CN102010135B - Method for preparing metal mask resistant to corrosion of hydrofluoric acid corrosive liquid - Google Patents
Method for preparing metal mask resistant to corrosion of hydrofluoric acid corrosive liquid Download PDFInfo
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- CN102010135B CN102010135B CN201010540144A CN201010540144A CN102010135B CN 102010135 B CN102010135 B CN 102010135B CN 201010540144 A CN201010540144 A CN 201010540144A CN 201010540144 A CN201010540144 A CN 201010540144A CN 102010135 B CN102010135 B CN 102010135B
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Abstract
The invention relates to a method for preparing an anticorrosive metal mask, in particular to a method for preparing a metal mask resistant to the corrosion of hydrofluoric acid corrosive liquid. The invention aims to solve the problems of undercut holes, local warping, peeling defects and the like of the conventional corroded mask. The method particularly comprises the following steps of: a, cleaning, namely performing corrosion soaking on a substrate to be coated in hydrofluoric acid and hydrogen peroxide mixed liquid or sulfuric acid and hydrogen peroxide mixed liquid, and performing megasonic cleaning on the substrate; and b, coating, namely (1) performing ion bombardment on Ar on the surface of the substrate; (2) sequentially coating a Cr film and a Cu film on the surface of the substrate under the condition of the temperature of between 100 and 220 DEG C, the sputtering pressure of 0.3 to 0.8 Pa and the sputtering power of 1.9 to 2.5 Kw; and (3) repeating the step (2) to coat the Cr film and the Cu film on the surface of the substrate again to form a double-layered or multilayered Cr/Cu metal mask. The method effectively reduces pinhole undercutting due to fine particles and film layer defects, improves the adhesion of the mask and effectively removes stress.
Description
Technical field
The present invention relates to a kind of noncorroding metal mask preparation method, particularly a kind of anti-hydrofluoric acid corrosive fluid corrosive metal mask preparation method.
Background technology
MEMS often adopts the crystalline material substrate to process various micro structural components, and its processing process mainly comprises substrate cleaning, thin film deposition, photoetching, corrosion etc.Cleaning mainly is the various impurity of removing substrate surface; Thin film deposition is that its effect is the corrosion of opposing corrosive fluid and makes electrode, lead-in wire at mode depositing metal films such as substrate surface employing magnetron sputtering or electron beam evaporations; Photoetching is that structure graph and electrode pattern are transferred on the substrate; Corrosion is the important step in the whole technological process, directly influences texture quality and device performance, adopts hydrofluoric acid (HF) type corrosive fluid that substrate is carried out chemical corrosion processing usually, and the part that is not corroded adopts the noncorroding metal mask to protect.
The preparation of noncorroding metal mask is the basis and the difficult point of chemical corrosion operation.The mask preparation has two basic demands: the first, and film adhesion is strong, stress is little, is destroyed or rete big area inefficacy (as hike up, peel, chap) with the edge that prevents rete and substrate interface place; The second, the compact structure of rete, impurity is few, preventing that corrosive fluid from seeing through rete space and impurity and arriving substrate surface and it is corroded form undercutting hole and damage rete, thereby influences the surface tissue quality of device and the electric property of rete.
The factor that influences substrate metallic membrane corrosion resistance mainly contains surface quality and the clean of substrate, the deposition method of mask, the processing parameter (substrate temperature, vaporator rate, vacuum tightness) of mask preparation etc.Substrate can be selected for use like silica glass or crystal, soda-lime glass, 7740 glass etc.The basic step of existing etching mask preparation is for cleaning and plated film; With 7740 substrate of glass is example; Carry out the cleaning of substrate earlier, the sheet glass of twin polishing is immersed in 120 ℃ the vitriol oil, adds an amount of ydrogen peroxide 50 cleaning 10min; To remove surperficial organism and particle etc., use deionized water rinsing, drying then; Substrate is put into the two-sided magnetron sputtering TiW/Au of coating equipment.
There are two obviously deficiencies in existing etching mask processing: the one, and in corrosive fluid, soak the back mask surface and have the undercutting hole, this is to be caused by the surface imperfection of film and environment particle contamination.Particulate secondary pollution in the residual and coating process of substrate cleaning process particulate before the plated film, particle has determined the quantity and the size of mask surface defective in the quantity and the size of substrate surface.In order to guarantee the erosion resistance of mask, must reduce the quantity and size and strictly controlled environment particle contamination of mask surface defective as far as possible; The 2nd, typical defects such as local warpage, peeling appear in mask surface after the chemical corrosion.This mainly is to be caused by the internal stress of rete and sticking power, like the sticking power between substrate forming residual stress, substrate and rete, two retes, and the thermal stresses that material thermal expansion coefficient difference and temperature variation cause in rete unrelieved stress, the deposition etc.Improve the substrate quality, improve between the double-layer films, the sticking power between film and the substrate, reduce the unrelieved stress of rete, reducing the superficial film defective is to improve the key of corrosion stability.
Summary of the invention
The objective of the invention is to solve problems such as the undercutting hole that exists behind the existing mask corrosion, local warpage, peeling defective, propose a kind of anti-hydrofluoric acid corrosive fluid corrosive metal mask preparation method.
The technical scheme that the present invention adopted is:
A kind of anti-hydrofluoric acid corrosive fluid corrosive metal mask preparation method comprises the steps:
Cleaning step;
The plated film step;
Wherein:
Institute's plated film is a multi-layer film structure in the said plated film step.
Aforesaid a kind of anti-hydrofluoric acid corrosive fluid corrosive metal mask preparation method, wherein: said cleaning step comprises the step of cleaning million.
Aforesaid a kind of anti-hydrofluoric acid corrosive fluid corrosive metal mask preparation method, wherein: said cleaning step also comprises the step that adopts hydrofluoric acid ydrogen peroxide 50 mixed solution or dioxysulfate water mixed liquid to treat film plating substrate corrosion immersion.
Aforesaid a kind of anti-hydrofluoric acid corrosive fluid corrosive metal mask preparation method, wherein: said corrosion is immersed under 60～120 ℃ of conditions to be carried out, and the corrosion soak time is 5～10 minutes, and said million scavenging periods are 5～15min.
Aforesaid a kind of anti-hydrofluoric acid corrosive fluid corrosive metal mask preparation method, wherein: said plated film step specifically comprises:
Treat the step that ion bombardment is carried out on the film plating substrate surface;
Adopt the magnetron sputtering mode to treat the step of film plating substrate plated film, the plated film condition is: 100～220 ℃ of temperature, sputtering pressure 0.3～0.8Pa, sputtering power 1.9～2.5Kw.
Aforesaid a kind of anti-hydrofluoric acid corrosive fluid corrosive metal mask preparation method, wherein: the ion bombardment in the said plated film step is Ar ion bombardment, the time is 5～10min, ion bombardment power 70～90w.
Aforesaid a kind of anti-hydrofluoric acid corrosive fluid corrosive metal mask preparation method, wherein: after said plated film step, also comprise annealing steps, said annealing steps carries out in vacuum annealing furnace.
Aforesaid a kind of anti-hydrofluoric acid corrosive fluid corrosive metal mask preparation method, wherein: the material of multilayer film is a multi-layer C r/Cu metal mask in the said plated film step, multi-layer C r/Pt metal mask or multi-layer C r/Au metal mask.
The invention has the beneficial effects as follows:
1), reduces because the pin hole undercutting that molecule and rete defective cause through taking the multilayer film mode.In the prior art because residual and substrate surface tiny dust particle that external environment causes behind the substrate cleaning; In the film deposition process; The limited particle secondary pollution that causes of the cleanliness factor of the purity of target, the purity of process gas, cavity is through exist the pin hole undercutting after the corrosive fluid immersion inevitably; The probability of particle and defective to occur very little with repeatedly being deposited on the wafer surface same position for rete thickening, can reduce the pin hole undercutting that causes owing to molecule and rete defective.
2) through in cleaning process, adding million cleaning steps, can remove submicron particles.
3) through in wafer cleans; Adopt HF acid or sulfuric acid that wafer is corroded in right amount; When increasing surface microroughness; Also can remove the particle contamination that surface working metamorphic layer and common cleaning are difficult to remove, strengthen the mechanical locking action of mask and wafer, promptly improve the sticking power of mask.
4) through using Ar icon bombardment cleaning wafer surface; Can remove the remaining pollutent of wafer surface to increase sticking power, improve the rete resistance to corrosion, increase ion bombardment power and can make the wafer surface pollution remove more thorough; But the excessive pollutent on surfaces such as coating equipment vacuum-chamber wall, workpiece plate that makes of power is sputtered out; Wafer surface deposits the very thin light blue film of one deck, influences the sticking power of film, and 70～90w is more suitable for bombardment power.
5) improve sticking power through optimizing the substrate storing temperature.Storing temperature is low during plated film, and sticking power is strong inadequately, is prone to cause the side direction undercutting, and the temperature high adhesive force is strong, but thermal stresses is big, is prone to cause the local peeling of rete.
6) through selecting the film material identical or approaching (like Cr etc.) for use, and optimize substrate heating temperature, further reduce thermal stresses with the substrate thermal expansivity.
7) through optimizing substrate temperature, sputtering power, process gas pressure and other parameters, obtain best coating process parameters combination, further reduce the generation of intrinsic stress.
8) through after the plated film step, increasing annealing steps, can release portion stress.
Description of drawings
Fig. 1 is an a kind of anti-hydrofluoric acid corrosive fluid corrosive metal mask preparing method's provided by the invention flow process chart.
Embodiment
Below in conjunction with accompanying drawing and embodiment a kind of anti-hydrofluoric acid corrosive fluid corrosive metal mask preparation method of the present invention is introduced:
Substrate to be coated is an example with quartz crystal and 7740 glass substrates among the embodiment, also can carry out plated film to other substrate.
Embodiment 1
Work flow is as shown in Figure 1:
A. clean: adopt hydrofluoric acid ydrogen peroxide 50 mixed solution, quartz crystal after corrosion is soaked 5～10 minutes under 60～120 ℃ of conditions, is adopted and cleans 5～15min million.
B. plated film: (1) is placed on cleaned quartz substrate in the magnetic control film coating machine, substrate surface is carried out the Ar ion bombardment of 5～10min, ion bombardment power 70～90w earlier; (2) under 100～220 ℃ of temperature, sputtering pressure 0.3～0.8Pa, sputtering power 1.9～2.5Kw condition, make substrate surface plate the Cr film of thickness 30nm and the Cu film of 300nm successively; (3) repeating step (2) at the Cr film of substrate surface plating thickness 30nm and the Cu film of 300nm, forms double-deck Cr/Cu metal mask once more.Also can repeat to plate more multiple layer metal mask as required.The thickness of said film and the type of metal mask can determine according to actual needs, are those skilled in the art's common practise.Also can carry out multicoating through the repeated using thermal evaporation method, thermal evaporation method is those skilled in the art's a common practise.
C. take out substrate after naturally cooling to room temperature, place the vacuum annealing furnace annealing.
Embodiment 2:
A. clean: adopt sulfuric acid to put into the ydrogen peroxide 50 mixed solution, to 7740 glass substrates under 80～120 ℃ of conditions, immersion corrosion about 8～10 minutes after, adopts cleaning 5～10min million.
B. plated film: (1) is placed on cleaned glass substrate in the magnetic control film coating machine, glass substrate surface is carried out the Ar ion bombardment of 5～7min, ion bombardment power 70～80w earlier; (2) under 100～150 ℃, 0.4～0.8Pa, 1.9～2.3Kw power condition, make substrate surface plate the Cr film of thickness 30nm and the Pt film of 300nm successively; (3) repeating step (2) at the Cr film of substrate surface plating thickness 30nm and the Pt film of 300nm, forms double-deck Cr/Pt metal mask once more.
C. take out substrate after naturally cooling to room temperature, place the vacuum annealing furnace annealing.
Embodiment 3:
A. clean: adopt the dioxysulfate water mixed liquid, 7740 glass substrates behind immersion corrosion 5～7min under 100～120 ℃ of conditions, are adopted and clean 5～8min million.
B. plated film: (1) is placed on cleaned glass substrate in the magnetic control film coating machine, substrate surface is carried out the Ar ion bombardment of 5～6min, ion bombardment power 70～80w earlier; (2) under 120～150 ℃, 0.6～0.8Pa, 1.9～2.2Kw power condition, make substrate surface plate the Cr film of thickness 30nm and the Au film of 300nm successively; (3) repeating step (2) at the Cr film of substrate surface plating thickness 30nm and the Au film of 300nm, forms double-deck Cr/Au metal mask once more.
C. take out substrate after naturally cooling to room temperature, place the vacuum annealing furnace annealing.
Present method takes the cleaning measure to remove the particle contamination that surface working metamorphic layer and common cleaning are difficult to remove; Improve substrate surface quality, degree of cleaning, reduced the unrelieved stress that substrate is processed; Increase surface microroughness, the undercutting hole number and the size of corrosion back mask reduce; In the further clean wafers surface amounts of residual contamination do of filming process ion bombardment; Increase adhesive force of mask, improve the rete resistance to corrosion, corrosion back undercutting hole number and size and skin effect phenomenon reduce; Adopt layered mask to reduce particle contamination; Also further reduce undercutting hole number and size, utilize naturally cooling and annealing way can reduce and discharge the unrelieved stress between film, the rete, the film skin effect phenomenon after the annealing obviously reduces.Adopt the mask of present method preparation to soak in the HF corrosive fluid of concentration 35～45% more than 20 hours, realize that thickness reaches the quartz construction device chemistry corrosion processing of 1.2mm 70～85 ℃ of temperature.
Claims (1)
1. an anti-hydrofluoric acid corroding metal mask preparation method comprises the steps:
Cleaning step: said cleaning step comprises that adopting hydrofluoric acid ydrogen peroxide 50 mixed solution or dioxysulfate water mixed liquid to treat film plating substrate corrodes step of soaking and the step of cleaning for million; Said corrosion is immersed under 60～120 ℃ of conditions to be carried out, and the corrosion soak time is 5～10 minutes; Said million scavenging periods are 5～15min;
The plated film step; Said plated film step specifically comprises:
Treat the film plating substrate surface and carry out Ar ion bombardment, the time is 5～10min, ion bombardment power 70～90w;
Adopt the magnetron sputtering mode to treat the step of film plating substrate plated film, the plated film condition is: 100～220 ℃ of temperature, sputtering pressure 0.3～0.8Pa, sputtering power 1.9～2.5Kw;
Institute's plated film is that multi-layer film structure and material are multi-layer C r/Cu metal mask, multi-layer C r/Pt metal mask or multi-layer C r/Au metal mask;
After said plated film step, also comprise annealing steps, said annealing steps carries out in vacuum annealing furnace.
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| CN102810464B (en) * | 2011-06-02 | 2015-07-01 | 无锡华润上华半导体有限公司 | Photoetching method |
| CN107299318B (en) * | 2017-05-31 | 2019-07-12 | 北京航天控制仪器研究所 | A kind of metal mask preparation method of resistance to BOE corrosion |
| CN108569850A (en) * | 2018-07-05 | 2018-09-25 | 深圳大学 | A kind of multiple layer metal mask seed layer and its manufacturing method for glass HF corrosion |
| CN110429158A (en) * | 2019-07-04 | 2019-11-08 | 云南师范大学 | The wet etching method of non-refrigerated infrared focal plane probe optical window |
| CN110845146A (en) * | 2019-10-10 | 2020-02-28 | 中国工程物理研究院电子工程研究所 | Composite mask structure for glass corrosion and glass corrosion method |
| CN110863175A (en) * | 2019-12-04 | 2020-03-06 | 深圳市腾深显示技术有限公司 | Surface treatment method of metal mask plate |
| CN111232915B (en) * | 2020-01-20 | 2023-10-10 | 北京晨晶电子有限公司 | Multi-layer mask layer structure, preparation method thereof and MEMS device |
| CN112666789B (en) * | 2020-12-02 | 2024-05-24 | 湖南普照信息材料有限公司 | Attenuation type high-uniformity phase shift photomask blank and preparation method thereof |
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| CN101424873A (en) * | 2008-12-11 | 2009-05-06 | 湖南普照信息材料有限公司 | Photo mask using soda-lime glass as substrate and method for manufacturing same |
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