CN111940394B - Quartz component regeneration cleaning method of semiconductor high-order process APC device - Google Patents
Quartz component regeneration cleaning method of semiconductor high-order process APC device Download PDFInfo
- Publication number
- CN111940394B CN111940394B CN202010691293.8A CN202010691293A CN111940394B CN 111940394 B CN111940394 B CN 111940394B CN 202010691293 A CN202010691293 A CN 202010691293A CN 111940394 B CN111940394 B CN 111940394B
- Authority
- CN
- China
- Prior art keywords
- cleaning
- hydrofluoric
- quartz component
- nitric acid
- polishing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
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
-
- 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
-
- 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
- B24B29/00—Machines or devices for polishing surfaces on work by means of tools made of soft or flexible material with or without the application of solid or liquid polishing agents
- B24B29/02—Machines or devices for polishing surfaces on work by means of tools made of soft or flexible material with or without the application of solid or liquid polishing agents designed for particular workpieces
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24C—ABRASIVE OR RELATED BLASTING WITH PARTICULATE MATERIAL
- B24C1/00—Methods for use of abrasive blasting for producing particular effects; Use of auxiliary equipment in connection with such methods
- B24C1/08—Methods for use of abrasive blasting for producing particular effects; Use of auxiliary equipment in connection with such methods for polishing surfaces, e.g. smoothing a surface by making use of liquid-borne abrasives
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/003—Supply-air or gas filters
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/004—Nozzle assemblies; Air knives; Air distributors; Blow boxes
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
The invention relates to the technical field of semiconductors. The regeneration cleaning method for the quartz component of the semiconductor high-order process APC device comprises the following steps: step one, carrying out micro powder sand blasting; step two, physical polishing and grinding; step three, flame polishing; step four, high-temperature annealing; step five, chemical cleaning; firstly, soaking the mixture for 10min by using an ammonia hydrogen peroxide solution at the temperature of 20-40 ℃; then, soaking for 5-20min by using a hydrofluoric/nitric acid solution; finally, soaking for 5-20min by using a hydrofluoric/nitric acid solution; step six, ultrasonic cleaning; and step seven, washing and drying. The invention reduces the cost and achieves the purpose of avoiding the corrosion problem of chemical stripping.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a cleaning method.
Background
In the manufacturing process of semiconductor devices, as the requirements of semiconductor processes are higher and higher, the requirements of parasitic current are higher and higher, wherein the requirements of copper purity for copper connecting wires are higher and higher, and APC (reactive mode pre-cleaning) devices for processes below 28nm are beneficial to improving the copper purity, and are widely applied.
In the process of purifying copper by introducing hydrogen into an APC device, under the condition of low vacuum degree, the hydrogen can deprive the medium oxygen of the silicon dioxide of a quartz component substrate in the device while purifying the copper on the surface of a silicon wafer, and the following chemical reactions occur: SiO 22+N2+H2→SiON+SixNy+H2O, so that the surface of the quartz member becomes rough in view of the by-product-SiON/SixNyThe material has strong acid and alkali resistance, and is difficult to remove by a chemical method under the condition of not damaging a quartz body (silicon dioxide) of a component material.
The traditional method for removing the by-products comprises the following steps:
1) firstly, 140 ℃ and 180 ℃ concentrated phosphoric acid remove SiON/SixNyThen rinsed with hot water and finally dehydrated. Disclosed in: book written by strong portraitureThe research on the hot phosphoric acid etching process in large scale integrated circuits, written in ShouFang, Wanhui, Rosensland, 2007, "etching rate of hot phosphoric acid in silicon nitride wet etching", published in journal of semiconductor technology.
The disadvantage is that the use of hot phosphoric acid to remove deposits requires special cleaning machines and is costly.
2) And (4) soaking in hydrofluoric acid at 40 ℃ to remove SixNy. The article "application of ceramic silicon nitride ceramics and research progress of acid corrosion" published on pages 8-14 of modern technologies of Jiangyu, Liqiang, Jiangyu in journal, Huan Changtian, 2011.
Use of HF to remove SiON/Si from quartz component surfacesxNyThe defect is that the quartz body is corroded for a long time and cannot be used.
Disclosure of Invention
In view of the problems of the prior art, the present invention provides a method for regenerating and cleaning a quartz component of an APC device for semiconductor high-order processing, so as to solve at least one of the above technical problems.
In order to achieve the above object, the present invention provides a method for regenerating and cleaning a quartz component of an APC apparatus for semiconductor high-order processing, comprising the steps of:
firstly, carrying out micro powder sand blasting to remove residues or sediments on the surface;
step two, carrying out physical polishing and grinding to ensure that the surface roughness of the quartz component is lower than 1.0 um;
step three, flame polishing is carried out, so that the surface roughness of the quartz component is lower than 0.5 um;
step four, high-temperature annealing;
step five, chemical cleaning;
firstly, soaking the mixture for 10min by using an ammonia hydrogen peroxide solution at the temperature of 20-40 ℃;
then, soaking for 5-20min by using a hydrofluoric/nitric acid solution;
finally, soaking for 5-20min by using a hydrofluoric/nitric acid solution;
step six, ultrasonic cleaning;
and step seven, washing and drying.
Further excellenceOptionally, in the first step, a gas protection jig is used for sand blasting, WA400# micro powder is used for sand blasting on the quartz component to remove residues or deposits on the surface, and the conveying gas pressure is 0.5-1Kg.cm2And the sand blasting time is 3-5 minutes.
Preferably, in the second step, the specific area is polished by using a rotary platform and adopting a certain amount of sieved silicon carbide abrasive, and the quartz component is polished for multiple times through multiple times of polishing of various sieved silicon carbide abrasive, wherein the thickness is firstly increased and then decreased, so that the surface roughness of the quartz component is lower than 1.0um, and the rotating speed of the rotary table is 30-75 rmp.
Further preferably, in the third step, polishing is performed by using an oxygen-hydrogen flame, so that a mirror surface effect with the roughness lower than 0.5um is obtained.
Further preferably, in the fourth step, the product is placed into a high temperature furnace for high temperature annealing at 1000-1150 ℃.
Preferably, in the fifth step, the ratio of the ammonia water hydrogen peroxide solution is NH4OH:H2O2:H2O ═ 0.5-1:0.5-2: 2-4; the proportion of the hydrofluoric/nitric acid solution is HF to HNO3:H2O＝1:5-10:44-60。
Preferably, in the fifth step, the concentration of the original solution in the ammonia water hydrogen peroxide solution is as follows: 28-30% of ammonia water and 28-30% of hydrogen peroxide; concentration of the original solution in the hydrofluoric/nitric acid solution: 69-70% of nitric acid and 49-50% of hydrofluoric acid.
Preferably, in the sixth step, the quartz component is subjected to ultrasonic cleaning, the temperature of ultrapure water in an ultrasonic groove is 20-38 ℃, the ultrasonic frequency is 40-80 KHz, and the ultrasonic cleaning time is 10-30 min. Then rinsed with ultra pure water and blown dry with 0.1 micron filtered nitrogen.
More preferably, in the sixth step and the seventh step, ultrapure water is adopted, and the ultrapure water is deionized water with the resistivity larger than 18M omega.
The invention has the following beneficial effects:
according to the regeneration method of the quartz component of the semiconductor high-order processing APC equipment etching device, the physical sand blasting is adopted to quickly remove the deposit, and the deposited film on the surface of the quartz component is removed in a short time; meanwhile, the surface roughness of the quartz component is reduced through physical grinding and polishing, flame polishing, high-temperature annealing and other treatments, and the problem that the surface roughness of a quartz product is increased in the using process is solved; the high-cleanness surface of the quartz component is obtained by chemical cleaning, and the aim of quartz regeneration cleaning in the high-order process is fulfilled. The invention reduces the cost and achieves the purpose of avoiding the corrosion problem of chemical stripping.
Drawings
FIG. 1 is a schematic flow chart of the present invention;
FIG. 2 is an external view of a quartz member before regeneration treatment;
FIG. 3 is an external view of the quartz component of FIG. 2 after treatment with the present invention;
FIG. 4 is a schematic view under a microscope of a quartz component before being recycled;
FIG. 5 is a schematic representation under a microscope after treatment with the present invention.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
Referring to fig. 1 to 5, the method for regenerating a quartz member (gas distribution plate) of the semiconductor APC apparatus of this embodiment comprises the steps of:
step one, carrying out micro powder sand blasting;
blasting sand by using a gas protection jig, performing WA400# micro powder blasting sand on the quartz component to remove residues or deposits on the surface, wherein the conveying gas pressure is 0.5-1Kg.cm2The sand blasting time is 3-5 minutes;
step two, physical grinding and polishing;
grinding a specific area by using a rotary platform and adopting a certain amount of sieved silicon carbide grinding materials, and grinding for multiple times (firstly, grinding and then grinding) through multiple kinds of sieved silicon carbide grinding materials to ensure that the surface roughness of a quartz component is lower than 1.0um and the rotating speed of a rotary table is 30-75 rmp;
step three, flame polishing;
polishing by using oxygen-hydrogen flame to obtain a mirror surface effect with the roughness lower than 0.5 um;
step four, high-temperature annealing;
putting the product into a high-temperature furnace, and carrying out high-temperature annealing at 1000-1150 ℃;
step five, chemical cleaning;
5.1) Using aqueous Ammonia dioxygen solution (NH)4OH:H2O2:H2O is 0.5-1:0.5-2:2-4), the solution temperature is 20-40 ℃, and the soaking time is 10 min.
5.2), using hydrofluoric/nitric acid solution (HF: HNO)3:H2O1: 5-10:44-60) for 5-20 min;
5.3), using hydrofluoric/nitric acid solution (HF: HNO)3:H2O1: 5-10:44-60) for 5-20 min;
step six, ultrasonic cleaning;
and (3) ultrasonically cleaning the quartz component, wherein the temperature of ultrapure water in an ultrasonic groove is 20-38 ℃, the ultrasonic frequency is 40-80 KHz, the ultrasonic cleaning time is 10-30min, and the quartz component is washed by the ultrapure water and dried by filtering nitrogen with the particle size of 0.1 micron.
And step seven, rinsing with ultrapure water and drying.
The comparison of the appearance of the quartz member (gas distribution plate) before and after cleaning and regeneration, as shown in fig. 2 and 3, through the above embodiment, the deposited film layer and the contaminant particles in fig. 2 are removed to show the flat and bright state in fig. 3 (in addition, fig. 4 is a microscopic picture of the surface of the product before cleaning, which shows the state of the deposit on the surface of the product and the roughness, and fig. 5 is a microscopic picture of the surface of the product after cleaning, which shows the flat and bright state). Through ICP-MS detection, the product can reach the cleanliness of silicon chip level (the metal ion level is 1-300E10 Atoms/cm)2)。
The foregoing is only a preferred embodiment of the present invention, and it should be noted that it is obvious to those skilled in the art that various modifications and improvements can be made without departing from the principle of the present invention, and these modifications and improvements should also be considered as the protection scope of the present invention.
Claims (5)
1. The method for regenerating and cleaning the quartz component of the semiconductor high-order process APC device is characterized by comprising the following steps:
firstly, carrying out micro powder sand blasting to remove residues or sediments on the surface;
in the first step, a gas protection jig is used for sand blasting, WA400# micro powder sand blasting is carried out on the quartz component, and the adopted conveying gas pressure is 0.5-1Kg2The sand blasting time is 3-5 minutes;
step two, carrying out physical polishing and grinding to ensure that the surface roughness of the quartz component is lower than 1.0 um;
polishing a specific area by using a rotary platform and adopting a certain amount of sieved silicon carbide abrasive materials, and polishing for multiple times by using multiple kinds of sieved silicon carbide abrasive materials, wherein the thickness is firstly increased and then the thickness is reduced, and the rotating speed of the rotary platform is 30-75 rmp;
step three, flame polishing is carried out, so that the surface roughness of the quartz component is lower than 0.5 um;
in the third step, polishing is carried out by using oxygen-hydrogen flame to obtain a mirror surface effect with the roughness lower than 0.5 um;
step four, high-temperature annealing; putting the product into a high-temperature furnace, and performing high-temperature annealing at 1000-1150 ℃;
step five, chemical cleaning;
firstly, soaking the mixture for 10min by using an ammonia hydrogen peroxide solution at the temperature of 20-40 ℃;
then, soaking for 5-20min by using a hydrofluoric/nitric acid solution;
finally, soaking for 5-20min by using a hydrofluoric/nitric acid solution;
step six, ultrasonic cleaning;
step seven, washing and drying;
through ICP-MS detection, the product reaches the cleanliness of a silicon wafer level, and the metal ion level is 1-300E10 atomms/cm2。
2. The method of claim 1, wherein the cleaning step further comprises the steps of: in the fifth step, the proportion of the ammonia water hydrogen peroxide solution is NH4OH:H2O2:H2O＝0.5-1:0.5-2:2-4；
The proportion of the hydrofluoric/nitric acid solution is HF to HNO3:H2O＝1:5-10:44-60。
3. The method of claim 1, wherein the cleaning step further comprises the steps of: in the fifth step, the concentration of the original liquid in the ammonia water hydrogen peroxide solution is as follows: 28-30% of ammonia water and 28-30% of hydrogen peroxide;
concentration of the original solution in the hydrofluoric/nitric acid solution: 69-70% of nitric acid and 49-50% of hydrofluoric acid.
4. The method of claim 1, wherein the cleaning step further comprises the steps of: and sixthly, ultrasonically cleaning the quartz component, wherein the temperature of ultrapure water in an ultrasonic groove is 20-38 ℃, the ultrasonic frequency is 40-80 KHz, the ultrasonic cleaning time is 10-30min, and then washing with ultrapure water and drying with 0.1 micron filtered nitrogen.
5. The method of claim 1, wherein the cleaning step further comprises the steps of: in the sixth step and the seventh step, ultrapure water is adopted, and the ultrapure water is deionized water with the resistivity larger than 18M omega.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010691293.8A CN111940394B (en) | 2020-07-17 | 2020-07-17 | Quartz component regeneration cleaning method of semiconductor high-order process APC device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010691293.8A CN111940394B (en) | 2020-07-17 | 2020-07-17 | Quartz component regeneration cleaning method of semiconductor high-order process APC device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111940394A CN111940394A (en) | 2020-11-17 |
| CN111940394B true CN111940394B (en) | 2022-01-21 |
Family
ID=73340044
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010691293.8A Active CN111940394B (en) | 2020-07-17 | 2020-07-17 | Quartz component regeneration cleaning method of semiconductor high-order process APC device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111940394B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114247699A (en) * | 2021-12-13 | 2022-03-29 | 安徽光智科技有限公司 | Ultrasonic demoulding method for crystal oscillation plate |
| CN114211405A (en) * | 2021-12-17 | 2022-03-22 | 富乐德科技发展（天津）有限公司 | Cleaning method for removing fluoride on surface of aluminum substrate |
| CN114536158B (en) * | 2022-01-19 | 2023-03-31 | 宁波云德半导体材料有限公司 | Processing method of quartz window of etching machine reaction chamber |
| CN114749407A (en) * | 2022-04-08 | 2022-07-15 | 安徽富乐德科技发展股份有限公司 | Ultrahigh-pressure physical film removing method for semiconductor component |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1004615B (en) * | 1987-07-20 | 1989-06-28 | 吉林工业大学 | Gas protection type sand blower |
| JP3210800B2 (en) * | 1994-04-12 | 2001-09-17 | ワッカー・エヌエスシーイー株式会社 | Semiconductor substrate cleaning method |
| CN101219429A (en) * | 2007-01-10 | 2008-07-16 | 北京北方微电子基地设备工艺研究中心有限责任公司 | Method for cleaning quartz parts surface in polycrystal etching cavity |
| CN108672375A (en) * | 2018-04-08 | 2018-10-19 | 苏州珮凯科技有限公司 | A kind of regeneration method of 8 cun of silicon wafer process ETCH8500 art quartz shading rings of semiconductor |
| CN109590267A (en) * | 2018-12-28 | 2019-04-09 | 深圳仕上电子科技有限公司 | Cleaning method |
| CN110510886A (en) * | 2019-09-18 | 2019-11-29 | 沈阳汉科半导体材料有限公司 | Chemical granulation processing method for quartz surface |
| CN111112212B (en) * | 2019-11-29 | 2021-07-30 | 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 |
-
2020
- 2020-07-17 CN CN202010691293.8A patent/CN111940394B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN111940394A (en) | 2020-11-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111940394B (en) | Quartz component regeneration cleaning method of semiconductor high-order process APC device | |
| WO2021043167A1 (en) | Final cleaning method for silicon carbide single-crystal polished wafer substrate | |
| US7250114B2 (en) | Methods of finishing quartz glass surfaces and components made by the methods | |
| JP2787788B2 (en) | Residue removal method | |
| US7498269B2 (en) | Cleaning methods for silicon electrode assembly surface contamination removal | |
| TWI283900B (en) | Removal of CMP and post-CMP residue from semiconductors using supercritical carbon dioxide process | |
| CN111900070A (en) | Regeneration cleaning and repairing method for silicon part of semiconductor high-order process etching device | |
| CN111900071A (en) | Regeneration method of silicon electrode component of etching device of semiconductor equipment | |
| JP2005093869A (en) | Method of regenerating silicon wafer, and regenerated wafer | |
| CN115254766A (en) | Cleaning regeneration method of aluminum oxide ceramic ejector of semiconductor equipment | |
| KR100654501B1 (en) | Wafer Polishing, Cleaning and Protective Films | |
| WO2023218828A1 (en) | Cleaning solution and wafer cleaning method | |
| WO1997008742A1 (en) | Procedure for drying silicon | |
| WO2011086876A1 (en) | Surface cleaning method for silicon wafer | |
| US20040266191A1 (en) | Process for the wet-chemical surface treatment of a semiconductor wafer | |
| KR102019817B1 (en) | Quarts surface treatment method | |
| EP2434004A1 (en) | Cleaning liquid and cleaning method | |
| KR20090121527A (en) | Recycling method of silicon wafer and its recycled divice | |
| KR102625872B1 (en) | Method for Surface Treatment of Aluminum Remote Plasma Source Chamber Comprising Physical Polishing and Anodizing | |
| TWI569894B (en) | Pollutant Treatment Method for Sprinkler with Silicon Carbide Coated | |
| JP2000164568A (en) | Manufacture of plasma etching electrode | |
| US20070034601A1 (en) | Surface treating method and surface-treating apparatus | |
| CN116351782A (en) | Surface high-cleanliness treatment method suitable for semiconductor equipment parts | |
| KR20080003616A (en) | Silica slurry for chemical mechanical polishing semiconductor devices including hydro peroxide | |
| KR20070070378A (en) | Chemical mechanical polishing device using hf vapor method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |