CN1674319A - Method for producing plane type gas sensor substrate by semiconductor technology - Google Patents
Method for producing plane type gas sensor substrate by semiconductor technology Download PDFInfo
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- CN1674319A CN1674319A CN 200510055225 CN200510055225A CN1674319A CN 1674319 A CN1674319 A CN 1674319A CN 200510055225 CN200510055225 CN 200510055225 CN 200510055225 A CN200510055225 A CN 200510055225A CN 1674319 A CN1674319 A CN 1674319A
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Abstract
A method for preparing planar gas sensor substrate. It includes cutting and polishing boronized glass or quarts being used as substrate material; washing and drying the material after it is soaked in hydrofluoric acid solution; carrying out the first photoetching with glue thickness of 0.5-2.0 micron, sputtering three metal film layer of Cr, Pt and Au in sequence on substrate, doing the second photoetching with glue thickness of 0.5-2.0 micron, corroding and washing; making high temperature anneal for substrate under nitrogen protection, soaking it in sulphuric acid, washing, drying by wind, scribing and splinting.
Description
Technical field
The present invention relates to a kind of manufacture method of gas sensor substrate, particularly a kind of method of making the plane type gas sensor substrate of semiconductor technology.
Background technology
The tradition gas sensor is the tube core of earthenware structure, forms by making by hand, and two shortcomings are arranged: the one, and sensitive electrode forms with the manual system of retouching of gold paste, and consistency is poor, is not suitable for producing in enormous quantities; The 2nd, mode of heating is that at the bottom of the heat utilization ratio, volume is big by earthenware substrate indirect, and element adds the heat power consumption height, is not suitable for the requirement of portable apparatus and building Based Intelligent Control weak electricity system.The plane type gas sensor element also there is exploration, generally be divided into two kinds, a kind of is the planar thick membrane component, utilize method for printing screen on ceramic flat surface, to print heater strip, signal electrode, thin film-forming method also is silk screen printing, and this method has solved the consistency problem of tube core electrode, but because screen printing technology limitation, die area is still bigger, and the high problem of power consumption still is not resolved; Another kind is the sputtered film element that semiconductor process techniques is made, this method had both solved the consistency problem of tube core electrode, die area is dwindled, improve the consistency of element greatly and reduce the element power consumption, but the thin film-forming method of this plane formula tube core is a spatter film forming, and the sensitive membrane component that makes is wayward, and is too low to the sensitivity of gas, the most important thing is poor stability, be difficult to commercialization.Therefore, for present gas sensor, under the prerequisite that guarantees certain sensitivity, stability, realizing that heating is low in energy consumption, high conformity, be fit to the gas sensor produced in batches, is that market is badly in need of.
At present the new mode of filming is that sputtering method prepares the requirement of sensitive material film at the bottom of to wick-based and is: sensitive material and die surfaces adhesiveness are good.
Summary of the invention
The present invention has overcome the deficiencies in the prior art, a kind of method of making the plane type gas sensor substrate of semiconductor technology is provided, utilize MEMS (microeletromechanical-system, MEMS (micro electro mechanical system)) processing technology is carried out physics, chemical treatment to the base material of plane type gas sensor, thereby has realized the suitability for industrialized production with the compact plane type gas sensor substrate of sensitive material.Specifically, the present invention utilizes the MEMS technology to make the plane tube core on boronation glass or quartz, thereby provides a kind of and the substrate compact gas sensor of sensitive material.
Method with the substrate of semiconductor technology making plane type gas sensor provided by the invention comprises the steps:
1, preparation base material:
Selection is the boronation glass of main component or quartzy as base material with silicon dioxide, after cutting, polishing, makes the thin slice that the surface has certain roughness.Wherein, the surface of certain degree of roughness can guarantee the anti-mechanical shock ability of sensitive thin film.
2, preliminary treatment before the metal electrode sputter:
Before the splash-proofing sputtering metal electrode, earlier activate glass surface, clean up again, reach enough degree of roughness to guarantee substrate material surface with acid solution, guarantee that simultaneously surface cleaning is pollution-free, to increase metal electrode and the adhesiveness of base material and the adhesiveness of sensitive material and substrate.
3, sputtering method prepares metal electrode:
On glass planar, utilize the photoetching, sputter, scribing technology of semiconductor technology to make microsize, that is, die-size is to 1mm * 3mm, metal electrode reaches μ m level) the tube core electrode structure, and carry out physics, chemical activation is handled.
4, electrode sputter reprocessing:
In substrate after the sputtering electrode, through high annealing, metal is combined closely with substrate, promptly can be made into the substrate of the plane type gas sensor that can combine closely with sensitive material.
Wherein, in above-mentioned the 1st step, also comprise the steps:
(1), with boronation glass or quartzy to cut into thick be 0.15 to 0.5 millimeter thin slice;
(2), the polishing, make sheet surface reach certain roughness, the surface particles diameter is 0.5 to 5 micron;
Use deionized water ultrasonic waves for cleaning, then use the absolute ethyl alcohol ultrasonic waves for cleaning (3), earlier;
(4), compressed air dries up substrate.
Wherein, in above-mentioned the 2nd step, also comprise the steps:
(1), base material is put into concentration is 20% to 80% buffered hydrofluoric acid solution, ultrasonic stirring 1 to 5 minute;
(2), base material put into the deionized water for ultrasonic ripple earlier clean, then put into the absolute ethyl alcohol ultrasonic waves for cleaning, till clean;
(3), dry up base material with compressed air.
Wherein, in above-mentioned the 3rd step, also comprise the steps:
(1), photoetching for the first time, thick 0.2 to 2.0 micron of glue;
(2), sputter: three-layer metal and thickness thereof are respectively: ground floor Cr, 100 ~ 400 ; Second layer Pt, 1000 ~ 4000 ; The 3rd layer of Au, 200 ~ 1000 .Adopt the batch (-type) sputter, too high that photoresist is roasting bad to prevent temperature;
(3), photoetching for the second time, thick 0.2 to 2.0 micron of glue;
(4), corrosion;
(5), clean.
Further, in above-mentioned steps (2), all substrate surface is bombarded activation, 5 to 30 minutes time before each splash-proofing sputtering metal.
Further, in above-mentioned steps (2), after the sputter second layer metal, before the bombardment activation substrate for the third time, also comprise the step that substrate is peeled off and cleaned.
Wherein, above-mentioned the 4th step also comprises:
(1), high annealing, substrate under nitrogen protection, 200 ℃ to 500 ℃ annealing 5 to 60 minutes;
(2), acid corrosion, substrate is to soak for 2 to 10 seconds in 5% to 25% the sulfuric acid in concentration;
(3), clean, successively use deionized water and absolute ethyl alcohol ultrasonic waves for cleaning clean;
(4), compressed air dries up;
(5), scribing, surplus thick be 20 to 100 microns;
(6), sliver.
Beneficial effect of the present invention is, select the close boronation glass of fusing point height, thermal coefficient of expansion and sensitive material or quartzy for use as base material, and utilize MEMS technology that base material is carried out physics and chemical activation and handle, thereby provide a kind of plane type gas sensor substrate that can combine closely with sensitive material; Simultaneously, MEMS technology has also guaranteed to utilize method provided by the invention can realize the suitability for industrialized production of above-mentioned plane formula sensor base as a kind of technology of maturation.
Embodiment
Embodiment one:
1, preparation base material:
(1) boronation glass is made the thick thin slice of 0.15mm through cutting, polishing, and the surface particles degree is 0.5 micron;
(2) boiled 20 minutes with dilute sulfuric acid;
(3) use absolute ethyl alcohol and deionized water ultrasonic waves for cleaning clean respectively;
(4) dry up with compressed air;
2, preliminary treatment before the metal electrode sputter:
(1) placing concentration is 20% buffered hydrofluoric acid solution, ultrasonic stirring 1 minute;
(2) be placed on earlier in deionized water and the absolute ethyl alcohol, clean with ultrasonic waves for cleaning;
(3) compressed air dries up;
3, sputtering method prepares metal electrode:
(1) photoetching for the first time, thick 0.5 micron of glue;
(2) substrate surface bombards activation for the first time, 5 minutes time;
(3) sputter adhesion layer metal, i.e. ground floor metal, Cr, thickness 100 ;
(4) substrate surface bombards activation for the second time, 5 minutes time;
(5) sputter second layer metal, Pt, thickness are 1000 ;
(6) peel off;
(7) clean;
(8) substrate surface bombards activation for the third time, 10 minutes time;
(9) sputter three-layer metal, Au, thickness are 200 ;
(10) photoetching for the second time, thick 0.5 micron of glue;
(11) corrosion;
(12) clean;
4, metal electrode sputter reprocessing:
(1) substrate is under nitrogen protection, 200 ℃ of high annealings 5 minutes;
(2) keep nitrogen, be chilled to room temperature and take out;
(3) in 5% sulfuric acid, soaked for 10 seconds;
(4) successively put into deionized water and absolute ethyl alcohol, clean with ultrasonic waves for cleaning;
(5) compressed air dries up;
(5) scribing, surplus thick 20 microns;
(6) sliver.
Embodiment two:
1, preparation base material:
(1) boronation glass is made the thick thin slice of 0.3mm through cutting, polishing, and the surface particles degree is 5 microns;
(2) boiled 40 minutes with dilute sulfuric acid;
(3) use absolute ethyl alcohol and deionized water ultrasonic waves for cleaning clean respectively;
(4) dry up with compressed air;
2, preliminary treatment before the metal electrode sputter:
(1) placing concentration is 50% buffered hydrofluoric acid solution, ultrasonic stirring 3 minutes;
(2) be placed on earlier in deionized water and the absolute ethyl alcohol, ultrasonic waves for cleaning is clean;
(3) dry up with compressed air;
3, sputtering method prepares metal electrode:
(1) photoetching for the first time, thick 1.2 microns of glue;
(2) substrate surface bombards activation for the first time, 15 minutes time;
(3) sputter adhesion layer metal, i.e. ground floor metal, Cr, thickness 200 ;
(4) substrate surface bombards activation for the second time, 15 minutes time;
(5) sputter second layer metal, Pt, thickness are 2000 ;
(6) peel off;
(7) clean;
(8) substrate surface bombards activation for the third time, 15 minutes time;
(9) sputter three-layer metal, Au, thickness are 500 ;
(10) photoetching for the second time, thick 1.2 microns of glue;
(11) corrosion;
(12) clean;
4, metal electrode sputter reprocessing:
(1) substrate is under nitrogen protection, 350 ℃ of high annealings 30 minutes;
(2) keep nitrogen, be chilled to room temperature and take out;
(3) in 15% dilute sulfuric acid, soaked for 5 seconds;
(4) be placed on earlier in deionized water and the absolute ethyl alcohol, clean with ultrasonic waves for cleaning;
(5) compressed air dries up;
(5) scribing, surplus thick 60 microns;
(6) sliver.
Embodiment three:
1, preparation base material:
(1) the thick thin slice of 0.5mm is made in quartzy process cutting, polishing, and the surface particles degree is 2.5 microns;
(2) boiled 60 minutes with dilute sulfuric acid;
(3) put into absolute ethyl alcohol and deionized water respectively, clean with ultrasonic waves for cleaning;
(4) dry up with compressed air;
2, preliminary treatment before the metal electrode sputter:
(1) placing concentration is 80% buffered hydrofluoric acid solution, ultrasonic stirring 5 minutes;
(2) successively put into deionized water and absolute ethyl alcohol, clean with ultrasonic waves for cleaning;
(3) dry up with compressed air;
3, sputtering method prepares metal electrode:
(1) photoetching for the first time, thick 2.0 microns of glue;
(2) substrate surface bombards activation for the first time, 30 minutes time;
(3) sputter adhesion layer metal, i.e. ground floor metal, Cr, thickness 400 ;
(4) substrate surface bombards activation for the second time, 30 minutes time;
(5) sputter second layer metal, Pt, thickness are 4000 ;
(6) peel off;
(7) clean;
(8) substrate surface bombards activation for the third time, 30 minutes time;
(9) sputter three-layer metal, Au, thickness are 1000 ;
(10) photoetching for the second time, thick 2.0 microns of glue;
(11) corrosion;
(12) clean;
4, metal electrode sputter reprocessing:
(1) substrate is under nitrogen protection, 500 ℃ of high annealings 60 minutes;
(2) keep nitrogen, be chilled to room temperature and take out;
(3) in 25% sulfuric acid, soaked for 2 seconds;
(4) successively put into deionized water and absolute ethyl alcohol, clean with ultrasonic waves for cleaning;
(5) compressed air dries up;
(5) scribing, surplus thick 100 microns;
(6) sliver.
More than by embodiment the present invention is described in detail, the technology of this area is to be understood that with personnel, in the scope that does not exceed spirit of the present invention and essence, the present invention is made certain modification and distortion, such as replacing compressed air to dry up substrate, still can realize purpose of the present invention with other modes.
Claims (4)
1, a kind of method of making the plane type gas sensor substrate with semiconductor technology comprises the steps:
(1) preparation base material:
With boronation glass or the quartzy thickness that cuts into is 0.15 to 0.5 millimeter thin slice, polishing then, making its surface roughness reach particle diameter is 0.5 to 5 micron, after boiling 20 to 60 minutes with dilute sulfuric acid again, put into deionized water respectively and absolute ethyl alcohol is clean with ultrasonic waves for cleaning, dry up with compressed air again;
(2) preliminary treatment before the metal electrode sputter:
With ready boronation glass of step (1) or the quartzy concentration that places is 20% to 80% buffered hydrofluoric acid solution, then successively clean with ultrasonic waves for cleaning in deionized water and absolute ethyl alcohol with ultrasonic stirring 1 to 5 minute, dries up with compressed air again;
(3) sputtering method prepares metal electrode, comprises the steps:
Photoetching for the first time, thick 0.5 to 2.0 micron of glue;
Adopt the batch (-type) sputtering method at substrate surface sputter Cr, Pt successively, Au three-layer metal film;
Photoetching for the second time, thick 0.5 to 2.0 micron of glue;
Corrosion;
Clean;
(4) metal electrode sputter reprocessing comprises the steps:
Substrate is under nitrogen protection, and annealing is 5 to 60 minutes in 200 ℃ to the 500 ℃ temperature ranges;
Keep nitrogen, be chilled to room temperature and take out;
In concentration is to soak for 2 to 10 seconds in 5% to 25% the sulfuric acid;
Priority puts into deionized water and absolute ethyl alcohol is clean with ultrasonic waves for cleaning;
Dry up with compressed air;
Scribing, surplus thick 20 to 100 microns;
Sliver.
2, method of making the plane type gas sensor substrate of semiconductor technology as claimed in claim 1, it is characterized in that, described step (3) also comprises the step of substrate surface being carried out three bombardment activation, and described three bombardment activation steps are in respectively before the sputter three-layer metal, and each time is 5 to 30 minutes.
3, method of making the plane type gas sensor substrate of semiconductor technology as claimed in claim 2, it is characterized in that described step (3) also is included in after the sputter second layer metal and to substrate surface bombards the step that activation is peeled off and cleaned substrate before for the third time.
4, as claim 2 or 3 described methods of making the plane type gas sensor substrate, it is characterized in that the thickness of described three-layer metal film Cr, Pt, Au is respectively: 100 to 400 , 1000 to 4000 , 200 to 1000 with semiconductor technology.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100552258A CN100349309C (en) | 2005-03-16 | 2005-03-16 | Method for producing plane type gas sensor substrate by semiconductor technology |
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| CNB2005100552258A CN100349309C (en) | 2005-03-16 | 2005-03-16 | Method for producing plane type gas sensor substrate by semiconductor technology |
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| CN1674319A true CN1674319A (en) | 2005-09-28 |
| CN100349309C CN100349309C (en) | 2007-11-14 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101329291B (en) * | 2007-06-20 | 2012-01-11 | 中国科学院微电子研究所 | Gas-sensitive sensor |
| CN109536990A (en) * | 2018-10-15 | 2019-03-29 | 华南理工大学 | A kind of flat thin-film electro catalyst operation electrode and its preparation method and application |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04208848A (en) * | 1990-11-30 | 1992-07-30 | Matsushita Electric Works Ltd | Electrochemical gas sensor and manufacture thereof |
| JPH11108886A (en) * | 1997-09-30 | 1999-04-23 | Akebono Brake Res & Dev Center Ltd | Co2 gas sensor |
| CN1186627C (en) * | 2003-02-28 | 2005-01-26 | 北京青鸟元芯微系统科技有限责任公司 | Chip of low power dissipation chemical gas sensor and its preparing method |
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2005
- 2005-03-16 CN CNB2005100552258A patent/CN100349309C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101329291B (en) * | 2007-06-20 | 2012-01-11 | 中国科学院微电子研究所 | Gas-sensitive sensor |
| CN109536990A (en) * | 2018-10-15 | 2019-03-29 | 华南理工大学 | A kind of flat thin-film electro catalyst operation electrode and its preparation method and application |
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| CN100349309C (en) | 2007-11-14 |
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