CN105136871A - Micro thermal conductivity detector structure and processing and manufacturing method thereof - Google Patents
Micro thermal conductivity detector structure and processing and manufacturing method thereof Download PDFInfo
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- CN105136871A CN105136871A CN201510349171.XA CN201510349171A CN105136871A CN 105136871 A CN105136871 A CN 105136871A CN 201510349171 A CN201510349171 A CN 201510349171A CN 105136871 A CN105136871 A CN 105136871A
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Abstract
The invention provides a micro thermal conductivity detector structure containing a thermistor, a detector body, a metal connection wire and electrodes; the micro thermal conductivity detector structure is characterized in that the detector body is formed by taking silicon slices, each having the upper surface and the lower surface insulated and each having the interior containing grooves, as cover plates, allowing groove positions to align and be laminated and carrying out silicon-silicon interface bonding sealing. The invention provides a processing and manufacturing method matched with the structure; the silicon slices are used as the upper cover plate and the lower cover plate of the thermal conductivity detector; through a standard MEMS body silicon release technology and a DRIE technology, the grooves are obtained at corresponding positions of the upper cover plate and the lower cover plate; a conventional semiconductor insulation material is adopted for completion of insulation of the cover plate surfaces; a semiconductor metal is used for preparing the metal connection wire and the electrodes; the thermistor is formed by a photoresist stripping process; finally the grooves of the upper cover plate and the lower cover plate align and are laminated and then are subjected to silicon-silicon interface bonding to complete sealing. The processing and manufacturing method is compatible with a conventional semiconductor process, the process is easy to implement, the technology is mature and the stability is good.
Description
Technical field
The present invention relates to MEMS processing and manufacturing technical field, particularly a kind of structure of Micro Thermal Conductivity Detector and machining manufacture thereof.
Background technology
Thermal conductivity detector (TCD) (TCD) is a kind of application common detector comparatively early, existing still in widespread use, is the important detector type of one of gas chromatograph.Conventional thermal conductivity detector (TCD) is made up of parts such as conductance cell, measurement bridge road, stabilized voltage supplys, and wherein conductance cell is one of core component, is made up of thermal sensing element and pond body.
Thermal sensing element adopts the metal materials such as Pt, Au, W to form.
The gage beam that thermal conductivity cell detector is generally equipped with thermal sensing element by two forms, and is to utilize tested gas different with the thermal conductivity coefficient of reference gas and the concentration detector of response.Because different gas has different thermal conductivity coefficients, when reference gas is simultaneously by 2 arms, have same impact to the heat transfer of two-arm, also identical on the impact of thermal sensing element temperature, thus the change in resistance of 2 thermal sensing elements is identical.When tested gas enters gage beam with reference gas, because the thermal conductivity coefficient of tested gas is different with the thermal conductivity coefficient of pure reference gas, thus make the temperature drop of 2 thermal sensing elements also different, cause the change in resistance of thermal sensing element to occur difference.
Existing commercially available thermal conductivity detector (TCD) is mostly, and first processes each building block respectively, then carries out mechanical package gained, and as the TCD product of Agilent, due to the restriction of machining, such thermal conductivity detector (TCD) is more difficult accomplishes microminiaturization.Some researchs carrying out TCD manufacture in conjunction with MEMS technology at present are also extensively being carried out, and comprise above-mentioned, by MEMS thermistor by bonding, are sealed in glass bulb.But, a lot of processing technologys of MEMS thermistor of the prior art and conductance cell, comprise manufacture material therefor and semiconductor technology incompatible, and more difficultly realize batch machining.For two thermal sensing elements of both arms thermal conductivity cell detector, owing to not being prepare so resistive performance there are differences inevitable simultaneously, this will cause systematical difference, reduces the precision of Measurement and analysis.Application number is the structure that the United States Patent (USP) of US8939012B2 proposes a kind of thermal conductivity detector (TCD), this patent lays particular emphasis on the optimization realizing units test performance, involved procedure of processing mostly is non-planar surface process, the repeatability of processing technology is difficult to ensure, and wherein some material and semiconductor technology can not be compatible.
Therefore, for improving the degree of compatibility of MEMS Micro Thermal Conductivity Detector job operation and semiconductor technology further, realize the high precision of device, microminiaturization and batch production, need the Micro Thermal Conductivity Detector structure of an exploitation based semiconductor material and with it supporting compatible with semiconductor technology, be easy to realize, the manufacture method of full automatic semiconductor machining means can be made full use of, to realize reducing production cost, take into account guarantee machining precision simultaneously, improve the object of the analytical performance of finished product.
Summary of the invention
Technical matters to be solved by this invention is the machining manufacture proposing a kind of Micro Thermal Conductivity Detector, adopt the basic compatible technique with conventional semiconductor process, realize device miniaturization and batch production, reduce production cost, and can machining precision be ensured and improve the analytical performance of finished product.
For solving the problems of the technologies described above, the present invention proposes a kind of Micro Thermal Conductivity Detector structure, using conventional semiconductor material completely, develop that match with proposed structure with machining manufacture that the is Micro Thermal Conductivity Detector of semiconductor technology compatibility simultaneously.
The present invention proposes a kind of Micro Thermal Conductivity Detector structure, comprise thermistor, pond body and metal connecting line and electrode, it is characterized in that described pond body be by two surface insulations and inside all containing reeded silicon chip as cover plate, aim at groove location, fit up and down, form through silicon silicon interface bonded seal.
Optionally, described lower cover realizes insulation by surface deposition Si3N4 and SiO2 or SiON and SiO2 Dual-layer insulated compound film, is all lower film with SiO2;
Preferably, the insulated compound film of described lower cover is that SiON and SiO2 forms Dual-layer combination, and SiO2 adopts thermal oxide to be formed, and thickness is
siON adopts PECVD to be formed, and thickness is
Optionally, the SiO2 that described upper cover plate insulation film adopts thermal oxide to generate, thicknesses of layers is
Optionally, the described upper and lower cover plates inner groovy degree of depth is 100 ~ 300 μm, and the length and width of upper cover plate groove are all greater than the groove of lower cover;
Optionally, described plain conductor and electrode are Au or Al of PVD deposit, and thickness is
described plain conductor live width is 2 ~ 5 μm;
Optionally, described thermistor material is metal W or Pt or Re and their synthetic material, and thickness is
The present invention proposes a kind of machining manufacture of Micro Thermal Conductivity Detector, described Micro Thermal Conductivity Detector comprises thermistor and pond body and metal connecting line and electrode, described pond body be by upper and lower two surface insulations and inside all containing reeded silicon chip as cover plate, described lower cover surface insulation material is the Dual-layer combination of Si3N4 and SiO2 or SiON and SiO2, it is all lower film with SiO2, described upper cover plate surface insulation material is SiO2, and described upper and lower cover plates is fitted with groove alignment, and its step comprises:
Step S01: lower cover forms insulation film, definition thermistor region;
Step S02: lower cover is formed plain conductor and electrode;
Step S03: lower cover is formed miniature thermistor, forms groove and discharges thermistor simultaneously;
Step S04: upper cover plate is formed insulation film and groove;
Step S05: two lid panel notches carry out silicon silicon interface bonding after aiming at laminating
Optionally, remove the topmost thin film of specific rectangular region inside surface insulating material on lower cover, define the area as thermistor region;
Preferably, the sidewall of the oblong openings of topmost thin film is angularly the angle of internal friction of 50 ~ 70 °.
Seen from the above description, the Micro Thermal Conductivity Detector structure that the present invention proposes, adopt silicon chip as the upper and lower cover plates of conductance cell, respectively groove is obtained at the correspondence position of upper and lower cover plates by standard MEMS body silicon release tech and DRIE (deep reaction ion etching) technique, use conventional semiconductor insulating material: SiO2, SiON or Si3N4 is by the thermal oxide in semiconductor technology, the method of CVD deposit completes lid surface insulation, metal connecting line and electrode is made with semiconductor alloy, thermistor is formed by photoresist stripping process, finally after the groove alignment of upper and lower cover plates is also fitted, carry out silicon silicon interface bonding, complete sealing.The material that structure of the present invention uses is semiconductor material, the common process of its process means mainly in manufacture of semiconductor.Therefore, technical scheme of the present invention and conventional semiconductor process compatibility, and technique is easy to realize, technology maturation, has good stability.
Replace glass bulb as the upper cover plate of conductance cell with silicon chip in the present invention, because the thermal conductivity of silicon is larger than conventional glass shell, contribute to improving analysis precision.
Further prioritization scheme is, on lower cover, thermistor region is defined in the inventive method, what be actually for the upper strata SiON film in the double layer of insulation of lower cover is graphical, make it formation oblong openings, remove the SiON film in opening, the position of this namely follow-up lower cover groove, etching stopping is on lower floor SiO2 film, simultaneously by adjustment etching technics make opening Bu Shi right angle, edge but in oblique angle, when its effect is the metal arm when subsequent technique deposit thermistor, metal is avoided to stride across the contingent Metal deposition uneven thickness of steep SiON thin films step or rupture.
The present invention is equally applicable to both arms conductance cell structure, and namely having two independently thermistors in lower cover silicon chip, is the thermistor of reference arm and gage beam respectively, utilizes tested gas different with the thermal conductivity coefficient of reference gas and the detection of concentration type is carried out in response.Because different gas has different thermal conductivity coefficients, when reference gas is simultaneously by 2 arms, have same impact to the heat transfer of two-arm, also identical on the impact of thermal sensing element temperature, thus the change in resistance of 2 thermal sensing elements is identical.When tested gas enters gage beam with reference gas, because the thermal conductivity coefficient of tested gas is different with the thermal conductivity coefficient of pure reference gas, thus make the temperature drop of 2 thermal sensing elements also different, cause the change in resistance of thermal sensing element to occur difference.This requires that two of both arms conductance cell thermistors must be consistent as far as possible.The inventive method is the preparation adopting photoresist stripping process simultaneously to complete two thermistors of reference arm and gage beam, at the accuracy adding that in semiconductor technology, deposited metal thickness is high, can ensure that two thermistor performances are consistent, reach minimizing systematical difference, make Measurement and analysis keep the effect of degree of precision.The inventive method utilizes the advantages such as the stability of manufacture of semiconductor comprehensive automation, technique high consistency and brilliance, and the Micro Thermal Conductivity Detector TCD manufactured by guarantee is significantly improved than the mechanical package TCD of prior art in the precision, accuracy of cost control, stable performance and testing result.The present invention simultaneously and conventional semiconductor process compatibility, can realize device miniaturization and batch production, save a large amount of man power and materials, reduce production cost further.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of Micro Thermal Conductivity Detector machining manufacture of the present invention.
Fig. 2, Fig. 3 a ~ 6a, Fig. 7 and Fig. 8 a is each step cross-sectional view of the embodiment of the present invention one.
Fig. 3 b ~ 6b, 8b are each step planar graph structural representations of the embodiment of the present invention one.
Fig. 9 is the gas passage planar structure schematic diagram of the embodiment of the present invention two.
Embodiment
For making content of the present invention clearly understandable, below in conjunction with Figure of description, content of the present invention is described further.Certain the present invention is not limited to this specific embodiment, and the general replacement known by those skilled in the art is also encompassed in protection scope of the present invention.
Secondly, the present invention utilizes schematic diagram to carry out detailed statement, and when describing example of the present invention in detail, for convenience of explanation, schematic diagram, should in this, as limitation of the invention not according to general ratio partial enlargement.
Below in conjunction with Figure of description, embodiments of the invention are further illustrated.
Embodiment one
The present embodiment is to collimate the processing and manufacturing flow process of general formula Micro Thermal Conductivity Detector, introduce the integrated manufacturing method that conductance cell comprises pond body (containing gas passage) and thermal sensing element wherein, this method avoid the uncertainty that tradition assembling processing is introduced, be more suitable for standardized production.Wherein two thermistors of the useful arm for referencial use of main devices and gage beam, and corresponding lead-in wire, electrode, supporting gas passage etc.Fig. 1 is the schematic flow sheet of Micro Thermal Conductivity Detector machining manufacture of the present invention.Concrete steps are as follows:
First, with reference to processing step S01 and Fig. 2: lower cover forms insulation film, definition thermistor region.
Select 6 cun of silicon chips as lower cover, Si substrate 100 forms double-layer compound film: SiO2/Si3N4 or SiO2/SiON, select SiO2/SiON in the present embodiment.Wherein SiO2 film 110 adopts thermal oxide to be formed, and thickness is
be preferably
siON film 120 adopts PECVD to be formed, and thickness is
be preferably
this composite membrane is used as insulation course, and SiO2, SiON double-layer films is used for the stress of balance film interlayer.
Consult Fig. 3 a, 3b.Carry out graphically to SiON rete 120, semiconductor common process (photoetching, etching) is adopted to realize, figure is defined as thermistor region, both arms conductance cell needs formation two independently thermistor region, one is reference arm thermistor region, another is gage beam thermistor region, and both can exchange.In the present embodiment, thermistor region is rectangle, is of a size of 20 μm × 60 μm.For subsequent technique is convenient, after graphical, the step of SiON rete 120 ' sidewall is inclined, and angle, between 50 ~ 70 °, is preferably 60 °.
Then, with reference to processing step S02 and Fig. 4 a, 4b, lower cover is formed plain conductor and electrode.
Consider the compatibility with semiconductor technology, plain conductor can select the metal materials such as Au, Al.The present embodiment selects Al as interconnected metal, and adopt PVD mode to form metallic diaphragm, thickness is
be preferably
then, carry out patterning process (photoetching, etching) to Al metal film and form wire and pressure point (electrode) figure 150, wire live width is 2 ~ 5 μm, and be preferably 3 μm, pressure point figure is 20 μm × 20 μm.Wire covers the step inclined-plane of SION.In the present embodiment, metal interconnection wire and test electrode must be formed for reference arm resistance and gage beam resistance.
Thereafter, with reference to processing step S03 and Fig. 5 a, 5b.Lower cover is formed miniature thermistor, form groove and discharge thermistor simultaneously.
The material of thermistor can select the metal of the higher temperature coefficients such as W, Pt, Re and relevant synthetic material.The present embodiment selects W as thermo-sensitive material, and thermistor is graphically adopt stripping technology (lift-off), respectively has a thermistor figure in the above-mentioned reference arm thermistor region mentioned and gage beam thermistor region.First in region, form litho pattern, then deposit forms W metallic diaphragm, thickness is
be preferably
then also deposit metallic diaphragm is in the above peeled off while removing photoresist, form W thermistor 160.The thermistor of the present embodiment is of a size of 5 μm × 60 μm, and thermistor extends along the long limit in thermistor region, crosses over thermistor region, and with cover the metal A l wire good contact on SION step inclined-plane.Containing two thermistors as reference arm and gage beam in the present embodiment, process preparation two thermistors by using the method for photoresist lift off simultaneously, the consistent of two resistive performances can be ensured, reduce systematical difference, make the Measurement and analysis of electric bridge keep degree of precision.
After thermistor and relevant supporting plain conductor and electrode structure are formed, because thermistor during test must entirety be in air-flow, need to form hanging structure.With reference to Fig. 6 a, 6b, adopt release process conventional in MEMS technology, first use HF gas attack SiO2 rete, at this SiON as mask, corrode Si substrate afterwards, form groove with XeF2, severity control, between 100 ~ 300 μm, is preferably 150 μm.Cavity 180 can be formed in thermistor region like this, make thermistor be in vacant state.Air release technique high selectivity can remove target layer, less to other materials damage, avoids the uncontrollable factor that liquid corrosion causes.So far, the basic structure in conductance cell lower cover has manufactured.
For forming sealing pipeline, needing manufacture one piece of upper cover plate in addition, still selecting silicon as backing material.With reference to processing step S04 and Fig. 7, adopt thermal oxidation technology to form SiO2 rete 210 first on the substrate 200, thickness is
be preferably
this rete plays insulation course effect.
With reference to Fig. 8 a, 8b, carry out photoetching process and form the photoetching offset plate figure corresponding to gas passage, described figure is the gas passage of upper cover plate, and its position needs to mate corresponding with lower cover groove location.Consider that the degree of accuracy of aligning can affect obturation effect, the length and width of upper cover plate groove are all greater than lower cover groove size, are 25 μm × 65 μm.Carry out DRIE etching to SiO2, Si, form groove, the degree of depth is 100 ~ 300 μm, is preferably 150 μm.Gained graphic diaphragm layer is Si substrate 200 ', SiO2 rete 210 ', wherein has gas passage 230.Remove photoresist and namely form cover plate of upper layer after cleaning.
After structure in upper and lower two cover plates all completes, with reference to processing step S05, both are aimed at the laggard line unit of laminating and close (SiO2-SiO2 interface), then can continue technique, comprise and carry out cutting formation separate unit, after sealing, form gas inlet-outlet and wire pin.
Embodiment two
Because gas flow is comparatively large to tests affect, can change the gas passage of upper cover plate substrate definition.As shown in Figure 9,310 ' be graphical after insulating thin layer, 330 is through-type gas passage.Concrete technology method is similar to embodiment one, and because the gas passage of upper cover plate adjusts, the pressure point position distribution of lower substrate also needs to be adjusted accordingly.
In addition, according to testing requirement, the inventive method can also be adopted to make the conductance cell structure of diffusion type, half diffusion type.
In sum, the machining manufacture of Micro Thermal Conductivity Detector provided by the invention adopts basic compatible processing technology and associated materials with conventional semiconductor process, contribute to realizing device miniaturization and batch production, the manufacture method of full automatic semiconductor machining means can be made full use of, realize reducing production cost, can machining precision be ensured simultaneously, improve the analytical performance of finished product.
Foregoing description is only the description to present pre-ferred embodiments, any restriction not to the scope of the invention, and any change that the those of ordinary skill in field of the present invention does according to above-mentioned disclosure, modification, all belong to the protection domain of claims.
Claims (10)
1. a Micro Thermal Conductivity Detector structure, comprise thermistor, pond body and metal connecting line and electrode, it is characterized in that described pond body be by two surface insulations and inside all containing reeded silicon chip as cover plate, aim at groove location, fit up and down, form through silicon silicon interface bonded seal.
2. Micro Thermal Conductivity Detector structure as claimed in claim 1, is characterized in that, described lower cover realizes insulation by surface deposition Si3N4 and SiO2 or SiON and SiO2 Dual-layer insulated compound film, is all lower film with SiO2.
3. Micro Thermal Conductivity Detector structure as claimed in claim 2, is characterized in that, the insulated compound film of described lower cover is that SiON and SiO2 forms Dual-layer combination, and SiO2 adopts thermal oxide to be formed, and thickness is
siON adopts PECVD to be formed, and thickness is
4. Micro Thermal Conductivity Detector structure as claimed in claim 1, is characterized in that, the SiO2 film that described upper cover plate insulation film adopts thermal oxide to generate, and thicknesses of layers is
5. Micro Thermal Conductivity Detector structure as claimed in claim 1, it is characterized in that, the described upper and lower cover plates inner groovy degree of depth is 100 ~ 300 μm, and the length and width of upper cover plate groove are all greater than the groove of lower cover.
6. Micro Thermal Conductivity Detector structure as claimed in claim 1, it is characterized in that, described plain conductor and electrode are Au or Al of PVD deposit, and thickness is
described plain conductor live width is 2 ~ 5 μm.
7. Micro Thermal Conductivity Detector structure as claimed in claim 1, is characterized in that, described thermistor material is metal W or Pt or Re and their synthetic material, and thickness is
8. the machining manufacture of a Micro Thermal Conductivity Detector, described Micro Thermal Conductivity Detector comprises thermistor and pond body and metal connecting line and electrode, described pond body be by upper and lower two surface insulations and inside all containing reeded silicon chip as cover plate, described lower cover surface insulation material is the Dual-layer combination of Si3N4 and SiO2 or SiON and SiO2, it is all lower film with SiO2, described upper cover plate surface insulation material is SiO2, and described upper and lower cover plates is fitted with groove alignment, and its step comprises:
Step S01: lower cover forms insulation film, definition thermistor region;
Step S02: lower cover is formed plain conductor and electrode;
Step S03: lower cover is formed miniature thermistor, forms groove and discharges thermistor simultaneously;
Step S04: upper cover plate is formed insulation film and groove;
Step S05: two lid panel notches carry out silicon silicon interface bonding after aiming at laminating.
9. Micro Thermal Conductivity Detector machining manufacture as claimed in claim 8, is characterized in that, removes the topmost thin film of specific rectangular region inside surface insulating material on lower cover, defines the area as thermistor region.
10. as right wants the Micro Thermal Conductivity Detector machining manufacture as described in 9, it is characterized in that, the sidewall of the oblong openings of described topmost thin film is angularly the angle of internal friction of 50 ~ 70 °.
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| CN113203769A (en) * | 2021-04-15 | 2021-08-03 | 电子科技大学 | High-air-tightness micro thermal conductivity detector and manufacturing method thereof |
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| CN108181415B (en) * | 2016-12-08 | 2023-05-12 | 中国科学院上海微***与信息技术研究所 | Thin film type micro heat conduction detector and preparation method thereof |
| CN108918743A (en) * | 2018-07-10 | 2018-11-30 | 中国科学院电子学研究所 | Micro thermal conductivity detector |
| CN109752418A (en) * | 2019-01-21 | 2019-05-14 | 中国科学院上海微***与信息技术研究所 | A kind of miniature thermal conductivity gas sensor |
| CN109752418B (en) * | 2019-01-21 | 2021-11-05 | 中国科学院上海微***与信息技术研究所 | Miniature thermal conductivity gas sensor |
| CN112034017A (en) * | 2020-09-16 | 2020-12-04 | 电子科技大学 | Wafer-level packaging-based micro thermal conductivity detector and preparation method thereof |
| CN113203769A (en) * | 2021-04-15 | 2021-08-03 | 电子科技大学 | High-air-tightness micro thermal conductivity detector and manufacturing method thereof |
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Application publication date: 20151209 |