CN1797806A - Gas sensor of hydrogen semiconductor transducer, and preparation method - Google Patents

Gas sensor of hydrogen semiconductor transducer, and preparation method Download PDF

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Publication number
CN1797806A
CN1797806A CNA2004101027578A CN200410102757A CN1797806A CN 1797806 A CN1797806 A CN 1797806A CN A2004101027578 A CNA2004101027578 A CN A2004101027578A CN 200410102757 A CN200410102757 A CN 200410102757A CN 1797806 A CN1797806 A CN 1797806A
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hydrogen
tin ash
sensing element
element according
layer
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CN100373652C (en
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王磊
熊玉华
杜军
毛昌辉
尉秀英
杨志民
秦光荣
苑鹏
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GRIMN Engineering Technology Research Institute Co Ltd
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Beijing General Research Institute for Non Ferrous Metals
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Abstract

Characters of the method are that n-SnO2-x thin membrane layer is prepared on Si(100) chip by using radio frequency sputtering technique; then, Pd-Ni layer is prepared on tin dioxide layer so as to form gas sensor in composite membrane of Pd-Ni/SnO2. Under environment of normal temperature, the gas sensor raises selectivity and sensibility for hydrogen. Features are: simple technique and low cost.

Description

Gas sensor of hydrogen semiconductor transducer and preparation method thereof
Technical field
The present invention relates to a kind of semiconductor transducer senser to the hydrogen sensitivity and preparation method thereof, belong to semiconductor transducer gas sensor manufacturing process technology field.
Background technology
Semiconductor gas sensor is meant and adopts semi-conducting material as senser, improves corresponding selectivity and sensitiveness by doping or surface modification technology.Because the variation of environmental gas composition causes the electrical property of semiconductor gas sensor and changes the kind and the concentration of the gas that exists in the testing environment by the sheet resistance of measuring semiconductor gas sensor.
As everyone knows, hydrogen is a kind of renewable and clean energy resource, has pollution-free, the reproducible energy, development along with fossil type fuel crunch and microelectronics industry, hydrogen uses frequent day by day in daily life, but the aerial concentration of hydrogen reaches 4.1%～75.6% will blast, therefore, hydrogen sensor just becomes extremely important for the hydrogen leak detection in the use of hydrogen, be generally used for hydrogen and detect chemical sensor based on the body doping stannic oxide, selectivity and sensitivity are relatively poor, can not satisfy hydrogen and leak the needs of monitoring in real time.
Summary of the invention
The purpose of this invention is to provide a kind of semiconductor transducer gas sensor that hydrogen is had high selectivity.
Another object of the present invention provides a kind of manufacture method of gas sensor of hydrogen semiconductor transducer, simple, cheap with preparation technology, as to have high selectivity and sensitivity hydrogen senser.
To achieve these goals, the present invention takes following technical scheme:
A kind of gas sensor of hydrogen semiconductor transducer is a sputter N type tin ash semiconductor film layer on Si (100) substrate, and forms Pd-Ni alloy firm layer, the Pd-Ni/SnO that is constituted on the tin ash layer 2The composite membrane gas sensor.
In above-mentioned gas sensor of hydrogen semiconductor transducer, described N type tin ash semiconductor film layer is a kind of film with (211) preferred orientation.
In above-mentioned gas sensor of hydrogen semiconductor transducer, described gas sensor of hydrogen semiconductor transducer surface also is provided with a pair of measurement electrode.
In above-mentioned gas sensor of hydrogen semiconductor transducer, the mass ratio of Ni and Pd is 0～0.15 in the described Pd-Ni alloy firm layer, and Ni/Pd ≠ 0.
A kind of method for preparing gas sensor of hydrogen semiconductor transducer, this side comprises the steps:
A. prepare the tin ash target: the tin ash micro mist is carried out hip treatment; Carry out surface grinding afterwards and handle, promptly obtain the tin ash target;
B. the Si single-chip to (100) face carries out surface treatment;
C. in multi-target magnetic control sputtering equipment, adopt the sputtering power scope of 60～120W, the underlayer temperature scope is controlled to be 25 ℃～400 ℃, and annealing region is controlled to be 100 ℃～700 ℃, at P O2/ P ArBe under 1: 1～1: 6 the atmosphere, on the Si single-chip through step (b) surface-treated (100) face, the tin ash target that uses step (a) to make is prepared the tin dioxide thin film layer, and sputtering time is 10～30 minutes;
D. adopt cosputtering method sputter Pd-Ni alloy firm layer on the tin ash surface, the thickness of thin layer is at 10～50nm; Can control Pd, Ni sputtering power adjustment respectively with the composition of realizing Pd, Ni;
E. the composite membrane that at last step (d) is made passes through in-situ annealing, and its annealing region is controlled to be 200～800 ℃, and the time is 3～8 hours, promptly makes Pd-Ni/SnO 2The composite membrane gas sensor.
In described step (d), by sputter Pd-Ni alloy firm layer, this alloy firm layer is in a kind of discontinuous state basically, also will carry out in-situ annealing by (e) step, realizes that the expansion of Pd-Ni layer, infiltration reach the modification to tin dioxide thin film.In the described step (e), the annealing heating rate is very low, and the time is generally greater than 3 hours.
In the manufacture method of a kind of hydrogen semiconductor sensor sensing element of the present invention, this method also comprises step (f): masking method is adopted on the surface at the tin dioxide thin film layer, and utilize magnetically controlled sputter method at two Cu electrodes of film two ends preparation, distance between electrodes equals the width of sample.
In the described step (f) of the manufacture method of a kind of hydrogen semiconductor sensor sensing element of the present invention, described masking method covers a tin ash layer part for adopt the glass baffle plate in sputter procedure, reserve the position of preparation electrode, prepare measurement electrode at reserved location.
In the described step (d) of the manufacture method of a kind of hydrogen semiconductor sensor sensing element of the present invention, in the sputter Pd-Ni alloy firm layer, the mass ratio of Ni and Pd is 0～0.15, and Ni/Pd ≠ 0 on the tin ash surface.
In the described step (a) of the manufacture method of a kind of hydrogen semiconductor sensor sensing element of the present invention, the purity of employed tin ash is 99.95%.
In the described step (a) of the manufacture method of a kind of hydrogen semiconductor sensor sensing element of the present invention, describedly the tin ash micro mist is carried out the hip treatment process be, the tin ash micro mist is carried out 16-20 hour dried under 100-130 ℃ of condition, under 1000-1200 ℃ of condition sintering 3-6 hour again.
In the described step (b) of the manufacture method of a kind of hydrogen semiconductor sensor sensing element of the present invention, described Si single-chip to (100) face carries out the surface-treated step and is, is described Si single-chip is adopted H 2SO 4+ K 2Cr 2O 7Washing lotion was soaked 22～28 hours, was that medium carries out ultrasonic waves for cleaning to the silicon chip that soaked with methyl alcohol, acetone, the ethanol of chemical pure concentration respectively then, obtained clean silicon substrate.
In the described step (b) of the manufacture method of a kind of hydrogen semiconductor sensor sensing element of the present invention, Si sheet washing lotion collocation method is: the H that with mass ratio is 1: 1 2SO 4With K 2Cr 2O 7Mix, the water-bath heating got final product in 0.5～2.5 hour, and the Si sheet cleaning process of soaking is: ultrasonic waves for cleaning is 5～30 minutes in the methyl alcohol, ultrasonic waves for cleaning 5～30 minutes in acetone then, ultrasonic waves for cleaning 5～30 minutes in ethanol at last.
Advantage of the present invention and effect are: the Pd-Ni/SnO of preparation 2The gas sensor of composite membrane can make this gas sensor for hydrogen good selectivity and high sensitivity be arranged, and therefore, it can be applied to fields such as gas leakage detection and gas analysis.The present invention has adopted the MULTILAYER COMPOSITE membrane technology, technology is simple, continuity is fine, once can finish all technology in an equipment, saves cost, consistency of product is fine, is beneficial to prepare gas sensor of hydrogen semiconductor transducer cheap, excellent performance.
Description of drawings
Fig. 1. be the structural representation of gas sensor of hydrogen semiconductor transducer of the present invention, Fig. 1 (a) is the gas sensor of hydrogen semiconductor transducer front view; Fig. 1 (b) is the gas sensor of hydrogen semiconductor transducer vertical view.
Fig. 2. Pd-Ni composition of layer ratio is to the influence curve of sensitivity in the expression hydrogen sensitive element.
Fig. 3. the underlayer temperature of preparation tin ash layer is to the influence curve of hydrogen sensitivity in the expression hydrogen sensitive element.
Fig. 4. the expression hydrogen sensitive element is to different reducing gas sensitivity and response time curve.
Embodiment
Below in conjunction with drawings and Examples the present invention is further narrated:
As shown in Figure 1, this gas sensor of hydrogen semiconductor transducer is a sputter N type tin ash semiconductor film layer 4 on Si (100) substrate 1, and forms Pd-Ni alloy firm layer 2, the Pd-Ni/SnO that is constituted on tin ash layer 4 2The composite membrane gas sensor.Also be provided with a pair of measurement electrode 3 on the gas sensor of hydrogen semiconductor transducer surface.
Embodiment one:
At first the tin ash micro mist is carried out hip treatment, its process is that the tin ash micro mist is carried out 18 hours dried under 110 ℃ of conditions, again sintering 4 hours under 1050 ℃ of conditions.
Si single-chip to (100) face carries out surface treatment then, and its process is that (100) face Si single-chip is adopted H 2SO 4+ K 2Cr 2O 7Washing lotion was soaked 24 hours, was that medium carries out ultrasonic waves for cleaning to the silicon chip that soaked with methyl alcohol, acetone, ethanol respectively then, obtained clean silicon substrate.
Prepare the tin ash semiconductive thin film again, sintered density is reached 90% tin ash target and carry out radio frequency sputtering, sputtering parameter: sputtering power 65W; Sputtering time 15 minutes; Underlayer temperature is 25 ℃; P O2/ P ArIt is 1: 4.Tin dioxide thin film in-situ annealing technology is 400 ℃, 6 hours.Deposition Cu electrode on the tin dioxide thin film for preparing adopts cosputtering deposition Pd-Ni alloy firm then on this basis, and Ni: Pd=0.05 (atomic ratio), film thickness are 35nm.Duplicature is in-situ annealing together, and annealing temperature is 600 ℃, 5 hours.Tin ash is through XRD, and XPS tests proof, and this film is a N type tin ash semiconductive thin film, and film has (211) preferred orientation.
Embodiment two: except that the preparation technology parameter of tin dioxide thin film is different from the embodiment one, the preparation method of remaining embodiment two each layer employing is identical with embodiment one.The preparation technology parameter of tin dioxide thin film is: sputtering power 98W; Sputtering time 15 minutes; Underlayer temperature is 400 ℃; P O2/ P ArIt is 1: 4.Tin dioxide thin film in-situ annealing technology is 700 ℃, 6 hours.Deposition Cu electrode on the tin dioxide thin film for preparing.Ni in the Pd-Ni alloy firm: Pd=0.1 (atomic ratio), thickness are 47nm, carry out 650 ℃ of following 5.5 hours annealing in process.Through XRD and XPS test proof, tin dioxide thin film is the N type semiconductor film, has obviously (211) preferred orientation.
Semiconductor transducer gas sensor among the present invention is when reality is used, when promptly in containing the environment of hydrogen, detecting, hydrogen molecule in the environment is decomposed into the H atom under the Pd-Ni catalytic action, the H atom sees through finishing coat and is caught by tin ash, chemical change takes place on the surface, cause the inner charge carrier of tin ash to reduce, electrical property changes, and therefore just can learn the concentration of hydrogen in the environment by measuring the gas sensor resistance sizes.Do not need senser is heated when work, transducer is worked at normal temperatures and pressures.
Hydrogen sensitive element sensitive property test is referring to Fig. 2., 3., 4.
Fig. 2. Pd-Ni composition of layer ratio is to the influence curve of sensitivity in the expression hydrogen sensitive element, and from scheming as seen Ni: Pd (atomic ratio) has the highest sensitivity to hydrogen when 0.09 left and right sides.
Fig. 3. the underlayer temperature of preparation tin ash layer is to the influence curve of hydrogen sensitivity in the expression hydrogen sensitive element, as seen from the figure, underlayer temperature has bigger influence to the structure and the electrical property of tin dioxide thin film, in underlayer temperature was in 290～320 ℃ scope, the tin ash hydrogen-sensitive element had higher sensitivity.
Fig. 4. the expression hydrogen sensitive element is to the sensitivity and the response time curve of different reducing gass.SnO 2 gas-sensitive element is all very high to the sensitivity of ethanol and hydrogen under the room temperature, after the present invention has adopted finishing, can distinguish ethanol and hydrogen effectively, has improved the selectivity to hydrogen greatly.From Fig. 4. as seen, to response time of hydrogen between 20 seconds～30 seconds, sensitivity is greater than 20.

Claims (12)

1. a gas sensor of hydrogen semiconductor transducer is characterized in that, sputter N type tin ash semiconductor film layer on Si (100) substrate, and on the tin ash layer, form Pd-Ni alloy firm layer, the Pd-Ni/SnO that is constituted 2The composite membrane gas sensor.
2. a kind of hydrogen semiconductor sensor sensing element according to claim 1 is characterized in that, described N type tin ash semiconductor film layer is a kind of film with (211) preferred orientation.
3. a kind of hydrogen semiconductor sensor sensing element according to claim 1 and 2 is characterized in that described gas sensor of hydrogen semiconductor transducer surface also is provided with a pair of measurement electrode.
4. a kind of hydrogen semiconductor sensor sensing element according to claim 1 and 2 is characterized in that the atomic ratio of Ni and Pd is 0～0.15 in the described Pd-Ni alloy firm layer, and Ni/Pd ≠ 0.
5. a method for preparing gas sensor of hydrogen semiconductor transducer is characterized in that, this side comprises the steps:
A. prepare the tin ash target: the tin ash micro mist is carried out hip treatment; Carry out surface grinding afterwards and handle, promptly obtain the tin ash target;
B. the Si single-chip to (100) face carries out surface treatment;
C. in multi-target magnetic control sputtering equipment, adopt the sputtering power scope of 60～120W, the underlayer temperature scope is controlled to be 25 ℃～400 ℃, and annealing region is controlled to be 100 ℃～700 ℃, at P O2/ P ArBe under 1: 1～1: 6 the atmosphere, on the Si single-chip through step (b) surface-treated (100) face, the tin ash target that uses step (a) to make is prepared the tin dioxide thin film layer, and sputtering time is 10～30 minutes;
D. adopt cosputtering method sputter Pd-Ni alloy firm layer on the tin ash surface, the thickness of thin layer is at 10～50nm;
E. the composite membrane that at last step (d) is made passes through in-situ annealing, and its annealing region is controlled to be 200～800 ℃, and the time is 3～8 hours, promptly makes Pd-Ni/SnO 2The composite membrane gas sensor.
6. the manufacture method of a kind of hydrogen semiconductor sensor sensing element according to claim 5, it is characterized in that, this method also comprises step (f): masking method is adopted on the surface at the tin dioxide thin film layer, and utilize magnetically controlled sputter method at two Cu electrodes of film two ends preparation, distance between electrodes equals the width of sample.
7. the manufacture method of a kind of hydrogen semiconductor sensor sensing element according to claim 6, it is characterized in that, in the described step (f), described masking method covers a tin ash layer part for adopt the glass baffle plate in sputter procedure, reserve the position of preparation electrode, prepare measurement electrode at reserved location.
8. the manufacture method of a kind of hydrogen semiconductor sensor sensing element according to claim 5, it is characterized in that, in described step (d), on the tin ash surface in the sputter Pd-Ni alloy firm layer, the mass ratio of Ni and Pd is 0～0.15, and Ni/Pd ≠ 0.
9. the manufacture method of a kind of hydrogen semiconductor sensor sensing element according to claim 5 is characterized in that, in described step (a), the purity of employed tin ash is 99.95%.
10. the manufacture method of a kind of hydrogen semiconductor sensor sensing element according to claim 5, it is characterized in that, in described step (a), describedly the tin ash micro mist is carried out the hip treatment process be, the tin ash micro mist is carried out 16-20 hour dried under 100-130 ℃ of condition, under 1000-1200 ℃ of condition sintering 3-6 hour again.
11. the manufacture method of a kind of hydrogen semiconductor sensor sensing element according to claim 5 is characterized in that, in described step (b), described Si single-chip to (100) face carries out the surface-treated step and is, is described Si single-chip is adopted H 2SO 4+ K 2Cr 2O 7Washing lotion was soaked 22～28 hours, was that medium carries out ultrasonic waves for cleaning to the silicon chip that soaked with methyl alcohol, acetone, the ethanol of chemical pure concentration respectively then, obtained clean silicon substrate.
12. the manufacture method of a kind of hydrogen semiconductor sensor sensing element according to claim 5 is characterized in that, in described step (b), Si sheet washing lotion collocation method is: the H that with mass ratio is 1: 1 2SO 4With K 2Cr 2O 7Mix, the water-bath heating got final product in 0.5～2.5 hour, and the Si sheet cleaning process of soaking is: ultrasonic waves for cleaning is 5～30 minutes in the methyl alcohol, ultrasonic waves for cleaning 5～30 minutes in acetone then, ultrasonic waves for cleaning 5～30 minutes in ethanol at last.
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CN101563599A (en) * 2006-12-22 2009-10-21 研究三角协会 Polymer nanofiber-based electronic nose
CN101251508B (en) * 2008-04-01 2011-06-22 重庆大学 Method for manufacturing gas sensor for testing hydrogen
CN101523200B (en) * 2006-08-11 2012-08-29 株式会社渥美精机 Hydrogen gas concentration sensor and apparatus for determining hydrogen gas concentration
CN102965622A (en) * 2012-12-19 2013-03-13 中国科学院微电子研究所 Preparation method of sensitive film doped with Au or Pt nanocrystals on surface
CN104272076A (en) * 2012-05-02 2015-01-07 Nwd技术公司 Leak detector
CN104568002A (en) * 2014-12-26 2015-04-29 昆山工研院新型平板显示技术中心有限公司 Environmental detection device
CN106395731A (en) * 2015-07-29 2017-02-15 盛思锐股份公司 Gas sensor, array and a method for manufacturing thereof
CN106661714A (en) * 2014-11-28 2017-05-10 瑞福龙株式会社 Method for forming tin oxide layer by means of tin metal target
CN106886735A (en) * 2016-11-28 2017-06-23 厦门英诺尔电子科技股份有限公司 A kind of electronic tag and system for gathering material concentration
CN107315070A (en) * 2017-07-05 2017-11-03 南京航空航天大学 A kind of structure of ultrasonic wave added type MOS gas sensors
CN108593720A (en) * 2018-07-10 2018-09-28 杭州高烯科技有限公司 A kind of gas molecule detector of quick response
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CN101523200B (en) * 2006-08-11 2012-08-29 株式会社渥美精机 Hydrogen gas concentration sensor and apparatus for determining hydrogen gas concentration
CN101563599A (en) * 2006-12-22 2009-10-21 研究三角协会 Polymer nanofiber-based electronic nose
CN101251508B (en) * 2008-04-01 2011-06-22 重庆大学 Method for manufacturing gas sensor for testing hydrogen
CN104272076B (en) * 2012-05-02 2016-05-04 Nwd技术公司 Leakage detector
CN104272076A (en) * 2012-05-02 2015-01-07 Nwd技术公司 Leak detector
CN102965622A (en) * 2012-12-19 2013-03-13 中国科学院微电子研究所 Preparation method of sensitive film doped with Au or Pt nanocrystals on surface
CN106661714A (en) * 2014-11-28 2017-05-10 瑞福龙株式会社 Method for forming tin oxide layer by means of tin metal target
CN104568002A (en) * 2014-12-26 2015-04-29 昆山工研院新型平板显示技术中心有限公司 Environmental detection device
CN106395731A (en) * 2015-07-29 2017-02-15 盛思锐股份公司 Gas sensor, array and a method for manufacturing thereof
CN106886735A (en) * 2016-11-28 2017-06-23 厦门英诺尔电子科技股份有限公司 A kind of electronic tag and system for gathering material concentration
WO2018094745A1 (en) * 2016-11-28 2018-05-31 厦门英诺尔电子科技股份有限公司 Electronic tag for collecting substance concentration, and system for collecting substance concentration
CN106886735B (en) * 2016-11-28 2023-07-11 厦门英诺尔电子科技股份有限公司 Electronic tag and system for collecting substance concentration
CN107315070A (en) * 2017-07-05 2017-11-03 南京航空航天大学 A kind of structure of ultrasonic wave added type MOS gas sensors
EP3802407A4 (en) * 2018-06-07 2022-07-27 Bar Ilan University Hydrogen sensors from organometallic precursors
CN108593720A (en) * 2018-07-10 2018-09-28 杭州高烯科技有限公司 A kind of gas molecule detector of quick response

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