CN105895521B - A kind of method of oxide etch - Google Patents
A kind of method of oxide etch Download PDFInfo
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- CN105895521B CN105895521B CN201610161102.0A CN201610161102A CN105895521B CN 105895521 B CN105895521 B CN 105895521B CN 201610161102 A CN201610161102 A CN 201610161102A CN 105895521 B CN105895521 B CN 105895521B
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- monocrystalline silicon
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- hydrofluoric acid
- silicon piece
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- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000000758 substrate Substances 0.000 claims abstract description 27
- 238000005530 etching Methods 0.000 claims abstract description 16
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 37
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 37
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims description 37
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims description 37
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 37
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 29
- 239000003153 chemical reaction reagent Substances 0.000 claims description 23
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 22
- 239000011521 glass Substances 0.000 claims description 13
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 239000000178 monomer Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000003999 initiator Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000004033 plastic Substances 0.000 claims description 4
- 229920003023 plastic Polymers 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical group F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract description 26
- 238000001259 photo etching Methods 0.000 abstract description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 4
- 238000002174 soft lithography Methods 0.000 abstract description 3
- 231100000419 toxicity Toxicity 0.000 abstract description 3
- 230000001988 toxicity Effects 0.000 abstract description 3
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 15
- 239000010408 film Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 8
- 235000013024 sodium fluoride Nutrition 0.000 description 8
- 239000011775 sodium fluoride Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 239000012047 saturated solution Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000001459 lithography Methods 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/311—Etching the insulating layers by chemical or physical means
- H01L21/31105—Etching inorganic layers
- H01L21/31111—Etching inorganic layers by chemical means
-
- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/311—Etching the insulating layers by chemical or physical means
- H01L21/31144—Etching the insulating layers by chemical or physical means using masks
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Physics & Mathematics (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The present invention relates to a kind of methods of oxide etch.Soft lithography relative to conventional lithographic techniques, have the advantages that it is convenient, flexible be easily achieved, moreover it can be used for the complicated space three-dimensional structure of etching.Common etching agent is hydrofluoric acid in photoetching, and hydrofluoric acid has very strong corrosivity and toxicity, is to be not suitable for application in the general laboratory of condition.The substitute of hydrofluoric acid is found, reduces and is endangered caused by being exposed in hydrofluoric acid environment, it is meaningful for photoetching.Fluoride is transferred to target substrate by stamping technique and realizes photoetching under simple condition by this patent, and the harm that hydrofluoric acid is reduced while photoetching is being realized instead of highly toxic hydrofluoric acid using the fluoride of hypotoxicity in patent.
Description
Technical field
The invention belongs to technical field of lithography, and in particular to a kind of method of silica imprint lithography.
Background technology
Coining is one of common soft lithography means in photoetching, which does not need expensive equipment, can realize
The etching of flexible substrates and three-dimensional structure.In recent years research shows that coining soft lithography in sensor, biotechnology and micro- electricity
The fields such as son have broad application prospects.Common etching agent is hydrofluoric acid in the photoetching process of silica, hydrofluoric acid strong toxicity,
Etching will carry out in stringent safeguard, and which has limited its applications under usual experiment condition.Find replacing for hydrofluoric acid
For object, reduction is exposed to the harm brought in hydrofluoric acid environment, undoubtedly meaningful for photoetching.This patent passes through pressure
Fluoride is transferred to target substrate and realizes photoetching under certain condition by print technology, and the fluoride of hypotoxicity is utilized in patent
The harm that hydrofluoric acid is reduced while photoetching is being realized instead of highly toxic hydrofluoric acid.
Invention content
The present invention is directed to stamping technique, it is proposed that a method of utilizing sodium fluoride etching oxidation silicon thin film.
The method of the present invention uses stamped method using surface figuratum dimethyl silicone polymer (PDMS) template as seal, by fluorine
Change sodium (NaF) solution and be transferred to silicon oxide surface, then the held for some time at a certain temperature in salt acid vapour, is aoxidizing
Silicon face etches pattern, completes transfer of the pattern on the surfaces PDMS to silicon oxide surface.
A kind of method of oxide etch of the invention comprises the concrete steps that：
The making of step (1), PDMS seals；
Take monomer：Initiator 10~3：Under 1 ratio, they are mixed, is then ceaselessly stirred using clean glass bar
It mixes about 1~3 hour, ensures that the gas that reaction generates constantly is run out of, while preventing reagent in reaction process from bonding；Stirring 1~3
After hour, obtained mix reagent is a kind of reagent that viscosity is big, and mix reagent is poured on grating, keeps reagent equal with glass bar
Even is coated in grating surface, stands 10~24 hours；After the completion of standing, PDMS is obtained within 5~10 hours in 50~70 DEG C of heating
Elastic film, PDMS film is obtained surface from grating surface mechanical stripping the PDMS seals of grating pattern.
Step (2), the etching of silica.
Surface growth is taken to have the 10mm X 8mm monocrystalline silicon pieces (SiO of 300nm thickness2/ Si), 5~15 are dripped on monocrystalline silicon piece
Microlitre NaF saturated solution solution cuts the PDMS seals of 10mm X 8mm, will be printed on the one side of grating pattern, covers monocrystalline silicon
On piece, being pressed in above seal with the object of 10~50g weights makes PDMS seals be contacted closely, then from monocrystalline silicon with monocrystalline silicon piece
Near piece, 2~10ml hydrochloric acid solutions are added dropwise apart from the place of 1~3cm of monocrystalline silicon piece edge.Whole process is in draught cupboard
It is carried out in the square container of 15mm X 15mm X15mm.PDMS seals are detached with monocrystalline silicon piece after 6~20 hours, are spent
Ionized water cleans monocrystalline silicon piece, and obtaining surface has the monocrystalline silicon piece of etching pattern.
The grating is glass raster, organic plastics grating.
The monocrystalline silicon piece is the substrate or silica glass substrate that monocrystalline silicon surface grows silica film.
Beneficial effects of the present invention：The method of the present invention replaces hydrofluoric acid by sodium fluoride, and sodium fluoride dosage is few, reduces
Toxicity in photoetching process；The photoetching of plane or three-dimensional silica matrices may be implemented using the invention simultaneously, method is simple, square
Just strong with operability.
Specific implementation mode
Embodiment 1：
Step (1), PDMS preparation process：
Monomer 15ml is taken, is put into beaker, then takes initiator 1.5ml, makes monomer：Initiator about 10：It, will under 1 ratio
They are mixed, and then use clean glass bar ceaselessly stir about 1 hour, ensure that the gas that reaction generates constantly is run out of,
Prevent reagent in reaction process from bonding simultaneously；After stirring 1 hour, obtained mix reagent is a kind of reagent that viscosity is big, will be mixed
It closes reagent to be poured on grating, so that reagent is uniformly coated in glass raster surface with glass bar, stand 10 hours；It stands and completes
Afterwards, PDMS elastic films are obtained within 5 hours in 50 DEG C of heating, PDMS film is obtained surface from grating surface mechanical stripping grating
The PDMS seals of pattern.
Step (2), the etching of silica.
Surface growth is taken to have the substrate of the 10mm X 8mm monocrystalline silicon surfaces growth silica film of 300nm thickness, drop 5 micro-
NaF saturated solution solution is risen, the PDMS seals of 10mm X 8mm is cut, there will be the one side for being printed on grating pattern, be covered in monocrystalline
Silicon face is grown on the substrate of silica film, and being pressed in above seal with the object of 10g weights makes PDMS seals be contacted with substrate
Closely, 2 milliliters of hydrochloric acid solutions then are added dropwise in the place apart from substrate edge 1cm.15mm X of the whole process in draught cupboard
It is carried out in the square container of 15mm X 15mm.By PDMS seals and substrate separation after 6 hours, substrate is cleaned with deionized water,
Obtaining surface has the substrate of etching pattern.
Embodiment 2：
Step (1), PDMS preparation process：Monomer 15ml is taken, is put into beaker, then takes initiator 5ml, makes monomer：Cause
Agent about 3：Under 1 ratio, they are mixed, then uses clean glass bar ceaselessly stir about 3 hours, ensures that reaction generates
Gas constantly run out of, while reagent being prevented in reaction process to bond；After stirring 3 hours, obtained mix reagent is a kind of
The big reagent of viscosity, mix reagent is poured on grating, so that reagent is uniformly coated in organic plastics grating surface with glass bar,
Stand 24 hours；After the completion of standing, PDMS elastic films are obtained within 10 hours in 70 DEG C of heating, by PDMS film from grating surface machine
Tool stripping, which obtains surface, the PDMS seals of grating pattern.
Step (2), the etching of silica.
Surface growth is taken to have the 10mm X 8mm silica glass substrates of 300nm thickness, 15 microlitres of NaF saturated solutions of drop molten
Liquid cuts the PDMS seals of 10mm X 8mm, will be printed on the one side of grating pattern, on covering substrate, is pressed in the object of 50g weights
So that PDMS seals is contacted with substrate closely above seal, 10ml hydrochloric acid solutions then are added dropwise in the place apart from substrate edge 3cm.
It is carried out in the square container of 15mm X 15mm X 15mm of the whole process in draught cupboard.After 20 hours by PDMS seals with
Substrate separation cleans substrate with deionized water, and obtaining surface has the substrate of etching pattern.
Embodiment 3：
Step (1), PDMS preparation process：Monomer 10ml is taken, is put into beaker, then takes initiator 2ml, makes monomer：Cause
Agent about 5：Under 1 ratio, they are mixed, then uses clean glass bar ceaselessly stir about 2 hours, ensures that reaction generates
Gas constantly run out of, while reagent being prevented in reaction process to bond；After stirring 2 hours, obtained mix reagent is a kind of
The big reagent of viscosity, mix reagent is poured on grating, so that reagent is uniformly coated in plastic grating surface with glass bar, is stood
15 hours；After the completion of standing, PDMS elastic films are obtained within 7 hours in 60 DEG C of heating, PDMS film is shelled from grating surface machinery
There are the PDMS seals of grating pattern from surface is obtained.
Step (2), the etching of silica.
It takes surface growth to have the 10mm X 8mm silica glass substrates of 300nm thickness, drips 8 microlitres of NaF saturated solution solution,
The PDMS seals for cutting 10mm X 8mm, will be printed on the one side of grating pattern, and on covering substrate, print is pressed in the object of 30g weights
So that PDMS seals is contacted with substrate closely above chapter, 5 milliliters of hydrochloric acid solutions then are added dropwise in the place apart from substrate edge 2cm.
It is carried out in the square container of 15mm X 15mm X 15mm of the whole process in draught cupboard.After 10 hours by PDMS seals with
Substrate separation cleans substrate with deionized water, and obtaining surface has the substrate of etching pattern.
Claims (3)
1. a kind of method of oxide etch, which is characterized in that this method specifically includes following steps：
The making of step (1), PDMS seals；
Take monomer：Initiator 10~3：Under 1 volume ratio, they are mixed, is then ceaselessly stirred using clean glass bar
It mixes 1~3 hour, after stirring 1~3 hour, mix reagent is poured on grating by obtained mix reagent, makes reagent with glass bar
It is uniformly coated in grating surface, stands 10~24 hours；After the completion of standing, obtained within 5~10 hours in 50~70 DEG C of heating
PDMS elastic films, PDMS film is obtained surface from grating surface mechanical stripping the PDMS seals of grating pattern；
Step (2), the etching of silica；
It is the 10mm X 8mm monocrystalline silicon pieces of 300nm to take surface growth to have thickness, and it is full that 5~15 microlitres of NaF are dripped on monocrystalline silicon piece
And solution, the PDMS seals of 10mm X 8mm are cut, the one side of grating pattern will be printed on, are covered on monocrystalline silicon piece, with 10~50g
The object of weight, which is pressed in above seal, makes PDMS seals be contacted with monocrystalline silicon piece closely, and then near from monocrystalline silicon piece, distance is single
2~10ml hydrochloric acid solutions are added dropwise in the place of 1~3cm of crystal silicon chip edge；15mm X 15mm X of the whole process in draught cupboard
It is carried out in the square container of 15mm；PDMS seals are detached with monocrystalline silicon piece after 6~20 hours, monocrystalline is cleaned with deionized water
Silicon chip, obtaining surface has the monocrystalline silicon piece of etching pattern.
2. a kind of method of oxide etch according to claim 1, it is characterised in that：The grating is glass light
Grid, organic plastics grating.
3. a kind of method of oxide etch according to claim 1, it is characterised in that：The monocrystalline silicon piece is monocrystalline
Silicon face grows the substrate of silica film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610161102.0A CN105895521B (en) | 2016-03-21 | 2016-03-21 | A kind of method of oxide etch |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610161102.0A CN105895521B (en) | 2016-03-21 | 2016-03-21 | A kind of method of oxide etch |
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| CN105895521A CN105895521A (en) | 2016-08-24 |
| CN105895521B true CN105895521B (en) | 2018-09-25 |
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| CN107699956A (en) * | 2017-11-17 | 2018-02-16 | 杭州电子科技大学 | A kind of method using two-dimentional molybdenum sulfide etching oxidation silicon |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101082769A (en) * | 2007-06-15 | 2007-12-05 | 中国科学院上海光学精密机械研究所 | Method for copying surface relief microstructure Dammann grating |
| CN102955355A (en) * | 2011-09-26 | 2013-03-06 | 上海市纳米科技与产业发展促进中心 | Method for preparing solvent permeation nanoimprint micro-nano structure |
| CN104238264A (en) * | 2014-09-10 | 2014-12-24 | 清华大学 | Solution-assisted soft imprinting method |
| CN105137712A (en) * | 2015-07-21 | 2015-12-09 | 苏州大学 | Method for constructing organic liquid crystal molecule single crystal micron line array patterning by utilizing nano imprinting technology |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102279517A (en) * | 2010-06-14 | 2011-12-14 | 清华大学 | Nano-imprinting method |
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- 2016-03-21 CN CN201610161102.0A patent/CN105895521B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101082769A (en) * | 2007-06-15 | 2007-12-05 | 中国科学院上海光学精密机械研究所 | Method for copying surface relief microstructure Dammann grating |
| CN102955355A (en) * | 2011-09-26 | 2013-03-06 | 上海市纳米科技与产业发展促进中心 | Method for preparing solvent permeation nanoimprint micro-nano structure |
| CN104238264A (en) * | 2014-09-10 | 2014-12-24 | 清华大学 | Solution-assisted soft imprinting method |
| CN105137712A (en) * | 2015-07-21 | 2015-12-09 | 苏州大学 | Method for constructing organic liquid crystal molecule single crystal micron line array patterning by utilizing nano imprinting technology |
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