be longer, so that the flow rate of the process gas into the LPCVD furnace is difficult to keep consistent, and therefore, the process gas distribution on the surfaces of the silicon wafers at different positions on the quartz boat is not uniform, and the film-forming thickness among the silicon wafers is not uniform. Therefore, the present inventors have observed the above-mentioned disadvantages and have come to the present invention by considering the need to improve the bonding strength between the quartz surface and the deposited layer and to improve the uniformity of the film thickness between silicon wafers.
Disclosure of Invention
In order to solve the above problems, the present invention provides a processing method for prolonging the service life of a quartz product for an LPCVD process, which can improve the bonding strength between the surface of the quartz product and a deposition layer, increase the surface area of the quartz product, further improve the yield of silicon wafers, and improve the uniformity of the film thickness between silicon wafers.
In order to achieve the purpose, the invention adopts the following technical scheme.
A processing method for prolonging the service life of quartz products for LPCVD process comprises the following steps.
Step 1, fire polishing: the quartz product for LPCVD process is fire polished to make its surface state consistent.
Step 2, annealing: and (3) placing the quartz product into an annealing furnace, raising the temperature to 1050-1125 ℃, keeping the temperature for 40-50 minutes, and then gradually cooling to room temperature to eliminate the internal stress of the quartz product so that the quartz product cannot be naturally cracked.
Step 3, shielding: the quartz product non-reaction surface is completely shielded by a shielding object.
Step 4, sand blasting: the quartz product is sandblasted to form a hilly surface on the unmasked portion of the quartz product surface, wherein the hilly surface has a plurality of sharp peaks.
Step 5, removing the shielding object: and removing the shielding matter covering the surface of the quartz product.
Step 6, first cleaning: the quartz product is cleaned by a cleaning agent, so that the fragile part of the hill-shaped surface is firstly removed by cleaning, and the particle part on the surface of the quartz product can be removed.
And 7, preparing an acidic chemical solution.
Step 8, chemical etching: the acid chemical solution is supplied to the surface of the quartz product for chemical etching, so that the hill-shaped surface is more uniform and smooth.
And 9, second cleaning: the quartz product was washed with pure water.
And step 10, detecting the roughness of the surface of the treated quartz component.
Further, in step 1, the quartz products for LPCVD process include quartz tube, quartz furnace core tube, quartz boat, quartz furnace door, quartz bracket, etc.
Further, in the step 2, the cooling temperature is room temperature.
Further, in step 3, the shielding object is an adhesive tape.
Further, in the step 6, the cleaning agent is an ultrasonic cleaning agent.
Further, in the steps 6 and 9, the cleaning time is 8-15 minutes, the ultrasonic power is 900, and the frequency (khz) is 28.
Further, in the step 7, the acidic chemical solution is composed of, by mass, 1 to 10 parts of hydrofluoric acid, 5 to 25 parts of deionized water, 25 to 35 parts of ammonium fluoride, 40 to 50 parts of formic acid, and 0.1 to 5 parts of citric acid.
Further, in the step 8, the acid chemical solution may be sprayed, completely precipitated, or completely soaked to chemically etch the surface of the quartz product, preferably in a spraying manner.
Further, in the step 8, the chemical etching time is 10-120 minutes, and the temperature is 20-45 ℃.
The Ra value of the surface of the quartz product is controlled by adjusting the chemical etching time to form a uniform and hilly surface. The surface average Ra value of the quartz product is adjusted to 0.5-8.0 μm. And the peak part of the hill-shaped surface is more rounded, as shown in fig. 4, the cross-sectional view of the quartz product prepared by the invention is shown.
Compared with the prior art, the invention has the beneficial effect that.
(1) The invention firstly leads the surface state of the quartz product to be consistent through the fire polishing step, then leads the unmasked part of the surface to form a hill-shaped surface through the sand blasting, and finally leads the hill-shaped surface to be more uniform and smooth through the chemical etching step, thereby leading the surface of the quartz product to be tightly and stably combined with the deposition layer, reducing the generation of particles in the process, not only having the defects of peak and crack formed by the sand blasting method, but also having the defects of uneven surface and over smooth part of surface formed by the known chemical method, prolonging the service life of the quartz product and improving the yield of silicon wafers.
(2) Because the hill-shaped surface is mainly formed on the reaction surface of the quartz product, more processing gas can be adsorbed on the surface in the process of forming the film, so that the concentration of the gas adsorbed by the silicon wafers arranged on the quartz product is more consistent, and the uniformity of the film forming thickness among the silicon wafers can be improved.
Drawings
FIG. 1 is a cross-sectional view of a fire polished quartz surface.
FIG. 2 is a cross-sectional view of a grit blasted quartz surface.
FIG. 3 is a cross-sectional view of a chemically machined quartz surface.
FIG. 4 is a cross-sectional view of a quartz surface formed by the steps of the present invention.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation. It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the invention.
A processing method for prolonging the service life of the surface of a quartz product used in an LPCVD process comprises the following steps.
Step 1, fire polishing: the quartz product for LPCVD process is fire polished to make its surface state consistent.
Step 2, annealing: and (3) placing the quartz product into an annealing furnace, raising the temperature to 1050-1125 ℃, keeping the temperature for 40-50 minutes, and then gradually cooling to room temperature to eliminate the internal stress of the quartz product so that the quartz product cannot be naturally cracked.
Step 3, shielding: the quartz product non-reaction surface is completely shielded by a shielding object.
Step 4, sand blasting: the quartz product is sandblasted to form a hilly surface on the unmasked portion of the quartz product surface, wherein the hilly surface has a plurality of sharp peaks.
Step 5, removing the shielding object: and removing the shielding matter covering the surface of the quartz product.
Step 6, first cleaning: the quartz product is cleaned by a cleaning agent, so that the fragile part of the hill-shaped surface is firstly removed by cleaning, and the particle part on the surface of the quartz product can be removed.
And 7, preparing an acidic chemical solution.
Step 8, chemical etching: the acid chemical solution is supplied to the surface of the quartz product for chemical etching, so that the hill-shaped surface is more uniform and smooth.
And 9, second cleaning: the quartz product was washed with pure water.
And step 10, detecting the roughness of the surface of the treated quartz component, wherein the treated quartz surface is shown as figure 4.
Further, in step 1, the quartz products for LPCVD process include quartz tube, quartz furnace core tube, quartz boat, quartz furnace door, quartz bracket, etc.
Further, in the step 2, the cooling temperature is room temperature.
Further, in step 3, the shielding object is an adhesive tape.
Further, in the step 6, the cleaning agent is an ultrasonic cleaning agent.
Further, in the steps 6 and 9, the cleaning time is 8-15 minutes, the ultrasonic power is 900, and the frequency (khz) is 28.
Further, in the step 7, the acidic chemical solution is composed of, by mass, 1 to 10 parts of hydrofluoric acid, 5 to 25 parts of deionized water, 25 to 35 parts of ammonium fluoride, 40 to 50 parts of formic acid, and 0.1 to 5 parts of citric acid.
Further, in the step 8, the acid chemical solution may be sprayed, completely precipitated, or completely soaked to chemically etch the surface of the quartz product, preferably in a spraying manner.
Further, in the step 8, the chemical etching time is 10-120 minutes, and the temperature is 20-45 ℃.
Example 1.
Step 1, fire polishing: the quartz product for LPCVD process is fire polished to make its surface state consistent.
Step 2, annealing: and (3) placing the quartz product into an annealing furnace, raising the temperature to 1125 ℃, keeping the temperature for 45 minutes, and gradually cooling to room temperature to eliminate the internal stress of the quartz product so that the quartz product cannot be naturally cracked.
Step 3, shielding: the quartz product non-reaction surface is completely shielded by a plurality of shielding matter masking paper.
Step 4, sand blasting: the quartz product is sandblasted to form a hilly surface on the unmasked portion of the quartz product surface, wherein the hilly surface has a plurality of sharp peaks.
Step 5, removing the shielding object: and removing the shielding matter covering the surface of the quartz product.
Step 6, first cleaning: the quartz product was cleaned with an ultrasonic cleaning agent for 10 minutes at an ultrasonic power of 900 and a frequency (khz) of 28. So that the weaker part of the hilly surface is removed by cleaning, and the particle part on the surface of the quartz product can be removed.
And 7, mixing 5 parts of hydrofluoric acid, 20 parts of deionized water, 30 parts of ammonium fluoride, 40 parts of formic acid and 5 parts of citric acid to prepare the acidic chemical solution.
Step 8, chemical etching: and (3) supplying an acidic chemical solution to the surface of the quartz product by adopting a complete precipitation method for chemical etching, wherein the etching temperature is 24 ℃ and the etching time is 60 minutes, so that the hilly surface is uniform and smooth.
And 9, second cleaning: the quartz product was cleaned with pure water for 10 minutes at an ultrasonic power of 900 and a frequency (khz) of 28.
And step 10, detecting the roughness of the surface of the treated quartz component, wherein the roughness Ra = 2.2.
Example 2.
Step 1, fire polishing: the quartz product for LPCVD process is fire polished to make its surface state consistent.
Step 2, annealing: and (3) placing the quartz product into an annealing furnace, raising the temperature to 1125 ℃, keeping the temperature for 45 minutes, and gradually cooling to room temperature to eliminate the internal stress of the quartz product so that the quartz product cannot be naturally cracked.
Step 3, shielding: the quartz product non-reaction surface is completely shielded by a plurality of shielding matter masking paper.
Step 4, sand blasting: the quartz product is sandblasted to form a hilly surface on the unmasked portion of the quartz product surface, wherein the hilly surface has a plurality of sharp peaks.
Step 5, removing the shielding object: and removing the shielding matter covering the surface of the quartz product.
Step 6, first cleaning: the quartz product was cleaned with an ultrasonic cleaning agent for 10 minutes at an ultrasonic power of 900 and a frequency (khz) of 28. So that the weaker part of the hilly surface is removed by cleaning, and the particle part on the surface of the quartz product can be removed.
And 7, mixing 5 parts of hydrofluoric acid, 10 parts of deionized water, 32 parts of ammonium fluoride, 49 parts of formic acid and 4 parts of citric acid to prepare an acidic chemical solution.
Step 8, chemical etching: and (3) supplying an acidic chemical solution to the surface of the quartz product by adopting a complete precipitation method for chemical etching, wherein the etching temperature is 24 ℃ and the etching time is 60 minutes, so that the hilly surface is uniform and smooth.
And 9, second cleaning: the quartz product was cleaned with pure water for 10 minutes at an ultrasonic power of 900 and a frequency (khz) of 28.
And step 10, detecting the roughness of the surface of the treated quartz component, wherein the roughness Ra = 2.5.
Example 3.
Step 1, fire polishing: the quartz product for LPCVD process is fire polished to make its surface state consistent.
Step 2, annealing: and (3) placing the quartz product into an annealing furnace, raising the temperature to 1125 ℃, keeping the temperature for 45 minutes, and gradually cooling to room temperature to eliminate the internal stress of the quartz product so that the quartz product cannot be naturally cracked.
Step 3, shielding: the quartz product non-reaction surface is completely shielded by a plurality of shielding matter masking paper.
Step 4, sand blasting: the quartz product is sandblasted to form a hilly surface on the unmasked portion of the quartz product surface, wherein the hilly surface has a plurality of sharp peaks.
Step 5, removing the shielding object: and removing the shielding matter covering the surface of the quartz product.
Step 6, first cleaning: the quartz product was cleaned with an ultrasonic cleaning agent for 10 minutes at an ultrasonic power of 900 and a frequency (khz) of 28. So that the weaker part of the hilly surface is removed by cleaning, and the particle part on the surface of the quartz product can be removed.
And 7, mixing 5 parts of hydrofluoric acid, 10 parts of deionized water, 32 parts of ammonium fluoride, 49 parts of formic acid and 4 parts of citric acid to prepare an acidic chemical solution.
Step 8, chemical etching: and supplying an acid chemical solution to the surface of the quartz product by a complete precipitation method for chemical etching, wherein the etching temperature is 24 ℃ and the etching time is 120 minutes, so that the hilly surface is uniform and smooth.
And 9, second cleaning: the quartz product was cleaned with pure water for 10 minutes at an ultrasonic power of 900 and a frequency (khz) of 28.
And step 10, detecting the roughness of the surface of the treated quartz component, wherein the roughness Ra = 3.8.
Comparative example 1.
The sand blasting method is to form high-speed blasting beams by using compressed air as power, and to spray diamond grinding sand grains to the surface of quartz to be treated at high speed, so that the appearance of the quartz surface is physically changed, and the quartz is provided with a sharp mountain peak-shaped surface. The roughness of the treated surface of the quartz member was measured, and the roughness Ra = 13.
Comparative example 2.
Performing surface polishing and annealing treatment on a quartz component to be treated, cleaning the surface of the treated quartz component by using deionized water, mixing analytically pure hydrofluoric acid with the solution concentration of 40% and solid analytically pure ammonium fluoride with the solution concentration of 99%, and adding analytically pure acetic acid with the solution concentration of 99.5% to prepare a treatment solution for later use, wherein the addition mass ratio of the components is as follows: hydrofluoric acid: ammonium fluoride: acetic acid 3:5: 9; raising the temperature of the treated solution to 33 ℃, and mechanically stirring for 62 min; taking out the treated quartz component, and washing for 15 min; the roughness Ra of the surface of the treated quartz member was measured to be 3.8.
Table 1 table of test results of examples and comparative examples.
The method of the invention has the advantages that the surface of the quartz product has no sharp peaks, microcracks and particle deposition, the hilly state is uniform, and the roughness meets the requirement; the surface of the quartz product manufactured by the sand blasting method has sharp peaks and microcracks, and the roughness does not meet the requirement. Although the surface roughness of the quartz product manufactured by the chemical method meets the requirement, the quartz product has uneven hilly shape, and part of hilly parts are too smooth.
Claims (10)
1. A processing method for prolonging the service life of a quartz product for an LPCVD process is characterized by comprising the following steps:
step 1, fire polishing: carrying out fire polishing on the quartz product for the LPCVD process;
step 2, annealing: placing the quartz product into an annealing furnace, heating to 1050-1125 ℃, keeping for 40-50 minutes, and gradually cooling to room temperature;
step 3, shielding: shielding the non-reaction surface of the quartz product by using a shielding object;
step 4, sand blasting: sand blasting is carried out on the quartz product;
step 5, removing the shielding object: removing the shielding matter covering the surface of the quartz product;
step 6, first cleaning: cleaning the quartz product with a cleaning agent;
step 7, preparing an acidic chemical solution;
step 8, chemical etching: supplying an acid chemical solution to the surface of the quartz product to perform chemical etching;
and 9, second cleaning: cleaning the quartz product with pure water;
and step 10, detecting the roughness of the surface of the treated quartz component.
2. The method as claimed in claim 1, wherein the quartz product for LPCVD process comprises quartz tube, quartz muffle tube, quartz boat, quartz furnace door, quartz bracket, etc. in step 1.
3. The method of claim 1, wherein the cooling temperature in step 2 is room temperature.
4. The method of claim 1, wherein in step 3, the masking material is an adhesive tape.
5. The method as claimed in claim 1, wherein in step 6, the cleaning agent is an ultrasonic cleaning agent.
6. The method as claimed in claim 1, wherein in steps 6 and 9, the cleaning time is 8-15 minutes, the ultrasonic power is 900, and the frequency is 28 khz.
7. The processing method for prolonging the service life of a quartz product for LPCVD process according to claim 1, wherein in step 7, the acidic chemical solution is composed of, by mass, 1-10 parts of hydrofluoric acid, 5-25 parts of deionized water, 25-35 parts of ammonium fluoride, 40-50 parts of formic acid, and 0.1-5 parts of citric acid.
8. The method as claimed in claim 1, wherein in step 8, the acidic chemical solution is sprayed, deposited completely or soaked completely to etch the surface of the quartz product.
9. The method as claimed in claim 1, wherein the chemical etching time in step 8 is 10-120 min and the temperature is 20-45 ℃.
10. The method according to claim 1, wherein the average Ra value of the surface of the final quartz product is adjusted to 0.5-8.0 μm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110509441.4A CN113213736A (en) | 2021-05-11 | 2021-05-11 | Processing method for prolonging service life of quartz product for LPCVD (low pressure chemical vapor deposition) process |
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| CN111112212A (en) * | 2019-11-29 | 2020-05-08 | 上海富乐德智能科技发展有限公司 | Quartz thermal screen plate regeneration method for integrated circuit manufacturing |
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