CN106770854A - A kind of high-aspect-ratio micro-scale gas chromatograph post chip and preparation method thereof - Google Patents
A kind of high-aspect-ratio micro-scale gas chromatograph post chip and preparation method thereof Download PDFInfo
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- CN106770854A CN106770854A CN201611184707.8A CN201611184707A CN106770854A CN 106770854 A CN106770854 A CN 106770854A CN 201611184707 A CN201611184707 A CN 201611184707A CN 106770854 A CN106770854 A CN 106770854A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
- G01N30/6052—Construction of the column body
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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Abstract
The invention discloses a kind of preparation method of high-aspect-ratio micro-scale gas chromatograph post chip, including make mask plate;Silicon chip is pre-processed;Spin coating photoetching process is carried out, is developed;Then layer of metal aluminium is sputtered again as masking layer, ultrasound is peeled off, and exposes the passage to be etched, carry out the parameter of deep dry etching, adjustment vertical etch and deposition protection;The identical substrate of two panels etched features is carried out into anode linkage, the chip double-side sputtered film heater and temperature detecting resistance completed in bonding are used for chromatographic column and heat and temperature adjusting;One layer of PDMS film is internally formed in micro-compliant mechanism using static painting method.Micro-scale gas chromatograph post prepared by the method, sidewall, depth-to-width ratio is big, and the depth-to-width ratio of micro-scale gas chromatograph post is doubled on the basis of original etching.Its preparation method is simple and reliable, and the micro-compliant mechanism chip sensitivity of preparation and resolution ratio are higher.
Description
Technical field
The present invention relates to technical field of chromatographic analysis, belong to Miniaturization of chromatograph application field, and in particular to a kind of advanced
Preparation method than micro-scale gas chromatograph post wide, the invention can be used to separate mixed gas.
Background technology
Gas-chromatography is a kind of chemical analysis technology for separating and detecting mixing gas component.Mixed gas are by color
During spectrum post, different component will be different due to its difference physically or chemically, its active force between fixing phase, lead
Mixing gas component is caused to separate and flowed out from chromatographic column end in the different time.Traditional gas chromatograph is main by carrier gas,
Injector, chromatographic column and detector are constituted, and core component chromatographic column is usually capillary column or packed column, but traditional color
There is volume greatly in spectrum post, disengaging time is long, and power consumption is big, it is impossible to the problems such as being applied to Site Detection.The key of Miniaturization of chromatograph
It is chromatographic column, and traditional three-dimensional chromatographic column is converted into by two-dimensional structure using the chromatographic column that micro-processing technology makes, while
Chromatographic column chip carries temperature adjusting function, and departing from bulky chromatographic column post case, disengaging time is shortened dramatically, power consumption
It is low, small volume, therefore turned into an important directions in chromatographic apparatus exploitation.
The Main Means of current chromatographic column miniaturization are, in silicon chip, to etch passage on the substrate such as glass and metal, then enter
Row anode linkage is made.Compatibility of the chromatographic column of silicon base due to its chemical inertness and with semiconductor technology, in addition
The development of MEMS technology reaches its maturity, and the chromatographic column etched on silicon chip has obtained quick development.The silicon base of early stage it is miniature
Chromatographic column is made using wet corrosion technique, and wet etching anisotropy is difficult effectively to control, thus make
Chromatographic column depth-to-width ratio is all smaller, and column capacity is also very limited, and separating power is weak.
The chromatogram channel design gas of high-aspect-ratio can be distributed quickly, strengthen separating power.With MEMS technology
Development, deep reaction ion etching technique provides technical conditions to make the structure of high-aspect-ratio.Using the logical of deep dry etching
Road inwall is steep, and with depth-to-width ratio higher, compared to wet corrosion technique, its controllability is stronger.General miniature gas phase color
Spectrum post is all to etch passage on a silicon substrate, followed by anode linkage technique by glass and wafer bonding, is formed closed
Passage.
The content of the invention
The technical problem to be solved in the present invention is directed to the channel aspect ratio that silicon base micro-compliant mechanism silicon glass is bonded together to form
It is difficult to improve, single-side heating is heated uneven problem, proposes a kind of high-aspect-ratio micro-scale gas chromatograph based on Si-Si bonding
The depth-to-width ratio of passage can be increased and is twice by the preparation method of post chip, the method on the basis of original etching, meanwhile, front
There are heater strip and temperature detecting resistance with the back side, channel interior is uniformly heated, the further separation for improving micro-compliant mechanism
Ability.
The present invention is adopted the following technical scheme that and is achieved:
A kind of preparation method of high-aspect-ratio micro-scale gas chromatograph post chip, comprises the following steps:
1) mask plate is made:The serpentine channel of continuous insertion is made on the glass substrate, is placed with passage in array point
The circular abutment of cloth, the spacing of column is in symmetrical not equidistantly distributed;
2) silicon chip pretreatment:Silicon chip is placed in the mixed solution of the concentrated sulfuric acid of heating and mistakeization hydrogen solution and cleans 5min,
Air blow drying is used after being rinsed well with deionized water, silicon chip is then dried;
3) photoetching:The spin coating photoresist on silicon chip, the silicon chip of the good photoresist of spin coating is placed in heating plate, drying;
4) develop:Silicon chip after drying is placed in photolithography table, mask plate alignment is adjacent to silicon chip, be immediately placed on after exposure
Middle baking is carried out in heating plate, then silicon chip is placed in tetramethyl ammonium hydroxide solution and is developed, is dried;
5) sputter:It is the aluminium lamination of 150nm to use and sputtered on magnetron sputtering technique silicon chip after development thickness, then by silicon
Piece is placed in ultrasound in acetone, and aluminium lamination is peeled off, and formation is suitable to the masking layer of deep dry etching;
6) deep dry etching:Using Bosch techniques, alternating is passed through SF6And C4F8Gas, 300 μm of etching depth, will etch
Chip afterwards is placed in the mixing liquor of the concentrated sulfuric acid of heating and hydrogenperoxide steam generator, and aluminium lamination thoroughly cleaning is clean after 10min;
7) anode linkage, fixing phase coating:Anode linkage will be carried out after the silicon chip alignment of two panels etching same depth, then
PDMS solution is coated in channel interior using static coating processes, thin film is formed after solidifying under solution vacuum;
8) it is last to sputter Ti 50nm and Pt 150nm respectively in chip double-side, form thin film heater and temperature detecting resistance.
Further, the step 2) and step 6) in, mixed solution is that the concentrated sulfuric acid and hydrogenperoxide steam generator press 3:1 volume
Than the mixed solution for being mixed and heated to 100~120 DEG C.
Further, the photoresist is N244.
Further, the step 3) in, the silicon chip of the good photoresist of spin coating is placed in 5~8min in 85~95 DEG C of heating plate
After dry.
Further, the step 4) in, being immediately placed in 110~120 DEG C of heating plate after 5~6s of exposure carries out middle baking 3
~5min, is then placed in 25~30s of development in the tetramethyl ammonium hydroxide solution that mass ratio is 2.5% by silicon chip.
Further, the step 2) and step 4) in, 10~15min of silicon chip is dried under conditions of 85~95 DEG C.
A kind of high-aspect-ratio micro-scale gas chromatograph post chip that the present invention makes, including two substrates, two substrate difference
Spectrum post passage of the identical in continuous insertion is etched, is placed with the circle of array distribution in each described chromatographic column passage
Column, passage surface is coated with fixing phase film;The back of each substrate is equipped with the thin film heater and thermometric of Ti/Pt sputterings
Resistance;Leave the entrance and exit of wedge shape in the side of substrate.
Further, the serpentine-like distribution of chromatographic column passage, a width of 200 μm of passage, etching depth is 300 μm, is had in passage
The circular abutment array of marshalling, a diameter of 30 μm of circular abutment, the spacing of column in symmetrical not equidistantly distributed, stand by two ends
Post is 30 μm apart from conduit wall, and spacing is 25 μm two-by-two for three columns.
Further, the wedge shaped entrance of chip sides and outlet, expose interface after scribing.
The present invention has the advantage that and good effect compared with prior art:Present invention firstly provides by two panels etched features
Identical silicon chip carries out anode linkage, and compared to traditional silicon glass bonding method, Si-Si bonding thermal coefficient of expansion is consistent, and bonding is more
Plus it is firm, most importantly the depth-to-width ratio of chromatographic column passage can be increased one on the basis of existing deep dry etching technology
Times, the method that further enhancing the separating power and resolution ratio of chromatographic column passage, double-faced sputter heater and temperature detecting resistance
The heterogeneity phantom of chromatographic column channel interior can be made more uniform;It is the preparation or even miniature chromatographic development of micro-compliant mechanism
There is provided certain basis.
Passage instead of traditional silicon glass and is bonded using two panels silicon base bonding.Wet etching instead of using stripping technology
Method, technique more preferably controls, and masking layer sharpness of border is more beneficial for follow-up deep dry etching.
Brief description of the drawings
Below in conjunction with the accompanying drawings and specific embodiment the present invention is described in further detail.
Fig. 1 is the generalized section of the high-aspect-ratio micro-scale gas chromatograph post chip of the embodiment of the present invention.
Fig. 2 (a) is the mask plate schematic diagram of inventive embodiments.Fig. 2 (b) is enlarged drawing at Fig. 2 (a) A.
Fig. 3 (a)-(e) is the process chart of high-aspect-ratio micro-scale gas chromatograph post chip preparation method.
Fig. 4 is the SEM figures after the high-aspect-ratio micro-scale gas chromatograph post chip depth dry etching of embodiments of the invention.
A () is the section electron microscope of passage, (b) is the electron microscope of corner.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with the accompanying drawings and specific implementation
The present invention is described in further detail for scheme, it should be pointed out that embodiments below is intended to be easy to reason of the invention
Solution, and do not play any restriction effect to it.
Fig. 1 is that the section of the high-aspect-ratio micro-scale gas chromatograph post chip based on silicon bonding of embodiments of the invention is illustrated
Figure.As shown in figure 1, the micro-compliant mechanism chip includes two substrates 1, two substrates etch the continuous insertion of identical respectively
Chromatographic column passage 2, also has circular abutment array in the chromatographic column passage 2 described in each, it is thin that passage surface is coated with fixing phase
Film 3.There are the thin film heater and temperature detecting resistance 4 that Ti/Pt is sputtered in the back of each substrate.Chip sides leave the entrance of wedge shape
5 is 280 μm with outlet 6, terminal end width.
Fig. 2 (a) is the schematic diagram of embodiments of the invention high-aspect-ratio micro-scale gas chromatograph post chip, and Fig. 2 (b) is Fig. 2
Enlarged drawing at the A of (a).Passageway pattern is snakelike winding distribution, and symmetrically a diameter of 30 μm are not arranged with equally spacedly in passage
Cylindrical-array, often row's arrangement 3, its spacing is respectively d1=30 μm, d2=25 μm.100 μm of channel wall thickness, width w=200 μ
M, r1=50 μm, r2=250 μm of its corner's internal diameter.
Based on further increase microchannel depth-to-width ratio target, including two panels depth dry etching depth identical silicon base with
And the serpentine channel and circular abutment array etched in substrate, the thin film heater at the back side, the fixation of temperature detecting resistance and coating
Phase film.The figure etched in two panels silicon base is completely the same, and circular abutment array and conduit wall are by lucky after anode linkage
Can laminating.
Fig. 3 (a)-(e) is the technique of the high-aspect-ratio micro-scale gas chromatograph post chip preparation method of embodiments of the invention
Flow chart.Comprise the following steps:
1) mask plate is designed and produced:According to the structure of design shown in Fig. 1,2, Fig. 1,2 (a)-(b) are made on the glass substrate
The serpentine channel of shown continuous insertion, is placed with the circular abutment of array distribution in passage, the spacing of column in it is symmetrical not
Equidistantly distributed.
2) silicon chip pretreatment:Cleaning silicon chip, by silicon chip be placed in 100~120 DEG C of heating the concentrated sulfuric acid and mistakeization hydrogen solution by
3:5~8min is cleaned in the mixed solution of 1 volume ratio mixing, air blow drying is used after being rinsed well with deionized water, then dried
Dry silicon chip.
3) photoetching:Silicon base from the polished silicon slice that thickness is 500 μm, the then front spin coating photoresist N244 on substrate,
The silicon chip of the good photoresist of spin coating is placed in 5~8min in 85~95 DEG C of heating plate, is dried;As shown in Fig. 3 (a).
4) develop:By step 3) in photoetching drying obtain silicon chip is placed in photolithography table, by mask plate alignment be adjacent to silicon chip,
Being immediately placed in 110~120 DEG C of heating plate after 5~6s of exposure carries out 3~5min of middle baking, and silicon chip then is placed in into mass ratio is
Develop 25~30s in 2.5% tetramethyl ammonium hydroxide solution, and 10~15min of silicon chip is dried under conditions of 85~95 DEG C;Will
The pattern transfer in mask plate shown in Fig. 2 (a), (b) on substrate, as shown in Fig. 3 (b).
5) sputter:Using magnetron sputtering technique by step 4) in the substrate of gained sputter one layer about using magnetron sputtering technique
150nm thick aluminium lamination, is then placed in silicon chip acetone ultrasound and peels off, masking layer is obtained, shown in such as Fig. 3 (c).
6) deep dry etching:Using Bosch techniques, alternating is passed through SF6And C4F8Gas, each serves as bombardment etching and protects
The effect of shield, by step 5) in the substrate of gained performed etching using deep dry etch process, about 300 μm of etching depth will be carved
Chip after erosion is placed in the concentrated sulfuric acid and hydrogenperoxide steam generator that are heated to 100~120 DEG C by 3:The mixed liquor of 1 volume ratio mixing
In solution, aluminium lamination thoroughly cleaning is clean after 8~10min;Removal masking layer is cleaned after the completion of etching, shown in such as Fig. 3 (d).
7) anode linkage, fixing phase coating:By step 6) in gained two panels silicon chip alignment after carry out anode linkage, key
Two panels substrate passageway wall and circular abutment array are fitted after conjunction.Conduit wall can just be aligned, and be existed by static coating processes
Channel interior coats fixing phase PDMS, and finally chip double-side sputtering Ti/Pt after bonding is used as thin film heater and thermometric electricity
Resistance, shown in such as Fig. 3 (e).
8) it is last to sputter Ti 50nm and Pt 150nm respectively in chip double-side, form thin film heater and temperature detecting resistance.
The present invention is described in further details below by specific embodiment.
Embodiment 1
Silicon chip is placed in 120 DEG C of heating, the concentrated sulfuric acid and hydrogenperoxide steam generator press 3:It is clear in the solution that 1 volume ratio is mixed into
5min is washed, air blow drying is used after being rinsed well with deionized water, silicon chip 10min is then dried at a temperature of 90 DEG C.On silicon chip
Spin coating photoresist N244,5min in 95 DEG C of heating plate is placed in by the silicon chip of the good photoresist of spin coating, drying.
Silicon chip after drying is placed in photolithography table, by mask plate alignment, silicon chip is adjacent to, the time for exposure sets 6s, exposure
Silicon chip afterwards will be immediately placed on and middle baking is carried out in 120 DEG C of heating plate, and the time is 3min, and silicon chip then is placed in into the four of 2.5%
Develop in ammonium hydroxide solution, developing time 30s, it can be seen that the figure of mask plate has been transferred into silicon chip after development
On, silicon chip 10min is dried under conditions of 90 DEG C.
It is the aluminium lamination of 150nm to use and sputtered on magnetron sputtering technique silicon chip after development thickness, is then placed in silicon chip
Ultrasound 3min, aluminium lamination is peeled off in acetone, forms the masking layer of deep dry etching.
Deep dry etching, using Bosch techniques, alternating is passed through SF6And C4F8Gas, two kinds of gases each serve as bombardment
Etching and the effect of protection, etching depth 300um, Fig. 4 (a)-(b) are the SEM figures of the passage after etching, by the chip after etching
It is placed in 120 DEG C of the concentrated sulfuric acid and hydrogenperoxide steam generator 3:In the solution that 1 volume ratio is made into, aluminium lamination thoroughly cleaning is done after 10min
Only.
Anode linkage is carried out after the silicon chip alignment that two panels etching is completed, then using static coating processes in channel interior
Coating PDMS solution, thin film is formed after solidifying under solution vacuum.It is last to sputter Ti 50nm, Pt 150nm in chip double-side,
Form thin film heater and temperature detecting resistance.
Embodiment 2
Silicon chip is placed in 100 DEG C of heating, the concentrated sulfuric acid and hydrogenperoxide steam generator press 3:It is clear in the solution that 1 volume ratio is mixed into
8min is washed, air blow drying is used after being rinsed well with deionized water, silicon chip 10min is then dried at a temperature of 85 DEG C.On silicon chip
Spin coating photoresist N244,8min in 85 DEG C of heating plate is placed in by the silicon chip of the good photoresist of spin coating, drying.
Silicon chip after drying is placed in photolithography table, by mask plate alignment, silicon chip is adjacent to, the time for exposure sets 5s, exposure
Silicon chip afterwards will be immediately placed on and middle baking is carried out in 110 DEG C of heating plate, and the time is 5min, and silicon chip then is placed in into the four of 2.5%
Develop in ammonium hydroxide solution, developing time 25s, it can be seen that the figure of mask plate has been transferred into silicon chip after development
On, silicon chip 15min is dried under conditions of 85 DEG C.
It is the aluminium lamination of 150nm to use and sputtered on magnetron sputtering technique silicon chip after development thickness, is then placed in silicon chip
Ultrasound 3min, aluminium lamination is peeled off in acetone, forms the masking layer of deep dry etching.
Deep dry etching, using Bosch techniques, alternating is passed through SF6And C4F8Gas, two kinds of gases each serve as bombardment
Chip after etching is placed in etching and the effect of protection, 300 μm of etching depth 100 DEG C of the concentrated sulfuric acid and hydrogenperoxide steam generator
3:In the solution that 1 volume ratio is made into, aluminium lamination thoroughly cleaning is clean after 8min.
Anode linkage is carried out after the silicon chip alignment that two panels etching is completed, then using static coating processes in channel interior
Coating PDMS solution, thin film is formed after solidifying under solution vacuum.It is last to sputter Ti 50nm, Pt 150nm in chip double-side,
Form thin film heater and temperature detecting resistance.
Described above is only presently preferred embodiments of the present invention, and right model of the invention can not be so limited with this
Enclose, those skilled in the art make a little simple modification, equivalent variations or modification using the technology contents of above-mentioned disclosure, still fall within
Within protection scope of the present invention.
Claims (9)
1. a kind of preparation method of high-aspect-ratio micro-scale gas chromatograph post chip, it is characterised in that comprise the following steps:
1) mask plate is made:The serpentine channel of continuous insertion is made on the glass substrate, is placed with array distribution in passage
Circular abutment, the spacing of column is in symmetrical not equidistantly distributed;
2) silicon chip pretreatment:Silicon chip is placed in the mixed solution of the concentrated sulfuric acid of heating and mistakeization hydrogen solution and cleans 5min, spent
Ionized water uses air blow drying after rinsing well, then dries silicon chip;
3) photoetching:The spin coating photoresist on silicon chip, the silicon chip of the good photoresist of spin coating is placed in heating plate, drying;
4) develop:Silicon chip after drying is placed in photolithography table, mask plate alignment is adjacent to silicon chip, heating is immediately placed on after exposure
Middle baking is carried out on plate, then silicon chip is placed in tetramethyl ammonium hydroxide solution and is developed, is dried;
5) sputter:It is the aluminium lamination of 150nm to use and sputtered on magnetron sputtering technique silicon chip after development thickness, then puts silicon chip
Ultrasound, aluminium lamination is peeled off in acetone, and formation is suitable to the masking layer of deep dry etching;
6) deep dry etching:Using Bosch techniques, alternating is passed through SF6And C4F8Gas, 300 μm of etching depth, after etching
Chip is placed in the mixing liquor of the concentrated sulfuric acid of heating and hydrogenperoxide steam generator, and aluminium lamination thoroughly cleaning is clean after 10min;
7) anode linkage, fixing phase coating:Anode linkage will be carried out after the silicon chip alignment of two panels etching same depth, then used
Static coating processes coat PDMS solution in channel interior, and thin film is formed after solidifying under solution vacuum;
8) it is last to sputter Ti 50nm and Pt 150nm respectively in chip double-side, form thin film heater and temperature detecting resistance.
2. the preparation method of high-aspect-ratio micro-scale gas chromatograph post chip as claimed in claim 1, it is characterised in that the step
It is rapid 2) and step 6) in, mixed solution is that the concentrated sulfuric acid and hydrogenperoxide steam generator press 3:1 volume ratio is mixed and heated to 100~
120 DEG C of mixed solution.
3. the preparation method of high-aspect-ratio micro-scale gas chromatograph post chip as claimed in claim 1, it is characterised in that the light
Photoresist is N244.
4. the preparation method of high-aspect-ratio micro-scale gas chromatograph post chip as claimed in claim 1, it is characterised in that the step
It is rapid 3) in, by the silicon chip of the good photoresist of spin coating be placed in 85~95 DEG C of heating plate after 5~8min dry.
5. the preparation method of high-aspect-ratio micro-scale gas chromatograph post chip as claimed in claim 1, it is characterised in that the step
It is rapid 4) in, be immediately placed in 110~120 DEG C of heating plate and carry out 3~5min of middle baking after 5~6s of exposure, then silicon chip is placed in
Mass ratio be 2.5% tetramethyl ammonium hydroxide solution in develop 25~30s.
6. the preparation method of high-aspect-ratio micro-scale gas chromatograph post chip as claimed in claim 1, it is characterised in that the step
It is rapid 2) and step 4) in, silicon chip 10~15min is dried under conditions of 85~95 DEG C.
7. a kind of high-aspect-ratio micro-scale gas chromatograph post chip, it is characterised in that the micro-scale gas chromatograph post chip includes two
Substrate (1), two substrates etch spectrum post passage (2) of the identical in continuous insertion respectively, in each chromatographic column passage
(2) it is placed with the circular abutment of array distribution in, passage surface is coated with fixing phase film (3);The back of each substrate is equal
It is provided with the thin film heater and temperature detecting resistance (4) of Ti/Pt sputterings;Leave entrance (5) and the outlet (6) of wedge shape in the side of substrate.
8. high-aspect-ratio micro-scale gas chromatograph post chip as claimed in claim 7, it is characterised in that the chromatographic column passage
(2) serpentine-like distribution, a width of 200 μm of passage, channel wall thickness is 100 μm, and etching depth is 300 μm, there is marshalling in passage
Circular abutment array, a diameter of 30 μm of circular abutment, in symmetrical not equidistantly distributed, two ends column is apart from passage for the spacing of column
Wall is 30 μm, and spacing is 25 μm two-by-two for three columns.
9. high-aspect-ratio micro-scale gas chromatograph post chip as claimed in claim 7, it is characterised in that the wedge shape of chip sides enters
Mouth and outlet, expose interface after scribing.
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CN113466393A (en) * | 2021-06-11 | 2021-10-01 | 西安交通大学 | Miniature gas chromatographic column capable of using air as carrier gas and its making method |
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