CN109277357B - Cleaning method suitable for ceramic parts with surface attachments - Google Patents
Cleaning method suitable for ceramic parts with surface attachments Download PDFInfo
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- CN109277357B CN109277357B CN201810945499.1A CN201810945499A CN109277357B CN 109277357 B CN109277357 B CN 109277357B CN 201810945499 A CN201810945499 A CN 201810945499A CN 109277357 B CN109277357 B CN 109277357B
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- soaking
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- 238000004140 cleaning Methods 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000000919 ceramic Substances 0.000 title claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 76
- 229910001868 water Inorganic materials 0.000 claims abstract description 50
- 238000001035 drying Methods 0.000 claims abstract description 27
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000002791 soaking Methods 0.000 claims abstract description 26
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 24
- 230000010355 oscillation Effects 0.000 claims abstract description 20
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 15
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000012360 testing method Methods 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 12
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 claims abstract description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000005201 scrubbing Methods 0.000 claims abstract description 7
- SWXQKHHHCFXQJF-UHFFFAOYSA-N azane;hydrogen peroxide Chemical compound [NH4+].[O-]O SWXQKHHHCFXQJF-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 230000010356 wave oscillation Effects 0.000 claims description 9
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 3
- 239000012498 ultrapure water Substances 0.000 claims description 3
- 238000011179 visual inspection Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims 6
- 230000000996 additive effect Effects 0.000 claims 6
- 230000006835 compression Effects 0.000 claims 1
- 238000007906 compression Methods 0.000 claims 1
- 239000012535 impurity Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 101100107923 Vitis labrusca AMAT gene Proteins 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- -1 deionized Water Chemical compound 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- B08B1/143—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B13/00—Accessories or details of general applicability for machines or apparatus for cleaning
-
- 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
- B08B3/02—Cleaning by the force of jets or sprays
-
- 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
Abstract
The invention discloses a cleaning method suitable for ceramic parts with surface attachments, which comprises the following steps: s1, chemical cleaning: soaking the workpiece by using an ammonia hydrogen peroxide solution with the volume ratio of H2O2：H2O：NH4OH ═ 2.5-3.5: (3.5-4.5): (0.5-1.5); s2, rinsing with pure water; s3, carrying out neutralization reaction by using hydrofluoric/nitric acid, wherein the hydrofluoric/nitric acid is prepared by mixing nitric acid and hydrofluoric acid, and the volume ratio of each solution is HNO3：HF：H2O ═ 17 to 23: (0.5-1.5): (17-23); s4, scrubbing; s5, soaking the workpiece in DI Water for more than 10 minutes at normal temperature; s6, testing the pH value of the surface of the workpiece; s7, ultrasonic oscillation cleaning; s8, testing the pH value of the surface of the workpiece; s9, drying by CDA; s10, ultrasonic oscillation cleaning; s11, heating and drying; and S12, naturally cooling.
Description
Technical Field
The invention discloses a method for cleaning a ceramic part, in particular to a method suitable for cleaning a ceramic part with surface attachments, and belongs to the technical field of special cleaning.
Background
Isolator Ring in AMAT eMax CT + parts, isolator Ring in AMAT DPS parts: the surfaces of Ceramic Lid, Gas Injector, Ion Port and screen Cover Ring are Ceramic as surface attachments, and after long-time use, the surface of a workpiece is inevitably attached with impurities, so that the workpiece is required to be cleaned regularly, the body of the workpiece is Ceramic, the surface is metal attachments (aluminum/photoresist), the impurities on the surface of the workpiece cannot be well removed by conventional workpiece surface cleaning means, and the cleaning effect is poor.
Disclosure of Invention
Aiming at the defect that the effect of removing impurities on the surface of a workpiece by using ceramic parts as attachments is poor in the prior art, the invention provides the cleaning method suitable for removing the impurities on the surface of the workpiece by using the ceramic parts as the attachments, which adopts a mode of combining chemical soaking and ultrasonic oscillation cleaning and can simply and quickly remove the impurities on the surface of the workpiece.
The technical scheme adopted by the invention for solving the technical problems is as follows: a cleaning method suitable for ceramic parts with surface attachments comprises the following steps:
s1, chemical cleaning: soaking the workpiece by using an ammonia hydrogen peroxide solution with the volume ratio of H2O2：H2O：NH4OH = (2.5-3.5): (3.5-4.5): (0.5-1.5), adopting ultrapure water with the resistivity more than or equal to 12M omega.CM, soaking the workpiece at the temperature of 5 ℃ plus or minus 5 ℃, reacting for 3-5 hours, and observing once every half hour until no residual film is left on the surface of the workpiece by visual inspection;
s2, rinsing with pure water: fishing out the workpiece processed in the step S1, and soaking and washing the workpiece in flowing pure water for more than 30 minutes;
s3, carrying out neutralization reaction by using hydrofluoric/nitric acid, wherein the hydrofluoric/nitric acid is prepared by mixing nitric acid and hydrofluoric acid, and the volume ratio of each solution is HNO3：HF：H2O=（17~23）：（0.5~1.5）：（17~23）；
S4, scrubbing: scrubbing a workpiece in DI Water by using dust-free cloth;
s5, soaking the workpiece in DI Water for more than 10 minutes at normal temperature;
s6, workpiece surface pH test: testing the pH value of the residual water on the surface of the workpiece if the pH value is higher than the preset value
If the pH value is less than 6 or more than 7, returning to the step S5, and soaking and cleaning again;
s7, ultrasonic oscillation cleaning: putting the components into a DI Water tank with ultrasonic waves, performing ultrasonic wave oscillation cleaning for more than 30 minutes, performing ultrasonic wave oscillation cleaning by adopting the ultrasonic waves with the effective power of 1.2Kw, and continuously introducing deionized Water into an ultrasonic cleaning tank during the ultrasonic wave oscillation cleaning to keep the Water in the Water tank overflowing continuously from the upper surface of the Water tank;
s8, workpiece surface pH test: testing the pH value of the residual water on the surface of the workpiece, if the pH value meets 6-7, switching to the next procedure, and if the pH value is less than 6 or more than 7, returning to the step S7, and soaking and cleaning again;
s9, CDA drying: drying the surface of the workpiece by using CDA filtered by a 0.1-micrometer filter;
s10, ultrasonic oscillation cleaning: cleaning in a workshop without a vehicle, putting the parts into a DI Water tank with ultrasonic waves, performing ultrasonic oscillation cleaning for more than 5 minutes, performing ultrasonic oscillation cleaning by adopting the ultrasonic waves with the effective power of 1.2Kw, and continuously introducing deionized Water into an ultrasonic cleaning tank during the ultrasonic oscillation cleaning to keep the Water in the Water tank overflowing continuously from the upper surface of the Water tank;
s11, heating and drying: baking, heating and drying the product by using an oven, wherein the drying temperature is 150 +/-10 ℃, and the drying time is more than 1H;
s12, natural cooling: and naturally cooling the heated and dried workpiece to room temperature.
The technical scheme adopted by the invention for solving the technical problem further comprises the following steps:
in the step S1, H2O2：H2O：NH4OH=3：4：1。
In step S2, pure water having a resistivity of 12M Ω · cm or more is used as the pure water.
In the step S3, hydrofluoric/nitric acid is HNO3：HF：H2O = 20: 1: and 20, carrying out soaking reaction at normal temperature for 10-30S.
In step S5, the DI Water resistivity is 5M Ω · cm or more, and the pH: 6-7.
In the step S9, the pressure of the compressed air is 2kgf/cm2The drying temperature is 100 +/-5 ℃, and the drying time is more than 30 minutes.
In step S10, the dust-free workshop is a 1000-level dust-free workshop.
The invention has the beneficial effects that: the invention adopts a mode of combining chemical soaking and ultrasonic oscillation cleaning, can simply and quickly remove impurities on the surface of the workpiece, and has small damage to the workpiece.
Detailed Description
The present embodiment is a preferred embodiment of the present invention, and other principles and basic structures that are the same as or similar to the present embodiment are within the scope of the present invention.
The invention mainly relates to a cleaning method suitable for ceramic parts with surface attachments, which comprises the following steps:
s1, chemical cleaning: in this embodiment, the workpiece is soaked with the ammonia hydrogen peroxide solution, and when soaking, the hydrogen peroxide solution submerges the workpiece, that is, the workpiece is ensured to be completely soaked in the hydrogen peroxide solution2O2：H2O：NH4OH = (2.5-3.5): (3.5-4.5): (0.5-1.5), preferably, H2O2：H2O：NH4OH = 3: 4: 1, in the embodiment, the adopted water is ultrapure water with the resistivity greater than or equal to 12 MOmega CM, the soaking temperature is 45 +/-5 ℃, the reaction time is 3-5 hours until no titanium film or titanium nitride film remains on the surface of the workpiece is observed visually, if the parent metal of the workpiece is Ti, the observation is carried out once every half hour, in the embodiment, the hydrogen peroxide adopts the hydrogen peroxide with the concentration of 30-32% by mass on the market, and the ammonia water adopts the ammonia water with the concentration of 25% by mass on the market;
in this embodiment, when the concentration of hydrogen peroxide in the mixed solution is less than 5%, the soaking solution needs to be replaced, and when replacing the liquid, a special measuring tool needs to be adopted to measure, and when replacing the liquid medicine, relevant recording work needs to be done, and the user needs to pay attention to the light and light placement so as to avoid unnecessary loss.
S2, rinsing with pure water: fishing out the workpiece processed in step S1, and adding flowing pure water (resistivity of
Pure water of more than 12M omega cm) for more than 30 minutes to remove the chemical liquid remained on the surface of the workpiece;
s3, carrying out a neutralization reaction by using hydrofluoric/nitric acid, wherein the hydrofluoric/nitric acid is prepared by mixing nitric acid and hydrofluoric acid at a volume ratio of HNO3：HF：H2O = (17 to 23): (0.5-1.5): (17-23), preferably HNO3：HF：H2O = 20: 1: 20, in the embodiment, the reaction is a soaking reaction at a normal temperature, and the reaction time is 10 to 30S, in the embodiment, the nitric acid is a commercially available concentrated nitric acid with a mass percentage concentration of 68%, in the specific implementation, nitric acids with other concentrations can be used for carrying out equivalent proportioning, in the embodiment, the hydrofluoric acid is a commercially available hydrofluoric acid with a mass percentage concentration of 55%, and in the specific implementation, nitric acids with other concentrations can be used for carrying out equivalent proportioning;
in this embodiment, when nitric acid concentration is less than 10%, need to change the hydrofluoric acid solution, when changing liquid, need adopt special measuring tool to measure and get, need do relevant record work when changing liquid medicine, pay attention to gently take to put to avoid causing unnecessary loss.
S4, scrubbing: scrubbing a workpiece in DI Water (namely deionized Water, the resistivity of the deionized Water is more than 5M omega cm, the pH value is 6-7) by adopting dust-free cloth, wherein in the embodiment, the dust-free cloth adopts 7447# industrial scouring pad;
s5, soaking the workpiece in DI Water (namely deionized Water, the resistivity of which is more than 5M omega cm, and the pH value is 6-7) at normal temperature for 10 minutes;
s6, workpiece surface pH test: testing the pH value of the residual water on the surface of the workpiece, if the pH value meets 6-7, switching to the next procedure, and if the pH value is less than 6 or more than 7, returning to the step S5, and soaking and cleaning again;
s7, ultrasonic oscillation cleaning: putting the product into a DI Water (namely deionized Water with the resistivity of more than 5M omega cm and the pH value of 6-7) tank with ultrasonic waves, and carrying out ultrasonic oscillation cleaning for 30 minutes, wherein in the embodiment, the ultrasonic waves with the effective power of 1.2Kw are adopted for ultrasonic oscillation cleaning to remove residual granular substances on the surface of a workpiece, and the deionized Water is continuously introduced into an ultrasonic cleaning tank during ultrasonic oscillation cleaning to keep the Water in the tank overflowing from the upper surface of the tank continuously so as to take away the oscillated granular substances;
s8, workpiece surface pH test: testing the pH value of the residual water on the surface of the workpiece if the pH value is higher than the preset value
If the pH value is less than 6 or greater than 7, the process returns to step S7,
soaking and cleaning again;
s9, CDA drying: drying the surface of the workpiece by CDA (oil and water removing compressed air) filtered by a 0.1 mu m filter, wherein the pressure of the compressed air is 2kgf/cm2The drying temperature is 100 +/-5 ℃, the drying time is more than 30 minutes, and residual moisture on the surface can be removed;
s10, ultrasonic oscillation cleaning: the cleaning is carried out in a non-vehicle workshop (in the embodiment, a 1000-grade non-dust workshop is adopted in the non-dust workshop), the parts are put into a DI Water tank (namely deionized Water with the resistivity of more than 5M omega cm and the pH value of 6-7) with ultrasonic waves, ultrasonic wave oscillation cleaning is carried out for 5 minutes, in the embodiment, the ultrasonic waves with the effective power of 1.2Kw are adopted for ultrasonic wave oscillation cleaning to remove residual particle substances on the surface of a workpiece, the deionized Water is continuously introduced into an ultrasonic cleaning tank during the ultrasonic wave oscillation cleaning, and the Water in the Water tank continuously overflows from the upper surface of the Water tank to take away the oscillated particle substances.
S11, heating and drying: and baking, heating and drying the product by using an oven, wherein the drying temperature is 150 +/-10 ℃, the drying time is more than 1H, and the product is isolated even if the products are not contacted with each other, so that incomplete drying is prevented.
S12, natural cooling: and naturally cooling the heated and dried workpiece to room temperature.
The invention adopts a mode of combining chemical soaking and ultrasonic oscillation cleaning, can simply and quickly remove impurities on the surface of the workpiece, and has small damage to the workpiece.
Claims (7)
1. A cleaning method suitable for ceramic parts with surface attachments is characterized by comprising the following steps: the method comprises the following steps:
s1, chemical cleaning: soaking the workpiece by using an ammonia hydrogen peroxide solution with the volume ratio of H2O2：H2O：NH4OH = (2.5-3.5): (3.5-4.5): (0.5-1.5), adopting ultrapure water with the resistivity more than or equal to 12M omega.CM, soaking at 45 +/-5 ℃, reacting for 3-5 hours, and observing once every half hour until no residual film is on the surface of the workpiece by visual inspection;
s2, rinsing with pure water: fishing out the workpiece processed in the step S1, and soaking and washing the workpiece in flowing pure water for more than 30 minutes;
s3, carrying out neutralization reaction by using hydrofluoric/nitric acid, wherein the hydrofluoric/nitric acid is prepared by mixing nitric acid and hydrofluoric acid, and the volume ratio of each solution is HNO3：HF：H2O=（17~23）：（0.5~1.5）：（17~23）；
S4, scrubbing: scrubbing a workpiece in DI Water by using dust-free cloth;
s5, soaking the workpiece in DI Water for more than 10 minutes at normal temperature;
s6, workpiece surface pH test: testing the pH value of the residual water on the surface of the workpiece if the pH value is higher than the preset value
If the pH value is less than 6 or more than 7, returning to the step S5, and soaking and cleaning again;
s7, ultrasonic oscillation cleaning: putting the components into a DI Water tank with ultrasonic waves, performing ultrasonic wave oscillation cleaning for more than 30 minutes, performing ultrasonic wave oscillation cleaning by adopting the ultrasonic waves with the effective power of 1.2Kw, and continuously introducing deionized Water into an ultrasonic cleaning tank during the ultrasonic wave oscillation cleaning to keep the Water in the Water tank overflowing continuously from the upper surface of the Water tank;
s8, workpiece surface pH test: testing the pH value of the residual water on the surface of the workpiece, if the pH value meets 6-7, switching to the next procedure, and if the pH value is less than 6 or more than 7, returning to the step S7, and soaking and cleaning again;
s9, CDA drying: drying the surface of the workpiece by using CDA filtered by a 0.1-micrometer filter;
s10, ultrasonic oscillation cleaning: cleaning in a workshop without a vehicle, putting the parts into a DI Water tank with ultrasonic waves, performing ultrasonic oscillation cleaning for more than 5 minutes, performing ultrasonic oscillation cleaning by adopting the ultrasonic waves with the effective power of 1.2Kw, and continuously introducing deionized Water into an ultrasonic cleaning tank during the ultrasonic oscillation cleaning to keep the Water in the Water tank overflowing continuously from the upper surface of the Water tank;
s11, heating and drying: baking, heating and drying the product by using an oven, wherein the drying temperature is 150 +/-10 ℃, and the drying time is more than 1H;
s12, natural cooling: and naturally cooling the heated and dried workpiece to room temperature.
2. The method according to claim 1, wherein the cleaning method is a method for cleaning a ceramic part with a surface additive comprising: in the step S1, H2O2：H2O：NH4OH=3：4：1。
3. The method according to claim 1, wherein the cleaning method is a method for cleaning a ceramic part with a surface additive comprising: in step S2, pure water having a resistivity of 12M Ω · cm or more is used as the pure water.
4. The method according to claim 1, wherein the cleaning method is a method for cleaning a ceramic part with a surface additive comprising: in the step S3, hydrofluoric/nitric acid is HNO3：HF：H2O = 20: 1: and 20, carrying out soaking reaction at normal temperature for 10-30S.
5. The method according to claim 1, wherein the cleaning method is a method for cleaning a ceramic part with a surface additive comprising: in step S5, the DI Water resistivity is 5M Ω · cm or more, and the pH: 6-7.
6. The method according to claim 1, wherein the cleaning method is a method for cleaning a ceramic part with a surface additive comprising: in the step S9, the compression is performedThe pressure of air was 2kgf/cm2The drying temperature is 100 +/-5 ℃, and the drying time is more than 30 minutes.
7. The method according to claim 1, wherein the cleaning method is a method for cleaning a ceramic part with a surface additive comprising: in step S10, the dust-free workshop is a 1000-level dust-free workshop.
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| CN111534825B (en) * | 2020-05-14 | 2022-05-31 | 富乐德科技发展（大连）有限公司 | Process for removing titanium and titanium nitride deposited film of stainless steel part of semiconductor equipment |
| CN112553630A (en) * | 2020-12-02 | 2021-03-26 | 江苏凯威特斯半导体科技有限公司 | Process for removing titanium or titanium nitride film on surface of semiconductor equipment |
| CN112934832A (en) * | 2021-04-19 | 2021-06-11 | 北京北方华创微电子装备有限公司 | Method for cleaning ceramic parts |
| CN113289959A (en) * | 2021-05-12 | 2021-08-24 | 上海富乐德智能科技发展有限公司 | Method for cleaning ceramic surface of electrostatic chuck part of semiconductor ETCH (electronic toll Collection) equipment |
| CN113245279A (en) * | 2021-05-20 | 2021-08-13 | 北京北方华创微电子装备有限公司 | Method for cleaning ceramic parts |
| CN114101191A (en) * | 2021-11-19 | 2022-03-01 | 横店集团东磁股份有限公司 | Cleaning method of walking roller used in solar single crystal cell etching process |
| CN114351154A (en) * | 2021-12-31 | 2022-04-15 | 卡贝尼新材料科技(上海)有限公司 | Method for cleaning double-layer attachments on surfaces of parts of semiconductor Cu processing equipment |
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