CN110571134B - Cleaning process for molybdenum and oxides thereof on baffle - Google Patents
Cleaning process for molybdenum and oxides thereof on baffle Download PDFInfo
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- CN110571134B CN110571134B CN201910721777.XA CN201910721777A CN110571134B CN 110571134 B CN110571134 B CN 110571134B CN 201910721777 A CN201910721777 A CN 201910721777A CN 110571134 B CN110571134 B CN 110571134B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
- H01L21/0206—Cleaning during device manufacture during, before or after processing of insulating layers
Abstract
The invention discloses a process for cleaning molybdenum and oxides thereof on the surface of a baffle, which comprises the following steps: using H2O2Soaking and cleaning the deposited film on the surface of the baffle plate by using the solution; soaking molybdenum and its oxide on the surface of baffle plate with alkaline liquorSoaking; washing the baffle plate by using high-pressure water; carrying out sand blasting treatment on the surface of the baffle; washing the baffle plate by using high-pressure water; carrying out dry ice cleaning on the baffle; carrying out ultrasonic cleaning on the baffle; the process solves the problems of great damage and great danger of acid liquor to the component body in the prior art, can effectively remove molybdenum and oxides thereof on the surface of the baffle, and cannot damage the baffle.
Description
Technical Field
The invention relates to the field of surface treatment, in particular to a cleaning process of molybdenum and oxides thereof on a baffle.
Background
In the process of manufacturing the TFT of the LCD and the OLED display screens, in order to reduce the impedance of peripheral guide lines or facilitate FPC bonding of module sections, a metal molybdenum Mo or an oxide MoOx thereof is sputtered in a TFT film, the material is continuously deposited on a baffle plate in a cavity in the sputtering process, the adhesion force of a deposition film and the baffle plate is reduced along with the increase of the thickness of a deposit, the deposition film can fall off to pollute the cavity, the defects of black spots, short circuits and the like are generated, the display quality of the LCD and the OLED display screens is influenced, so parts exposed in the process environment in the cavity need to be precisely regenerated, the service life of the parts is prolonged, the process environment is ensured to meet the process requirements of the display screens, the product quality is improved, and the process cost of clients is reduced.
A common cleaning method for deposited films of molybdenum Mo and its oxides (MoOx) is to use HNO3/H2SO4Soaking and cleaning with HF or other acid solution or mixed acid, blasting surface, cleaning with deionized water, and drying in clean drying oven. The acid liquor used in the cleaning process is volatile and has high risk, particularly HF has corrosiveness, and can prevent cleaning equipment, a tank body, waste gas treatment and other auxiliary facilities and personnelThe protection requirement is high, the cleaning time is long, acid liquor is easy to cause great damage to a part body, and after subsequent surface treatment, sand grains used for surface treatment are not easy to be completely cleaned, so that the standard exceeding of particles on the surface of the part can be caused, and the service performance of the part is influenced.
Disclosure of Invention
The invention solves the problems of great damage and great danger of acid liquor to the component body in the prior art, and provides a cleaning process of molybdenum and oxides thereof on a baffle plate, which can effectively remove molybdenum Mo and oxides thereof MoOx films attached to the surfaces of metal titanium, plastic and ceramic components during application and avoid great damage to the component body.
The invention is realized by the following technical scheme:
a cleaning process of molybdenum and oxides thereof on the surface of a baffle plate comprises the following steps:
s1: using H2O2Soaking and cleaning the deposited film on the surface of the baffle plate by using the solution;
s2: soaking molybdenum and oxides thereof on the surface of the baffle plate by using alkaline liquid medicine;
s3: washing the baffle plate by using high-pressure water;
s4: drying the baffle plate, and then carrying out sand blasting treatment on the surface;
s5: washing the baffle plate by using high-pressure water;
s6: carrying out dry ice cleaning on the baffle;
s7: carrying out ultrasonic cleaning on the baffle;
s8: the cleaned parts are dried.
Preferably, said H2O2The mass fraction of the solution is 20-40%, the soaking time of the baffle is 2-3 h, then the product soaked in the liquid medicine is cleaned by pure water, and the step is finished in a cleaning tank. The molybdenum Mo and the oxide MoOx thereof react with hydrogen peroxide to produce the high molybdic acid, and the chemical reaction process is as follows:
H2O2+Mo→H2MoOX+O2↑
due to H2O2Can not be mixed with plasticsThe reaction of the material and the ceramic forms a thin and compact oxide film on the surface when reacting with metal to prevent the further reaction, so that H2O2Substantially without corrosion of the parts of the substrate (metal, plastic, ceramic, etc.).
Cleaning molybdenum and oxides thereof on the surface of the baffle by using alkaline liquor, wherein the step is carried out in an alkaline liquor tank;
preferably, the alkali liquor is sodium hydroxide or potassium hydroxide solution.
Preferably, the concentration of the sodium hydroxide solution in S2 is naoh (g): h2O (mL) is 1: 6-1:10, the concentration of the potassium hydroxide solution being KOH (g): h2O (mL) is 1: the soaking time is 1-3h at the soaking temperature of 50-60 ℃ and the soaking time is 6-1: 10.
The alkali liquor reacts with molybdenum oxide Mo and oxide MoOx thereof on the surface of the baffle and metal aluminum Al of the meltallizing isolating layer to clean the molybdenum oxide Mo and oxide MoOx thereof and the metal aluminum, taking KOH as an example, the chemical reaction is as follows:
MoOX+KOH→K2MoO4+H2O
Al+KOH+H2O→KAlO2+H2↑
the metal molybdenum Mo and the oxide MoOx and the metal aluminum on the surface of the baffle can be completely cleaned through two-step reaction, and basically no damage is caused to the base material of the baffle.
Preferably, the pressure of the high pressure water in S3 is 16-18Mpa, and the baffle cleaned by the alkaline chemical liquid is washed by the high pressure water to remove the excessive chemical liquid on the surface of the product and remove the excessive deposition film on the surface of the product by the impact of the water.
And (3) carrying out sand blasting treatment on the surface of the part by using a sand blasting machine to clean and repair the surface. Preferably, the surface sand blasting material is white corundum Al with the grain diameter of 30-400 meshes2O3The particle size is selected according to the requirement of surface roughness.
And the pressure of the high-pressure water in the S5 is 16-18Mpa, and the baffle after sand blasting is washed by the high-pressure water so as to remove redundant large particles on the surface of the baffle during the sand blasting process.
Preferably, the dry ice cleaning step is to spray dry ice onto the surface of the baffle by compressed air.
And (4) placing the baffle subjected to high-pressure water washing in dry ice cleaning equipment, and treating the surface by using dry ice to remove the residues of the sand blasting particles on the surface of the part in the step S4. The dry ice equipment functions include: a dry ice generator, a compressed air source.
And placing the baffle cleaned by the dry ice in an ultrasonic groove for ultrasonic cleaning. The tank body function includes: ultrasonic wave (with do not harm the product as the standard, be 30 ~ 40KHZ usually), overflow (make the cell body water keep certain cleanliness factor), filtration (the suspended solid passes through the filter and filters, pollution abatement).
And (5) placing the baffle subjected to the pure water soaking treatment in a clean drying box for drying. Preferably, the drying temperature is 180-.
The cleaning process is applied to cleaning molybdenum Mo and oxide MoOx films on the surfaces of metals (such as titanium, aluminum and other alloys), plastics and ceramic parts.
The product obtained by the cleaning process is provided by the invention.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. hydrogen peroxide is used to replace conventional strong acid, so that the problems of great damage and great risk of the acid liquor to the part body in the prior art are solved, and H2O2Will not react with plastics and ceramics, will form a thin and compact oxide film on the surface with metal to prevent further reaction, H2O2Substantially without causing corrosion to the components of the metal substrate.
2. By controlling the concentration of the alkali liquor, metal molybdenum (Mo) and oxides thereof (MoOx) on the surface of the baffle can be cleaned, metal aluminum can also be cleaned, and the base material of the baffle is basically not damaged.
3. The surface sand blasting treatment can be used for cleaning and repairing the baffle, and the high-pressure water can be used for removing redundant liquid medicine on the surface of the product and removing redundant deposited films on the surface of the product through the impact force of water; dry ice treating the surface removes the abrasive blasting particles from the surface of the part.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a diagram of the apparatus of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
Example 1
Placing the decomposed ceramic baffle plates into a cleaning tank, separating the baffle plates by using magnetic substances to ensure that the cleaning surfaces of the baffle plates cannot be contacted and shielded with each other, and adding H with the mass fraction of 20% into the tank2O2And soaking the deposited film on the surface of the baffle for 3 hours until no reaction process exists. After the liquid medicine is cleaned, opening a liquid discharge pipe of the tank body, discharging the liquid medicine through a filter, and injecting pure water into the tank body for rinsing to remove the product of the reaction of the liquid medicine on the surface of the baffle plate and the molybdenum Mo and the oxide MoOx thereof; will pass through H2O2The cleaned parts were loaded with naoh (g) concentration: h2O (mL) is 1: 6, heating the tank liquor to 50 ℃ in advance in the caustic soda tank body of the sodium hydroxide solution, taking out the baffle from the interior of the tank body after reacting for 3 hours, and soaking the baffle in a pure water tank to remove the caustic soda and reaction residues on the surface of the baffle; placing the component on a high-pressure washing table top, cleaning the surface of the component by using 16Mpa high-pressure water, removing redundant liquid medicine on the surface of the product and redundant deposited films on the surface of the product by the impact force of water, and ensuring that the liquid medicine on the surface of the component and the reactants participating in the cleaning are completely cleaned; white corundum Al with grain diameter of 30 meshes for sand blasting machine2O3Sand blasting treatment of baffle surfacePolishing and slightly cleaning the surface, and slightly repairing micro scratches, scratches and the like on the surface of the component under the CAD pressure of 0.6 Mpa; placing the component on a high-pressure washing table top, cleaning the surface of the component by using high-pressure water of 16Mpa, and removing sand grains remained on the surface of the component in the sand blasting process; placing the baffle subjected to sand blasting in dry ice cleaning equipment, and spraying dry ice on the surface of the baffle by the dry ice generated in a dry ice generator through compressed air so as to remove sand grains and other tiny particles attached in gaps on the surface of the component; placing the baffle cleaned by the dry ice in an ultrasonic groove for ultrasonic cleaning and soaking, wherein the ultrasonic frequency is 30 KHZ; and (3) putting the cleaned baffle into a clean drying oven at 180 ℃ for drying for 2 hours, completely removing the water on the surface of the part, cooling to 40 ℃, and taking out the part.
Example 2
Placing the decomposed plastic baffle plates into a cleaning tank, separating the baffle plates by using magnetic substances to ensure that the cleaning surfaces of the baffle plates on the cleaning surface of the baffle plates can not be contacted and shielded, and adding H with the mass fraction of 40% into the tank2O2And soaking the deposited film on the surface of the baffle for 2 hours until no reaction process exists. After the liquid medicine is cleaned, opening a liquid discharge pipe of the tank body, discharging the liquid medicine through a filter, and injecting pure water into the tank body for rinsing to remove the product of the reaction of the liquid medicine on the surface of the baffle plate and the molybdenum Mo and the oxide MoOx thereof; will pass through H2O2The cleaned parts were loaded with a koh (g) concentration: h2O (mL) is 1:10, heating the tank liquor to 60 ℃ in advance in a potassium hydroxide solution alkaline liquor tank body, taking out the baffle from the interior of the tank body after reacting for 1h, and putting the baffle into a pure water tank for soaking so as to remove alkaline liquor and reaction residues on the surface of the baffle; placing the component on a high-pressure washing table top, cleaning the surface of the component by using 18Mpa high-pressure water, removing redundant liquid medicine on the surface of the product and redundant deposited films on the surface of the product by the impact force of water, and ensuring that the liquid medicine on the surface of the component and the reactants participating in the cleaning are completely cleaned; white corundum Al with grain size of 400 meshes for sand blasting machine2O3Sand blasting treatment is carried out on the surface of the baffle, the surface is polished and slightly cleaned, and micro repairing is carried out on micro scratches, scratches and the like on the surface of the componentCAD pressure is 0.7 Mpa; placing the component on a high-pressure washing table top, cleaning the surface of the component by using high-pressure water of 18Mpa, and removing sand grains remained on the surface of the component in the sand blasting process; placing the baffle subjected to sand blasting in dry ice cleaning equipment, and spraying dry ice on the surface of the baffle by the dry ice generated in a dry ice generator through compressed air so as to remove sand grains and other tiny particles attached in gaps on the surface of the component; placing the baffle cleaned by the dry ice in an ultrasonic groove for ultrasonic cleaning and soaking, wherein the ultrasonic frequency is 40 KHZ; and (3) putting the cleaned baffle into a clean drying oven at 200 ℃ for drying for 1 hour, completely removing the water on the surface of the part, cooling to 50 ℃, and taking out the part.
Example 3
Placing the decomposed titanium metal baffle plates into a cleaning tank, separating the baffle plates by using magnetic substances to ensure that the cleaning surfaces of the baffle plates cannot be contacted and shielded, and adding H with the mass fraction of 30% into the tank2O2And soaking the deposited film on the surface of the baffle for 2.5 hours until no reaction progress exists. After the liquid medicine is cleaned, opening a liquid discharge pipe of the tank body, discharging the liquid medicine through a filter, and injecting pure water into the tank body for rinsing to remove the product of the reaction of the liquid medicine on the surface of the baffle plate and the molybdenum Mo and the oxide MoOx thereof; will pass through H2O2The cleaned parts were loaded with naoh (g) concentration: h2O (mL) is 1: 8, heating the tank liquor to 55 ℃ in advance in a sodium hydroxide solution alkaline liquor tank body, taking out the baffle from the interior of the tank body after reacting for 2 hours, and soaking the baffle in a pure water tank to remove alkaline liquor and reaction residues on the surface of the baffle; placing the component on a high-pressure washing table top, cleaning the surface of the component by using 17Mpa high-pressure water, removing redundant liquid medicine on the surface of the product and redundant deposited films on the surface of the product by the impact force of water, and ensuring that the liquid medicine on the surface of the component and the reactants participating in the cleaning are completely cleaned; white corundum Al with grain size of 100 meshes for sand blasting machine2O3Performing sand blasting treatment on the surface of the baffle, polishing and slightly cleaning the surface, and slightly repairing micro scratches, scratches and the like on the surface of the component, wherein the CAD pressure is 0.65 Mpa; the parts were placed on a high pressure rinse table using a 17Mpa heightPressing water to clean the surface of the part and remove sand grains remained on the surface of the part in the sand blasting process; placing the baffle subjected to sand blasting in dry ice cleaning equipment, and spraying dry ice on the surface of the baffle by the dry ice generated in a dry ice generator through compressed air so as to remove sand grains and other tiny particles attached in gaps on the surface of the component; placing the baffle cleaned by the dry ice in an ultrasonic groove for ultrasonic cleaning and soaking, wherein the ultrasonic frequency is 35 KHZ; and (3) putting the cleaned baffle into a clean drying oven at 190 ℃ for drying for 1.5 hours, completely removing the water on the surface of the part, cooling to 45 ℃, and taking out the part.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. A cleaning process of molybdenum and oxides thereof on the surface of a baffle plate is characterized by comprising the following steps:
s1: using H2O2Soaking and cleaning the deposited film on the surface of the baffle by using solution, wherein H is2O2The mass fraction of the solution is 20-40%, and the soaking time of the baffle is 2-3 h;
s2: soaking molybdenum and oxides thereof on the surface of the baffle by using alkaline liquid medicine, wherein the alkaline liquid medicine is sodium hydroxide or potassium hydroxide solution;
s3: washing the baffle plate by using high-pressure water;
s4: drying the baffle plate, and then carrying out sand blasting treatment on the surface;
s5: washing the baffle plate by using high-pressure water;
s6: carrying out dry ice cleaning on the baffle;
s7: carrying out ultrasonic cleaning on the baffle;
s8: the cleaned parts are dried.
2. The cleaning process according to claim 1, wherein the concentration of the sodium hydroxide solution in S2 is NaOH (g): h2O (mL) is 1: 6-1:10, the concentration of the potassium hydroxide solution being KOH (g): h2O (mL) is 1: the soaking time is 1-3h at the soaking temperature of 50-60 ℃ and the soaking time is 6-1: 10.
3. The cleaning process according to claim 1, wherein the pressure of the high pressure water in S3 and S5 is 16-18 MPa.
4. The cleaning process as claimed in claim 2, wherein the drying temperature in S4 is 180-200 ℃, the drying time is 1-2 hours, and the surface blasting material is white corundum Al with a particle size of 30-400 meshes2O3。
5. The cleaning process of claim 1, wherein the dry ice cleaning step is spraying dry ice onto the surface of the baffle by compressed air.
6. The cleaning process as claimed in claim 1, wherein the drying temperature is 180-200 ℃ and the drying time is 1-2 hours.
7. Use of the cleaning process according to any one of claims 1 to 6 for cleaning molybdenum Mo and oxide MoOx films on the surfaces of metal, plastic and ceramic parts.
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| CN201910721777.XA CN110571134B (en) | 2019-08-06 | 2019-08-06 | Cleaning process for molybdenum and oxides thereof on baffle |
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| CN114558822B (en) * | 2021-12-15 | 2023-04-07 | 杭州盾源聚芯半导体科技有限公司 | Cleaning method of injection pipe |
| CN114196900B (en) * | 2021-12-17 | 2023-08-08 | 富乐德科技发展（天津）有限公司 | Surface treatment method for stainless steel component in semiconductor chip manufacturing industry |
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| US6794292B2 (en) * | 2001-07-16 | 2004-09-21 | United Microelectronics Corp. | Extrusion-free wet cleaning process for copper-dual damascene structures |
| US7205233B2 (en) * | 2003-11-07 | 2007-04-17 | Applied Materials, Inc. | Method for forming CoWRe alloys by electroless deposition |
| CN1947870B (en) * | 2006-05-12 | 2011-01-19 | 浙江昱辉阳光能源有限公司 | Method for cleaning waste silicon materials |
| US8586472B2 (en) * | 2010-07-14 | 2013-11-19 | Infineon Technologies Ag | Conductive lines and pads and method of manufacturing thereof |
| CN103151423B (en) * | 2013-02-28 | 2015-09-16 | 常州捷佳创精密机械有限公司 | A kind of polycrystalline silicon texturing cleaning process |
| KR20170044968A (en) * | 2015-10-16 | 2017-04-26 | 삼성전자주식회사 | Method of cleaning a substrate and fabrication method of semiconductor device using the same |
| CN109628965B (en) * | 2019-01-30 | 2021-02-12 | 云谷（固安）科技有限公司 | Metal workpiece cleaning process |
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