CN105693102B - The harsh etching method of quartz glass acid etch mask and quartz glass pendulum - Google Patents
The harsh etching method of quartz glass acid etch mask and quartz glass pendulum Download PDFInfo
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- CN105693102B CN105693102B CN201610019313.0A CN201610019313A CN105693102B CN 105693102 B CN105693102 B CN 105693102B CN 201610019313 A CN201610019313 A CN 201610019313A CN 105693102 B CN105693102 B CN 105693102B
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- quartz glass
- mask
- pendulum
- etching method
- glass substrate
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Classifications
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- 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
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/26—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment
- C08L23/28—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment by reaction with halogens or compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/26—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment
- C08J2323/28—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment by reaction with halogens or halogen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
Abstract
The present invention relates to a kind of quartz glass acid etch mask and the harsh etching methods of quartz glass pendulum.The mask is using fluorine carbon paste as matrix, and by adding the curing agent of its mass fraction 5 15%, 1 20% diluent adjusts latex film property;Wherein, the fluorine carbon paste is the polymer that fluorine atom some or all of replaces in polyethylene or polypropylene hydrogen atom to obtain.The mask hydrofluoric acid resistant performance is excellent, and with the harsh etching method of above-mentioned mask without special brass, Teflon mold, dimensional accuracy is high, and can reduce processing cost.
Description
Technical field
The present invention relates to the preparation methods of a kind of mask and quartz glass pendulum, more particularly to a kind of quartz glass acid
The harsh etching method of etching mask and quartz glass pendulum.
Background technology
Currently, the harsh etching technique of quartz glass pendulum flexible beam using the special etched mold such as brass, tetrafluoroethene and
Acidproof fluorine silicone rubber mask protection is not required to etched portions, so that acidproof mask and quartz glass is in close contact by pressing mold;It is logical
The method processing mask for crossing mechanical compaction or laser cutting, is allowed to identical as platen shape, only exposes rectangular opening to etch stone
English glass pendulum flexible beam, then place it in a certain concentration and the hydrofluoric acid solution of temperature and carry out acid etch.
However it is had the following disadvantages in the above method:(1) fluorine silicone rubber can not long-time hydrofluoric acid resistant;(2) it is to ensure pendulum
Piece flexible beam is unanimous between the higher and lower levels and bilateral symmetry is processed into the dimensional accuracy height of special die center platen so as to cause mold
This height;(3) also it is difficult to ensure that pressing plate, mask, pendulum three assemble alignment during the installation process, batch consistency is poor.
Invention content
It is a primary object of the present invention to provide the harsh of a kind of quartz glass acid etch mask and quartz glass pendulum
Etching method, the technical problem to be solved is that so that quartz glass acid etch mask is had prolonged tolerance energy to hydrofluoric acid
Power, and it is made to can be applied in the harsh etching method of quartz glass pendulum, thus more suitable for practicality.
The object of the invention to solve the technical problems is realized using following technical scheme.The present invention proposes a kind of
Quartz glass acid etch mask, using fluorine carbon paste as matrix, by adding the curing agent of its mass fraction 5-15%, 1-20%
Diluent adjusts latex film property;Wherein, the fluorine carbon paste is some or all of in fluorine atom substitution polyethylene or polypropylene
The polymer that hydrogen atom obtains.
Preferably, quartz glass acid etch mask is to mix the fluorine carbon paste, curing agent and diluent, stirring,
Stand what 30-45min was obtained.
The present invention also proposes a kind of harsh etching method of quartz glass pendulum, includes the following steps:
(1) mask coats:Mask is coated on quartz glass substrate surface, the mask covers the quartz glass substrate
All surfaces, the mask are quartz glass acid etch mask above-mentioned;
(2) pattern is cut:After the mask carries out spontaneous curing on the quartz glass substrate, in the mask
On be cut into predetermined pattern, remove the mask in predetermined pattern, expose quartz glass substrate;
(3) it is heating and curing:The quartz glass substrate of the mask with predetermined pattern is heated, increase mask with
The adhesive force of Quartz glass surfaces;
(4) it etches:It is performed etching in merging hydrofluoric acid solution;
(5) demoulding:After etching, whole masks of Quartz glass surfaces are removed.
Preferably, the harsh etching method of the quartz glass pendulum, wherein the mask coating includes:In quartzy glass
The first surface of glass substrate coats mask, and carries out spontaneous curing;Then, it is covered in the second surface of quartz glass and side coating
Film.
Preferably, the harsh etching method of the quartz glass pendulum, the cutting pattern include being cut using laser
It cuts, the mask on the laser while two surfaces of glass-cutting substrate.
Preferably, the harsh etching method of the quartz glass pendulum, the laser are saturating to the quartz glass substrate
It crosses rate and is more than 85%.
Preferably, the harsh etching method of the quartz glass pendulum, it is described be heating and curing including:By glass substrate and glue
Film is heated to 50-80 DEG C, and keeps 30-180min.
Preferably, the harsh etching method of the quartz glass pendulum, the demoulding include:By the pendulum leaching after etching
In organic solvent, until mask is completely dissolved, the organic solvent is ethyl alcohol or acetone to bubble.
Preferably, the mask coating of the harsh etching method of the quartz glass pendulum, the Quartz glass surfaces is thick
Degree is 0.05-0.2mm.
Preferably, the harsh etching method of the quartz glass pendulum, perform etching in the hydrofluoric acid solution including:
Etch rate 1.0-2.0um/min, etch period are more than 250min.
By above-mentioned technical proposal, the harsh etching method of quartz glass acid etch mask and quartz glass pendulum of the present invention
At least there are following advantages:
Quartz glass acid etch mask proposed by the present invention, by using fluorine carbon paste as primary raw material and by with it is solid
The cooperation of agent and diluent has successfully obtained a kind of mask glue to hydrofluoric acid with well tolerable performance, in -50-120
It DEG C can be used for a long time, long to the tolerance time of a concentration of 40% hydrofluoric acid, the glued membrane of 0.1mm thickness is at 20 DEG C, 40% levels of hydrogen fluorine
Impregnated in acid solution 20 hours anacidities it is swollen, deformation occur.
The harsh etching method of the quartz glass pendulum of the present invention, by coating above-mentioned quartz glass acid etch mask,
Brass and Teflon mold in the prior art are saved, is avoided since pressing plate and mask, pressing plate and pressing plate position uneven make
At pendulum etched features it is asymmetric, upper and lower mask can once be cut by using to the high saturating laser of quartz glass
Type improves the dimensional accuracy of quartz glass pendulum.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, it is described in detail as after with presently preferred embodiments of the present invention below.
Specific implementation mode
It is of the invention to reach the technological means and effect that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Preferred embodiment, it is specific real to a kind of preparation method of the quartz glass pendulum acid etch mask proposed according to the present invention
Mode, structure, feature and its effect are applied, is described in detail as after.In the following description, different " embodiment " or " embodiment "
What is referred to is not necessarily the same embodiment.In addition, the special characteristic, structure or feature in one or more embodiments can be by any conjunction
Conformal formula combination.
Embodiment 1
The embodiment of the present invention proposes a kind of quartz glass acid etch mask, using fluorine carbon paste as matrix, by adding it
The curing agent of mass fraction 5-15%, the diluent of 1-20% adjust latex film property;Wherein, the fluorine carbon paste takes for fluorine atom
For the polymer that hydrogen atom obtains some or all of in polyethylene or polypropylene, solid content is more than 50%.Above-mentioned quartzy glass
The specific preparation method of glass acid etch mask is to mix the fluorine carbon paste, curing agent and diluent, and stirring stands 30-
Bubble in glue is discharged in 45min.The curing agent and diluent is used cooperatively with above-mentioned fluorine carbon paste:Curing agent is not only fluorine
The necessary material of carbon paint drying, even more the important composition ingredient of fluorine carbon paste film forming matter;The effect of diluent is to adjust glue to glue
Degree, so as to coat or spray with glass surface and control film thickness, amount of diluent is higher, is more easy to get relatively thin glue
Film.Fluorine carbon paste, curing agent, the diluent of the hydrofluoric acid resistant are the production of Shanghai Dubbo Paar new material Science and Technology Ltd.
DB-60 series, wherein fluorine carbon paste are hydrogen moieties in polyethylene or Polypropylene structural or all are replaced by fluorine atoms to be formed
Fluoroolefins vinyl ether co-polymer, molecular formula is as follows:
Wherein, fluorine content is more than 19%, adjusts glue weatherability;R1 and R2 is alkyl, and it is soluble, transparent that glue is adjusted
Property, glossiness, hardness and flexibility;R3 and R4 is alkylidene, adjusts glue curability, adhesion and pigment score respectively
Property.
The film of formation can be used for a long time at -50-120 DEG C, hydrofluoric acid resistant solution.
Curing agent is crosslinked with the hydroxyl on fluorine carbon paste strand and is reacted for aliphatic isocyanates, formation-NH-
CO- keys.
Diluent is butyl acetate, can dissolve film forming polymer, adjust the viscosity and rheological characteristic of glue.
According to the method for the above embodiments, the following instance for the quartz glass acid etch mask being prepared, tool
The composition of body and as shown in table 1 below to the tolerance time of hydrofluoric acid, wherein the glued membrane that the tolerance time refers to 0.1mm thickness exists
40% hydrofluoric acid impregnates the time for starting to occur falling off in 20 DEG C of hydrofluoric acid solutions.
1 quartz glass acid etch of table is specifically formed with mask and to the tolerance time of hydrofluoric acid
Embodiment 2
The embodiment of the present invention also proposes a kind of harsh etching method of quartz glass pendulum flexible beam, includes mainly:Mask
Coating cutting pattern, is heating and curing, etches and demoulding.
The mask coating step is to coat mask on quartz glass substrate surface, the mask covers the quartz
The all surfaces of glass substrate, the mask are above-mentioned quartz glass acid etch mask, the Quartz glass surfaces
Mask coating thickness be 0.05-0.2mm;Preferably, mask first is coated in the first surface of quartz glass substrate, and carried out certainly
So solidification;Then, mask is coated in the second surface of quartz glass and side, then carries out spontaneous curing.The spontaneous curing
Refer in room temperature environment, glued membrane about 8-10h under curing agent effect completes solidification, and the glued membrane through spontaneous curing is flexible, with glass
Glass substrate adhesive force is weaker, is easily peeled off under external force.
The cutting pattern step is, after the mask carries out spontaneous curing on the quartz glass substrate,
It is cut into predetermined pattern on the mask, removes the mask in predetermined pattern, exposes quartz glass substrate;Preferably, institute
The cutting pattern stated is using laser cutting, and the laser is to use near ultraviolet to near-infrared laser, in this wave band quartz glass
Transmitance 85% or more, laser can glass-cutting substrate two sides simultaneously glued membrane, so that it is guaranteed that the etching on quartz glass two sides
The consistency of position.Glued membrane is removed with tweezers or other tools after laser cutting, so that glass substrate is exposed and needs acid etch
Position.
The heat-curing step is to heat the quartz glass substrate of the mask with predetermined pattern,
Increase the adhesive force of mask and Quartz glass surfaces;Preferably, glass substrate and glued membrane are slowly heated to 50-80 DEG C, constant temperature 30-
180min thoroughly excludes the diluent components in glued membrane;Glued membrane hardness increases after being heating and curing, and also increases with glass attachment power,
Outer force effect cannot remove glued membrane.
The etch step will perform etching in the quartz glass substrate merging hydrofluoric acid solution after solidification, described
Hydrofluoric acid concentration is 40% (mass fraction), and 20 DEG C of etch rate 1.0-2.0um/min, etch period is more than 250min.
The demoulding step after etching, removes whole masks of Quartz glass surfaces.Pendulum after etching is immersed in
It 8-24 hours in organic solvent, or is completely dissolved to mask, the organic solvent is ethyl alcohol or acetone.
Example 6
The harsh etching method of quartz glass pendulum flexible beam, the mask glue described in first preparating example 1.Cleaning glass substrate removes
The impurity such as dust, greasy dirt are used in combination non-dust cloth to wipe substrate clean.Using centrifugation sol evenning machine example 1 is coated to glass substrate
The mask glue.The glass substrate area is 380mm2, often glue amount needed for face is 0.05ml;Glass substrate is fixed on even
Shelves (2-5rad/s) at a slow speed is set as on glue machine, drawing 0.05ml epoxy glues with suction pipe drops in glass substrate first surface center, waits for
Uniformly spontaneous curing 8h is removed in coating to substrate outer to mask glue.The mask glue described in examples detailed above 1 is reconfigured again, with same
It is 0.12mm thick that quadrat method, which gives second surface gluing, the glued membrane,.It can be cut with ultraviolet laser after mask glue spontaneous curing
It cuts.3.8*10.8mm rectangles are cut in pendulum flexible beam position, the rectangle on glass substrate two sides is removed with tweezers, etches pendulum
The mask of flexible beam is molded.The molding substrate of mask is placed on electric furnace, is slowly heated to 50 DEG C, is removed after toasting 60min
Substrate natural cooling, mask fabrication are completed.In 20 DEG C of temperature, hydrofluoric acid concentration 40%, quartz glass etch rate 1.0um/
Under the conditions of min, flexible beam etch period 300min, flexible beam is thinned to 30um, and mask is not permeated, deformed.Pendulum acid etch is complete
Cheng Hou is impregnated 8h in ethanol, and glued membrane is completely dissolved, and next step operation can be carried out by cleaning up.
Example 7
The harsh etching method of quartz glass pendulum flexible beam, the mask glue described in first preparating example 5.Cleaning glass substrate removes
The impurity such as dust, greasy dirt are used in combination non-dust cloth to wipe substrate clean.Glass substrate gluing is given using centrifugation sol evenning machine.It is described
Glass substrate area is 380mm2, often glue amount needed for face is 0.03ml;Glass substrate is fixed on sol evenning machine and is set as shelves at a slow speed
(2-5rad/s) draws 0.03ml epoxy glues with suction pipe and drops in substrate first surface center, wait for glue uniformly outside coating to substrate
Remove spontaneous curing 10h in edge.Above-mentioned glue is reconfigured again, and second surface gluing, the film thickness are given with same method
For 0.07mm.It can be cut with ultraviolet laser after glued membrane spontaneous curing.3.8*10.8mm is cut in pendulum flexible beam position
Rectangle is removed the rectangle on glass substrate two sides with tweezers, and the mask of etching pendulum flexible beam is molded.By the molding base of mask
Piece is placed on electric furnace, is slowly heated to 50 DEG C, removes substrate natural cooling after toasting 30min, mask fabrication is completed.In temperature 20
DEG C, hydrofluoric acid concentration 40%, under the conditions of quartz glass etch rate 1.2um/min, flexible beam etch period 300min, flexible beam
It is thinned to 30um, mask is not permeated, deformed.After the completion of pendulum acid etch, 8h in ethanol is impregnated, glued membrane is completely dissolved,
Next step operation can be carried out by cleaning up.
Example 8:
The harsh etching method of quartz glass pendulum flexible beam, the mask glue described in first preparating example 3.Cleaning glass substrate removes
The impurity such as dust, greasy dirt are used in combination non-dust cloth to wipe substrate clean.Glass substrate gluing is given using centrifugation sol evenning machine.It is known
Glass substrate area is 380mm2, often glue amount needed for face is 0.07ml;Glass substrate is fixed on sol evenning machine and is set as shelves at a slow speed
(2-5rad/s) draws 0.07ml epoxy glues with suction pipe and drops in substrate first surface center, wait for glue uniformly outside coating to substrate
Remove spontaneous curing 9h in edge.Above-mentioned glue is reconfigured again, gives the second surface gluing, the film thickness to be with same method
0.17mm.It can be cut with ultraviolet laser after glued membrane spontaneous curing.3.8*10.8mm squares are cut in pendulum flexible beam position
Shape is removed the rectangle on glass substrate two sides with tweezers, and the mask of etching pendulum flexible beam is molded.By the molding substrate of mask
It is placed on electric furnace, is slowly heated to 80 DEG C, remove substrate natural cooling after toasting 60min, mask fabrication is completed.In temperature 20
DEG C, hydrofluoric acid concentration 40%, under the conditions of quartz glass etch rate 2.0um/min, flexible beam etch period 300min, flexible beam
It is thinned to 30um, mask is not permeated, deformed.After the completion of pendulum acid etch, 10h in ethanol is impregnated, glued membrane is completely dissolved,
Next step operation can be carried out by cleaning up.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, according to
According to the technical spirit of the present invention to any simple modification, equivalent change and modification made by above example, this hair is still fallen within
In the range of bright technical solution.
Claims (10)
1. a kind of quartz glass acid etch mask, which is characterized in that it includes:Using fluorine carbon paste as matrix, by adding its matter
The diluent of the curing agent, 1-20% of measuring score 5-15% adjusts latex film property;Wherein, the fluorine carbon paste replaces for fluorine atom
The polymer that hydrogen atom obtains some or all of in polyethylene or polypropylene.
2. quartz glass acid etch mask according to claim 1, which is characterized in that by the fluorine carbon paste, solidification
Agent and diluent mixing, stirring stand 30-45min.
3. a kind of harsh etching method of quartz glass pendulum, which is characterized in that including:
Mask coats:Mask is coated on quartz glass substrate surface, the mask covers whole tables of the quartz glass substrate
Face, the mask are quartz glass acid etch mask as claimed in claim 1 or 2;
Cut pattern:After the mask carries out spontaneous curing on the quartz glass substrate, cut on the mask
Go out predetermined pattern, remove the mask in predetermined pattern, exposes quartz glass substrate;
It is heating and curing:The quartz glass substrate with predetermined pattern mask is heating and curing, mask and quartz are increased
The adhesive force of glass surface;
Etching:It is performed etching in merging hydrofluoric acid solution;
Demoulding:After etching, whole masks of Quartz glass surfaces are removed.
4. the harsh etching method of quartz glass pendulum according to claim 3, which is characterized in that the mask coating packet
It includes:Mask is coated in the first surface of quartz glass substrate, and carries out spontaneous curing;Then, in the second surface of quartz glass
And side coats mask.
5. the harsh etching method of quartz glass pendulum according to claim 3, which is characterized in that the cutting pattern packet
It includes, using laser cutting, the mask on the laser while two surfaces of glass-cutting substrate.
6. the harsh etching method of quartz glass pendulum according to claim 5, which is characterized in that the laser is to the stone
The transmitance of English glass substrate is more than 85%.
7. the harsh etching method of quartz glass pendulum according to claim 3, which is characterized in that the packet that is heating and curing
It includes:Glass substrate and glued membrane are heated slowly to 50-80 DEG C, and keep 30-180min.
8. the harsh etching method of quartz glass pendulum according to claim 3, which is characterized in that the demoulding includes:It will
Pendulum after etching impregnates in organic solvent, until mask is completely dissolved, the organic solvent is ethyl alcohol or acetone.
9. according to the harsh etching method of claim 3-8 any one of them quartz glass pendulums, which is characterized in that the stone
The mask coating thickness of English glass surface is 0.05-0.2mm.
10. according to the harsh etching method of claim 3-8 any one of them quartz glass pendulums, which is characterized in that described
Performed etching in hydrofluoric acid solution including:1.0-2.0 μm of etch rate/min, etch period are more than 250min.
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US10410883B2 (en) * | 2016-06-01 | 2019-09-10 | Corning Incorporated | Articles and methods of forming vias in substrates |
US10794679B2 (en) | 2016-06-29 | 2020-10-06 | Corning Incorporated | Method and system for measuring geometric parameters of through holes |
US11078112B2 (en) | 2017-05-25 | 2021-08-03 | Corning Incorporated | Silica-containing substrates with vias having an axially variable sidewall taper and methods for forming the same |
US10580725B2 (en) | 2017-05-25 | 2020-03-03 | Corning Incorporated | Articles having vias with geometry attributes and methods for fabricating the same |
CN107915202B (en) * | 2017-11-13 | 2020-04-24 | 东南大学 | Method for rapidly determining any tangential wet etching structure morphology of quartz |
CN108101386A (en) * | 2017-12-18 | 2018-06-01 | 信利光电股份有限公司 | A kind of mobile terminal cover board lithographic method and mobile terminal cover board |
US11554984B2 (en) | 2018-02-22 | 2023-01-17 | Corning Incorporated | Alkali-free borosilicate glasses with low post-HF etch roughness |
CN111847847B (en) * | 2020-07-30 | 2022-05-06 | 保定开拓精密仪器制造有限责任公司 | Preparation method of quartz pendulous reed |
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KR100697979B1 (en) * | 2005-09-26 | 2007-03-23 | 제일모직주식회사 | Antireflective hardmask composition |
CN101154036A (en) * | 2007-09-06 | 2008-04-02 | 北京科技大学 | Method for controlling glass etching depth with optical-controlling method |
CN105223776B (en) * | 2015-11-05 | 2019-05-10 | 吉林大学 | Negative fluorine-contained photoetching compositions and it is used to prepare MZI type thermo-optic switch |
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