CN106770854B - A kind of high-aspect-ratio micro-scale gas chromatograph column chip and preparation method thereof - Google Patents
A kind of high-aspect-ratio micro-scale gas chromatograph column chip and preparation method thereof Download PDFInfo
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- CN106770854B CN106770854B CN201611184707.8A CN201611184707A CN106770854B CN 106770854 B CN106770854 B CN 106770854B CN 201611184707 A CN201611184707 A CN 201611184707A CN 106770854 B CN106770854 B CN 106770854B
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- G—PHYSICS
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- 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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- G01N30/6052—Construction of the column body
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- G—PHYSICS
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- 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
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Abstract
The invention discloses a kind of preparation methods of high-aspect-ratio micro-scale gas chromatograph column chip, including production mask plate；Silicon wafer pretreatment；Carry out spin coating photoetching process, development；Then one layer of metallic aluminium is sputtered again as masking layer, and ultrasound removing exposes the channel to be etched, and carries out deep dry etching, the parameter of adjustment vertical etch and deposition protection；The identical substrate of two panels etched features is subjected to anode linkage, is used for chromatographic column heating and temperature regulation in the chip double-side sputtered film heater and temperature detecting resistance of bonding completion；One layer of PDMS film is formed inside micro-compliant mechanism using static coating method.The micro-scale gas chromatograph column of this method preparation, sidewall, depth-to-width ratio is big, and the depth-to-width ratio of micro-scale gas chromatograph column is doubled on the basis of original etching.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 profundity
Than the preparation method of micro-scale gas chromatograph column, which can be used for separating mixed gas width.
Background technique
Gas-chromatography is a kind of for separating and detecting the chemical analysis technology of mixing gas component.Mixed gas passes through color
When composing column, for different components due to its difference physically or chemically, the active force between stationary phase will be different, lead
It causes mixing gas component separation and is flowed out in the different time from chromatographic column end.Traditional gas chromatograph mainly by carrier gas,
Sample injector, chromatographic column and detector composition, core component chromatographic column is usually capillary column or packed column, but traditional color
The problems such as composing column, that there are volumes is big, and disengaging time is long, and power consumption is big, may not apply to on-site test.The key of Miniaturization of chromatograph
It is chromatographic column, and the chromatographic column of micro-processing technology production is used to convert two-dimensional structure for traditional three-dimensional chromatographic column, simultaneously
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, it is small in size, therefore have become an important directions in chromatographic apparatus exploitation.
At present chromatographic column micromation main means be channel is etched on silicon wafer, the substrates such as glass and metal, then into
Row anode linkage is made.The chromatographic column of silicon base due to its chemical inertness and with the compatibility of semiconductor technology, in addition
The development of MEMS technology reaches its maturity, and the chromatographic column etched on silicon wafer 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 capacity is weak.
The chromatography channel design gas of high-aspect-ratio can be distributed quickly, enhance separating capacity.With MEMS technology
Development, deep reaction ion etching technique provide technical conditions to make the structure of high-aspect-ratio.Using the logical of deep dry etching
Road inner wall is steep, and depth-to-width ratio with higher, compared to wet corrosion technique, controllability is stronger.General miniature gas phase color
Composing column is all to etch channel on a silicon substrate, followed by anode linkage technique by glass and wafer bonding, is formed closed
Channel.
Summary of the invention
The channel aspect ratio that the technical problem to be solved by the present invention is to bond together to form for silicon base micro-compliant mechanism silicon glass
It is difficult to improve, the even problem of single-side heating uneven heating, proposes a kind of high-aspect-ratio micro-scale gas chromatograph based on Si-Si bonding
The preparation method of column chip, this method can increase the depth-to-width ratio in channel on the basis of original etching to be twice, 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, which adopts the following technical scheme that, to be achieved:
A kind of preparation method of high-aspect-ratio micro-scale gas chromatograph column chip, comprising the following steps:
1) it makes mask plate: making the serpentine channel continuously penetrated through on the glass substrate, be placed in channel in array point
The spacing of the circular abutment of cloth, column is distributed in symmetrical unequal spacing；
2) silicon wafer pre-processes: silicon wafer is placed in the concentrated sulfuric acid of heating and the mixed solution of mistakeization hydrogen solution and cleans 5min,
Air blow drying is used after being rinsed well with deionized water, then dries silicon wafer；
3) photoetching: the silicon wafer of the good photoresist of spin coating is placed in heating plate by the spin coating photoresist on silicon wafer, drying；
4) develop: the silicon wafer after drying is placed in photolithography table, mask plate alignment is adjacent to silicon wafer, is immediately placed on after exposure
It is dried in being carried out in heating plate, then silicon wafer is placed in tetramethyl ammonium hydroxide solution and develops, dry；
5) it sputters: the aluminium layer using sputtering on magnetron sputtering technique silicon wafer after development with a thickness of 150nm, then by silicon
Piece is placed in ultrasound in acetone, and aluminium layer is removed, and forms the masking layer for being suitable for deep dry etching；
6) deep dry etching: using Bosch technique, and alternating is passed through SF6And C4F8Gas, will etch by 300 μm of etching depth
Chip afterwards is placed in the concentrated sulfuric acid of heating and the mixing liquor of hydrogenperoxide steam generator, and aluminium layer thoroughly cleans up after 10min；
7) Si-Si bonding, stationary phase coating: Si-Si bonding will be carried out after the silicon wafer alignment of two panels etching same depth, then
PDMS solution is coated in channel interior using static coating processes, forms thin film after solidifying under solution vacuum；
8) Ti 50nm and Pt 150nm is finally sputtered respectively in chip double-side, form thin film heater and temperature detecting resistance.
Further, in the step 2) and step 6), mixed solution is the volume that the concentrated sulfuric acid and hydrogenperoxide steam generator press 3:1
Than the mixed solution for being mixed and heated to 100~120 DEG C.
Further, the photoresist is N244.
Further, in the step 3), the silicon wafer of the good photoresist of spin coating is placed in 5~8min in 85~95 DEG C of heating plate
After dry.
Further, it in the step 4), is immediately placed on after 5~6s of exposure in 110~120 DEG C of heating plate in carrying out and dries 3
Silicon wafer is then placed in the tetramethyl ammonium hydroxide solution that mass ratio is 2.5% 25~the 30s that develops by~5min.
Further, in the step 2) and step 4), 10~15min of silicon wafer is dried under conditions of 85~95 DEG C.
A kind of high-aspect-ratio micro-scale gas chromatograph column chip that the present invention makes, including two substrates, two substrate difference
It etches identical in the spectrum column channel continuously penetrated through, the circle in array distribution is placed in each chromatographic column channel
Column, channel surface are coated with stationary phase film；The back of each substrate is equipped with the thin film heater and thermometric of Ti/Pt sputtering
Resistance；There are the entrance and exits of wedge shape for the side of substrate.
Further, the serpentine-like distribution in chromatographic column channel, channel width are 200 μm, and etching depth is 300 μm, are had in channel
The circular abutment array of marshalling, circular abutment diameter are 30 μm, and the spacing of column is distributed in symmetrical unequal spacing, and both ends are vertical
Column is 30 μm apart from conduit wall, and spacing is 25 μm to three columns two-by-two.
Further, interface is exposed after scribing in the wedge shaped entrance of chip sides and outlet.
The present invention has the advantage that compared with prior art and good effect: present invention firstly provides by two panels etched features
Identical silicon wafer carries out Si-Si bonding, and compared to traditional silicon glass bonding method, Si-Si bonding thermal expansion coefficient is consistent, and bonding is more
It is firm to add, and most importantly the depth-to-width ratio in chromatographic column channel can be increased one on the basis of existing deep dry etching technology
Times, further enhance the separating capacity and resolution ratio in chromatographic column channel, the method for double-faced sputter heater and temperature detecting resistance
The heterogeneity phantom of chromatographic column channel interior can be made more uniform；For the preparation or even miniature chromatographic development of micro-compliant mechanism
Provide certain basis.
Channel is bonded using two panels silicon base and is bonded instead of traditional silicon glass.Using stripping technology instead of wet etching
Method, technique more preferably controls, masking layer sharpness of border, is more advantageous to subsequent deep dry etching.
Detailed description of the invention
With reference to the accompanying drawing and specific embodiment the present invention is described in further detail.
Fig. 1 is the diagrammatic cross-section of the high-aspect-ratio micro-scale gas chromatograph column 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 flow chart of high-aspect-ratio micro-scale gas chromatograph column chip preparation method.
Fig. 4 is the SEM figure after the high-aspect-ratio micro-scale gas chromatograph column chip depth dry etching of the embodiment of the present invention.
(a) it is the section electron microscope in channel, (b) is the electron microscope of corner.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawing and specific implementation
The present invention is described in further detail for scheme, it should be pointed out that following embodiments is intended to convenient for reason of the invention
Solution, and do not play any restriction effect to it.
Fig. 1 is the section signal of the high-aspect-ratio micro-scale gas chromatograph column chip based on silicon bonding of the embodiment of the present invention
Figure.As shown in Figure 1, the micro-compliant mechanism chip includes two substrates 1, two substrates etch respectively identical continuously to be penetrated through
Chromatographic column channel 2, there are also circular abutment arrays in each chromatographic column channel 2, and it is thin that channel surface is coated with stationary phase
Film 3.The thin film heater and temperature detecting resistance 4 that the back of each substrate has Ti/Pt to sputter.There are the entrances of wedge shape for chip sides
5 and outlet 6, terminal end width be 280 μm.
Fig. 2 (a) is the schematic diagram of the embodiment of the present invention high-aspect-ratio micro-scale gas chromatograph column chip, and Fig. 2 (b) is Fig. 2
(a) enlarged drawing at A.Passageway pattern is snakelike winding distribution, and being arranged with diameter to symmetrical unequal spacing in channel is 30 μm
Cylindrical-array, every row arrange 3, and 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 corner's internal diameter.
Based on the target for further increasing microchannel depth-to-width ratio, including the identical silicon base of two panels depth dry etching depth 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 lucky after Si-Si bonding
It can fitting.
Fig. 3 (a)-(e) is the technique of the high-aspect-ratio micro-scale gas chromatograph column chip preparation method of the embodiment of the present invention
Flow chart.The following steps are included:
1) it designs and produces mask plate: according to the structure of design shown in Fig. 1,2, making Fig. 1,2 (a)-(b) on the glass substrate
Shown in the serpentine channel that continuously penetrates through, be placed with the circular abutment in array distribution in channel, the spacing of column in it is symmetrical not
Equidistantly distributed.
2) silicon wafer pre-process: cleaning silicon chip, by silicon wafer be placed in 100~120 DEG C of heating the concentrated sulfuric acid and mistakeization hydrogen solution by
5~8min is cleaned in the mixed solution of the volume ratio mixing of 3:1, air blow drying is used after being rinsed well with deionized water, is then dried
Dry silicon wafer.
3) photoetching: it is 500 μm of polished silicon slice that silicon base, which selects thickness, then the positive spin coating photoresist N244 on substrate,
The silicon wafer 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 photoetching in step 3) dry to obtain silicon wafer is placed in photolithography table, mask plate alignment is adjacent to silicon wafer,
It is immediately placed on after 5~6s of exposure in 110~120 DEG C of heating plate in carrying out and dries 3~5min, silicon wafer, which is then placed in mass ratio, is
Develop 25~30s in 2.5% tetramethyl ammonium hydroxide solution, and 10~15min of silicon wafer is dried under conditions of 85~95 DEG C；It will
In pattern transfer to substrate in mask plate shown in Fig. 2 (a), (b), as shown in Fig. 3 (b).
5) it sputters: substrate obtained in step 4) being sputtered one layer about using magnetron sputtering technique using magnetron sputtering technique
Then silicon wafer is placed in the removing of acetone ultrasound, masking layer is made, as shown in Fig. 3 (c) by the aluminium layer of 150nm thickness.
6) deep dry etching: using Bosch technique, and alternating is passed through SF6And C4F8Gas each serves as bombardment etching and protects
Substrate obtained in step 5) is performed etching using deep dry etch process, about 300 μm of etching depth, will be carved by the effect of shield
Chip after erosion be placed in be heated to 100~120 DEG C the concentrated sulfuric acid and hydrogenperoxide steam generator by 3:1 volume ratio mix mixed liquor
In solution, aluminium layer is thoroughly cleaned up after 8~10min；Cleaning removal masking layer after the completion of etching, as shown in Fig. 3 (d).
7) Si-Si bonding, stationary phase coating: Si-Si bonding, key will be carried out after the alignment of two panels silicon chip obtained in step 6)
Two panels substrate passageway wall and circular abutment array are bonded after conjunction.Conduit wall can just be aligned, and be existed by static coating processes
Channel interior coats stationary phase PDMS, and finally chip double-side sputtering Ti/Pt after bonding is as thin film heater and thermometric electricity
Resistance, as shown in Fig. 3 (e).
8) Ti 50nm and Pt 150nm is finally sputtered 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 wafer is placed in 120 DEG C of heating, it is clear in the solution that the concentrated sulfuric acid and hydrogenperoxide steam generator are mixed by the volume ratio of 3:1
5min is washed, air blow drying is used after being rinsed well with deionized water, silicon wafer 10min is then dried at a temperature of 90 DEG C.On silicon wafer
The silicon wafer of the good photoresist of spin coating is placed in 5min in 95 DEG C of heating plate by spin coating photoresist N244, drying.
Silicon wafer after drying is placed in photolithography table, by mask plate alignment, is adjacent to silicon wafer, 6s, exposure is arranged in the time for exposure
Silicon wafer afterwards will be immediately placed in 120 DEG C of heating plate to be dried in progress, and silicon wafer is then placed in the four of 2.5% by time 3min
Develop in ammonium hydroxide solution, developing time 30s, it can be seen that the figure of mask plate has been transferred into silicon wafer after development
On, silicon wafer 10min is dried under conditions of 90 DEG C.
Using the aluminium layer sputtered on the silicon wafer of magnetron sputtering technique after development with a thickness of 150nm, then silicon wafer is placed in
Ultrasound 3min, aluminium layer is removed in acetone, forms the masking layer of deep dry etching.
Deep dry etching, using Bosch technique, alternating is passed through SF6And C4F8Gas, two kinds of gases each serve as bombardment
The effect of etching and protection, etching depth 300um, Fig. 4 (a)-(b) are the SEM figures in the channel after etching, by the chip after etching
Be placed in 120 DEG C of the concentrated sulfuric acid and solution that the volume ratio of hydrogenperoxide steam generator 3:1 is made into, aluminium layer thoroughly cleans dry after 10min
Only.
Si-Si bonding is carried out after the silicon wafer that two panels etching is completed is aligned, then using static coating processes in channel interior
PDMS solution is coated, forms thin film after solidifying under solution vacuum.Ti 50nm, Pt 150nm finally are sputtered in chip double-side,
Form thin film heater and temperature detecting resistance.
Embodiment 2
Silicon wafer is placed in 100 DEG C of heating, it is clear in the solution that the concentrated sulfuric acid and hydrogenperoxide steam generator are mixed by the volume ratio of 3:1
8min is washed, air blow drying is used after being rinsed well with deionized water, silicon wafer 10min is then dried at a temperature of 85 DEG C.On silicon wafer
The silicon wafer of the good photoresist of spin coating is placed in 8min in 85 DEG C of heating plate by spin coating photoresist N244, drying.
Silicon wafer after drying is placed in photolithography table, by mask plate alignment, is adjacent to silicon wafer, 5s, exposure is arranged in the time for exposure
Silicon wafer afterwards will be immediately placed in 110 DEG C of heating plate to be dried in progress, and silicon wafer is then placed in the four of 2.5% by time 5min
Develop in ammonium hydroxide solution, developing time 25s, it can be seen that the figure of mask plate has been transferred into silicon wafer after development
On, silicon wafer 15min is dried under conditions of 85 DEG C.
Using the aluminium layer sputtered on the silicon wafer of magnetron sputtering technique after development with a thickness of 150nm, then silicon wafer is placed in
Ultrasound 3min, aluminium layer is removed in acetone, forms the masking layer of deep dry etching.
Deep dry etching, using Bosch technique, alternating is passed through SF6And C4F8Gas, two kinds of gases each serve as bombardment
Chip after etching, is placed in 100 DEG C of the concentrated sulfuric acid and hydrogenperoxide steam generator by the effect of etching and protection by 300 μm of etching depth
In the solution that the volume ratio of 3:1 is made into, aluminium layer is thoroughly cleaned up after 8min.
Si-Si bonding is carried out after the silicon wafer that two panels etching is completed is aligned, then using static coating processes in channel interior
PDMS solution is coated, forms thin film after solidifying under solution vacuum.Ti 50nm, Pt 150nm finally are sputtered in chip double-side,
Form thin film heater and temperature detecting resistance.
Described above is only presently preferred embodiments of the present invention, so cannot limit right model of the invention with this
It encloses, 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 (5)
1. a kind of preparation method of high-aspect-ratio micro-scale gas chromatograph column chip, which comprises the following steps:
1) it makes mask plate: making the serpentine channel continuously penetrated through on the glass substrate, be placed in channel in array distribution
The spacing of circular abutment, column is distributed in symmetrical unequal spacing；
2) silicon wafer pre-processes: silicon wafer being placed in the concentrated sulfuric acid of heating and the mixed solution of mistakeization hydrogen solution and cleans 5min, spent
Ionized water uses air blow drying after rinsing well, then dries silicon wafer；
3) photoetching: the silicon wafer of the good photoresist of spin coating is placed in heating plate, in 85~95 DEG C of item by the spin coating photoresist on silicon wafer
10~15min is dried under part；
4) develop: the silicon wafer after drying is placed in photolithography table, mask plate alignment is adjacent to silicon wafer, heating is immediately placed on after exposure
It is dried in being carried out on plate, silicon wafer is then placed in development in tetramethyl ammonium hydroxide solution, dries 10 under conditions of 85~95 DEG C
~15min；
5) it sputters: using sputtering on magnetron sputtering technique silicon wafer after development with a thickness of the aluminium layer of 150nm, then setting silicon wafer
It is ultrasonic in acetone, aluminium layer is removed, the masking layer for being suitable for deep dry etching is formed；
6) deep dry etching: using Bosch technique, and alternating is passed through SF6And C4F8Gas, 300 μm of etching depth, after etching
Chip is placed in the concentrated sulfuric acid of heating and the mixing liquor of hydrogenperoxide steam generator, and aluminium layer thoroughly cleans up after 10min；
7) Si-Si bonding, stationary phase coating: Si-Si bonding will be carried out after the silicon wafer alignment of two panels etching same depth, then used
Static coating processes coat PDMS solution in channel interior, form thin film after solidifying under solution vacuum；
8) Ti 50nm and Pt 150nm is finally sputtered respectively in chip double-side, form thin film heater and temperature detecting resistance；
In the step 2) and step 6), mixed solution is that the concentrated sulfuric acid and hydrogenperoxide steam generator are mixed and added by the volume ratio of 3:1
The mixed solution of heat to 100~120 DEG C；
In the step 3), the silicon wafer of the good photoresist of spin coating is placed in 85~95 DEG C of heating plate after 5~8min and is dried；
In the step 4), 3~5min of baking in progress is immediately placed in 110~120 DEG C of heating plate after exposing 5~6s, then
Silicon wafer is placed in the tetramethyl ammonium hydroxide solution that mass ratio is 2.5% 25~the 30s that develops.
2. high-aspect-ratio micro-scale gas chromatograph column chip 6 as described in claim 1, preparation method, which is characterized in that described
Photoresist is N244.
3. a kind of high-aspect-ratio micro-scale gas chromatograph column chip of claim 1 the method preparation, which is characterized in that this is miniature
Gas chromatographic column chip includes two substrates (1), and two substrates etch identical in the spectrum column channel continuously penetrated through respectively
(2), the circular abutment in array distribution is placed in each chromatographic column channel (2), channel surface is coated with stationary phase
Film (3)；The back of each substrate is equipped with the thin film heater and temperature detecting resistance (4) of Ti/Pt sputtering；The side of substrate there are
The entrance (5) of wedge shape and outlet (6).
4. high-aspect-ratio micro-scale gas chromatograph column chip according to claim 3, which is characterized in that the chromatographic column channel
(2) serpentine-like distribution, channel width are 200 μm, and channel wall thickness is 100 μm, and etching depth is 300 μm, there is marshalling in channel
Circular abutment array, circular abutment diameter are 30 μm, and the spacing of column is distributed in symmetrical unequal spacing, and both ends column is apart from channel
Wall is 30 μm, and spacing is 25 μm to three columns two-by-two.
5. high-aspect-ratio micro-scale gas chromatograph column chip as claimed in claim 3, which is characterized in that the wedge shape of chip sides enters
Mouth and outlet, expose interface after scribing.
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| CN108254465B (en) * | 2018-01-16 | 2021-04-09 | 中国科学院电子学研究所 | Density distribution type micro chromatographic column chip and manufacturing method thereof |
| CN110562911A (en) * | 2019-09-18 | 2019-12-13 | 北京理工大学 | Micro-nano structure forming and manufacturing method using supporting layer |
| CN110862088B (en) * | 2019-10-30 | 2020-11-13 | 南京大学 | Preparation method of silicon nanoneedle array with ultra-high depth-to-width ratio |
| CN111398496B (en) * | 2020-02-20 | 2023-03-21 | 江苏大学 | Micro gas chromatographic column in staggered array arrangement |
| CN113466393B (en) * | 2021-06-11 | 2022-07-12 | 西安交通大学 | Miniature gas chromatographic column capable of using air as carrier gas and its making method |
| CN115055173A (en) * | 2022-05-27 | 2022-09-16 | 中国科学院上海微***与信息技术研究所 | All-silicon micro-chromatographic column with high depth-to-width ratio and preparation method thereof |
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