CN107299318A - A kind of metal mask preparation method of resistance to BOE corrosion - Google Patents
A kind of metal mask preparation method of resistance to BOE corrosion Download PDFInfo
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- CN107299318A CN107299318A CN201710399984.9A CN201710399984A CN107299318A CN 107299318 A CN107299318 A CN 107299318A CN 201710399984 A CN201710399984 A CN 201710399984A CN 107299318 A CN107299318 A CN 107299318A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/40—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal all coatings being metal coatings
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/25—Metals
- C03C2217/251—Al, Cu, Mg or noble metals
- C03C2217/254—Noble metals
- C03C2217/255—Au
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/25—Metals
- C03C2217/257—Refractory metals
- C03C2217/26—Cr, Mo, W
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/154—Deposition methods from the vapour phase by sputtering
- C03C2218/156—Deposition methods from the vapour phase by sputtering by magnetron sputtering
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/31—Pre-treatment
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The present invention relates to a kind of metal mask preparation method of resistance to BOE corrosion, the preparation method of the metal mask layer of resistance to BOE corrosion is particularly coated with quartz crystal.The present invention specifically includes cleaning step and plating steps.The present invention remarkable result be：1. realize and carry out the etching process of resistance to BOE with individual layer Cr/Au mask layers；2. the problems such as solving and occur surface undercutting, bulge after existing Cr/Au mask layers corrosion, or even come off；3. individual layer Cr/Au mask layers transfer litho pattern precision is high, can control within 1um；4. preparation process is simple, it is easy to control, and prepares with low cost, suitable batch production.
Description
Technical field
The invention belongs to the preparation method of metal mask, the metal that resistance to BOE corrosion is particularly coated with quartz crystal is covered
The preparation method of film layer.
Background technology
Quartz crystal is that one kind is shaken the extraordinary piezoelectric of frequency stability, is frequently used for preparing quartzy sound in inertia field
The sensitive structures such as fork.The processing of quartz crystal structure mainly use BOE wet corrosion techniques, specifically include quartz crystal cleaning,
The steps such as metal mask preparation, photoetching and BOE corrosion.BOE corrosion needs plated film quartz crystal being placed in corrosive liquid for a long time
Immersion, thus metal mask resistance to BOE corrosivity be shaping structures key point.The metal of conventional resistance to BOE corrosion at present
The method of mask mainly by plating multilayer film production, this method has the following disadvantages：
(1) preparation process of multilayer film is complicated, and operating process is very easy to pollute sample, and influence film layer is attached
Put forth effort；
(2) because follow-up plating membrane sample needs to carry out photoetching process to realize that structure graph is shifted, in corrosion multiple layer metal
During film, side undercut necessarily causes pattern line loss of significance；
(3) preparation of multilayer film needs to carry out multiple coating process process, and efficiency is low, and cost is high, is not suitable for batch production.
The content of the invention
The purpose of the present invention：Be in view of the shortcomings of the prior art there is provided a kind of technical process is simple, it is lower-cost resistance to
The preparation method of the single-layer metal film of BOE corrosion.
The technical solution adopted in the present invention is：
A kind of metal mask preparation method of resistance to BOE corrosion, step is as follows：
Step a：Object to be coated is cleaned；
Step b；Coating film treatment is carried out to the object after cleaning；
When carrying out coating film treatment, using individual layer Cr/Au masks.
The step a is specially：Object is placed in the concentrated sulfuric acid and hydrogen peroxide mixing cleaning fluid and soaked.
The mixing rinse liquid temperature is 80~130 DEG C, 15~30min of soak time.
The step b carries out coating film treatment to the object after cleaning, specifically includes following steps：
(1) object after cleaning is put into sputtering coating equipment, carries out vacuumize process；
(2) Cr films are plated by the way of magnetron sputtering；
(3) Au films are plated by the way of magnetron sputtering；
(4) natural cooling is carried out to the object after plated film.
Step (1) vacuumize process is specially to be evacuated to below 5E-7Torr.
The step (2) is when Cr films are plated by the way of magnetron sputtering, sputter gas is N2With Ar gaseous mixture, gas is sputtered
Press as 5~10mTorr, coating temperature is 100~350 DEG C, sputtering power is 100~300W.
The step (3) is when Au films are plated by the way of magnetron sputtering, sputter gas is Ar, and sputtering pressure is 5~
10mTorr, coating temperature is 100~350 DEG C, and sputtering power is 100~300W.
N2With N in Ar gaseous mixture2Shared volume ratio is 40%~60%.
The object is quartz crystal, quartz glass or monocrystalline silicon.
What the present invention was brought compared with prior art has the beneficial effect that：
(1) in cleaning step, by heating the concentrated sulfuric acid and hydrogen peroxide mixing cleaning fluid, sample table flour can effectively be removed
Dirt, particulate matter and organic pollution, improve the adhesive force of subsequent metal mask；
(2) present invention is passed through a certain proportion of N using when plating Cr films2Preparing monofilm realizes the resistance to BOE of metal mask
Etching characteristic, the method for realizing the metal mask etching characteristic of resistance to BOE relative to use multilayer film process for plating conventional at present,
Ensure to simplify technological process while performance, reduce cost；
(3) because follow-up plating membrane sample needs to carry out photoetching process to realize that structure graph is shifted, single-layer metal film is corroded
Obtained pattern line precision is high, can control within 1um, is conducive to improving the sample structure precision after BOE corrosion；
(4) the natural cooling step after being terminated by coating process, it is possible to reduce due to caused by heating in technical process
Plate membrane stress.
Brief description of the drawings
Fig. 1 is the process chart of the inventive method.
Embodiment
The invention will be further described with reference to the accompanying drawings and examples：
In BOE wet corrosion techniques, it will usually serve as mask using Cr/Au metal films are coated with target surface
Layer.BOE is HF and NH4The mixed solution that F is prepared with certain proportion, with stronger corrosivity, the individual layer that conventional method is coated with
The corrosion resistance of Cr/Au mask layers can not meet the requirement of BOE wet corrosion techniques, and general use is coated with multi-layer C r/Au at present
Metal film improves the resistance to BOE corrosivity of mask layer.The present invention is made by being passed through a certain proportion of nitrogen in plating Cr film steps
The corrosion resistance for obtaining be coated with individual layer Cr/Au mask layers meets the requirement of BOE wet corrosion techniques.
As shown in figure 1, the present invention proposes a kind of metal mask preparation method of resistance to BOE corrosion, step is as follows：
Step a：Object to be coated is cleaned；
Specially：Object is placed in the concentrated sulfuric acid and hydrogen peroxide mixing cleaning fluid and soaked.It is 80 to mix rinse liquid temperature
~130 DEG C, 15~30min of soak time.The concentrated sulfuric acid and hydrogen peroxide mixing can produce a large amount of bubble (O2) and discharge heat, bubble
The dust and particle deposition of target surface can be taken away, the concentrated sulfuric acid can erode organic pollution, and heating is conducive to target
Thing thoroughly cleaning is clean.
Step b；Coating film treatment is carried out to the object after cleaning；
The main innovation of the present invention is concentrated on：When carrying out coating film treatment, using individual layer Cr/Au masks.It is many with current technology
Layer Cr/Au masks are compared, and the advantage of the individual layer wet etching of resistance to BOE Cr/Au masks is huge, mainly includes：1. technological process is simple,
Only need to carry out a Cr/Au mask coating operation, greatly save the process time；2. process costs are cheap, the technique of monofilm into
The half of this only multilayer film is even lower；3. subsequent diagram transfer precision is high, it is ensured that pattern line precision 1um with
It is interior, and multilayer film is extremely difficult to same precision；4. mask ply stress is small, monofilm can be reduced preferably by different metal material
Expect the mask layer stress value that coefficient of thermal expansion different band is come.
Coating film treatment, specifically includes following steps：
(1) object after cleaning is put into sputtering coating equipment, carries out vacuumize process；Vacuumize process is specific
To be evacuated to below 5E-7Torr, sputtering coating equipment is equipment generally in the art, it is also possible to which thermal evaporation filming equipment is carried out
Plated film, manufacturer, model of filming equipment etc. are not limited, and sputter coating principle is known in the art general knowledge；
(2) Cr films are plated by the way of magnetron sputtering；Filming parameter is as follows：Sputter gas is N2With Ar gaseous mixture, splash
Pressure of emanating is 5~10mTorr, and coating temperature is 100~350 DEG C, and sputtering power is 100~300W.N2With N in Ar gaseous mixture2
Shared volume ratio is 40%~60%.
(3) Au films are plated by the way of magnetron sputtering；Filming parameter is as follows：Sputter gas is Ar, sputtering pressure is 5~
10mTorr, coating temperature is 100~350 DEG C, and sputtering power is 100~300W；
(4) natural cooling is carried out to the object after plated film.
Present invention is described using quartz crystal substrate as object to be coated for following embodiments.
Embodiment one：
Step a, cleaning：Quartz crystal substrate is put into H2O2：Dense H2SO4=1：In 3 proportions cleaning fluid, plus
Heat soaks 20~30min to 110 DEG C, and taking-up is cleaned with warm water.
Step b, plated film：1. the quartz crystal substrate for cleaning drying is put into sputter coating machine, is evacuated to 3E-
7Torr；2. heated quartz crystal substrates are to 320 DEG C or so；3. Ar and N is flowed into2, change N2Shared volume ratio carries out A, B, C, D, E
Totally 5 groups of contrast tests, A, B, C, D, E N2Shared volume ratio is respectively 20%, 40%, 50%, 60% and 80%, keeps sputtering
Chamber air pressure is 5mTorr, and sputtering power is 150W, completes the thick Cr films of 30nm and is coated with；4. Ar is flowed into, holding sputtering chamber air pressure is
10mTorr, sets sputtering power as 200W, completes the thick Au films of 200nm and is coated with；5. room temperature is naturally cooled to, plated film stone is taken out
English crystal substrates.
The quartz crystal substrate for being coated with individual layer Cr/Au masks obtained in respectively testing A, B, C, D, E is placed in temperature and is
60~80 DEG C of BOE (40%HF solution:40%NH4F solution=1:1) in corrosive liquid, soak 30 hours.Corrosion results are carried out
Analysis, the quartz crystal substrate surface individual layer Cr/Au masks in B, C, D experiment stand intact, and resistance to BOE corrosivity is very good；A and
There is bulge in quartz crystal substrate surface individual layer Cr/Au masks in E experiments, and a small amount of undercutting hole occur, it is impossible to meet mask layer
The resistance to corrosive demands of BOE.
Embodiment two：
Step a, cleaning：Quartz crystal substrate is put into H2O2：Dense H2SO4=1：In 5 proportions cleaning fluid, plus
Heat soaks 15~25min to 130 DEG C, and taking-up is cleaned with warm water.
Step b, plated film：1. the quartz crystal substrate for cleaning drying is put into sputter coating machine, is evacuated to setting value
1E-7Torr；2. heated quartz crystal substrates are to 240 DEG C or so；3. Ar and N is flowed into2, N2Shared volume ratio 55%, keeps sputtering
Chamber air pressure is 10mTorr, and sputtering power is 150W, completes the thick Cr films of 20nm and is coated with；4. Ar is flowed into, holding sputtering chamber air pressure is
10mTorr, sets sputtering power as 200W, completes the thick Au films of 300nm and is coated with；5. room temperature is naturally cooled to, plated film stone is taken out
English crystal substrates.
The quartz crystal substrate for being coated with individual layer Cr/Au masks of acquisition is placed in the BOE (40%HF that temperature is 40~60 DEG C
Solution:40%NH4F solution=1:2) in corrosive liquid, soak 20 hours.Corrosion results are analyzed, quartz crystal substrate table
Face individual layer Cr/Au masks stand intact, and resistance to BOE corrosivity is very good.
Individual layer Cr/Au metal masks prepared by the inventive method are in BOE (the 40%HF solution that temperature is 60 DEG C:40%
NH4F solution=1:1) soaked 35 hours in corrosive liquid, complete thickness and be molded for 300um quartz crystal structure.
The content not being described in detail in description of the invention belongs to the known technology of those skilled in the art.
Claims (9)
1. a kind of metal mask preparation method of resistance to BOE corrosion, step is as follows：
Step a：Object to be coated is cleaned；
Step b；Coating film treatment is carried out to the object after cleaning；
It is characterized in that：When carrying out coating film treatment, using individual layer Cr/Au masks.
2. a kind of metal mask preparation method of resistance to BOE corrosion as claimed in claim 1, it is characterised in that：The step a tools
Body is：Object is placed in the concentrated sulfuric acid and hydrogen peroxide mixing cleaning fluid and soaked.
3. a kind of metal mask preparation method of resistance to BOE corrosion as claimed in claim 2, it is characterised in that：The mixing is clear
Wash temperature is 80~130 DEG C, 15~30min of soak time.
4. a kind of metal mask preparation method of resistance to BOE corrosion as claimed in claim 1, it is characterised in that：B pairs of the step
Object after cleaning carries out coating film treatment, specifically includes following steps：
(1) object after cleaning is put into sputtering coating equipment, carries out vacuumize process；
(2) Cr films are plated by the way of magnetron sputtering；
(3) Au films are plated by the way of magnetron sputtering；
(4) natural cooling is carried out to the object after plated film.
5. a kind of metal mask preparation method of resistance to BOE corrosion as claimed in claim 4, it is characterised in that：The step (1)
Vacuumize process is specially to be evacuated to below 5E-7Torr.
6. a kind of metal mask preparation method of resistance to BOE corrosion as claimed in claim 4, it is characterised in that：The step (2)
When Cr films are plated by the way of magnetron sputtering, sputter gas is N2With Ar gaseous mixture, sputtering pressure is 5~10mTorr, plated film
Temperature is 100~350 DEG C, and sputtering power is 100~300W.
7. a kind of metal mask preparation method of resistance to BOE corrosion as claimed in claim 4, it is characterised in that：The step (3)
When Au films are plated by the way of magnetron sputtering, sputter gas is Ar, and sputtering pressure is 5~10mTorr, coating temperature is 100~
350 DEG C, sputtering power is 100~300W.
8. a kind of metal mask preparation method of resistance to BOE corrosion as claimed in claim 6, it is characterised in that：N2With Ar mixing
N in gas2Shared volume ratio is 40%~60%.
9. such as a kind of metal mask preparation method of resistance to BOE corrosion according to any one of claims 1 to 8, it is characterised in that：
The object is quartz crystal, quartz glass or monocrystalline silicon.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710399984.9A CN107299318B (en) | 2017-05-31 | 2017-05-31 | A kind of metal mask preparation method of resistance to BOE corrosion |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710399984.9A CN107299318B (en) | 2017-05-31 | 2017-05-31 | A kind of metal mask preparation method of resistance to BOE corrosion |
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| CN107299318A true CN107299318A (en) | 2017-10-27 |
| CN107299318B CN107299318B (en) | 2019-07-12 |
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Cited By (3)
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| 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 |
| CN111232915A (en) * | 2020-01-20 | 2020-06-05 | 北京晨晶电子有限公司 | Multilayer mask layer structure, preparation method thereof and MEMS device |
| CN111498797A (en) * | 2020-03-31 | 2020-08-07 | 北京航天控制仪器研究所 | Manufacturing method of wafer-level glass cavity |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111232915A (en) * | 2020-01-20 | 2020-06-05 | 北京晨晶电子有限公司 | Multilayer mask layer structure, preparation method thereof and MEMS device |
| 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 |
| CN111498797A (en) * | 2020-03-31 | 2020-08-07 | 北京航天控制仪器研究所 | Manufacturing method of wafer-level glass cavity |
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| CN107299318B (en) | 2019-07-12 |
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