CN101419179A - Nano-silicon air-sensitive material and gas sensor - Google Patents
Nano-silicon air-sensitive material and gas sensor Download PDFInfo
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- CN101419179A CN101419179A CNA2008101831219A CN200810183121A CN101419179A CN 101419179 A CN101419179 A CN 101419179A CN A2008101831219 A CNA2008101831219 A CN A2008101831219A CN 200810183121 A CN200810183121 A CN 200810183121A CN 101419179 A CN101419179 A CN 101419179A
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Abstract
The invention discloses a nano-silicon gas sensitive material and a gas sensitive element belonging to the filed of new material technology and nano materials, and is characterized in that the gas sensitive material based on nano-silicon and the gas sensitive element sensitive to nitrogen-oxygen compound gases such as nitric oxide, nitrogen dioxide and the like and gases such as ammonia gas and the like can be prepared through preparing the nano-silicon by erosion of metallic catalyst silicon and adding proper catalyst such as platinum (or gold) and the like. The gas sensitive element has the advantages of good selectivity, good temperature resistance and moisture resistance, good stability, long service life, no environment pollution, stable process, good repeatability, and convenient batch production.
Description
Technical field
The present invention relates to a kind of nano-silicon air-sensitive material and gas sensor, belong to new material technology and field of nanometer material technology.
Background technology
The all gases especially detection monitoring of inflammable gas and poisonous gas has become current urgent problem, the research of gas-sensitive nano material is to improving sensitivity, selectivity and the long-time stability of gas sensitive, and how to reduce working temperature and shorten aspects such as response temperature time and play great function.Present Research at the gas-sensitive nano material of gases such as hydrogen, sulfuretted hydrogen, hydrocarbon, oxynitrides, ethanol, acetone has been done certain research, and the trend of development has been made prospect.
Because pressing for of commercial production and environment measuring, the research of gas sensor and application and development are very active always.Gas sensor is a kind of novel micro analytical technology, and it is that specific gaseous species and concentration thereof are become the function element that signals such as photoelectricity are represented.Because gas sensitivity height, selectivity is good, easy to carry and microminiaturized, characteristics such as on-the site analysis and monitoring be can be used for, detection forecast and automaton harmful, flammable explosive gas therefore in environmental monitoring, petrochemical complex and daily life, more and more are used as.The subject matter that present traditional gas sensor exists is the requirement that characteristics such as sensitivity and selectivity can not satisfy the ultramicron fast detecting, but adopts the conventional gas sensitive material to be difficult to reach the level of ultramicron fast detecting.
Nearest nano materials research is found, after sensor material enters nanoscale, utilizes its surface effect and scale effect can increase substantially the detection sensitivity of sensor, thereby is that realization ultramicron fast detecting sensor has been opened up a brand-new thinking.The nanometer gas sensor has the irreplaceable advantage of conventional sensors: the one, and nano material has huge interface, and a large amount of gas passages are provided, thereby has improved sensitivity greatly; The 2nd, the size of having dwindled sensor greatly.Nanometer technology provides a series of good nanometer gas-sensing function materials for the development of novel nano gas sensor, as nanotube, nano belt, nano wire, nano-porous materials etc.The research of nano material gas sensor has obtained considerable progress both at home and abroad at present.People such as Kong were made as chemical sensor with single Single Walled Carbon Nanotube in 2000 first, were used for detecting NO
2And NH
3[Kong J, Franklin NR, Zhou CW, Chapline MG, Peng S, Cho KJ, Dai HJ.Nanotube molecular wires aschemical sensors, Science 2000,287,622-625]; Calendar year 2001 king middle forest seminar is with single SnO
2Nano belt is made into gas sensor, is used for measure CO and NO
2[Comini E, Faglia G, Sberveglieri G, Pan ZW, Wang ZL.Stable and highly sensitive gas sensors based on semiconducting oxide nanobelts, Applied PhysicsLetters 2002,81,1869-1871].Fe has studied in domestic Li Yadong seminar [8]
2O
3/ ZnO core-shell nano bar structure is to the detectivity of low concentration inflammable gas.Li Shu soup seminar of City University of Hong Kong finds to have very high NH with the gas sensor of silicon nanowires preparation
3, water vapour sensitivity, and at room temperature can monitor [Zhou XT, Hu JQ, Li CP in real time, MaDDD, Lee CS, Lee ST.Silicon nanowires as chemical sensors, Chemical Physical Letters 2003,369,220-224].
On the large-area nano silicon line technology of preparing and solar battery technology basis of our invention [referring to: Chinese patent CN1382626; Chinese patent application numbers 2005100117533; Chinese patent application CN200810084205.7; KuiqingPeng, Mingliang Zhang, Aijiang Lu, NingBew Wong, Ruiqin Zhang, Shuit-Tong Lee.Ordered Sinanowire arrays via Nanosphere Lithography and Metal-induced etching.Applied Physics Letters2007,90,163123], we have invented a kind of nano-silicon air-sensitive material and gas sensor that has the technology with proprietary intellectual property rights preparation based on us.
Summary of the invention
The present invention seeks to design and a kind of have highly sensitive nano-silicon air-sensitive material and gas sensor thereof are provided.
Nano-silicon air-sensitive material and gas sensor technology that the present invention proposes, it is characterized in that: described method is carried out successively as follows:
1) silicon chip is passed through the acetone ultrasonic cleaning successively, washed with de-ionized water, acidic cleaning solution solution-treated are cleaned in the alcohol vibration; The purpose of cleaning silicon chip is the silicon face that obtains to clean;
2) silver (or gold) film that the clean silicon surface deposition 20-200nm that utilizes vacuum thermal evaporation technology (or electroless plating technology) to obtain in step (1) is thick immerses the silicon chip of the Ag film that deposits and contains HF+H
2O
2+ H
2O (also can utilize Fe (NO
3)
3Deng the H in the oxygenant replacement corrosive liquid
2O
2) closed container in, handled 4-180 minutes between the room temperature-80 degree centigrade, can obtain nano-silicon air-sensitive material;
3) step (1) is obtained in the mixed solution that cleaning silicon wafer directly is soaked into hydrofluorite and silver nitrate, handled 4-100 minutes between the room temperature-80 degree centigrade, can obtain nano-silicon air-sensitive material;
4) utilize technology such as electroless plating or plating to obtain nano silicon material surface deposition one deck nanometer platinum (or gold) particle, can obtain nano-silicon air-sensitive material in step (2) and (3);
5) obtain the metal Ohmic electrode that two of nano silicon material surface preparation keep at a certain distance away in step (2), can become a simple gas sensor after drawing outer lead;
6) obtain nano silicon material surface in step (2) and respectively prepare a metal Ohmic electrode, can become a simple gas sensor after drawing outer lead with the back side;
7) obtain the metal Ohmic electrode that two of nano silicon material surface preparation keep at a certain distance away in step (3), can become a simple gas sensor after drawing outer lead;
8) obtain nano silicon material surface in step (3) and respectively prepare a metal Ohmic electrode, can become a simple gas sensor after drawing outer lead with the back side;
9) obtain two metal Ohmic electrodes that keep at a certain distance away of nano silicon material face preparation in step (4), can become a simple gas sensor after drawing outer lead;
10) obtain nano silicon material surface in step (4) and respectively prepare a metal Ohmic electrode, can become a simple gas sensor after drawing outer lead with the back side;
In the preparation method of above-mentioned silicon nanowire array, described acidic cleaning solution is H
2SO
4: H
2O
2=4:1 (V/V), treatment conditions kept 40-60 minutes after being heated to fluidized state.Sulfuric acid concentration is 98%.
In the preparation method of above-mentioned silicon nanowire array, described step 2 hydrofluoric acid concentration scope is 0.2-10mol/L, and the concentration of hydrogen peroxide scope is 0.02-2mol/L, and ferric nitrate content is between 0.01mol/l-0.50mol/l.
In the preparation method of above-mentioned silicon nanowire array, described step 3 fluohydric acid content is between 0.2mol/l-10mol/l, and silver nitrate content is between 0.005mol/l-0.10mol/l.
Description of drawings
Fig. 1 is nano-silicon air-sensitive material of the present invention and gas sensor synoptic diagram thereof.
1 metal Ohmic electrode
2 metal Europe rice electrodes
3 Nano thin film layers
4 silicon substrates
5 back electrodes
Embodiment 1
Deposit the thick Ag film of 30nm at cleaned silicon chip surface with thermal evaporation, the sample that will deposit silverskin again immerses in the closed container kettle contain hydrofluorite and mixed solution of hydrogen peroxide (concentration of hydrofluorite and hydrogen peroxide is respectively 1.0mol/L and 0.1mol/L) to be handled 20 minutes, can obtain the large-area nano silicon materials.At the metal Ohmic electrode that the nano silicon material surface deposition keeps at a certain distance away, can become a simple gas sensor after drawing outer lead.
Embodiment 2
At the cleaned silicon chip surface thick Ag film of electroless deposition 30nm, the sample that will deposit silverskin again immerses in the closed container kettle contain hydrofluorite and mixed solution of hydrogen peroxide (concentration of hydrofluorite and hydrogen peroxide is respectively 4.0mol/L and 0.2mol/L) to be handled 30 minutes, can obtain the large-area nano silicon materials.At the metal Ohmic electrode that the nano silicon material surface deposition keeps at a certain distance away, can become a simple gas sensor after drawing outer lead.
Embodiment 3
Directly immerse in the closed container kettle that contains hydrofluorite and silver nitrate mixed solution (concentration of hydrofluorite and silver nitrate is respectively 4.0mol/L and 0.02mol/L) at cleaned silicon chip and handled 30 minutes, can obtain the large-area nano silicon materials.At the metal Ohmic electrode that the nano silicon material surface deposition keeps at a certain distance away, can become a simple gas sensor after drawing outer lead.
At the cleaned silicon chip surface thick Ag film of electroless deposition 30nm, the sample that will deposit silverskin again immerses in the closed container kettle contain hydrofluorite and mixed solution of hydrogen peroxide (concentration of hydrofluorite and hydrogen peroxide is respectively 4.0mol/L and 0.2mol/L) to be handled 40 minutes, can obtain the large-area nano silicon materials.After distinguishing the plated metal Ohmic electrode, draw outer lead, the nano silicon material surface and the back side can become a simple gas sensor.
Directly immerse in the closed container kettle that contains hydrofluorite and silver nitrate mixed solution (concentration of hydrofluorite and silver nitrate is respectively 4.0mol/L and 0.02mol/L) at cleaned silicon chip and handled 60 minutes, can obtain the large-area nano silicon materials.After distinguishing the plated metal Ohmic electrode, draw outer lead, the nano silicon material surface and the back side can become a simple gas sensor.
Embodiment 6
Directly immerse in the closed container kettle that contains hydrofluorite and silver nitrate mixed solution (concentration of hydrofluorite and silver nitrate is respectively 4.5mol/L and 0.01mol/L) at cleaned silicon chip and handled 40 minutes, can obtain the large-area nano silicon materials.At the metal Ohmic electrode that the nano silicon material surface deposition keeps at a certain distance away, can become a simple gas sensor after drawing outer lead.
Embodiment 7
Deposit the thick Ag film of 30nm at cleaned silicon chip surface with thermal evaporation, the sample that will deposit silverskin again immerses in the closed container kettle contain hydrofluorite and mixed solution of hydrogen peroxide (concentration of hydrofluorite and hydrogen peroxide is respectively 4.5mol/L and 2.0mol/L) to be handled 20 minutes, can obtain the large-area nano silicon materials.At the metal Ohmic electrode that the nano silicon material surface deposition keeps at a certain distance away, can become a simple gas sensor after drawing outer lead.
Embodiment 8
Deposit the thick Ag film of 50nm at cleaned silicon chip surface with thermal evaporation, the sample that will deposit silverskin again immerses in the closed container kettle contain hydrofluorite and mixed solution of hydrogen peroxide (concentration of hydrofluorite and hydrogen peroxide is respectively 4.5mol/L and 0.5mol/L) to be handled 20 minutes, can obtain the large-area nano silicon materials.At the metal Ohmic electrode that the nano silicon material surface deposition keeps at a certain distance away, can become a simple gas sensor after drawing outer lead.
Claims (4)
1, nano-silicon air-sensitive material and gas sensor is characterized in that: described method is carried out successively as follows:
1) silicon chip is passed through the acetone ultrasonic cleaning successively, the alcohol vibration is cleaned, washed with de-ionized water, and acidic cleaning solution is handled; The purpose of cleaning silicon chip is the silicon face that obtains to clean;
2) clean silicon surface deposition one deck silver (or gold) film that utilizes vacuum thermal evaporation technology (or electroless plating technology) to obtain in step (1) immerses the silicon chip of the Ag film that deposits and contains HF+H
2O
2+ H
2O (also can utilize Fe (NO
3)
3Deng the H in the oxygenant replacement corrosive liquid
2O
2) closed container in, handled 4-180 minutes between the room temperature-80 degree centigrade, can obtain nano-silicon air-sensitive material;
3) step (1) is obtained in the mixed solution that cleaning silicon wafer directly is soaked into hydrofluorite and silver nitrate, handled 4-180 minutes between the room temperature-80 degree centigrade, can obtain nano-silicon air-sensitive material;
4) utilize technology such as electroless plating or plating to obtain nano silicon material surface deposition one deck nanometer platinum (or gold) particle, can obtain nano-silicon air-sensitive material in step (2) and (3);
5) obtain the metal Ohmic electrode that two of nano silicon material surface preparation keep at a certain distance away in step 2 (or step 3,4), can become a simple gas sensor after drawing outer lead;
6) obtain nano silicon material surface in step 2 (or step 3,4) and respectively prepare a metal Ohmic electrode, can become a simple gas sensor after drawing outer lead with the back side;
2, the preparation method of nano-silicon air-sensitive material according to claim 1 and gas sensor is characterized in that: described acidic cleaning solution is H
2SO
4: H
2O
2=4:1 (V/V), treatment conditions kept 40-60 minutes after being heated to fluidized state.Sulfuric acid concentration is 98%.
3, the preparation method of nano-silicon air-sensitive material according to claim 1 and gas sensor, it is characterized in that: described step 2 hydrofluoric acid concentration scope is 0.2-10mol/L, the concentration of hydrogen peroxide scope is 0.02-2mol/L, and ferric nitrate content is between 0.01mol/l-0.50mol/l.
4, the preparation method of nano-silicon air-sensitive material according to claim 1 and gas sensor is characterized in that: described step 3 fluohydric acid content is between 0.2mol/l-10mol/l, and silver nitrate content is between 0.005mol/l-0.10mol/l.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101793855A (en) * | 2010-03-26 | 2010-08-04 | 北京师范大学 | Gas sensor with silicon micro-nano structure and manufacturing method thereof |
| CN101830509A (en) * | 2010-05-20 | 2010-09-15 | 武汉理工大学 | Beta-AgVO3 nanowire hydrogen sulfide gas sensing material and method for manufacturing gas sensor by using same |
| CN102180518A (en) * | 2011-01-25 | 2011-09-14 | 湖北大学 | Large-scale preparation method of niobium pentoxide nanowires and hydrogen-sensitive element thereof |
| CN102201486A (en) * | 2010-03-26 | 2011-09-28 | 北京师范大学 | Preparation technology for silicon nano-aperture array photovoltaic material and photovoltaic cell |
| CN104502422A (en) * | 2014-12-19 | 2015-04-08 | 清华大学 | Method for preparing porous silicon nanowire NO2 gas sensor |
| CN107102033A (en) * | 2016-02-23 | 2017-08-29 | 延世大学校产协力团 | Hydrogen sensor and preparation method thereof |
| CN107673355A (en) * | 2017-09-22 | 2018-02-09 | 杭州汇健科技有限公司 | A kind of gas sensing material for low-power-consumptiohigh-sensitivity high-sensitivity methane transducer |
| CN115287589A (en) * | 2022-01-12 | 2022-11-04 | 青岛大学 | Preparation method and application of gas sensor based on coiled silicon nano-film |
-
2008
- 2008-12-12 CN CNA2008101831219A patent/CN101419179A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101793855A (en) * | 2010-03-26 | 2010-08-04 | 北京师范大学 | Gas sensor with silicon micro-nano structure and manufacturing method thereof |
| CN102201486A (en) * | 2010-03-26 | 2011-09-28 | 北京师范大学 | Preparation technology for silicon nano-aperture array photovoltaic material and photovoltaic cell |
| CN102201486B (en) * | 2010-03-26 | 2014-04-16 | 北京师范大学 | Preparation technology for silicon nano-aperture array photovoltaic material and photovoltaic cell |
| CN101830509A (en) * | 2010-05-20 | 2010-09-15 | 武汉理工大学 | Beta-AgVO3 nanowire hydrogen sulfide gas sensing material and method for manufacturing gas sensor by using same |
| CN102180518A (en) * | 2011-01-25 | 2011-09-14 | 湖北大学 | Large-scale preparation method of niobium pentoxide nanowires and hydrogen-sensitive element thereof |
| CN104502422B (en) * | 2014-12-19 | 2017-04-12 | 清华大学 | Method for preparing porous silicon nanowire NO2 gas sensor |
| CN104502422A (en) * | 2014-12-19 | 2015-04-08 | 清华大学 | Method for preparing porous silicon nanowire NO2 gas sensor |
| CN107102033A (en) * | 2016-02-23 | 2017-08-29 | 延世大学校产协力团 | Hydrogen sensor and preparation method thereof |
| JP2017151081A (en) * | 2016-02-23 | 2017-08-31 | インダストリー−アカデミック・コーポレーション・ファウンデーション・ヨンセイ・ユニヴァーシティ | Hydrogen sensor and method for manufacturing the same |
| CN107102033B (en) * | 2016-02-23 | 2020-01-03 | 新星C&T | Hydrogen sensor and preparation method thereof |
| CN107673355A (en) * | 2017-09-22 | 2018-02-09 | 杭州汇健科技有限公司 | A kind of gas sensing material for low-power-consumptiohigh-sensitivity high-sensitivity methane transducer |
| CN115287589A (en) * | 2022-01-12 | 2022-11-04 | 青岛大学 | Preparation method and application of gas sensor based on coiled silicon nano-film |
| CN115287589B (en) * | 2022-01-12 | 2024-01-30 | 青岛大学 | Preparation method and application of gas sensor based on curled silicon nano film |
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Application publication date: 20090429 |