CN108181415A - Micro- thermal conductivity detector (TCD) of film-type and preparation method thereof - Google Patents

Micro- thermal conductivity detector (TCD) of film-type and preparation method thereof Download PDF

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Publication number
CN108181415A
CN108181415A CN201611124545.9A CN201611124545A CN108181415A CN 108181415 A CN108181415 A CN 108181415A CN 201611124545 A CN201611124545 A CN 201611124545A CN 108181415 A CN108181415 A CN 108181415A
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film
micro
tcd
thermal conductivity
medium
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CN108181415B (en
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冯飞
侯磊
田博文
李昕欣
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Shanghai Institute of Microsystem and Information Technology of CAS
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Shanghai Institute of Microsystem and Information Technology of CAS
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/62Detectors specially adapted therefor
    • G01N30/64Electrical detectors
    • G01N30/66Thermal conductivity detectors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81BMICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B1/00Devices without movable or flexible elements, e.g. microcapillary devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00436Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
    • B81C1/00444Surface micromachining, i.e. structuring layers on the substrate
    • B81C1/00468Releasing structures
    • B81C1/00476Releasing structures removing a sacrificial layer
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00642Manufacture or treatment of devices or systems in or on a substrate for improving the physical properties of a device
    • B81C1/0065Mechanical properties
    • B81C1/00666Treatments for controlling internal stress or strain in MEMS structures
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C3/00Assembling of devices or systems from individually processed components
    • B81C3/001Bonding of two components
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

Abstract

The present invention provides a kind of micro- thermal conductivity detector (TCD) of film-type and preparation method thereof, and the micro- thermal conductivity detector (TCD) of the film-type has sandwich structure, is glass substrate, the silicon chip with very low power and the glass with micro- raceway groove successively from below to up;For cross network structure fabrication in silicon chip surface and among being suspended in microchannel, structure is the thermistor protected by two layers of silica/silicon nitride film;Critical process includes passing through deep reaction ion etching(DRIE)Technique etching silicon wafer back side silicon release cross network structure, the making of detector chip is led by the completion of electrostatic bonding twice low-grade fever.Two layers of silica/silicon nitride film up and down of the thermistor of the present invention not only plays a protective role to it; and symmetrical due to structure can also play the role of stress equilibrium; the deformation of cross network structure is reduced, substantially increases the intensity and stability of thermistor support construction;Cross network structure is discharged using a step DRIE techniques so that very low power sidewall, device dead volume are small.

Description

Micro- thermal conductivity detector (TCD) of film-type and preparation method thereof
Technical field
The invention belongs to microelectromechanical systems field, more particularly to a kind of micro- thermal conductivity detector (TCD) of film-type and its making Method.
Background technology
Thermal conductivity detector (TCD) is a kind of important detector of gas chromatograph, and this detector is only to the dense of detected gas Degree is sensitive, and almost all gas is all responded.Traditional gas chromatography thermal conductivity detector is generally added using stainless steel or ceramics Work forms, and volume is big, weight weight, and power consumption is big, more importantly since processing technology restricts, and traditional thermal conductivity detector (TCD) generally all has There is a larger dead volume, about tens to several hectolambdas, which has limited the reductions of thermal conductivity detector (TCD) Monitoring lower-cut.
With the development of MEMS (Micro-electro-mechanical system) technology, designed using MEMS technology, The low-grade fever of making, which leads detector chip, has many advantages, such as small, light-weight, small power consumption, and what is more important is based on MEMS technology The dead volume of the thermal conductivity detector (TCD) of making is greatly lowered and (is generally less than 1 microlitre, be nanoliter magnitude), and Monitoring lower-cut is up to several Ppm is even less than 1ppm.
In existing low-grade fever leads detector technologies scheme, thermistor be made on supporting layer and be suspended in micro- raceway groove it In, but there are Railway Projects:
1st, the supporting layer of thermistor is generally silicon nitride monofilm or silicon nitride/Si oxide compound film structure, due to answering The problems such as power is excessive or mismatch problems, and the structure after release can occur fracture, moderate finite deformation, collapse, this support construction are stablized Property is poor, easily by airflow influence.
2nd, based on potassium hydroxide (KOH) anisotropic etch or two step deep reaction ion etching techniques, (DRIE, the first step are Anisotropic etching, second step are isotropic etching) discharge support construction and shape from positive (thermistor side) corrosion silicon Into corresponding micro- raceway groove, excessive extra dead volume can be brought.
In order to obtain high performance micro- thermal conductivity detector (TCD), the above problem is the research of this field for being engaged in micro- thermal conductivity detector (TCD) The technical issues of personnel need to put forth effort to solve.
Invention content
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide a kind of micro- thermal conductivity detector (TCD)s of film-type And preparation method thereof, the supporting layer for solving thermistor in the prior art, which is easily broken off, and extra dead volume is excessive etc. asks Topic.
In order to achieve the above objects and other related objects, the present invention provides a kind of micro- thermal conductivity detector (TCD) of film-type, including:Silicon Substrate is formed with very low power structure in the silicon substrate;It is formed by first medium film-thermistor-second medium film Graphical stacked structure is hung in the positive very low power structure of the silicon substrate;Sheet glass with micro- raceway groove, is bonded to The silicon substrate front, and the graphical stacked structure is located in micro- raceway groove of the sheet glass;Glass substrate, bonding In the back side of the silicon substrate.
A kind of preferred embodiment of the micro- thermal conductivity detector (TCD) of film-type as the present invention, the very low power structure run through the silicon Substrate face and the back side.
As a kind of preferred embodiment of the micro- thermal conductivity detector (TCD) of film-type of the invention, pad is also formed in the silicon substrate Groove is formed with pad structure in the pad recess, and the pad structure is electrical connected with the thermistor.
A kind of preferred embodiment of the micro- thermal conductivity detector (TCD) of film-type as the present invention, metal used by the thermistor Including one kind in Pt/Ti laminations, Ni/Cr laminations, W/Ti laminations and W/Re laminations.
A kind of preferred embodiment of the micro- thermal conductivity detector (TCD) of film-type as the present invention, the first medium film and second Jie The planar structure of matter film be cross network structure, and in the cross network structure have multiple extensions, each extension with The silicon substrate connection, to support the cross network structure.
A kind of preferred embodiment of the micro- thermal conductivity detector (TCD) of film-type as the present invention, the thermistor are serrated along institute The extension of cross network structure is stated, and is connected between the pad structure.
A kind of preferred embodiment of the micro- thermal conductivity detector (TCD) of film-type as the present invention, the first medium film and second Jie Matter film includes the laminated construction of one or two kinds of compositions of silicon oxide film and silicon nitride film.
Preferably, the first medium film and second medium film form folded for silicon oxide film and silicon nitride film Layer structure, the first medium film are from bottom to top silicon oxide film and silicon nitride film laminated construction, the second medium Film is from bottom to top silicon nitride film and silicon oxide film laminated construction.
A kind of preferred embodiment of the micro- thermal conductivity detector (TCD) of film-type as the present invention, the first medium film and second Jie Matter film is wraps up the thermistor or the clamping thermistor.
A kind of preferred embodiment of the micro- thermal conductivity detector (TCD) of film-type as the present invention, the graphical stacked structure are hung on The middle section of the positive very low power structure of the silicon substrate, and the middle section in micro- raceway groove of the sheet glass.
A kind of preferred embodiment of the micro- thermal conductivity detector (TCD) of film-type as the present invention, it is the sheet glass and silicon substrate, described Glass substrate and silicon substrate are electrostatic bonding.
The present invention also provides a kind of preparation method of the micro- thermal conductivity detector (TCD) of film-type, the preparation method includes step:Step It is rapid 1) to provide a silicon substrate, deposit first medium film in the surface of silicon;Step 2), in the first medium film Upper deposited metal simultaneously graphically forms thermistor;Step 3), in depositing on the thermistor and first medium layer film Second medium film, formation first medium film-thermistor-the Film patterning to the first medium film and second medium The graphical stacked structure of second medium film;Step 4) provides a sheet glass for carrying micro- raceway groove, is bonded the sheet glass and institute Silicon substrate is stated, and the graphical stacked structure is located in micro- raceway groove of the sheet glass;Step 5), from back-etching institute Silicon substrate is stated, releases the graphical stacked structure of the first medium film-thermistor-second medium film;Step 6), One glass substrate is provided, and the glass substrate is bonded to the back side of the silicon substrate.
A kind of preferred embodiment of the preparation method of the micro- thermal conductivity detector (TCD) of film-type as the present invention, step 1) is in deposition the Further included before one dielectric film on the silicon substrate formed pad area groove the step of;After step 2) deposited metal, graphically Pad structure is formed in the pad recess simultaneously, the pad structure is electrical connected with the thermistor;In step 3), It is Film patterning to the first medium film and second medium while expose the bonding region of the pad structure and silicon substrate Domain.
A kind of preferred embodiment of the preparation method of the micro- thermal conductivity detector (TCD) of film-type as the present invention, it is described in step 2) Metal includes one kind in Pt/Ti laminations, Ni/Cr laminations, W/Ti laminations and W/Re laminations.
A kind of preferred embodiment of the preparation method of the micro- thermal conductivity detector (TCD) of film-type as the present invention, step 3) are graphical Afterwards, the planar structure of the first medium film and second medium film is cross network structure, and the cross network structure In have multiple extensions, each extension is in the graphical stacking of the first medium film-thermistor-second medium film It after structure release, is connect with the silicon substrate, to support the cross network structure.
A kind of preferred embodiment of the preparation method of the micro- thermal conductivity detector (TCD) of film-type as the present invention, the thermistor are in Zigzag extends along the cross network structure, and is connected between the pad structure.
A kind of preferred embodiment of the preparation method of the micro- thermal conductivity detector (TCD) of film-type as the present invention, the first medium are thin Film and second medium film include the laminated construction of one or two kinds of compositions of silicon oxide film and silicon nitride film.
Preferably, the first medium film and second medium film form folded for silicon oxide film and silicon nitride film Layer structure, the first medium film are from bottom to top silicon oxide film and silicon nitride film laminated construction, the second medium Film is from bottom to top silicon nitride film and silicon oxide film laminated construction.
A kind of preferred embodiment of the preparation method of the micro- thermal conductivity detector (TCD) of film-type as the present invention, the first medium are thin Film and second medium film is wrap up the thermistor or the clamping thermistor.
A kind of preferred embodiment of the preparation method of the micro- thermal conductivity detector (TCD) of film-type as the present invention, the graphical stacking Structure hangs on the middle section of the positive very low power structure of the silicon substrate, and in step 4), the sheet glass and described After silicon substrate bonding, the graphical stacked structure is located at the middle section in micro- raceway groove of the sheet glass.
A kind of preferred embodiment of the preparation method of the micro- thermal conductivity detector (TCD) of film-type as the present invention in step 5), uses Deep reaction ion etching technique releases the first medium film-thermistor-the second and is situated between from silicon substrate described in back-etching The graphical stacked structure of matter film.
A kind of preferred embodiment of the preparation method of the micro- thermal conductivity detector (TCD) of film-type as the present invention, the glass in step 4) Piece is bonded with the glass substrate in silicon substrate, step 6) with silicon substrate using static bonding process.
As described above, micro- thermal conductivity detector (TCD) of film-type of the present invention and preparation method thereof, has the advantages that:
1) two layers of silica/silicon nitride film up and down of thermistor of the invention not only plays a protective role to it, separately On the one hand due to the symmetrical deformation that can also play the role of stress equilibrium, reduce cross network structure of structure, thus Substantially increase the intensity and stability of thermistor support construction;
2) present invention discharges cross network structure using a step deep reaction ion etching DRIE techniques so that very low power side wall Steep, device dead volume is small.
Description of the drawings
Fig. 1 is shown as the schematic diagram of the cross network structure in the micro- thermal conductivity detector (TCD) of film-type of the present invention.
Fig. 2 is shown as micro- thermal conductivity detector (TCD) of the tool there are four thermistor.
Fig. 3 is shown as the Wheatstone bridge that four thermistors are formed.
Fig. 4~Figure 12 is shown as the structure that each step of production method of the micro- thermal conductivity detector (TCD) of film-type of the present invention is presented Schematic diagram, wherein, Figure 12 is shown as the micro- thermal conductivity detector (TCD) structure diagram of film-type.
Component label instructions
1 silicon substrate
11 very low power structures
12 cross network structures
2 oxide layers
3 pad recess
41 first medium films
42 second medium films
51 thermistors
52 pad structures
6 have the sheet glass of micro- raceway groove
7 glass substrates
81st, 83 microchannel
The interface channel of 82 installation capillaries
Specific embodiment
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through in addition different specific realities The mode of applying is embodied or practiced, the various details in this specification can also be based on different viewpoints with application, without departing from Various modifications or alterations are carried out under the spirit of the present invention.
Please refer to Fig.1~Figure 12.It should be noted that the diagram provided in the present embodiment only illustrates this in a schematic way The basic conception of invention, package count when only display is with related component in the present invention rather than according to actual implementation in illustrating then Mesh, shape and size are drawn, and kenel, quantity and the ratio of each component can be a kind of random change during actual implementation, and its Assembly layout kenel may also be increasingly complex.
As shown in FIG. 11 and 12, the micro- thermal conductivity detector (TCD) of film-type of the invention have sandwich structure, from below to up according to Secondary is glass substrate 7, the silicon substrate 1 with very low power and the sheet glass with micro- raceway groove 6.Cross network structure 12 is made in silicon substrate 1 surface and the middle section (distance of cross network structure to very low power two side walls is equal) for being suspended in very low power, such as Figure 11 And shown in 12, structure is the thermistor 51 protected by two layers of silica/silicon nitride film, is respectively from top to down:Oxygen SiClx/silicon nitride, thermistor 51, nitridation silicon/oxidative silicon, it is notable that in order to more clearly draw thermistor 51 Structure does not draw the silica/silicon nitride on upper strata in Fig. 1.In addition, it is necessary to explanation is:The friendship of other structures can be used Pitch 51 structure of reticular structure 12 and thermistor, it is not limited to structure shown in FIG. 1.This new structure design solves well It has determined two problems of the prior art:First, two layers of silica/silicon nitride film up and down of thermistor 51 not only plays it To protective effect, on the other hand since the symmetrical of structure can also play the role of stress equilibrium, cross network knot is reduced The deformation of structure 12;Second, using step DRIE techniques release cross network structure 12, very low power sidewall, device dead volume It is small.
A thermistor 51 is only depicted in Figure 11 and Figure 12, it is however generally that, a micro- thermal conductivity detector (TCD) includes four A thermistor 51R1, R2, R3, R4, as shown in Fig. 2, wherein R1, R4 are located in a microchannel 81, and in addition R2, R3 are located at In one microchannel 83, there are one the interface channels 82 of installation capillary respectively at the both ends of each microchannel.R1、R2、R3、R4 A Wheatstone bridge is formed according to as shown in Figure 3 being linked in sequence.
As shown in FIG. 11 and 12, the present embodiment provides a kind of micro- thermal conductivity detector (TCD) of film-type, including:Silicon substrate 1, it is described Very low power structure 11 is formed in silicon substrate 1;It is formed by first medium film 41- thermistor 51- second mediums film 42 Graphical stacked structure is hung in the positive very low power structure 11 of the silicon substrate 1;Sheet glass 6 with micro- raceway groove, key Together in 1 front of silicon substrate, and the graphical stacked structure is located in micro- raceway groove of the sheet glass 6;Glass lined Bottom 7 is bonded to the back side of the silicon substrate 1.
As an example, the very low power structure 11 is through 1 front of silicon substrate and the back side.
As an example, being also formed with pad recess 3 in the silicon substrate 1, pad structure is formed in the pad recess 52, the pad structure 52 is electrical connected with the thermistor 51.Metal includes Pt/Ti used by the thermistor 51 One kind in lamination, Ni/Cr laminations, W/Ti laminations and W/Re laminations.
As an example, the planar structure of the first medium film 41 and second medium film 42 is cross network structure 12, and there are multiple extensions in the cross network structure 12, each extension is connect with the silicon substrate 1, with described in support Cross network structure 12.The thermistor 51 is serrated to be extended, and be connected to the weldering along the cross network structure 12 Between dish structure 52.
As an example, the first medium film 41 and second medium film 42 include silicon oxide film and silicon nitride film One or two kinds of compositions laminated construction.The first medium film 41 and second medium film 42 is wrap up the temperature-sensitive electricity Resistance 51 or the clamping thermistor 51.
As an example, the graphical stacked structure is located at the middle section in micro- raceway groove of the sheet glass 6.
As an example, the sheet glass 6 is electrostatic bonding with silicon substrate 1, the glass substrate 7 and silicon substrate 1.
As shown in Fig. 4~Figure 12, the present embodiment also provides a kind of preparation method of the micro- thermal conductivity detector (TCD) of film-type, the system Preparation Method includes step:
As shown in Fig. 4~Fig. 6, step 1) is carried out first, a silicon substrate 1 is provided, in forming pad area on the silicon substrate 1 Groove as shown in Fig. 4~Fig. 5, then deposits first medium film 41, as shown in Figure 6 in 1 surface of silicon substrate.
As shown in fig. 6, then carrying out step 2), heat is formed in deposited metal on the first medium film 41 and graphically Quick resistance 51.
As an example, the metal includes one kind in Pt/Ti laminations, Ni/Cr laminations, W/Ti laminations and W/Re laminations.
In addition, in the present embodiment, it is graphical to form weldering in the pad recess 3 simultaneously after step 2) deposited metal Dish structure 52, the pad structure 52 are electrical connected with the thermistor 51.
As shown in Fig. 7~Fig. 8, step 3) is then carried out, is deposited on the thermistor 51 and first medium layer film Second medium film 42 graphically forms first medium film 41- to the first medium film 41 and second medium film 42 The graphical stacked structure of thermistor 51- second mediums film 42.
As an example, after step 3) is graphical, the planar structure of the first medium film 41 and second medium film 42 For cross network structure 12, and there are multiple extensions in the cross network structure 12, as shown in Figure 1, each extension is in institute After the graphical stacked structure release for stating first medium film 41- thermistor 51- second mediums film 42, with the silicon substrate 1 connection, to support the cross network structure 12.
Extend as an example, the thermistor 51 is serrated along the cross network structure 12, and be connected to described Between pad structure 52, as shown in Figure 1.
As an example, the first medium film 41 and second medium film 42 is wrap up the thermistor 51 or clamping The thermistor 51.
As an example, the first medium film 41 and second medium film 42 include silicon oxide film and silicon nitride film One or two kinds of compositions laminated construction.In the present embodiment, the first medium film 41 is thin for silica from bottom to top Film and silicon nitride film laminated construction, the second medium film 42 is silicon nitride film and silicon oxide film lamination from bottom to top Structure, i.e., what is contacted with the thermistor 51 is silicon nitride film, and silicon oxide film is then located at the silicon nitride film Except, the silicon oxide film is set to except silicon nitride film, can more effectively protect the thermistor 51, is increased The antioxygenic property of thermistor 51 and anti-etching/corrosivity of laminated construction.
Two layers of silica/silicon nitride film up and down of the thermistor 51 of the present invention not only plays a protective role to it, separately On the one hand due to the symmetrical deformation that can also play the role of stress equilibrium, reduce cross network structure 12 of structure, from And substantially increase the intensity and stability of 51 support construction of thermistor.
As an example, in step 3), the first medium film 41 and second medium film 42 are graphically exposed simultaneously The bond area of the pad structure 52 and silicon substrate 1.
As shown in figure 9, then carry out step 4), provide one carry micro- raceway groove sheet glass 6, be bonded the sheet glass 6 and The silicon substrate 1, and cause the graphical stacked structure be located in micro- raceway groove of the sheet glass 6, the sheet glass 6 it is micro- Very low power on raceway groove and the silicon substrate 1 collectively constitutes the microchannel 81,83 of the micro- thermal conductivity detector (TCD) of film-type.
As an example, after the sheet glass 6 and the silicon substrate 1 are bonded, the graphical stacked structure is located at the glass Middle section in micro- raceway groove of glass piece 6.
As an example, the sheet glass 6 in step 4) is bonded with silicon substrate 1 using static bonding process.
It should be noted that the specific size of micro- raceway groove and the very low power on silicon substrate can be with coming according to actual needs on glass It determines.The size of micro- raceway groove can be determined by the control corrosion rate time on glass;The depth of very low power on silicon substrate is by silicon chip Thickness determines.
As shown in Figure 10, step 5) is then carried out, from silicon substrate 1 described in back-etching, it is thin to release the first medium The graphical stacked structure of film 41- thermistor 51- second mediums film 42.
As an example, it releases described first from silicon substrate 1 described in back-etching using deep reaction ion etching technique and is situated between The graphical stacked structure of matter film 41- thermistor 51- second mediums film 42.The present invention is carved using a step deep reactive ion Lose DRIE techniques release cross network structure 12 so that very low power sidewall, device dead volume are small.
As shown in FIG. 11 and 12, step 6) is finally carried out, provides a glass substrate 7, and the glass substrate 7 is bonded In the back side of the silicon substrate 1.
As an example, the glass substrate 7 is bonded with silicon substrate 1 using static bonding process.
In a specific implementation process, the preparation method of the micro- thermal conductivity detector (TCD) of film-type includes the following steps:
1) silicon substrate 1 is provided, oxidation is carried out to the silicon substrate 1 and forms oxide layer 2 simultaneously graphically, as shown in Figure 4;
2) corroded using KOH and pad recess 3, corrosion depth is more than 0.5 micron and less than 10 microns, as shown in Figure 5;
3) silicon oxide deposition/silicon nitride film, then splash-proofing sputtering metal Pt/Ti or Ni/Cr or W/Ti or W/Re, and figure Change, form thermistor 51 and metal pad, as shown in Figure 6;
4) deposit silicon nitride/silicon oxide film, as shown in Figure 7;
5) etch silicon nitride/silicon oxide film exposes the silicon of pad area and bonding region (it is worth noting that, temperature-sensitive is electric Silicon nitride/silicon oxide film of 51 top of resistance and silica/silicon nitride of lower section can be with fully wrapped around metal Pr/Ti or Ni/Cr Or W/Ti or W/Re, Pr/Ti or Ni/Cr or W/Ti or W/Re can also be clamped), as shown in Figure 8;
6) sheet glass 6 for having micro- raceway groove will be corroded and 1 front of silicon substrate carries out electrostatic bonding, as shown in Figure 9;
7) DRIE etches the back side silicon of silicon substrate 1, discharges cross network structure 12, as shown in Figure 10;
8) back side silicon of silicon substrate 1 and glass substrate 7 carry out electrostatic bond and merge scribing formation low-grade fever leading detector chip, such as Shown in Figure 11 and Figure 12.
As described above, micro- thermal conductivity detector (TCD) of film-type of the present invention and preparation method thereof, has the advantages that:
1) two layers of silica/silicon nitride film up and down of thermistor 51 of the invention not only plays a protective role to it, On the other hand due to the symmetrical deformation that can also play the role of stress equilibrium, reduce cross network structure 12 of structure, So as to substantially increase the intensity and stability of 51 support construction of thermistor;
2) present invention is using step deep reaction ion etching DRIE techniques release cross network structure 12 so that very low power side Wall is steep, and device dead volume is small.
So the present invention effectively overcomes various shortcoming of the prior art and has high industrial utilization.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe The personage for knowing this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as Into all equivalent modifications or change, should by the present invention claim be covered.

Claims (22)

1. a kind of micro- thermal conductivity detector (TCD) of film-type, it is characterised in that:Including:
Silicon substrate is formed with very low power structure in the silicon substrate;
The graphical stacked structure formed by first medium film-thermistor-second medium film, hangs on the silicon substrate Positive very low power structure in;
Sheet glass with micro- raceway groove is bonded to the silicon substrate front, and it is described so that the graphical stacked structure is located at In micro- raceway groove of sheet glass;
Glass substrate is bonded to the back side of the silicon substrate.
2. the micro- thermal conductivity detector (TCD) of film-type according to claim 1, it is characterised in that:The very low power structure is through described Silicon substrate front and the back side.
3. the micro- thermal conductivity detector (TCD) of film-type according to claim 1, it is characterised in that:It is also formed with welding in the silicon substrate Disk groove is formed with pad structure in the pad recess, and the pad structure is electrical connected with the thermistor.
4. the micro- thermal conductivity detector (TCD) of film-type according to claim 1, it is characterised in that:It is golden used by the thermistor Belong to the one kind included in Pt/Ti laminations, Ni/Cr laminations, W/Ti laminations and W/Re laminations.
5. the micro- thermal conductivity detector (TCD) of film-type according to claim 1, it is characterised in that:The first medium film and second The planar structure of dielectric film is cross network structure, and has multiple extensions, each extension in the cross network structure It is connect with the silicon substrate, to support the cross network structure.
6. the micro- thermal conductivity detector (TCD) of film-type according to claim 5, it is characterised in that:The thermistor is serrated edge The cross network structure extension, and be connected between the pad structure.
7. the micro- thermal conductivity detector (TCD) of film-type according to claim 1, it is characterised in that:The first medium film and second Dielectric film includes the laminated construction of one or two kinds of compositions of silicon oxide film and silicon nitride film.
8. the micro- thermal conductivity detector (TCD) of film-type according to claim 7, it is characterised in that:The first medium film and second The laminated construction that dielectric film is formed for silicon oxide film and silicon nitride film, the first medium film are from bottom to top oxidation Silicon thin film and silicon nitride film laminated construction, the second medium film are folded from bottom to top for silicon nitride film with silicon oxide film Layer structure.
9. the micro- thermal conductivity detector (TCD) of film-type according to claim 1, it is characterised in that:The first medium film and second Dielectric film is wraps up the thermistor or the clamping thermistor.
10. the micro- thermal conductivity detector (TCD) of film-type according to claim 1, it is characterised in that:The graphical stacked structure hangs It is hung on the middle section of the positive very low power structure of the silicon substrate, and the central area in micro- raceway groove of the sheet glass Domain.
11. the micro- thermal conductivity detector (TCD) of film-type according to claim 1, it is characterised in that:The sheet glass and silicon substrate, institute It is electrostatic bonding that glass substrate, which is stated, with silicon substrate.
12. a kind of preparation method of the micro- thermal conductivity detector (TCD) of film-type, which is characterized in that the preparation method includes step:
Step 1) provides a silicon substrate, and first medium film is deposited in the surface of silicon;
Step 2) forms in deposited metal on the first medium film and graphically thermistor;
Step 3) is thin to the first medium in deposition second medium film on the thermistor and first medium layer film Film and the Film patterning graphical stacked structure for forming first medium film-thermistor-second medium film of second medium;
Step 4) provides a sheet glass for carrying micro- raceway groove, is bonded the sheet glass and the silicon substrate, and cause the figure Change stacked structure to be located in micro- raceway groove of the sheet glass;
Step 5) from silicon substrate described in back-etching, releases the first medium film-thermistor-second medium film Graphical stacked structure;
Step 6) provides a glass substrate, and the glass substrate is bonded to the back side of the silicon substrate.
13. the preparation method of the micro- thermal conductivity detector (TCD) of film-type according to claim 12, it is characterised in that:Step 1) is heavy It is further included before product first medium film in pad area groove is formed on the silicon substrate the step of;After step 2) deposited metal, figure Shapeization forms pad structure in the pad recess simultaneously, and the pad structure is electrical connected with the thermistor;Step 3) it is Film patterning to the first medium film and second medium while expose the key of the pad structure and silicon substrate in Close region.
14. the preparation method of the micro- thermal conductivity detector (TCD) of film-type according to claim 12, it is characterised in that:In step 2), The metal includes one kind in Pt/Ti laminations, Ni/Cr laminations, W/Ti laminations and W/Re laminations.
15. the preparation method of the micro- thermal conductivity detector (TCD) of film-type according to claim 12, it is characterised in that:Step 3) figure After change, the planar structure of the first medium film and second medium film is cross network structure, and the cross network knot There are multiple extensions, each extension is in the graphical heap of the first medium film-thermistor-second medium film in structure After stack structure release, it is connect with the silicon substrate, to support the cross network structure.
16. the preparation method of the micro- thermal conductivity detector (TCD) of film-type according to claim 15, it is characterised in that:The temperature-sensitive electricity Resistance is serrated to be extended, and be connected between the pad structure along the cross network structure.
17. the preparation method of the micro- thermal conductivity detector (TCD) of film-type according to claim 12, it is characterised in that:Described first is situated between Matter film and second medium film include the laminated construction of one or two kinds of compositions of silicon oxide film and silicon nitride film.
18. the preparation method of the micro- thermal conductivity detector (TCD) of film-type according to claim 17, it is characterised in that:Described first is situated between The laminated construction that matter film and second medium film are formed for silicon oxide film and silicon nitride film, the first medium film is certainly It is lower and upper for silicon oxide film and silicon nitride film laminated construction, the second medium film from bottom to top for silicon nitride film with Silicon oxide film laminated construction.
19. the preparation method of the micro- thermal conductivity detector (TCD) of film-type according to claim 12, it is characterised in that:Described first is situated between Matter film and second medium film is wrap up the thermistor or the clamping thermistor.
20. the preparation method of the micro- thermal conductivity detector (TCD) of film-type according to claim 12, it is characterised in that:It is described graphical Stacked structure hangs on the middle section of the positive very low power structure of the silicon substrate, and in step 4), the sheet glass and After the silicon substrate bonding, the graphical stacked structure is located at the middle section in micro- raceway groove of the sheet glass.
21. the preparation method of the micro- thermal conductivity detector (TCD) of film-type according to claim 12, it is characterised in that:In step 5), Using deep reaction ion etching technique from silicon substrate described in back-etching, the first medium film-thermistor-the is released The graphical stacked structure of second medium film.
22. the preparation method of the micro- thermal conductivity detector (TCD) of film-type according to claim 12, it is characterised in that:In step 4) Sheet glass is bonded with the glass substrate in silicon substrate, step 6) with silicon substrate using static bonding process.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011044547A2 (en) * 2009-10-09 2011-04-14 Services Petroliers Schlumberger Micro-thermal conductivity detector, method to fabricate such and chromatography system using such
CN102730622A (en) * 2011-04-01 2012-10-17 中国科学院电子学研究所 Integrated chip of micro thermal conductive detector and manufacturing method for same
CN104764773A (en) * 2015-04-20 2015-07-08 中国科学院电子学研究所 Cantilever beam type metal oxide detector and manufacturing method thereof
CN104828771A (en) * 2015-03-16 2015-08-12 中国科学院电子学研究所 Micro thermal conductivity detector with integrated filtering structure and manufacturing method
CN105136871A (en) * 2015-06-19 2015-12-09 上海集成电路研发中心有限公司 Micro thermal conductivity detector structure and processing and manufacturing method thereof
CN105765378A (en) * 2014-04-14 2016-07-13 西门子公司 A thermal conductivity detector

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011044547A2 (en) * 2009-10-09 2011-04-14 Services Petroliers Schlumberger Micro-thermal conductivity detector, method to fabricate such and chromatography system using such
CN102549422A (en) * 2009-10-09 2012-07-04 普拉德研究及开发股份有限公司 Micro-thermal conductivity detector, method to fabricate such and chromatography system using such
CN102730622A (en) * 2011-04-01 2012-10-17 中国科学院电子学研究所 Integrated chip of micro thermal conductive detector and manufacturing method for same
CN105765378A (en) * 2014-04-14 2016-07-13 西门子公司 A thermal conductivity detector
CN104828771A (en) * 2015-03-16 2015-08-12 中国科学院电子学研究所 Micro thermal conductivity detector with integrated filtering structure and manufacturing method
CN104764773A (en) * 2015-04-20 2015-07-08 中国科学院电子学研究所 Cantilever beam type metal oxide detector and manufacturing method thereof
CN105136871A (en) * 2015-06-19 2015-12-09 上海集成电路研发中心有限公司 Micro thermal conductivity detector structure and processing and manufacturing method thereof

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
B. C. KAANTA 等: "High Sensitivity Micro-Thermal Conductivity Detector for Gas Chromatography" *
D. CRUZ 等: "Microfabricated thermal conductivity detector for the micro-ChemLabTM" *
SUN J H 等: "Design, modeling, microfabrication and characterization of novel micro thermal conductivity detector" *
孙建海 等: "基于MEMS技术的微型热导检测器的研制" *

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