CN207623299U - The micro- gas chromatographic column of silicon substrate - Google Patents
The micro- gas chromatographic column of silicon substrate Download PDFInfo
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- CN207623299U CN207623299U CN201721816759.2U CN201721816759U CN207623299U CN 207623299 U CN207623299 U CN 207623299U CN 201721816759 U CN201721816759 U CN 201721816759U CN 207623299 U CN207623299 U CN 207623299U
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Abstract
The utility model proposes a kind of micro- gas chromatographic column of silicon substrate, is designed on the inner surface of micro- raceway groove of silicon microfluidic chromatography column and prepare one layer of fine and closely woven silicon nanowires forest, nano wire line footpath is typically distributed across between several nanometers to tens nanometers.This fine and closely woven silicon nanowires forest greatly increases the surface area of silicon microfluidic chromatography column, to be effectively improved column capacity, separating degree and the column effect of silicon microfluidic chromatography column.
Description
Technical field
The utility model belongs to microelectromechanical systems field, more particularly to a kind of micro- gas chromatographic column of silicon substrate and its system
Preparation Method.
Background technology
The major function of gas chromatographic column is detached to mixing sample gas to be analyzed, it is gas chromatograph
Core component.Traditional gas chromatographic column includes capillary column, packed column etc., since volume is larger, needs special column oven
It is heated for it, power consumption reaches several kilowatts, therefore in order to realize that the micromation of gas chromatograph, the micromation of gas chromatographic column are extremely closed
It is important.
Since the end of the seventies in last century, the method making that people begin attempt on a silicon substrate by corrosion/etching is micro-
Chromatographic column chip.In order to improve the separative efficiency of silicon substrate microfluidic chromatography column, design is optimized to its geometry in researcher, and
Achieve impressive progress：Snakelike layout, which is better than spiral shape, to be shown to the layout research of chromatographic column on a silicon substrate；Chromatographic column is transversal
There is round and rectangle in face, and the rectangle column performance of high-aspect-ratio is more preferably.
Microfluidic chromatography post separation performance is directly related with its surface area, in order to improve its column capacity, separating degree and column effect, needs
Increase microfluidic chromatography column column internal surface area.For this purpose, the utility model proposes a kind of novel silicon microfluidic chromatographies and preparation method.
Utility model content
In view of the foregoing deficiencies of prior art, the purpose of this utility model is to provide a kind of micro- gas-chromatographies of silicon substrate
Column and preparation method thereof, for solving the problems, such as that the surface area of micro- gas chromatographic column in the prior art is relatively low.
In order to achieve the above objects and other related objects, the utility model provides a kind of preparation of the micro- gas chromatographic column of silicon substrate
Method, the preparation method include step：1) silicon substrate is provided, micro- raceway groove is made in the silicon substrate；2) metal is used
Assisted Chemical Etching Process technique prepares silicon nanowires forest in the inner surface of micro- raceway groove；And 3) encapsulation cover plate is provided, it will
The encapsulation cover plate is bonded with the silicon substrate, to close micro- raceway groove, forms the micro- logical of the micro- gas chromatographic column of silicon substrate
Road.
Preferably, also with one kind in multiple trench cells and the formed group of multiple micro-pillar arrays in micro- raceway groove
Or two kinds, the silicon nanowires forest is prepared in the multiple trench cells and the multiple micro-pillar array surface.
Preferably, step 2) includes：The silicon substrate 2-1) is put into the first mixing comprising hydrofluoric acid and deionized water
In solution, to remove the oxide layer of micro- channel surface；2-2) silicon substrate is put into comprising silver nitrate, hydrofluoric acid and is gone
In second mixed solution of ionized water, in the inner surface deposited metal silver of micro- raceway groove；2-3) silicon substrate is put into
Including in the third mixed solution of hydrofluoric acid, hydrogen peroxide and deionized water, the inner surface of micro- raceway groove is corroded, in
The inner surface of micro- raceway groove forms the silicon nanowires forest：And 2-4) silicon substrate is put into salpeter solution, with
Remove the metallic silver of micro- raceway groove inner surface.
Preferably, step 2-2) in, the ratio of the silver nitrate, hydrofluoric acid and deionized water is between 4mL~12mL：10~
30mL：Between 40~80ml, the concentration of the silver nitrate is between 0.001~0.2mol/L, and the time of the deposition is between 1
Between~20min.
Preferably, step 2-3) in, the ratio of the hydrofluoric acid, hydrogen peroxide and deionized water is between 5~35ml：1~
10ml：Between 10~60ml, the temperature of the corrosion between 20~60 DEG C, time of the corrosion between 1~10min it
Between.
Preferably, step 2-4) in, the mass fraction of the salpeter solution between 55%~75%, the removal
Time is between 10~50min.
Preferably, step 2-2) while the deposition uniform oscillation treatment, step 2-3 are carried out to the silicon substrate)
Uniform oscillation treatment is carried out to the silicon substrate while corrosion.
Preferably, step 1) further includes the steps that making micro-fluidic port, the preparation side in the both ends of micro- raceway groove
Method further includes step 4)：Scribing obtains the micro- gas chromatographic column chip of silicon substrate, and installs capillary in the micro-fluidic port.
Preferably, the encapsulation cover plate includes silicon cover board, and the silicon cover board is prepared in region corresponding with the micro- raceway groove
There is silicon nanowires forest, closing technique by silicon-silicon bond is bonded the silicon cover board with the silicon substrate.
Preferably, the encapsulation cover plate includes the glass cover-plate of twin polishing, is bonded to using anode linkage method described
On the bonding face of silicon substrate, bonding temperature is between 200-450 DEG C, and bonding voltage is between 600-1400V.
Preferably, further include step：It is formed accordingly in silicon nanowires forest surface based on component needed to be separated
Decorative material.
Preferably, the decorative material includes octadecyl trichlorosilane alkane, octadecyldimethylchlorosilane and octadecane
One kind in base trimethoxy silane.
Preferably, the step of forming the decorative material include：Step a), it includes toluene and the decorative material to prepare
The mixed liquor is injected into micro- raceway groove and reacts by mixed liquor；And step b), alcohol washes institute is used after reaction
Micro- raceway groove is stated, and all removes the alcohol in micro- raceway groove under vacuum or low pressure environment.
Preferably, the line footpath of the silicon nanowires in the silicon nanowires forest is between 1~100 nanometer.
The utility model also provides a kind of micro- gas chromatographic column of silicon substrate, including：Silicon substrate；Micro- raceway groove is formed in the silicon
In substrate；Micro-fluidic port is formed in micro- raceway groove both ends；Silicon nanowires forest is prepared in micro- raceway groove；And envelope
Capping plate is bonded to the surface of silicon, to close micro- raceway groove, forms the microchannel of the micro- gas chromatographic column of silicon substrate.
Preferably, also with one kind in multiple trench cells and the formed group of multiple micro-pillar arrays in micro- raceway groove
Or two kinds, the silicon nanowires forest is prepared in the multiple trench cells and the multiple micro-pillar array surface.
Preferably, the encapsulation cover plate includes silicon cover board, and the silicon cover board is prepared in region corresponding with the micro- raceway groove
There is silicon nanowires forest, closing technique by silicon-silicon bond is bonded the silicon cover board with the silicon substrate.
Preferably, further include：The corresponding of silicon nanowires forest surface is formed in based on component needed to be separated to repair
Exterior material.
Preferably, the decorative material includes octadecyl trichlorosilane alkane, octadecyldimethylchlorosilane and octadecane
One kind in base trimethoxy silane.
Preferably, the encapsulation cover plate includes the glass cover-plate of twin polishing, is bonded to by anode linkage method described
On the bonding face of silicon substrate.
Preferably, the line footpath of the silicon nanowires in the silicon nanowires forest is between 1~100 nanometer.
As described above, micro- gas chromatographic column of the silicon substrate of the utility model and preparation method thereof, has the advantages that：
The utility model is gloomy by being distributed one layer of fine and closely woven silicon nanowires on the inner surface of micro- raceway groove of silicon microfluidic chromatography column
Woods greatly increases the surface area of silicon microfluidic chromatography column, to be effectively improved the column capacity of silicon microfluidic chromatography column, separating degree and
Column is imitated.
Description of the drawings
Each step of preparation method that Fig. 1~Fig. 4 is shown as the micro- gas chromatographic column of silicon substrate of the utility model embodiment 1 is in
Existing structural schematic diagram.
Each step of preparation method that Fig. 5~Fig. 6 is shown as the micro- gas chromatographic column of silicon substrate of the utility model embodiment 2 is in
Existing structural schematic diagram.
Fig. 7 is shown as the silicon microfluidic chromatography column that the micro- raceway groove inner surface of the utility model contains one layer of fine and closely woven silicon nanowires forest
Structural scan electron microscope.
Fig. 8 is shown as the scanning electron microscope (SEM) photograph of the silicon nanowires forest of the micro- trench bottom of the utility model.
Fig. 9 is shown as the scanning electron microscope (SEM) photograph of the silicon nanowires forest of the micro- trench sidewalls of the utility model.
Figure 10 is shown as the scanning electron microscope (SEM) photograph of the silicon nanowires forest of micro-post surface in the micro- raceway groove of the utility model.
Component label instructions
1 micro- raceway groove
11 microtrabeculaes
12 micro- trench sidewalls
13 micro- trench bottoms
14 micro-fluidic ports
2 silicon substrates
21 silicon nitride films
22 photoresists
3 glass cover-plates
4 silicon nanowires forests
5 silicon cover boards
Specific implementation mode
Illustrate that the embodiment of the utility model, those skilled in the art can be by this theorys below by way of specific specific example
Content disclosed by bright book understands other advantages and effect of the utility model easily.The utility model can also be by addition
Different specific implementation modes are embodied or practiced, and the various details in this specification can also be based on different viewpoints and answer
With carrying out various modifications or alterations under the spirit without departing from the utility model.
Please refer to Fig.1~Figure 10.It should be noted that the diagram provided in the present embodiment only illustrates this in a schematic way
The basic conception of utility model, when only display is with related component in the utility model rather than according to actual implementation in illustrating then
Component count, shape and size are drawn, when actual implementation kenel, quantity and the ratio of each component can be a kind of random change
Become, and its assembly layout kenel may also be increasingly complex.
Embodiment 1
As shown in Figure 1 to 4, the present embodiment provides a kind of preparation method of the micro- gas chromatographic column of silicon substrate, the preparation sides
Method includes step：
As shown in Fig. 1~Fig. 2, step 1) is carried out first, a silicon substrate 2, the grown silicon nitride on the silicon substrate 2 are provided
Film 21, and spin coating photoresist 22 are formed the mask graph of silicon nitride and photoresist 22 using photo etching process, then adopted
Micro- raceway groove 1 is made in the silicon substrate 2 with DRIE techniques, then removes the photoresist 22, and micro- raceway groove 1 can be in past
It returns bending to extend, micro- raceway groove 1 includes bottom 13 and side wall 12.
As an example, also having in multiple trench cells and the formed group of 11 array of multiple microtrabeculaes in micro- raceway groove 1
One or two.
As an example, step 1) further includes the steps that making micro-fluidic port 14 in the both ends of micro- raceway groove 1.
It should be noted that the quantity of contained microtrabeculae 11 and aligning method do not limit to illustrated case in micro- raceway groove 1,
In addition, 11 array of the microtrabeculae can not also be contained in micro- raceway groove 1.
As shown in figure 3, step 2) is then carried out, using metal Assisted Chemical Etching Process technique in the interior table of micro- raceway groove 1
Face prepares silicon nanowires forest 4, and the silicon nanowires forest 4 can be prepared in the multiple trench cells and the multiple simultaneously
11 array surface of microtrabeculae.
As an example, step 2) includes：The silicon substrate 2 2-1) is put into first mixing comprising hydrofluoric acid and deionized water
It closes in solution, to remove the oxide layer on 1 surface of micro- raceway groove；2-2) silicon substrate 2 is put into comprising silver nitrate, hydrofluoric acid
And in the second mixed solution of deionized water, in the inner surface deposited metal silver of micro- raceway groove 1；2-3) by the silicon substrate
2 are put into the third mixed solution comprising hydrofluoric acid, hydrogen peroxide and deionized water, are carried out to the inner surface of micro- raceway groove 1 rotten
Erosion, the silicon nanowires forest 4 and 2-4 are formed with the inner surface in micro- raceway groove 1) silicon substrate 2 is put into nitric acid
In solution, the metallic silver to remove 1 inner surface of micro- raceway groove finally removes the silicon nitride film 21, to expose the silicon
The bonding face of substrate 2.
Preferably, step 2-2) in, the ratio of the silver nitrate, hydrofluoric acid and deionized water is between 4mL~12mL：10~
30mL：Between 40~80ml, the concentration of the silver nitrate is between 0.001~0.2mol/L, and the time of the deposition is between 1
Between~20min.
Preferably, step 2-3) in, the ratio of the hydrofluoric acid, hydrogen peroxide and deionized water is between 5~35ml：1~
10ml：Between 10~60ml, the temperature of the corrosion between 20~60 DEG C, time of the corrosion between 1~10min it
Between.
Preferably, step 2-4) in, the mass fraction of the salpeter solution between 55%~75%, the removal
Time is between 10~50min.
Preferably, step 2-2) while the deposition uniform oscillation treatment, step 2-3 are carried out to the silicon substrate 2)
Uniform oscillation treatment is carried out to the silicon substrate 2 while the corrosion.
Specifically, the present embodiment uses two-step method metal Assisted Chemical Etching Process (Two-step metal-assisted
Chemical etching) technique prepares fine and closely woven silicon nanowires forest 4 in 1 inner surface of micro- raceway groove；The two-step method gold
Belonging to Assisted Chemical Etching Process technique detailed process includes：
1) by the silicon substrate 2 be put into 70ml hydrofluoric acid, 140ml deionized waters mixed solution in react 10min, to go
Except the oxide layer on 1 surface of micro- raceway groove.The utility model first removes the oxide layer on 1 surface of micro- raceway groove, follow-up to ensure
The reaction efficiency of metal Assisted Chemical Etching Process, and distributing homogeneity, density and the quality of silicon nanowires forest 4 can be improved.
2) deposition of Ag：It takes 1g silver nitrates to be put into the silver nitrate solution for being configured to 0.02mol/L in 300ml aqueous solutions, takes
A concentration of 0.02mol/L silver nitrates of 8ml, and it is mixed into solution with 20ml hydrofluoric acid, 60ml deionized waters, removing oxide layer will be removed
Silicon substrate 2, which is put into solution, uniformly vibrates 6min.
3) prepared by silicon nanowires：The silicon substrate 2 for depositing Ag is put by 20ml hydrofluoric acid, 2ml hydrogen peroxide and 30ml are gone
The mixed solution that ionized water is prepared, 2.5min is heated at 40 DEG C, heating process pays attention to uniformly vibrating.
4) removal of Ag：After corroding, silicon substrate 2 is immersed to removal 2 table of silicon substrate in 68% salpeter solution immediately
The silver in face, soaking time 30min.
By above-mentioned metal Assisted Chemical Etching Process, it is good to obtain pattern, is evenly distributed, high density and quality is good
Silicon nanowires forest 4, substantially increase surface area, to be effectively improved the column capacity of silicon microfluidic chromatography column, separating degree and
Column is imitated.Preferably, the line footpath of the silicon nanowires in the silicon nanowires forest 4 is between 1~100 nanometer.
As shown in figure 4, then carrying out step 3), provide an encapsulation cover plate, by the encapsulation cover plate and the silicon substrate 2 into
Line unit closes, and to close micro- raceway groove 1, forms the microchannel of the micro- gas chromatographic column of silicon substrate.
As an example, the encapsulation cover plate includes the glass cover-plate 3 of twin polishing, institute is bonded to using anode linkage method
On the bonding face for stating silicon substrate 2, bonding temperature is between 200-450 DEG C, and bonding voltage is between 600-1400V.
As an example, further including step：It is formed accordingly in 4 surface of silicon nanowires forest based on component needed to be separated
Decorative material.The decorative material includes octadecyl trichlorosilane alkane, octadecyldimethylchlorosilane and octadecyl three
One kind in methoxy silane.The step of forming the decorative material include：Step a), it includes toluene and the modification material to prepare
The mixed liquor is injected into micro- raceway groove 1 and reacts by the mixed liquor of material；And step b), alcohol is used after reaction
Micro- raceway groove 1 is cleaned, and all removes the alcohol in micro- raceway groove 1 under vacuum or low pressure environment.
Finally, step 4) is carried out：Scribing obtains the micro- gas chromatographic column chip of silicon substrate, and is installed in the micro-fluidic port 14
Capillary.
As shown in figure 4, the present embodiment also provides a kind of micro- gas chromatographic column of silicon substrate, including：Silicon substrate 2；Micro- raceway groove 1, shape
In silicon substrate 2 described in Cheng Yu；Micro-fluidic port 14 is formed in 1 both ends of micro- raceway groove；Silicon nanowires forest 4 is prepared in described
In micro- raceway groove 1；And encapsulation cover plate, it is bonded to 2 surface of the silicon substrate, to close micro- raceway groove 1, forms the micro- gas phase of silicon substrate
The microchannel of chromatographic column.
Also with one kind or two in multiple trench cells and the formed group of 11 array of multiple microtrabeculaes in micro- raceway groove 1
Kind, the silicon nanowires forest 4 is prepared in 11 array surface of the multiple trench cells and the multiple microtrabeculae.
The micro- gas chromatographic column of silicon substrate further includes：It is formed in the silicon nanowires forest 4 based on component needed to be separated
The corresponding decorative material on surface.The decorative material include octadecyl trichlorosilane alkane, octadecyldimethylchlorosilane and
One kind in octadecyl trimethoxysilane.
As an example, the encapsulation cover plate includes the glass cover-plate 3 of twin polishing, institute is bonded to by anode linkage method
On the bonding face for stating silicon substrate 2.
Preferably, the line footpath of the silicon nanowires in the silicon nanowires forest 4 is between 1~100 nanometer.
Fig. 7 is shown as the silicon microfluidic chromatography column that the micro- raceway groove inner surface of the utility model contains one layer of fine and closely woven silicon nanowires forest
Structural scan electron microscope.Fig. 8 is shown as the scanning electron microscope (SEM) photograph of the silicon nanowires forest of the micro- trench bottom of the utility model.Fig. 9 is aobvious
It is shown as the scanning electron microscope (SEM) photograph of the silicon nanowires forest of the micro- trench sidewalls of the utility model.Figure 10 is shown as the micro- raceway groove of the utility model
The scanning electron microscope (SEM) photograph of the silicon nanowires forest of interior micro-post surface.As seen from the figure, the utility model passes through in the micro- of silicon microfluidic chromatography column
It is distributed one layer of fine and closely woven silicon nanowires forest 4 on the inner surface of raceway groove 1, greatly increases the surface area of silicon microfluidic chromatography column, from
And it is effectively improved column capacity, separating degree and the column effect of silicon microfluidic chromatography column.
Embodiment 2
As shown in Fig. 1~Fig. 3 and Fig. 5~Fig. 6, the present embodiment provides a kind of preparation method of the micro- gas chromatographic column of silicon substrate,
Its basic step such as embodiment 1, wherein difference from example 1 is that：The encapsulation cover plate includes silicon cover board 5, described
Silicon cover board 5 is prepared in region corresponding with micro- raceway groove 1 silicon nanowires forest 4, and technique is closed by the silicon by silicon-silicon bond
Cover board 5 is bonded with the silicon substrate 2.For example, patterned silicon nitride mask layer is formed prior to 5 surface of silicon cover board,
Then it uses the method such as step 2) to prepare the silicon in the surface in the silicon cover board 5 region corresponding with micro- raceway groove 1 to receive
Rice noodles forest 4 closes technique finally by silicon-silicon bond and is bonded the silicon cover board 5 with the silicon substrate 2.
As shown in fig. 6, the present embodiment also provides a kind of micro- gas chromatographic column of silicon substrate, basic structure such as embodiment 1,
In, difference from example 1 is that：The encapsulation cover plate include silicon cover board 5, the silicon cover board 5 in micro- raceway groove 1
Prepared by corresponding region have silicon nanowires forest 4, and closing technique by silicon-silicon bond carries out the silicon cover board 5 with the silicon substrate 2
Bonding.
The present embodiment, can be into one by making the silicon nanowires forest 4 corresponding with micro- raceway groove 1 on silicon cover board
Step improves the surface area of silicon microfluidic chromatography column, to further increase column capacity, separating degree and the column effect of silicon microfluidic chromatography column.
As described above, micro- gas chromatographic column of the silicon substrate of the utility model and preparation method thereof, has the advantages that：
The utility model is gloomy by being distributed one layer of fine and closely woven silicon nanowires on the inner surface of micro- raceway groove 1 of silicon microfluidic chromatography column
Woods 4 greatly increases the surface area of silicon microfluidic chromatography column, to be effectively improved column capacity, the separating degree of silicon microfluidic chromatography column
It is imitated with column.
So the utility model effectively overcomes various shortcoming in the prior art and has high industrial utilization.
The above embodiments are only illustrative of the principle and efficacy of the utility model, new not for this practicality is limited
Type.Any person skilled in the art can all carry out above-described embodiment under the spirit and scope without prejudice to the utility model
Modifications and changes.Therefore, such as those of ordinary skill in the art without departing from the revealed essence of the utility model
All equivalent modifications completed under refreshing and technological thought or change, should be covered by the claim of the utility model.
Claims (6)
1. a kind of micro- gas chromatographic column of silicon substrate, which is characterized in that including：
Silicon substrate；
Micro- raceway groove is formed in the silicon substrate；
Micro-fluidic port is formed in micro- raceway groove both ends；
Silicon nanowires forest is prepared in micro- raceway groove；And
Encapsulation cover plate is bonded to the surface of silicon, to close micro- raceway groove, forms the micro- logical of the micro- gas chromatographic column of silicon substrate
Road.
2. the micro- gas chromatographic column of silicon substrate according to claim 1, it is characterised in that：Also there are multiple ditches in micro- raceway groove
One or both of road unit and the formed group of multiple micro-pillar arrays, the silicon nanowires forest are prepared in the multiple ditch
Road unit and the multiple micro-pillar array surface.
3. the micro- gas chromatographic column of silicon substrate according to claim 1, it is characterised in that：Further include：Based on needed to be separated group
Divide the corresponding decorative material for being formed in silicon nanowires forest surface.
4. the micro- gas chromatographic column of silicon substrate according to claim 1, it is characterised in that：The encapsulation cover plate includes twin polishing
Glass cover-plate, be bonded to by anode linkage method on the bonding face of the silicon substrate.
5. the micro- gas chromatographic column of silicon substrate according to claim 1, it is characterised in that：The encapsulation cover plate includes silicon cover board,
The silicon cover board is prepared in region corresponding with the micro- raceway groove silicon nanowires forest, and closing technique by silicon-silicon bond will be described
Silicon cover board is bonded with the silicon substrate.
6. the micro- gas chromatographic column of silicon substrate according to Claims 1 to 5 any one, it is characterised in that：The silicon nanowires
The line footpath of silicon nanowires in forest is between 1~100 nanometer.
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| CN201721816759.2U CN207623299U (en) | 2017-12-22 | 2017-12-22 | The micro- gas chromatographic column of silicon substrate |
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|---|---|---|---|
| CN201721816759.2U CN207623299U (en) | 2017-12-22 | 2017-12-22 | The micro- gas chromatographic column of silicon substrate |
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| CN207623299U true CN207623299U (en) | 2018-07-17 |
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2017
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