CN113414890B - Processing method of quartz product for vacuum sealing - Google Patents
Processing method of quartz product for vacuum sealing Download PDFInfo
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- CN113414890B CN113414890B CN202110634594.1A CN202110634594A CN113414890B CN 113414890 B CN113414890 B CN 113414890B CN 202110634594 A CN202110634594 A CN 202110634594A CN 113414890 B CN113414890 B CN 113414890B
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 161
- 239000010453 quartz Substances 0.000 title claims abstract description 157
- 238000007789 sealing Methods 0.000 title claims abstract description 23
- 238000003672 processing method Methods 0.000 title abstract description 11
- 239000012043 crude product Substances 0.000 claims abstract description 67
- 239000000047 product Substances 0.000 claims abstract description 66
- 238000005406 washing Methods 0.000 claims abstract description 66
- 238000004140 cleaning Methods 0.000 claims abstract description 36
- 238000000227 grinding Methods 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 238000005520 cutting process Methods 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 12
- 238000009835 boiling Methods 0.000 claims abstract description 8
- 238000004806 packaging method and process Methods 0.000 claims abstract description 7
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 40
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 40
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 36
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 235000021314 Palmitic acid Nutrition 0.000 claims description 20
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims description 20
- 239000003208 petroleum Substances 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 18
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 16
- 238000010992 reflux Methods 0.000 claims description 16
- 238000002390 rotary evaporation Methods 0.000 claims description 16
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical compound BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 239000012044 organic layer Substances 0.000 claims description 12
- RQTDWDATSAVLOR-UHFFFAOYSA-N 4-[3,5-bis(4-hydroxyphenyl)phenyl]phenol Chemical compound C1=CC(O)=CC=C1C1=CC(C=2C=CC(O)=CC=2)=CC(C=2C=CC(O)=CC=2)=C1 RQTDWDATSAVLOR-UHFFFAOYSA-N 0.000 claims description 10
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical group [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 9
- 229910052740 iodine Inorganic materials 0.000 claims description 9
- 239000011630 iodine Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 8
- 239000012065 filter cake Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 8
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 8
- 239000005457 ice water Substances 0.000 claims description 8
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 8
- 238000003828 vacuum filtration Methods 0.000 claims description 8
- 238000003754 machining Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229940095676 wafer product Drugs 0.000 claims description 6
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052794 bromium Inorganic materials 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- 238000004440 column chromatography Methods 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 239000003480 eluent Substances 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical class [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- 229910021645 metal ion Inorganic materials 0.000 abstract description 8
- 230000003749 cleanliness Effects 0.000 abstract description 5
- 239000000428 dust Substances 0.000 abstract description 5
- 230000002209 hydrophobic effect Effects 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 239000004065 semiconductor Substances 0.000 abstract description 4
- 239000004519 grease Substances 0.000 abstract description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract description 3
- 238000005238 degreasing Methods 0.000 abstract description 2
- 238000005498 polishing Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- 239000003599 detergent Substances 0.000 description 5
- 241000519995 Stachys sylvatica Species 0.000 description 4
- 125000001246 bromo group Chemical group Br* 0.000 description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 150000007942 carboxylates Chemical group 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000012459 cleaning agent Substances 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000007792 addition Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002173 cutting fluid Substances 0.000 description 1
- 239000010730 cutting oil Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28D—WORKING STONE OR STONE-LIKE MATERIALS
- B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
- B28D5/04—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by tools other than rotary type, e.g. reciprocating tools
- B28D5/045—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by tools other than rotary type, e.g. reciprocating tools by cutting with wires or closed-loop blades
-
- 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
- B24B7/00—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor
- B24B7/20—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground
- B24B7/22—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground for grinding inorganic material, e.g. stone, ceramics, porcelain
- B24B7/228—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground for grinding inorganic material, e.g. stone, ceramics, porcelain for grinding thin, brittle parts, e.g. semiconductors, wafers
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/09—Preparation of carboxylic acids or their salts, halides or anhydrides from carboxylic acid esters or lactones
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/30—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
- C07C67/307—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by introduction of halogen; by substitution of halogen atoms by other halogen atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/30—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
- C07C67/31—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by introduction of functional groups containing oxygen only in singly bound form
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/04—Carboxylic acids or salts thereof
- C11D1/06—Ether- or thioether carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/24—Mineral surfaces, e.g. stones, frescoes, plasters, walls or concretes
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Detergent Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a processing method of a quartz product for vacuum sealing, which relates to the field of high-purity quartz processing.A high-purity quartz material is subjected to wire cutting, plane grinding, processing center processing and surface polishing, degreasing cleaning, boiling cleaning, ultrasonic cleaning, chemical cleaning and packaging to obtain the quartz product with good surface appearance state, wherein a key vacuum surface of the quartz product is effectively ensured, the process route is simple, the size precision is high, the quartz product can be manufactured in batches, and the requirements of equipment in the current semiconductor industry can be met; according to the processing method, the quartz crude product is placed in washing liquid for chemical cleaning, the washing liquid is prepared by dissolving a washing auxiliary agent in water, the molecules of the washing auxiliary agent are of a molecular structure with four benzene rings and three hydrophobic long chains, the surface activity is high, grease, dust and metal ions can be separated from the surface of the quartz crude product and enter water, and the surface of the quartz product is sufficiently washed and high in cleanliness.
Description
Technical Field
The invention relates to the field of high-purity quartz processing, in particular to a processing method of a quartz product for vacuum sealing.
Background
The oxygen and the silicon are combined in nature to form silicon oxide, including silica sand and colorless crystals, which are mined and smelted into quartz, and then manufactured into a final quartz product;
the quartz material has the characteristics of high hardness and frangibility, so quartz processing is always a difficult point in the industry, the quartz product processed in the industry at present has low dimensional precision and a rough surface state, and oil stains, dust and metal ions are easy to adhere to the quartz product in the production process, so that the requirement of the semiconductor industry is difficult to meet;
in view of the above technical drawbacks, a solution is proposed.
Disclosure of Invention
In order to overcome the technical problems described above, the present invention aims to provide a method for processing a vacuum-sealed quartz product, comprising: clamping a quartz round ingot on a wire cutting machine, cutting to form a quartz round wafer, performing plane grinding processing on the quartz round wafer, performing processing center processing after the plane grinding of the quartz round wafer, performing cleaning processing after the processing of the quartz round wafer, performing precision grinding processing after the quartz round wafer is cleaned, placing a quartz round wafer product subjected to precision grinding processing in a processing center according to product characteristics to finish machining to meet the product size requirement, performing mechanical grinding processing on one surface for vacuum sealing on a machine tool to obtain a quartz crude product, placing the quartz crude product in a dewaxing tank and a boiling tank for cleaning, placing the quartz crude product in an ultrasonic cleaning tank for ultrasonic cleaning, adding a cleaning assistant into clear water to prepare into cleaning solution, placing the quartz crude product in the cleaning solution for cleaning, performing final detection on the quartz crude product, and using the cleaning solution again after the quartz crude product is qualified, and then the quartz is cleaned by pure water, so that the problems that the existing quartz product is low in size precision and relatively rough in surface state, oil stains, dust and metal ions are easy to adhere to the quartz product in the production process, and the requirement of the semiconductor industry is difficult to meet are solved.
The purpose of the invention can be realized by the following technical scheme:
a method of processing a quartz product for vacuum sealing, comprising the steps of:
the method comprises the following steps: clamping a quartz round ingot on a wire cutting machine, cutting to form a quartz round ingot, wherein wire cutting ensures that the consumption of raw materials is reduced and the cut surface is smooth, and the next procedure can be performed without grinding assistance;
step two: carrying out plane grinding on the quartz wafer to ensure that the flatness and parallelism requirements are within 0.05 mm;
step three: after the plane of the quartz wafer is ground, machining center machining is carried out, the characteristics of a part of products are roughly machined, and a single side is left for the allowance of 4-6 mm;
step four: after being processed by a quartz wafer processing center, the quartz wafer processing center is cleaned and used for removing cutting fluid on the surface of a product and ensuring the clean circulation of the product;
step five: after being cleaned, the quartz wafer is subjected to precision grinding processing, so that the surface roughness of the product is ensured to meet the requirement;
step six: placing the quartz wafer product subjected to precision grinding processing in a processing center for finish machining according to product characteristics to meet the product size requirement, and performing mechanical grinding processing on one surface for vacuum sealing on a machine tool to ensure that the surface has no undesirable phenomena of tool marks, scratches and cracks to obtain a quartz crude product;
step seven: putting the quartz crude product in a dewaxing tank and a boiling tank, respectively cleaning for 20-30min, and removing cutting oil and product attached impurities;
step eight: placing the quartz crude product in an ultrasonic cleaning tank, and ultrasonically cleaning for 20-30min to remove product impurities;
step nine: adding a washing assistant into clear water to prepare washing liquid with the molar concentration of 0.05-0.5mol/L, and washing the quartz crude product in the washing liquid for 30-50min to remove metal ions and impurities;
step ten: and finally detecting the quartz crude product, washing the quartz crude product for 20-30min by using washing liquid after the quartz crude product is qualified, then washing the quartz crude product by using pure water to ensure the cleanliness of the product, drying the cleaned quartz crude product, finally packaging and warehousing the dried quartz crude product to obtain the quartz product for vacuum sealing.
As a further scheme of the invention: the preparation process of the washing assistant is as follows:
s1: adding palmitic acid into a three-neck flask provided with a reflux condenser pipe and a stirrer, moving the three-neck flask into a water bath kettle, completely melting the palmitic acid at 65-70 ℃, dropwise adding thionyl chloride into the three-neck flask, controlling the dropwise adding time to be 2-3h, leading out generated sulfur dioxide and hydrogen chloride gas, absorbing the generated hydrogen dioxide and hydrogen chloride gas by using a sodium hydroxide solution, continuing to perform constant-temperature reaction for 30-50min after dropwise adding, then adding a catalyst under the condition of heating to 85-90 ℃, dropwise adding liquid bromine at the stirring speed of 100-200r/min, controlling the dropwise adding time to be 6-7h, continuing to perform constant-temperature reaction for 1h after dropwise adding, then cooling to 50-60 ℃, dropwise adding anhydrous methanol, controlling the dropwise adding time to be 1-2h, and refluxing for 2-4h after dropwise adding, after the reaction is finished, cooling the product to room temperature, adding a saturated sodium sulfite solution to remove excessive bromine, then distilling under reduced pressure to remove excessive methanol, standing for layering, separating an organic layer, washing with distilled water for 3-5 times, then adding anhydrous magnesium sulfate for drying, and then distilling under reduced pressure to obtain an intermediate 1;
the reaction principle is as follows:
s2: adding 1, 3, 5-tri (4-hydroxyphenyl) benzene and N, N-dimethylformamide into a three-neck flask, adding anhydrous potassium carbonate under the protection of nitrogen, then adding the intermediate 1 solution at one time when the temperature is raised to 60 ℃, reacting at constant temperature for 2-3h, then raising the temperature to 80-90 ℃, continuing to react for 20-30h, cooling to room temperature after the reaction is finished, carrying out vacuum filtration, carrying out reduced pressure rotary evaporation on the filtrate to remove N, N-dimethylformamide, adding the rotary evaporation product into a separating funnel, adding petroleum ether, adding ice water, washing an organic layer for 3-4 times, separating the organic layer, drying with anhydrous magnesium sulfate, performing reduced pressure rotary evaporation to remove the petroleum ether, performing column chromatography separation on a rotary evaporation product, starting using the petroleum ether as an eluent, and then using the petroleum ether and ethyl acetate according to a volume ratio of 10: 1 to obtain an intermediate 2;
the reaction principle is as follows:
s3: adding the intermediate 2, sodium hydroxide and absolute ethyl alcohol a into a flask provided with a reflux condenser tube, refluxing for 10-15h at the temperature of 80-90 ℃, centrifuging a reaction product after the reaction is finished, carrying out vacuum filtration, washing a filter cake for 3-5 times by using absolute ethyl alcohol b, then placing the filter cake in a vacuum drying oven, and drying to constant weight at the temperature of 55-65 ℃ to obtain a washing auxiliary agent;
the reaction principle is as follows:
the method comprises the steps of placing a quartz crude product into washing liquid for chemical cleaning, wherein the washing liquid is prepared by dissolving a washing assistant in water, reacting palmitic acid, thionyl chloride and liquid bromine under the catalysis of an iodine simple substance to enable bromine atoms to substitute hydrogen atoms on the palmitic acid to generate carboxylic acid containing bromine atoms, then carrying out esterification reaction on the carboxylic acid and anhydrous methanol to generate an intermediate 1, carrying out substitution reaction on the intermediate 1 and 1, 3, 5-tri (4-hydroxyphenyl) benzene to generate an intermediate 2, and carrying out reaction on the intermediate 2 and sodium hydroxide to generate the washing assistant, so that a molecular structure with four benzene rings and three hydrophobic long chains is formed, the hydrophobic performance of the washing assistant is enhanced, and higher surface activity can be generated, therefore, stains such as grease, dust and the like can be wrapped on the surface of the quartz crude product and can enter water after being separated from the surface of the quartz crude product, the washing assistant is also in a carboxylate structure and has negative charges after being ionized in water, can be complexed with metal ions, so that the metal ions are also separated from the surface of the crude quartz product, and the crude quartz product has the advantages of sufficient surface washing and high cleanliness.
As a further scheme of the invention: in the step S1, the dosage ratio of the palmitic acid, the thionyl chloride, the liquid bromine and the anhydrous methanol is 0.58 mol: 0.80 mol: 0.73 mol: 80mL, wherein the catalyst is an iodine simple substance, and the dosage of the iodine simple substance is 5-10% of the total weight of the palmitic acid and the thionyl chloride.
As a further scheme of the invention: the using amount ratio of the 1, 3, 5-tris (4-hydroxyphenyl) benzene, N-dimethylformamide, anhydrous potassium carbonate, intermediate 1 solution, petroleum ether and ice water in step S2 was 0.027 mol: 100mL of: 30g of: 50mL of: 60mL of: 80mL of the intermediate 1 solution is intermediate 1, and the molar ratio of the intermediate 1 is 0.100 mol: 50mL of the aqueous solution was dissolved in N, N-dimethylformamide.
As a further scheme of the invention: the using ratio of the intermediate 2, the sodium hydroxide and the absolute ethyl alcohol a in the step S3 is 0.023 mol: 0.077 mol: 100 mL.
The invention has the beneficial effects that:
the invention relates to a processing method of a quartz product for vacuum sealing, which comprises the steps of clamping a quartz round ingot on a wire cutting machine, cutting to form a quartz wafer, carrying out plane grinding processing on the quartz wafer, carrying out processing center processing after the plane grinding of the quartz wafer, carrying out cleaning processing after the processing of the quartz wafer, carrying out precision grinding processing after the quartz wafer is cleaned, placing the quartz wafer product after the precision grinding processing in a processing center for finish machining according to the product characteristics to meet the product size requirement, carrying out mechanical grinding processing on the surface for vacuum sealing on a machine tool to obtain a quartz crude product, placing the quartz crude product in a dewaxing tank and a boiling tank for cleaning, placing the quartz crude product in an ultrasonic cleaning tank for ultrasonic cleaning, adding a cleaning assistant into clear water to prepare a cleaning solution, placing the quartz crude product in the cleaning solution for cleaning, carrying out final detection on the quartz crude product, washing the quartz crude product with washing liquid again after the quartz crude product is qualified, then washing the quartz crude product with pure water, drying the cleaned quartz crude product, and finally packaging and warehousing the quartz crude product to obtain the quartz product for vacuum sealing; the quartz material used by the processing method is a high-purity quartz material, and is processed by wire cutting, plane grinding, processing center processing and surface polishing, degreasing and cleaning, boiling and cleaning, ultrasonic cleaning, chemical cleaning and packaging, the quartz product processed by the processing method has good surface appearance state, the key vacuum surface of the quartz product is effectively ensured, the process route is simple, the size precision is high, batch manufacturing can be realized, and the requirements of equipment in the current semiconductor industry can be met;
in the processing method, a quartz crude product is placed in a washing liquid for chemical cleaning, the washing liquid is prepared by dissolving a washing assistant in water, palmitic acid, thionyl chloride and liquid bromine react under the catalysis of a simple substance of iodine, so that hydrogen atoms on the palmitic acid are replaced by bromine atoms to generate carboxylic acid containing bromine atoms, then the carboxylic acid is esterified with anhydrous methanol to generate an intermediate 1, then the intermediate 1 is replaced by 1, 3, 5-tri (4-hydroxyphenyl) benzene to generate an intermediate 2, the intermediate 2 is reacted with sodium hydroxide to generate the washing assistant, thereby forming a molecular structure of four benzene rings and three hydrophobic long chains, enhancing the hydrophobic property of the molecular structure, generating higher surface activity, and therefore, stains such as grease, dust and the like can be wrapped on the surface of the quartz crude product and enter water after being separated from the surface of the quartz crude product, and the washing assistant is also in a carboxylate structure, the quartz crude product has negative charge after ionization in water and can be complexed with metal ions, so that the metal ions are also separated from the surface of the quartz crude product, and the surface of the quartz crude product is sufficiently washed, and the cleanliness is high.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
this example is a detergent builder, and the preparation process of the detergent builder is specifically as follows:
s1: adding palmitic acid into a three-neck flask provided with a reflux condenser pipe and a stirrer, moving the three-neck flask into a water bath kettle, completely melting the palmitic acid under the condition of 65 ℃, dropwise adding thionyl chloride into the three-neck flask, controlling the dropwise adding time to be 2 hours, leading out generated sulfur dioxide and hydrogen chloride gas, absorbing the generated sulfur dioxide and hydrogen chloride gas by using a sodium hydroxide solution, continuing to perform constant-temperature reaction for 30 minutes after the dropwise adding is finished, then heating to 85 ℃, adding a catalyst, dropwise adding liquid bromine under the condition of stirring speed of 100r/min, controlling the dropwise adding time to be 6 hours, continuing to perform constant-temperature reaction for 1 hour after the dropwise adding is finished, then cooling to 50 ℃, dropwise adding anhydrous methanol, controlling the dropwise adding time to be 1 hour, refluxing for 2 hours after the dropwise adding is finished, cooling the product to room temperature after the reaction is finished, then adding a saturated sodium sulfite solution to remove excessive bromine, then, carrying out reduced pressure distillation to remove excessive methanol, standing for layering, separating an organic layer, washing with distilled water for 3 times, adding anhydrous magnesium sulfate for drying, and then carrying out reduced pressure distillation to obtain an intermediate 1; controlling the dosage ratio of palmitic acid, thionyl chloride, liquid bromine and absolute methanol to be 0.58 mol: 0.80 mol: 0.73 mol: 80mL, wherein the catalyst is an iodine simple substance, and the dosage of the iodine simple substance is 5% of the total weight of the palmitic acid and the thionyl chloride;
s2: adding 1, 3, 5-tri (4-hydroxyphenyl) benzene and N, N-dimethylformamide into a three-neck flask, adding anhydrous potassium carbonate under the protection of nitrogen, then adding the intermediate 1 solution at one time when the temperature is raised to 60 ℃, reacting at constant temperature for 2-3h, then raising the temperature to 80 ℃, continuing to react for 20h, cooling to room temperature after the reaction is finished, carrying out vacuum filtration, carrying out reduced pressure rotary evaporation on the filtrate to remove N, N-dimethylformamide, adding the rotary evaporation product into a separating funnel, adding petroleum ether, adding ice water, washing an organic layer for 3-4 times, separating the organic layer, drying with anhydrous magnesium sulfate, performing reduced pressure rotary evaporation to remove the petroleum ether, performing column chromatography separation on a rotary evaporation product, starting using the petroleum ether as an eluent, and then using the petroleum ether and ethyl acetate according to a volume ratio of 10: 1 to obtain an intermediate 2; controlling the dosage ratio of 1, 3, 5-tri (4-hydroxyphenyl) benzene, N-dimethylformamide, anhydrous potassium carbonate, the intermediate 1 solution, petroleum ether and ice water to be 0.027 mol: 100mL of: 30g of: 50mL of: 60mL of: 80mL of intermediate 1 solution as intermediate 1 according to 0.100 mol: 50mL of solution formed by dissolving the materials in N, N-dimethylformamide;
s3: adding the intermediate 2, sodium hydroxide and absolute ethyl alcohol a into a flask provided with a reflux condenser tube, refluxing for 10 hours at the temperature of 80 ℃, centrifuging a reaction product after the reaction is finished, carrying out vacuum filtration, washing a filter cake for 3 times by using absolute ethyl alcohol b, then placing the filter cake into a vacuum drying oven, and drying to constant weight at the temperature of 55 ℃ to obtain a washing assistant; controlling the dosage ratio of the intermediate 2, sodium hydroxide and absolute ethyl alcohol a to be 0.023 mol: 0.077 mol: 100 mL.
Example 2:
this example is a detergent builder, and the preparation process of the detergent builder is specifically as follows:
s1: adding palmitic acid into a three-neck flask provided with a reflux condenser pipe and a stirrer, moving the three-neck flask into a water bath kettle, completely melting the palmitic acid at the temperature of 70 ℃, dropwise adding thionyl chloride into the three-neck flask, controlling the dropwise adding time to be 3h, leading out generated sulfur dioxide and hydrogen chloride gas, absorbing the sulfur dioxide and hydrogen chloride gas by using a sodium hydroxide solution, continuing to perform constant-temperature reaction for 50min after the dropwise adding is finished, then heating to 90 ℃, adding a catalyst, dropwise adding liquid bromine at the stirring speed of 200r/min, controlling the dropwise adding time to be 7h, continuing to perform constant-temperature reaction for 1h after the dropwise adding is finished, then cooling to 60 ℃, dropwise adding anhydrous methanol, controlling the dropwise adding time to be 2h, refluxing for 4h after the dropwise adding is finished, cooling the product to room temperature after the reaction is finished, and then adding a saturated sodium sulfite solution to remove excessive bromine, then, carrying out reduced pressure distillation to remove excessive methanol, standing for layering, separating an organic layer, washing with distilled water for 5 times, adding anhydrous magnesium sulfate for drying, and then carrying out reduced pressure distillation to obtain an intermediate 1; controlling the dosage ratio of palmitic acid, thionyl chloride, liquid bromine and absolute methanol to be 0.58 mol: 0.80 mol: 0.73 mol: 80mL, wherein the catalyst is an iodine simple substance, and the dosage of the iodine simple substance is 10% of the total weight of the palmitic acid and the thionyl chloride;
s2: adding 1, 3, 5-tris (4-hydroxyphenyl) benzene and N, N-dimethylformamide into a three-neck flask, adding anhydrous potassium carbonate under the condition of introducing nitrogen for protection, then heating to 60 ℃, adding an intermediate 1 solution at one time, reacting at constant temperature for 3 hours, heating to 90 ℃, continuing to react for 30 hours, cooling to room temperature after the reaction is finished, carrying out vacuum filtration, carrying out reduced pressure rotary evaporation on the filtrate to remove the N, N-dimethylformamide, adding the rotary evaporation product into a separating funnel, adding petroleum ether firstly, adding ice water, washing an organic layer for 4 times, separating the organic layer, drying with anhydrous magnesium sulfate, carrying out reduced pressure rotary evaporation to remove the petroleum ether, carrying out column chromatography separation on the rotary evaporation product, starting using the petroleum ether as an eluent, and then using the petroleum ether and ethyl acetate according to the volume ratio of 10: 1 to obtain an intermediate 2; controlling the dosage ratio of 1, 3, 5-tri (4-hydroxyphenyl) benzene, N-dimethylformamide, anhydrous potassium carbonate, the intermediate 1 solution, petroleum ether and ice water to be 0.027 mol: 100mL of: 30g of: 50mL of: 60mL of: 80mL of intermediate 1 solution as intermediate 1 according to 0.100 mol: 50mL of solution formed by dissolving the materials in N, N-dimethylformamide;
s3: adding the intermediate 2, sodium hydroxide and absolute ethyl alcohol a into a flask provided with a reflux condenser tube, refluxing for 15h at the temperature of 90 ℃, centrifuging a reaction product after the reaction is finished, carrying out vacuum filtration, washing a filter cake for 5 times by using absolute ethyl alcohol b, then placing the filter cake into a vacuum drying oven, and drying to constant weight at the temperature of 65 ℃ to obtain a washing assistant; controlling the dosage ratio of the intermediate 2, sodium hydroxide and absolute ethyl alcohol a to be 0.023 mol: 0.077 mol: 100 mL.
Example 3:
the embodiment is a processing method of a quartz product for vacuum sealing, which comprises the following steps:
the method comprises the following steps: clamping a quartz round ingot on a linear cutting machine, and cutting to form a quartz round wafer;
step two: carrying out plane grinding processing on the quartz wafer;
step three: processing by a processing center after grinding the plane of the quartz wafer;
step four: cleaning after processing by a quartz wafer processing center;
step five: after being cleaned, the quartz wafer is subjected to precision grinding processing;
step six: placing the quartz wafer product subjected to precision grinding processing in a processing center for finish machining according to product characteristics to meet the product size requirement, and performing mechanical grinding processing on the surface for vacuum sealing on a machine tool to obtain a quartz crude product;
step seven: putting the quartz crude product in a dewaxing tank and a boiling tank, and cleaning for 20min respectively;
step eight: placing the quartz crude product in an ultrasonic cleaning tank for ultrasonic cleaning for 20 min;
step nine: adding the washing assistant from example 1 into clean water to prepare washing liquid with the molar concentration of 0.05mol/L, and placing the quartz crude product into the washing liquid for washing for 30 min;
step ten: and finally detecting the quartz crude product, washing the quartz crude product for 20min by using a washing solution after the quartz crude product is qualified, then washing the quartz crude product by using pure water, drying the cleaned quartz crude product, and finally packaging and warehousing the quartz crude product to obtain the quartz product for vacuum sealing.
Example 4:
the embodiment is a processing method of a quartz product for vacuum sealing, comprising the following steps:
the method comprises the following steps: clamping a quartz round ingot on a linear cutting machine, and cutting to form a quartz round wafer;
step two: carrying out plane grinding processing on the quartz wafer;
step three: processing by a processing center after grinding the plane of the quartz wafer;
step four: cleaning after processing by a quartz wafer processing center;
step five: after being cleaned, the quartz wafer is subjected to precision grinding processing;
step six: placing the quartz wafer product subjected to precision grinding processing in a processing center for finish machining according to product characteristics to meet the product size requirement, and performing mechanical grinding processing on the surface for vacuum sealing on a machine tool to obtain a quartz crude product;
step seven: putting the quartz crude product in a dewaxing tank and a boiling tank, and cleaning for 30min respectively;
step eight: placing the quartz crude product in an ultrasonic cleaning tank for ultrasonic cleaning for 30 min;
step nine: adding the washing assistant from example 2 into clean water to prepare washing liquid with the molar concentration of 0.5mol/L, and placing the quartz crude product into the washing liquid for washing for 50 min;
step ten: and finally detecting the quartz crude product, washing the quartz crude product for 30min by using a washing solution after the quartz crude product is qualified, then washing the quartz crude product by using pure water, drying the cleaned quartz crude product, and finally packaging and warehousing the quartz crude product to obtain the quartz product for vacuum sealing.
Comparative example 1:
comparative example 1 differs from example 4 in that washing with a washing liquid was not conducted.
Comparative example 2:
comparative example 2 differs from example 4 in that the detergent used was a quartz crystal piece cleaning agent supplied under application No. CN 201510290690.3.
The cleanliness of the quartz products of the examples 3-4 and the comparative examples 1-2 is detected, the stain adhesion condition on the surface of the quartz product is visually observed by a 4X 10 times microscope, the watermark residue condition on the surface of the quartz product is visually detected under a black bottom spotlight, and the detection results are shown in the following table;
sample (I) | Stain attachment | Watermark remaining situation |
Example 3 | No dirt and small white spot | No watermark residue |
Example 4 | No dirt and small white spot | No watermark residue |
Comparative example 1 | Has more dirty and small white spots | Multiple watermark residual |
Comparative example 2 | Has little dirt and white spots | Few no watermarks |
From the above table detection results, it can be seen that there are many stains attached to the surface of the quartz product cleaned without using the cleaning solution, and after drying, there are watermarks, which proves that there are many stains remaining, and when the quartz crystal wafer cleaning agent is used as the cleaning solution, the stains attached to the surface of the quartz product can be effectively removed, but the cleaning effect of the cleaning solution provided in the present invention is still not as good, which indicates that the cleaning solution provided in the present invention has high dirt removing ability, and can simultaneously remove a variety of stains.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (4)
1. A method of processing a quartz product for vacuum sealing, comprising the steps of:
the method comprises the following steps: clamping a quartz round ingot on a linear cutting machine, and cutting to form a quartz round wafer;
step two: carrying out plane grinding processing on the quartz wafer;
step three: processing by a processing center after grinding the plane of the quartz wafer;
step four: cleaning after processing by a quartz wafer processing center;
step five: after being cleaned, the quartz wafer is subjected to precision grinding processing;
step six: placing the quartz wafer product subjected to precision grinding processing in a processing center for finish machining according to product characteristics to meet the product size requirement, and performing mechanical grinding processing on the surface for vacuum sealing on a machine tool to obtain a quartz crude product;
step seven: putting the quartz crude product in a dewaxing tank and a boiling tank, and respectively cleaning for 20-30 min;
step eight: placing the quartz crude product in an ultrasonic cleaning tank, and ultrasonically cleaning for 20-30 min;
step nine:
s1: adding palmitic acid into a three-neck flask provided with a reflux condenser pipe and a stirrer, moving the three-neck flask into a water bath kettle, completely melting the palmitic acid at 65-70 ℃, dropwise adding thionyl chloride into the three-neck flask, controlling the dropwise adding time to be 2-3h, leading out generated sulfur dioxide and hydrogen chloride gas, absorbing the generated hydrogen dioxide and hydrogen chloride gas by using a sodium hydroxide solution, continuing to perform constant-temperature reaction for 30-50min after dropwise adding, then adding a catalyst under the condition of heating to 85-90 ℃, dropwise adding liquid bromine at the stirring speed of 100-200r/min, controlling the dropwise adding time to be 6-7h, continuing to perform constant-temperature reaction for 1h after dropwise adding, then cooling to 50-60 ℃, dropwise adding anhydrous methanol, controlling the dropwise adding time to be 1-2h, and refluxing for 2-4h after dropwise adding, after the reaction is finished, cooling the product to room temperature, adding a saturated sodium sulfite solution to remove excessive bromine, then distilling under reduced pressure to remove excessive methanol, standing for layering, separating an organic layer, washing with distilled water for 3-5 times, then adding anhydrous magnesium sulfate for drying, and then distilling under reduced pressure to obtain an intermediate 1;
s2: adding 1, 3, 5-tri (4-hydroxyphenyl) benzene and N, N-dimethylformamide into a three-neck flask, adding anhydrous potassium carbonate under the protection of nitrogen, then adding the intermediate 1 solution at one time when the temperature is raised to 60 ℃, reacting at constant temperature for 2-3h, then raising the temperature to 80-90 ℃, continuing to react for 20-30h, cooling to room temperature after the reaction is finished, carrying out vacuum filtration, carrying out reduced pressure rotary evaporation on the filtrate to remove N, N-dimethylformamide, adding the rotary evaporation product into a separating funnel, adding petroleum ether, adding ice water, washing an organic layer for 3-4 times, separating the organic layer, drying with anhydrous magnesium sulfate, performing reduced pressure rotary evaporation to remove the petroleum ether, performing column chromatography separation on a rotary evaporation product, starting using the petroleum ether as an eluent, and then using the petroleum ether and ethyl acetate according to a volume ratio of 10: 1 to obtain an intermediate 2;
s3: adding the intermediate 2, sodium hydroxide and absolute ethyl alcohol a into a flask provided with a reflux condenser tube, refluxing for 10-15h at the temperature of 80-90 ℃, centrifuging a reaction product after the reaction is finished, carrying out vacuum filtration, washing a filter cake for 3-5 times by using absolute ethyl alcohol b, then placing the filter cake in a vacuum drying oven, and drying to constant weight at the temperature of 55-65 ℃ to obtain a washing auxiliary agent;
s4: adding a washing assistant into clear water to prepare washing liquid with the molar concentration of 0.05-0.5mol/L, and placing the quartz crude product into the washing liquid for washing for 30-50 min;
step ten: and finally detecting the quartz crude product, washing the quartz crude product for 20-30min by using a washing solution after the quartz crude product is qualified, then washing the quartz crude product by using pure water, drying the cleaned quartz crude product, and finally packaging and warehousing the quartz crude product to obtain the quartz product for vacuum sealing.
2. The method for processing a quartz product for vacuum sealing according to claim 1, wherein the amount ratio of palmitic acid, thionyl chloride, liquid bromine, and anhydrous methanol in step S1 is 0.58 mol: 0.80 mol: 0.73 mol: 80mL, wherein the catalyst is an iodine simple substance, and the dosage of the iodine simple substance is 5-10% of the total weight of the palmitic acid and the thionyl chloride.
3. The method for processing a quartz product for vacuum sealing according to claim 1, wherein the amount ratio of 1, 3, 5-tris (4-hydroxyphenyl) benzene, N-dimethylformamide, anhydrous potassium carbonate, intermediate 1 solution, petroleum ether, ice water in step S2 is 0.027 mol: 100mL of: 30g of: 50mL of: 60mL of: 80mL of the intermediate 1 solution is intermediate 1, and the molar ratio of the intermediate 1 is 0.100 mol: 50mL of the aqueous solution was dissolved in N, N-dimethylformamide.
4. The method for processing a quartz product for vacuum sealing according to claim 1, wherein the intermediate 2, sodium hydroxide and absolute ethyl alcohol a in the step S3 are used in an amount ratio of 0.023 mol: 0.077 mol: 100 mL.
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