CN101037185A - Method for making nano-groove on quartz glass - Google Patents
Method for making nano-groove on quartz glass Download PDFInfo
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- CN101037185A CN101037185A CN 200710036417 CN200710036417A CN101037185A CN 101037185 A CN101037185 A CN 101037185A CN 200710036417 CN200710036417 CN 200710036417 CN 200710036417 A CN200710036417 A CN 200710036417A CN 101037185 A CN101037185 A CN 101037185A
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Abstract
The invention relates to a nano-channel preparing method on a piece of quartz glass, characterized in that the crucial technology for preparing comprises three steps of photoetching, wet etching and linking, wherein the wet etching solution preparation is one of the crucial steps of the MEMS processing technology, and can directly influence the graphic structure of the nano-channels. The invention employs the quartz glass as the substrate material, the technology is simple and has no need of reactive ion etching equipment, and the depth error of the nano-channel can be precisely controlled to be +/-1nm or so by regulating the etching time and temperature on the basis of the prepared etching solution.
Description
Technical field
The present invention relates to the preparation method of nano-channel on a kind of quartz glass, belong to the Micrometer-Nanometer Processing Technology field.
Background technology
Micro-total analysis system (micro total analytical system, μ TAS) claims that again chip lab (Lab-on-a-chip) is the notion that is proposed by Manz et al. in the nineties in last century, be with micro-electromechanical technology (micro-electromechanical systems, MEMS) and analytical chemistry detect and to combine, sample preparation related in the fields such as biological and chemical, biology and chemical reaction, separate, basic operation units such as detection are integrated or be integrated into substantially on more than one square centimeters the chip, in order to finishing different biological or chemical courses of reaction, and the technology that its product is analyzed.Through the development of more than ten years, very fast to development aspect nucleic acid, protein, organic compound and separate inorganic ions, analysis and the detection system on microchip, there has been integrated commercialization micro-total analysis system to occur.Recently the fluid behaviour under the nanoscale is subjected to extensive concern, when line size is reduced to nano-scale, the liquid in its raceway groove will show with the micro-meter scale fluid different fluid behaviour, for example EOF reduces, flow rate of liquid increase etc.This has opened up new field for the research of micro-total analysis system, existing report with the nano-fluid characteristic be applied to that the preenrichment of albumen, supper-fast sample are mixed, the transfer of charged reactant etc.Present stage, the processing nano-channel is mainly used the method for reactive ion etching (RIE), under vacuum state, the gas that feeds reaction chamber is applied radio-frequency power supply, thus gas molecule is dissociated and under the effect of electrode the etching material that needs of accelerating impact negative electrode reach the purpose of etching material.Need special consersion unit also need prepare the reacting gas of different flow according to different materials, and the processing charges costliness.
Summary of the invention
The object of the present invention is to provide a kind of method of making nano-groove on quartz glass, specifically on silica glass material, adopt a kind of preparation method of photoetching, wet etching and the bonding techniques realization nano-groove of standard.Method is easy, uses basic MEMS processing technology, need not special installation.
The key technology that the present invention solves has the following aspects:
1. the configuration of wet etching liquid
Adopted present widely used wet corrosion technique, this is the committed step in the micromachining technology.For wet etching, the pattern of etching depends mainly on the material to be corroded and the composition of corrosive liquid.Therefore the configuration of corrosive liquid directly affects the graphic structure of nano-channel, is the critical process of this preparation method.
2. the control of corrosion depth
In the wet etching, corrosion depth is relevant with a plurality of factors, comprising: the environment temperature of material property, corrosive liquid proportioning, corrosion.Under the prerequisite that material property is determined, the present invention adopts under the water-bath corrodes operation, and the temperature of control corrosion operating environment is at 40 ℃; The proportioning of strict control corrosive liquid.Control the nanoscale Corrosion of Pipeline degree of depth thus.
Specifically, the invention provides a kind of Fabrication of nanostructures method of simple possible, concrete technological process comprises following several committed step:
1. photoetching
To plate the quartz glass plate of chromium layer, used acetone, ethanol and deionized water to clean repeatedly; Use nitrogen to dry up and put to 120 ℃ of oven dry; Evaporation HMDO HMDS again is to increase the surface of glass slide adhesiveness; Under 4000rpm, get rid of photoresist 6809; Go forward to dry by the fire at 100 ℃ of hot plates; Working strength is 12mW/cm
2Litho machine, photoetching 12s; Place the 18s that develops in the developer solution, washed with de-ionized water.
2. wet etching
Plasma is removed the photoresist in the residual pipeline; 120 ℃ of post bakes; Use the chromium corrosive liquid, remove visuals chromium layer; The quartz glass corrosive liquid of putting into 40～50 ℃ of constant temperature stirs, and carries out the nanotubes corrosion.
3. bonding
Use is low-temperature bonding method in water: after the nano-channel corrosion finishes, use washed with de-ionized water, put into the chromium corrosive liquid the remaining chromium layer in surface is removed; Then substrate and cover plate are put into Piranha (volume ratio H
2SO
4: H
2O
2=4: after 1) washing lotion is cleaned; Then at affine washing lotion (volume ratio NH
3H
2O: H
2O: H
2O
2=6: 3: 1) hot plate 30min in, washed with de-ionized water is used in the back; The chip bonding (pre-bonding) of fitting in the water: directly substrate and cover plate are fitted in deionized water, transfer in the vacuum drying chamber then.Set the vacuum drying chamber temperature and be 100 ℃ and open vavuum pump, close vavuum pump after continuing to vacuumize 30min, keep 100 ℃, 2h; Bonding: powered-down cools off naturally after slowly being heated to 200 ℃ of maintenance 6h, realizes the making of nano-groove, can be used for the nano-fluid The Characteristic Study.
Concrete making step sees embodiment 1 and 2 for details, no longer repeats at this.
Nanoscale pipeline of the present invention is that frame is at two microns pipeline enclosure nanotubes or rice font nano-groove chip.
Advantage and beneficial effect that the present invention adopts are:
1. the processing base material of the present invention's employing is a quartz glass, has good little working properties, and with MEMS processing technology compatibility, the source is abundant;
2. machining process of the present invention is simple, does not need specific apparatus such as reactive ion etching;
3. according to the corrosive liquid of preparation, regulate the degree of depth and width that etching time and corrosion temperature can be controlled nano-channel accurately, error is about ± 1nm.
Description of drawings
Fig. 1 nano-channel manufacture craft flow chart
(a) chromium plating on quartz substrate (b) steaming HMDS (c) resist coating 6809 (d) photoetching (e) corrosion chromium layer (f) glass corrosion (g) removes photoresist and chromium layer (h) bonding
Fig. 2 nano-channel structure chart
(a) nano-channel AFM design sketch (b) nano-channel structure photo (in the circle is the nano-channel of frame at two microns pipeline enclosures)
The specific embodiment
The present invention is further illustrated below in conjunction with embodiment:
Embodiment 1:
Make the 50nm nanochannel at the micron pipeline enclosure.
1) photoetching for the first time
1, cleans: use acetone, ethanol and deionized water ultrasonic cleaning substrate 5min successively respectively; Nitrogen dries up; Oven dry (120 ℃) 20min
2, evaporation organosilicon oxide (HMDS); Be coated with 6809 photoresists, with 4000rpm speed whirl coating 30s
3, preceding baking: 100 ℃, 6min
4, photoetching: working strength is 12mW/cm
2Litho machine, photoetching 12s
5, develop: 18s
6, bottoming film 10S
7,120 ℃ of baking oven 30min of post bake
2) trunk line corrosion
1, dechromises: remove visuals chromium layer with chromium corrosive liquid (ammonium ceric nitrate 400g+ perchloric acid 110mL, deionized water is settled to 1.76L)
2, washed with de-ionized water is 10 times
3, glass corrosion: quartz glass corrosive liquid (the volume ratio HF: H that puts into 40-50 ℃ of constant temperature
2O
2: corrosion 40-50min HAC=2: 1: 1), obtain wide 50 microns, dark about 10 microns main channel, regulate the degree of depth and width that etching time and temperature can accurately be controlled nano-channel, error is ± 1nm.
4, washed with de-ionized water is 10 times
3) photoetching for the second time is to make the raceway groove of nanostructured
1, cleans: use acetone, ethanol, deionized water ultrasonic cleaning substrate 5min respectively; Nitrogen dries up; 120 ℃ of oven dry 20min
2, whirl coating, photoresist 6809 4000rpm, 30s thickness: 0.9 μ m
3, preceding baking: 100 ℃, 6min (hot plate)
4, aim at photoetching: employing intensity is 12mW/cm
2Litho machine photoetching 12s
5, develop: 18s
6, bottoming film 10s
7,120 ℃ of baking oven 30min of post bake
4) nanotubes is made
1, dechromises: the chromium layer that removes visuals with chromium corrosive liquid (ammonium ceric nitrate 400g+ perchloric acid 110mL, deionized water is settled to 1.76L)
2, nanometer corrosion: quartz glass corrosive liquid (the volume ratio HF: H that puts into 40-50 ℃ of constant temperature
2O
2: HAC=2: 5: 5) stir, 50-70s, dark about 50nm, according to the corrosive liquid of preparation, to regulate etching time and temperature and can accurately control corrosion depth, error is ± 1nm;
5) punching: spark hole diameter on the substrate relevant position is the hole of 2mm, as liquid storage tank.
6) bonding
1, acetone removes the remained on surface photoresist, ethanol and washed with de-ionized water
2, dechromise in the surface: substrate is put into the chromium corrosive liquid for preparing, the 3min layer that dechromises in ultrasonic pond
3, with acetone, ethanol and deionized water ultrasonic cleaning substrate, cover plate 5min successively
4, the Piranha washing lotion is cleaned.Substrate, cover plate are put into Piranha washing lotion (volume ratio H
2SO
4: H
2O
2=4: 1), hot plate 10～15min; Increase surface affinity; Washed with de-ionized water
5, at affine washing lotion (volume ratio NH
3H
2O: H
2O: H
2O
2=6: 3: 1) hot plate 30min in; Washed with de-ionized water 10-15 time
6, the chip bonding (pre-bonding) of fitting in the water: directly substrate and cover plate are fitted in deionized water, transfer in the vacuum drying chamber then.Set the vacuum drying chamber temperature and be 100 ℃ and open vavuum pump, close vavuum pump after continuing to vacuumize 30min, keep 100 ℃
7, bonding: powered-down cools off naturally after slowly rising to 200 ℃ of 6h, realizes that low-temperature bonding makes the nano-groove chip, is used for the nano-fluid analysis.
Embodiment 2:
Make " rice " font 100nm nanochannel chip.
1) photoetching (nanostructured)
1, cleans: use acetone, ethanol, deionized water ultrasonic cleaning substrate 5min respectively; Nitrogen dries up; Oven dry (120 ℃) 20min
2, whirl coating, photoresist 68094000rpm, 30s thickness: 0.9 μ m
3, preceding baking: 100 ℃, 6min (hot plate)
4, aim at photoetching: employing intensity is 12mW/cm
2Litho machine photoetching 12s
5, develop: 18s
6, bottoming film 10S
7,120 ℃ of baking oven 30min of post bake
2) nanotubes is made
1, dechromises: remove visuals chromium layer with chromium corrosive liquid (ammonium ceric nitrate 400g+ perchloric acid 110mL, deionized water is settled to 1.76L)
2, nanometer corrosion: the quartz glass corrosive liquid (HF: H that puts into 40-50 ℃ of constant temperature
2O
2: HAC=2: 5: 5, volume ratio) stir, 100-120s is dark about 100nm; According to the corrosive liquid of preparation, regulate etching time and temperature, can accurately control the degree of depth of nano-channel, error is about ± 1nm;
3) punching: spark hole diameter on the substrate relevant position is the hole of 2mm, as liquid storage tank.
4) bonding
1, acetone removes the remained on surface photoresist, ethanol and washed with de-ionized water
2, dechromise in the surface: substrate is put into the chromium corrosive liquid for preparing, the 3min layer that dechromises in ultrasonic pond
3, acetone, ethanol, deionized water ultrasonic cleaning substrate, cover plate 5min
4, the Piranha washing lotion is cleaned.Substrate, cover plate are put into Piranha washing lotion (volume ratio H
2SO
4: H
2O
2=4: 1), hot plate 10～15min; Increase surface affinity; Washed with de-ionized water
5, at affine washing lotion (volume ratio NH
3H
2O: H
2O: H
2O
2=6: 3: 1) hot plate 30min in; Washed with de-ionized water 10 times
6, the chip bonding (pre-bonding) of fitting in the water: directly substrate and cover plate are fitted in deionized water, transfer in the vacuum drying chamber then.Set the vacuum drying chamber temperature and be 100 ℃ and open vavuum pump, close vavuum pump after continuing to vacuumize 30min, keep 100 ℃
7, bonding: after slowly rising to 200 ℃ of 6h, powered-down cools off naturally, realizes that low-temperature bonding makes the nano-groove chip, is used for the nano-fluid analysis.
Claims (10)
1, the preparation method of nano-channel on a kind of quartz glass is characterized in that described nanoscale pipeline is that the making step of frame nanotubes between two micron tube is:
A) photoetching for the first time
(a) clean: the quartz glass plate 5min that has plated the chromium layer respectively with acetone, ethanol, deionized water ultrasonic cleaning; Nitrogen dries up; Oven dry;
(b) evaporation HMDO; Be coated with 6809 photoresists, with 4000rpm speed whirl coating;
(c) preceding baking: 100 ℃, 6min;
(d) photoetching: working strength is 12mW/cm
2Litho machine, photoetching 12s;
(e) develop: 18s, and deionization cleans;
(f) bottoming film 10S;
(g) 120 ℃ of baking oven 30min of post bake;
B) trunk line corrosion
(a) dechromise: use by ammonium ceric nitrate 400g+ perchloric acid 110mL, deionized water is settled to the chromium corrosive liquid of 1.76L preparation and removes visuals chromium layer;
(b) washed with de-ionized water is 10 times;
(c) glass corrosion: the volume ratio HF that puts into 40-50 ℃ of constant temperature: H
2O
2: HAC=2: corrode in the quartz glass corrosive liquid of forming at 1: 1, obtain wide 50 microns, dark 10 microns main channel;
(d) washed with de-ionized water is 10 times
C) photoetching for the second time is to make the pipeline of nanostructured
(a) clean: use acetone, ethanol, deionized water ultrasonic cleaning substrate 5min respectively; Nitrogen dries up; Oven dry 20min;
(b) whirl coating, photoresist 6809 4000rpm, 30s thickness: 0.9 μ m;
(c) preceding baking: 100 ℃, 6min;
(d) aim at photoetching: employing intensity is 12mW/cm
2Litho machine photoetching 12s;
(e) develop: 18s;
(f) bottoming film 10s;
(g) 120 ℃ of baking oven 30min of post bake;
D) nanotubes is made
(a) dechromise: use by ammonium ceric nitrate 400g+ perchloric acid 110mL, deionized water is settled to the chromium layer that chromium corrosive liquid that 1.76L is mixed with is removed visuals;
(b) nanometer corrosion: put into 40-50 ℃ of constant temperature by volume ratio HF: H
2O
2: HAC=2: the quartz glass corrosive liquid of forming at 5: 5 stirs, 50-70s, and corrosion depth is 50nm;
E) punching: with spark hole diameter on the substrate relevant position is the hole of 2mm, as liquid storage tank;
F) bonding
(a) acetone removes the remained on surface photoresist, ethanol and washed with de-ionized water;
(b) dechromise in the surface: substrate is put into the chromium corrosive liquid for preparing, the 3min layer that dechromises in ultrasonic pond; Described chromium corrosive liquid is formed identical with (a) among the above-mentioned steps B;
(c) acetone, ethanol, deionized water ultrasonic cleaning substrate, cover plate 5min;
(d) washing lotion is cleaned, and substrate, cover plate are put into volume ratio H
2SO
4: H
2O
2=4: 1 Piranha washing lotion is hotted plate 10～15min; Increase surface affinity; And use washed with de-ionized water;
(e) again at volume ratio NH
3H
2O: H
2O: H
2O
2=6: hot plate 30min in 3: 1 the affine washing lotion; Washed with de-ionized water;
(f) the pre-bonding of applying chip in the water: directly substrate and cover plate are fitted in deionized water, transfer in the vacuum drying chamber then.Set the vacuum drying chamber temperature and be 100 ℃ and open vavuum pump, close vavuum pump after continuing to vacuumize 30min, keep 100 ℃
(g) bonding: after slowly rising to 200 ℃, powered-down cools off naturally, realizes that low-temperature bonding makes the nano-groove chip, is used for the nano-fluid analysis.
2, by the preparation method of nano-channel on the described quartz glass of claim 1, it is characterized in that the bake out temperature of in first time lithography step (a) is 120 ℃, the time is 20 minutes.
3, by the preparation method of nano-channel on the described quartz glass of claim 1, it is characterized in that in the whirl coating time of the lithography step first time (b) be 30s.
4, by the preparation method of nano-channel on the described quartz glass of claim 1, it is characterized in that the quartz glass etching time is 40-50min among (c) in the trunk line corrosion step, according to the corrosive liquid of preparation, adjusting corrosive liquid humidity error is ± 1nm.
5, by the preparation method of nano-channel on the described quartz glass of claim 1, it is characterized in that the bonding time in (g) is 6h in the bonding step.
6, the preparation method of nano-channel on a kind of quartz glass is characterized in that described " rice " font receives the making step of sheet channel chip and be:
A) lithographic nano structure
(a) clean: the quartz glass substrate 5min that has plated the chromium layer respectively with acetone, ethanol, deionized water ultrasonic cleaning; Nitrogen dries up; Oven dry;
(b) whirl coating, photoresist 6809 whirl coating speed are 4000rpm;
(c) preceding baking: 100 ℃, 6min;
(d) aim at photoetching: employing intensity is 12mW/cm
2Litho machine photoetching 12s;
(e) develop: 18s;
(f) bottoming film 10S;
(g) 120 ℃ of baking oven 30min of post bake;
B) nanotubes is made
(a) dechromise: use by ammonium ceric nitrate 400g+ perchloric acid 110mL, deionized water is settled to the chromium corrosive liquid of 1.76L preparation and removes visuals chromium layer;
(b) nanometer corrosion: what put into 40-50 ℃ of constant temperature is HF: H by volume ratio
2O
2: HAC=2: the quartz glass corrosive liquid of forming at 5: 5 stirs, and corrosion depth is 100nm;
C) punching: spark hole diameter on the substrate relevant position is the hole of 2mm, as liquid storage tank;
D) bonding
(a) remove the remained on surface photoresist with acetone earlier, again with ethanol and washed with de-ionized water;
(b) dechromise in the surface: substrate is put into the chromium corrosive liquid for preparing, the 3min layer that dechromises in ultrasonic pond; Described chromium corrodes (a) described composition in the same step (B);
(c) acetone, ethanol, deionized water ultrasonic cleaning substrate, cover plate 5min
(d) washing lotion is cleaned. substrate, cover plate are put into volume ratio H
2SO
4: H
2O
2=4: 1 Piranha washing lotion is hotted plate 10～15min; Increase surface affinity; Washed with de-ionized water;
(e) be NH in volume ratio again
3H
2O: H
2O: H
2O
2=6: hot plate 30min in 3: 1 the affine washing lotion; Washed with de-ionized water;
(f) chip of fitting in the water; Pre-bonding: directly substrate and cover plate are fitted in deionized water, transfer in the vacuum drying chamber then. set the vacuum drying chamber temperature and be 100 ℃ and open vavuum pump, close vavuum pump after continuing to vacuumize 30min, keep 100 ℃;
(g) bonding: after slowly rising to 200 ℃, powered-down cools off naturally, realizes that low-temperature bonding makes the nano-groove chip, is used for the nano-fluid analysis.
7, by the preparation method of nano-channel on the described quartz glass of claim 6, the bake out temperature that it is characterized in that (a) in the lithographic nano configuration steps is 120 ℃, and the time is 20 minutes.
8, by the preparation method of nano-channel on the described quartz glass of claim 6, the whirl coating time that it is characterized in that (b) in the lithographic nano configuration steps is 30s, and thickness is 0.9 μ m.
9, press the preparation method of nano-channel on the described quartz glass of claim 6, it is characterized in that the quartz glass etching time at nanotubes making step (b) removal visuals chromium layer is 100-120s, regulate the time of corrosion and the degree of depth of temperature control nano-channel, error is ± 1nm.
10,, it is characterized in that in the bonding step bonding time is 6h under 200 ℃ of conditions by the preparation method of nano-channel on the described quartz glass of claim 6.
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|---|---|---|---|
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|---|---|---|---|
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| CN108658036B (en) * | 2018-04-16 | 2019-02-26 | 广东工业大学 | A kind of synchronization wet etching processing method of differentiation micro-structure |
| US10468265B1 (en) | 2018-04-16 | 2019-11-05 | Guangdong University Of Technology | Method for synchronous wet etching processing of differential microstructures |
| CN112334230A (en) * | 2018-06-14 | 2021-02-05 | 康宁股份有限公司 | Nanographered surfaces for microfluidic devices and methods of making the same |
| CN109607471A (en) * | 2018-12-11 | 2019-04-12 | 吉林大学 | The super-micro syringe and preparation method thereof of picoliters magnitude based on patterned surface |
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| CN112916059A (en) * | 2021-01-22 | 2021-06-08 | 宜兴市晶科光学仪器有限公司 | Preparation method of novel micro-flow-channel flow cell |
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