CN103776940A - Arrayed micro gas chromatographic column chip with super-large contact area - Google Patents
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- CN103776940A CN103776940A CN201210398713.9A CN201210398713A CN103776940A CN 103776940 A CN103776940 A CN 103776940A CN 201210398713 A CN201210398713 A CN 201210398713A CN 103776940 A CN103776940 A CN 103776940A
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Abstract
The invention discloses an arrayed micro gas chromatographic column chip with a super-large contact area. The chip comprises a silicon substrate (5), channels (2) and arrayed vertical pillars (3) processed on the silicon substrate (5), the arrayed vertical pillars (3) are distributed in the channels (2), a layer of porous silicon (7) grows on the surface of each of the channels (2) and the arrayed vertical pillars (3) through an electrochemical corrosion method after the arrayed vertical pillars (3) and the channels (2) are processed, and the surface of the porous silicon (7) is fixed with a stationary phase. The chip comprises a sealing layer (6) sealing the channels (2) on the silicon substrate (5) in a bonding manner. The porous silicon of the chip has a loose and porous structure, so the surface area of the chip increases thousands of times; and the surface of the porous silicon is fixed with the stationary phase, so the bonding area of the stationary phase in the chromatographic column can be greatly increased, and is 5-10 times higher than that the bonding area of the stationary phase in a chromatographic column having an empty channel structure. The change of the speed and the pressure of a gas flow in channels having the above structure is much smaller than the change of the speed and the pressure of a gas flow in chromatographic columns having the empty channel structure, so the mixed gas separation capability is greatly improved.
Description
Technical field
The invention belongs to technical field of chromatographic analysis, be specifically related to array micro-scale gas chromatograph post chip of a kind of super large contact area and preparation method thereof, the present invention reaches the separation that is suitable for mixed gas, can be applied to field environment monitoring, biochemical war agent, food security, illicit drugs inspection, early diagnosis of cancer etc.
Background technology
Gas chromatographic column is one of key component of chromatographic analysis system, and its effect is the separation realizing mixed gas.Traditional chromatographic analysis systems adopts packed column or capillary column mostly, and this chromatographic column is generally long, takies volumetric spaces larger, and analysis speed is slow, is difficult to adapt to the demand that on-the-spot express-analysis detects.
The needs that detect in order to adapt to multi-field on-the site analysis, the micro-scale gas chromatograph post based on MEMS technology, because its ability with small structure and quick separating mixture enjoys favor.Therefore, micro-scale gas chromatograph post chip technology has obtained unprecedented development, has occurred take materials such as silicon, glass, metals as substrate the micro-scale gas chromatograph post chip of various shapes.
But existing these micro-scale gas chromatograph post chips, owing to being subject to the restriction of size, the length of chromatographic column is very limited, thereby fixing attaching surface in chromatographic column raceway groove amasss fewer, has limited fully contacting of mixed gas and fixing phase; On the other hand, the miniature chromatographic column of these sky raceway grooves, the pressure in its raceway groove and gas velocity change greatly, and pressure and flow velocity are the key factors that affects chromatographic column separating property.Therefore, these above unfavorable factors, have limited the ability of the separation component of chromatographic column, particularly to those complicated potpourris, separate difficulty especially, greatly reduce the responding ability to low concentration sample, have restricted the detection limit of detecting device.
Summary of the invention
(1) technical matters that will solve
Technical matters to be solved by this invention is to propose a kind of high resolving power, the overall good gas chromatographic column chip of separation efficiency, so that pressure change and the velocity variations of air-flow in chromatographic column is as far as possible little, and the bond area in chromatographic column is fixed in raising to greatest extent, thereby combination gas physical efficiency is fully contacted mutually with fixing in chromatogram raceway groove, reach the object that improves the resolution to mixed gas separation and overall separation efficiency.
(2) technical scheme
For solving above-mentioned technology department topic, the present invention proposes a kind of array micro-scale gas chromatograph post chip, comprises a substrate and the raceway groove of a connection forming in this substrate, and this chip also comprises multiple columns, it is formed in described raceway groove, and its short transverse is consistent with the depth direction of described raceway groove.
According to one embodiment of the present invention, there is porous silicon layer at the Surface Creation of described multiple columns and described raceway groove.
According to one embodiment of the present invention, be fixed with the fixing phase of one deck on the surface of described porous silicon layer.
According to one embodiment of the present invention, described porous silicon layer be shaped as dendroid, spongy or cellular.
According to one embodiment of the present invention, the width of each column in described multiple columns be described raceway groove width 1/10 to 1/2.
According to one embodiment of the present invention, 1/20 to 1/2 of the width that the spacing between the column of described multiple columns is raceway groove.
According to one embodiment of the present invention, described spacing is described channel width 1/10.
According to one embodiment of the present invention, the shape of cross section of described column is circle, quadrilateral or triangle.
According to one embodiment of the present invention, described chip also comprises a sample air intake opening and a sample gas outlet, and described sample air intake opening is positioned at one end of described raceway groove, is connected with a sampling system; Described sample gas outlet is positioned at the other end of raceway groove, is connected with a detecting device.
According to one embodiment of the present invention, described chip also has a sealant above described substrate.
The present invention also proposes a kind of method of manufacturing array micro-scale gas chromatograph post chip, comprises the steps: to form a substrate raceway groove of a connection, forms multiple columns in described raceway groove; In described substrate, seal a sealant.
According to one embodiment of the present invention, after forming described column, at porous silicon layer of superficial growth of described raceway groove and column.
According to one embodiment of the present invention, described porous silicon layer is by adopting electrochemical erosion method to prepare in HF ethanolic solution.
According to one embodiment of the present invention, after forming described sealant, in the fixing phase in the surface of described porous silicon.
(3) beneficial effect
Gas chromatographic column chip of the present invention arranges array column in raceway groove, and at the surface of raceway groove and superficial growth one deck porous silicon of array column, because the structure of porous silicon is loose porous shape, thousands of times of increases of its surface area, in the fixing phase of porous silicon surface, increase considerably fixing bond area in chromatographic column again.The chromatographic column of the empty channel structure of its Area Ratio, improve 5-10 doubly.
And gas of the present invention thinks that the interior gas velocity of raceway groove and the pressure change of chromatographic column chip are more much smaller than the chromatographic column of empty channel structure.Therefore, the array micro-scale gas chromatograph post chip of this super large contact area, the ability of its separating mixed gas is greatly improved.
Accompanying drawing explanation
Fig. 1 is the diagrammatic cross-section of the array micro-scale gas chromatograph post chip of the super large contact area of embodiments of the invention;
Fig. 2 is raceway groove and the array column pictorial diagram of the array micro-scale gas chromatograph post chip of the super large contact area of embodiments of the invention;
Fig. 3 is the structural representation (looking down from sealant) of the array micro-scale gas chromatograph post chip of the super large contact area of embodiments of the invention;
Fig. 4 is the process flow diagram of the manufacture method of embodiments of the invention.
Embodiment
The present invention proposes a kind of array micro-scale gas chromatograph post chip of super large contact area, by in micro-scale gas chromatograph stria road, array column is set, and by the method for galvanic corrosion, by micro-scale gas chromatograph post channel surface and array column superficial growth one deck porous silicon, because the structure of porous silicon is loose porous shape, thousands of times of increases of its surface area, therefore again in the fixing phase of porous silicon surface, can increase considerably fixing bond area in chromatographic column.
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, array micro-scale gas chromatograph post chip to super large contact area of the present invention and preparation method thereof elaborates.
Fig. 1 is the structural representation of the array micro-scale gas chromatograph post chip of the super large contact area of embodiments of the invention.As shown in Figure 1, this chip comprises a substrate 5, and from the upper surface of this substrate 5, and along the raceway groove 2 that is formed with a connection on its thickness direction, the degree of depth of described raceway groove 2 is less than the thickness of described substrate 5.In each described raceway groove 2, be distributed with multiple columns 3, the short transverse of described column 3 is consistent with the depth direction of described raceway groove 2.Multiple columns 3 in each raceway groove 2 form a column array, are therefore referred to as array column 3.All grow and have a porous silicon layer 7 on the surface of raceway groove 2r surface and array column 3.Above described substrate 5, also have a sealant 6, sealing layer 6, for sealing the raceway groove 2 of described substrate 5, is also fixed with the fixing phase of one deck on the surface of porous silicon 7.
According to the present invention, described chip also comprises a sample air intake opening 1 and sample gas outlet 4, and the position of sample air intake opening 1 is positioned at one end of described raceway groove 2, and it is connected with a sampling system, and sample gas outlet 4 is positioned at the other end of raceway groove 2, is connected with a detecting device.Analytic sample enters this gas chromatographic column chip through sample air intake opening 1, by the fixing phase adsorption and desorption on porous silicon 7 surfaces, due to the asynchronism(-nization) that phase adsorption and desorption experiences that is fixed of each component, therefore can realize the separation of each gas composition, thereby make the gas separating enter detecting device from sample gas outlet 4 one by one.
According to the present invention, the material of described substrate 5 is silicon.The thickness of described substrate is conventionally between 350 microns to 1000 microns, and in the present embodiment, the thickness of substrate is 500 microns.
Described raceway groove 2 is passages of air-flow, described array column 3 is equivalent to a kind of carrier, on the one hand, because column 3 is arranged in raceway groove 2, can prevent that gas velocity and pressure from changing excessive, on the other hand, because the surface area ratio of column is larger, the bond area that can increase fixing phase is made after porous silicon on its surface, more can significantly improve the bond area of fixing phase.
According to a kind of embodiment of the present invention, the degree of depth of described raceway groove 2 equates with the height of described array column 3.
As long as it is unimpeded that described raceway groove 2 meets air-flow, its shape of cross section can be varied, can be screw type, folding shape or snakelike, and the cross-sectional area of each column of described array column 3 is also changeable, but can not cause the obstruction of air-flow as good.Its cross sectional shape can be circle, quadrilateral or triangle, etc.The column number of the array column 3 comprising in described each raceway groove 2, is determined by the impact on gas velocity, conventionally on the section of each passage, have 2-10 column, the diameter of single column or width be raceway groove 2 width 1/10 to 1/2.In an embodiment of the present invention, in the section of each raceway groove 2, there are 4 columns.According to the present invention, the spacing between the column of described array column 3 can be the 1/20-1/2 of channel width, and in the present embodiment, described spacing is channel width 1/10.The distribution of described array column 3 in described raceway groove 2 can be regular distribution (various regular formation), can be also random distribution (random formation).
According to the present invention, the material that forms described array column 2 determines by the manufacturing process of chip, and in the present embodiment, it is by carrying out deep etching to substrate 5 or chemical corrosion forms, and therefore its constituent material is consistent with substrate.
Described sealant 6 is by forming with the material that bonding is carried out in substrate 5, and such as glass, silicon etc., in the present embodiment, adopt glass as sealant material.
Described porous silicon 7, it is the surface that is grown in raceway groove 2 and column 3, method by galvanic corrosion obtains, because porous silicon has loose porous structure, its surface area can thousands ofly increase, one deck porous silicon of all growing on the surface of raceway groove 2 and column 3, just can significantly expand the bond area of fixing phase, improve the separating power of chromatographic column, the thickness of porous silicon layer is generally no more than the diameter (or width) of column, in an embodiment of the present invention, the thickness of porous silicon and the radius of column are consistent.Described fixing phase, it is the surface that is fixed on porous silicon, when mixed gas is through fixing phase time, because its time to gas with various adsorption and desorption is different, thereby realize the separation to the each component of mixed gas, and its fixing means can be static, dynamic or other painting method, in an embodiment of the present invention, adopt the method for dynamic coating.
Fig. 2 is raceway groove and the array column pictorial diagram of the array micro-scale gas chromatograph post chip of the super large contact area of embodiments of the invention, to obtain in substrate 5 by deep etching or chemical corrosion, in an embodiment of the present invention, to obtain by deep etching technology etching, the height of the degree of depth of raceway groove 2 and column 3 can be from 50 microns-500 microns, in an embodiment of the present invention, the height of the degree of depth of raceway groove 2 and column 3 is all 250 microns.
Fig. 3 is the structural representation (vertical view from sealant 6 toward substrate 5) of the array micro-scale gas chromatograph post chip of the super large contact area of embodiments of the invention.Its principle of work is: mixed gas sample enters in raceway groove 2 through sample air intake opening 1, each component of mixed gas is by the fixing absorption mutually of porous silicon surface, desorption again, after each component is separated, discharge from sample air intake opening 4 successively, the gas of discharge is directly sent to detecting device and is carried out component detection (detecting device can be thermal conductivity detector (TCD), photoionization detector, flame ionization ditector, surface acoustic wave detector etc.) again.
The porous silicon of embodiments of the invention adopts electrochemical erosion method to prepare porous silicon in HF ethanolic solution, and it is shaped as dendroid, spongy or cellular.
More than describe concrete structure and the principle of work thereof of the array micro-scale gas chromatograph post chip of super large contact area of the present invention, described the method for manufacturing this chip below by specific embodiment and with reference to Fig. 4.
The method for making of micro-shape gas chromatographic column chip of the present invention comprises the steps:
First, preparation substrate 5.In the time of preparation substrate 5, first need base material to carry out pre-service, to remove surperficial impurity, in the present embodiment, we select N-type or P type silicon chip as base material, this silicon chip are carried out twin polishing and are cleaned, to remove surperficial impurity.
After base material is carried out to pre-service; the sealer when one deck of growing in this substrate 5 is again made porous silicon and the protective seam of one deck deep etching; for example; in an embodiment of the present invention; on silicon base material, first pass through LPCVD or PECVD growth one deck silicon nitride; with as growth protective seam at substrate 5 upper surfaces and column 3 upper surfaces when porous silicon, the thickness of silicon nitride layer can be
between, in the present embodiment, select thickness to be
(as shown in a figure of Fig. 4).Again on silicon nitride layer with the method such as electron beam or sputter deposition one deck mask layer, as the mask of deep etching, it can be aluminium lamination, the thickness range of aluminium lamination can be
between select, be also in the present embodiment
(as shown in the b figure of Fig. 4).
Then, in described substrate 5, form the raceway groove 2 of a connection, and simultaneously at the interior formation array of described raceway groove 2 column 3, described array column 3 is the arrays that are made up of multiple columns.
According to this embodiment of the invention, in this step, first remove aluminium lamination (as shown in the c figure of Fig. 4) with photoetching, wet corrosion technique, utilize reactive ion etching process to remove silicon nitride layer (as shown in the d figure of Fig. 4), expose the region that will form described raceway groove 2 and array column 3, recycling deep etching formula technique etching obtains this raceway groove 2 and array column 3.In an embodiment of the present invention, utilize H
3pO
4wet etching removes aluminium lamination, so uses SF
6as etchant gas, answer ion etching technique to remove silicon nitride layer, recycling SF
6and CCl
2f
2as etchant gas, utilize deep etching formula technique etching to obtain this raceway groove 2 and array column 3 (as shown in the e figure of Fig. 4)
The cross-sectional width of the raceway groove 2 obtaining according to the present invention can be between 50-400 micron, length (from the sample air intake opening 1 of chromatographic column to the raceway groove total length sample gas outlet 4) between 0.5-6 rice, the degree of depth is between 50-400 micron.In this embodiment, width, length and the degree of depth are respectively 250 microns 3 meters and 250 microns.
In described array column 3, the spacing between spacing, column and column between sidewall and the column of raceway groove 2 can be selected between 10-50 micron, and the diameter of single column can be selected at 10-100 micron.In the present embodiment, the spacing between spacing, column and column between sidewall and the column of raceway groove 2 is respectively 20 microns, 20 microns, and the diameter of single column is 40 microns.
Then at the raceway groove 2 forming and superficial growth one deck porous silicon of array column 3, the thickness of porous silicon can be selected between 1 micron-50 microns, in an embodiment of the present invention, the thickness of porous silicon is 20 microns, the shape of porous silicon can be dendroid, spongy or cellular, in an embodiment of the present invention, porous silicon be shaped as spongy.
According to this embodiment of the invention, in this step, porous silicon 7 is by adopting electrochemical erosion method to prepare (as shown in the f figure of Fig. 4) in HF ethanolic solution.
Finally, will in substrate 5, seal a sealant 6, obtain micro-scale gas chromatograph post chip.
After forming described raceway groove 2 and array column 3, with SF6 as etchant gas, answer ion etching technique to remove the silicon nitride layer outside raceway groove in substrate 5 (as shown in the g figure of Fig. 4), again by sealing technologies such as bonding technologies, substrate 5 is aimed at and sealed with the layer being made up of encapsulant, thereby obtain micro-scale gas chromatograph post chip (as shown in the h figure of Fig. 4).The material of the sealant 6 adopting can be glass or silicon.Bonding technology can anode linkage technique or static bonding process.
According to the preferred embodiment of the present invention, after forming sealant 6, on the surface of described porous silicon 7, by static, the dynamic or fixing phase of additive method, then continue to pass into N in chromatographic column
2as protection gas, aging 4-6 hour at the temperature of 120-250 ℃.Can obtain the array micro-scale gas chromatograph post chip of this super large contact area, and for to mixed gas high-resolution separation.
As mentioned above, the bond area in gas chromatographic column of the present invention can improve 5-10 doubly than the chromatographic column of empty channel structure, and this structure, and in its raceway groove, gas velocity and pressure change are more much smaller than the chromatographic column of empty channel structure.Therefore, the array micro-scale gas chromatograph post chip of this super large contact area, its theoretical plate tower number can be largely increased with the resolution that component is separated, thereby realizes the high-resolution separation to various potpourris.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (14)
1. an array micro-scale gas chromatograph post chip, comprises a substrate (5) and the raceway groove (2) in the upper connection forming of this substrate (5), it is characterized in that, this chip also comprises:
Multiple columns (3), it is formed in described raceway groove, and its short transverse is consistent with the depth direction of described raceway groove (2).
2. array micro-scale gas chromatograph post chip as claimed in claim 1, is characterized in that, has porous silicon layer (7) at the Surface Creation of described multiple columns (3) and described raceway groove (2).
3. array micro-scale gas chromatograph post chip as claimed in claim 2, is characterized in that, is fixed with the fixing phase of one deck on the surface of described porous silicon layer (7).
4. array micro-scale gas chromatograph post chip as claimed in claim 2, is characterized in that, described porous silicon layer (7) be shaped as dendroid, spongy or cellular.
5. array micro-scale gas chromatograph post chip as claimed in claim 1, is characterized in that, the width of each column in described multiple columns (3) be described raceway groove (2) width 1/10 to 1/2.
6. array micro-scale gas chromatograph post chip as claimed in claim 1, is characterized in that, the spacing between the column of described multiple columns (3) be raceway groove (2) width 1/20 to 1/2.
7. array micro-scale gas chromatograph post chip as claimed in claim 1, is characterized in that, described spacing be described raceway groove (2) width 1/10.
8. array micro-scale gas chromatograph post chip as claimed in claim 1, is characterized in that, the shape of cross section of described column (3) is circle, quadrilateral or triangle.
9. array micro-scale gas chromatograph post chip as claimed in claim 1, it is characterized in that, described chip also comprises a sample air intake opening (1) and a sample gas outlet (4), described sample air intake opening (1) is positioned at one end of described raceway groove (2), is connected with a sampling system;
Described sample gas outlet (4) is positioned at the other end of raceway groove (2), is connected with a detecting device.
10. array micro-scale gas chromatograph post chip as claimed in claim 1, is characterized in that, described chip also has a sealant (6) in the top of described substrate (5).
The method of 11. 1 kinds of manufacturing array micro-scale gas chromatograph post chips, is characterized in that comprising the steps:
The raceway groove (2) that forms a connection in a substrate (5) forms multiple columns (3) in described raceway groove;
At described substrate (5) sealant of upper sealing (6).
The method of 12. manufacturing array micro-scale gas chromatograph post chips as claimed in claim 11, it is characterized in that, forming described column (3) afterwards, at a porous silicon layer of superficial growth (7) of described raceway groove (2) and column (3).
The method of 13. manufacturing array micro-scale gas chromatograph post chips as claimed in claim 12, is characterized in that, described porous silicon layer (7) is by adopting electrochemical erosion method to prepare in HF alcoholic solution.
The method of 14. manufacturing array micro-scale gas chromatograph post chips as claimed in claim 11, is characterized in that, is forming described sealant (6) afterwards, in the fixing phase in the surface of described porous silicon (7).
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