CN103578938B - A kind of Sn mixed ZnO semiconductor material and preparation method and application thereof - Google Patents
A kind of Sn mixed ZnO semiconductor material and preparation method and application thereof Download PDFInfo
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- CN103578938B CN103578938B CN201310587104.2A CN201310587104A CN103578938B CN 103578938 B CN103578938 B CN 103578938B CN 201310587104 A CN201310587104 A CN 201310587104A CN 103578938 B CN103578938 B CN 103578938B
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- H—ELECTRICITY
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/403—Cells and electrode assemblies
- G01N27/414—Ion-sensitive or chemical field-effect transistors, i.e. ISFETS or CHEMFETS
- G01N27/4141—Ion-sensitive or chemical field-effect transistors, i.e. ISFETS or CHEMFETS specially adapted for gases
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/0257—Doping during depositing
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
Abstract
The present invention relates to one Sn mixed ZnO semiconductor material and preparation method and the application of this kind of material, belong to technical field of semiconductor film preparation. The preparation method is that, Sn powder and Zn powder are blended in the oxygen atmosphere with argon and heat with CVD(chemical vapour deposition (CVD)) deposit to device surface formation Sn mixed ZnO semiconductor material. Described materials microstructure structure is the mixing network structure being of a size of 40 ~ 100nm nanoneedle and 200 ~ 500nm nanometer rods. The present invention is capable of the controllable growth of Sn doping zinc oxide nanometer thin film; The detection being capable of under room temperature to the gas such as acetone, ethanol, say, that adopt the method can prepare room temperature gas sensing property components and parts, it is possible to realize the selectivity of gas sensor under room temperature condition: ethanol is better than acetone gas sensing property. The preparation method growth temperature provided is low, and equipment is simple, and cost is low, it does not have environmental pollution.
Description
Technical field
The invention belongs to technical field of semiconductor film preparation, relate to gas sensor and nano material preparation technology, particularly relate to one Sn mixed ZnO semiconductor material and preparation method and the application of this kind of material.
Background technology
Semiconductor gas sensor is very low with its manufacturing cost, long service life, recovery time and response time ratio very fast and highly sensitive, be used widely in gasmetry and monitoring. Wherein by the ZnO nano film structure of different element dopings because the photoelectric properties of its uniqueness are shown one's talent in numerous semiconductor gas sensor structural materials. As with the Mg nano-ZnO thin film adulterated to H2There is the gas sensing property (YanxiaLiu that comparison is high, TaoHang, YizhuXie, ZhongBao, JieSong, HongliangZhang, ErqingXie.SensorsandActuatorsB, 160 (2011) 266 270.), gas sensing property research (XuedaLi to acetone and ethanol when with Sn doping zinc oxide nanometer thin film high temperature, YongqinChang, YiLong.MaterialsScienceandEngineeringC, 32 (2012) 817 821.). At present, the method preparing ZnO nano-structure is relatively more, mainly has chemical vapour deposition technique (CVD), sol-gal process, the sedimentation method, hydro-thermal method, microemulsion method, electrochemical process, organic precursor thermal decomposition method, magnetron sputtering method etc. Wherein CVD is to utilize hot conditions reactant to issue biochemical reaction at gaseous condition, and in cooling procedure, coagulation grows up formation particle deposition at substrate surface. Nano-ZnO thin film structure prepared by this method has that pattern is various, better crystallinity degree, purity high, particle dispersion is good, can the advantage such as synthesis in a large number.
At present the bottleneck problem to the research of ZnO semiconductor gas sensor is how to realize under room temperature the good gas sensing property to surveyed gas by controlling the nano structural material of different element doping and synthesis different-shape.It has been reported that the article gone out is substantially under hot conditions just has gas sensing property (YanxiaLiu, TaoHang, YizhuXie, ZhongBao, JieSong, HongliangZhang, ErqingXie.SensorsandActuatorsB, 160 (2011) 266 270.).
Summary of the invention
The technical problem to be solved in the present invention is, existing ZnO semi-conducting material is due to the reason such as element doping, organizational structure, in gas sensor application aspect, just there is good gas sensing property and selectivity only under the high temperature conditions, its application is extremely restricted, the present invention controls Sn in doping and the tissue topography of ZnO so that its room temperature gas sensing property is substantially improved and selectivity is more notable by composition and preparation method, can be used for the application of room temperature air sensor.
For solving the problems referred to above, the technical scheme that the present invention takes is as follows.
A kind of preparation method of Sn mixed ZnO semiconductor material, described preparation method is, Sn powder and Zn powder is blended in the oxygen atmosphere with argon and heats with CVD(chemical vapour deposition (CVD)) deposit to device surface formation Sn doping zinc oxide nanometer thin film.
The preferred version of above-mentioned preparation method is, the preparation process including following: 1) adopt the method for preset electrode to prepare gas sensor; 2) CVD(chemical vapour deposition (CVD) is adopted) method prepares Sn doping zinc oxide nanometer thin film on gas sensor, first Zn powder is mixed with the stirring of Sn powder, by staggered relatively in porcelain boat to mixed powder and gas sensor, porcelain boat is put in heating furnace, heat after 630 DEG C ~ 650 DEG C insulation, be Ar gas atmosphere in heating process; Insulating process is Ar gas, O2The mixed atmosphere of gas; 3) take out porcelain boat after insulation, after room temperature air cooling, obtain Sn mixed ZnO semiconductor material.
The preferred version of above-mentioned preparation method is, the mass ratio of described Zn powder and Sn powder is 4:1 ~ 7:3.
The preferred version of above-mentioned preparation method is, described heating and thermal insulation technique is, behind the heating rate of 13��18 DEG C/min to 630 DEG C ~ 650 DEG C, is incubated 10��20min.
The preferred version of above-mentioned preparation method is, described Ar gas, O2Respectively, in heating process, Ar throughput is set as 80 ~ 100sccm, O to the control flow of gas2Throughput is set as 0sccm; In insulating process, Ar throughput is set as 100 ~ 120sccm, O2Throughput is set as 8 ~ 10sccm.
The preferred version of above-mentioned preparation method is, the preparation method of described gas sensor is, first sheet glass is put in beaker, carry out ultrasonic cleaning, dry up standby after cleaning, both are sufficiently stirred for according to the ratio of 3 ~ 3.5g:1ml by argentum powder and conducting resinl and are mixed into starchiness, as binding agent, copper wire is fixed on sheet glass with it, elargol is dried in atmosphere, whole element is placed in drying basin and dries 10 ~ 12h, then it is put into again in drying baker, processes at 100 DEG C ~ 150 DEG C and take out that to be placed again in drying basin standby after 1.5 ~ 2h.
The invention still further relates to a kind of Sn mixed ZnO semiconductor material, described materials microstructure structure is nanoneedle 40 ~ 100nm mixing network structure being of a size of with nanometer rods 200 ~ 500nm.
The preferred version of above-mentioned semi-conducting material is, the ratio of the described material gas sensing property response value S resistance that is material in test gas and resistance in atmosphere, when alcohol concentration is 326ppm, S value is more than 250.
The invention still further relates to the application of Sn mixed ZnO semiconductor material, described Sn mixed ZnO semiconductor material can be applicable to gas sensor.
The preferred version of above-mentioned application is, ethanol and acetone can be detected and monitor by described material at ambient temperature.
The present invention it is possible to realize the controllable growth of Sn doping zinc oxide nanometer thin film relative to the beneficial effect of prior art; The detection being capable of under room temperature to the gas such as acetone, ethanol, say, that adopt the method can prepare room temperature gas sensing property components and parts, it is possible to realize the selectivity of gas sensor under room temperature condition: ethanol is better than acetone gas sensing property. The preparation method growth temperature provided is low, and equipment is simple, and cost is low, it does not have environmental pollution.
Accompanying drawing explanation
Fig. 1 is the material of the embodiment 1 preparation gas-sensitive reaction curve to ethanol;
Fig. 2 is the material of the embodiment 1 preparation selectivity curve to ethanol and acetone;
Fig. 3 is the material of the embodiment 1 preparation gas sensing property response value to variable concentrations ethanol;
Fig. 4 is the material of the embodiment 2 preparation gas-sensitive reaction curve to ethanol;
Fig. 5 is the material of the embodiment 2 preparation selectivity curve to ethanol and acetone;
Fig. 6 is the material of the embodiment 2 preparation gas sensing property response value to variable concentrations ethanol.
Detailed description of the invention
Embodiment 1
The preparation of a kind of Sn mixed ZnO semiconductor material and air-sensitive method of testing, the concrete steps including following: 1) weigh Zn powder (analytical pure) 0.32g and Sn powder (analytical pure) 0.08g(Zn:Sn=4:1), put into porcelain boat; 2) surface being placed horizontally in porcelain boat by electrode microscope slide preset in drying basin and gas sensor mixed powder, fixes with copper wire and puts into tube furnace quartz ampoule middle section; 3) heating process is warming up to 650 DEG C with the speed of 13 DEG C/min, is incubated 10min; 4) in heating process, Ar throughput is set as 100sccm, O2Throughput is set as 0sccm, and in insulating process, Ar throughput is set as 100sccm, O2Throughput is set as 10sccm; 5), after insulation terminates, sample air cooling is taken out to room temperature;
The preparation method of gas sensor is, first sheet glass is put in beaker, carry out ultrasonic cleaning, dry up standby after cleaning, both are sufficiently stirred for according to the ratio of 3g:1ml by argentum powder and conducting resinl and are mixed into starchiness, as binding agent, copper wire is fixed on sheet glass with it, elargol is dried in atmosphere, whole element is placed in drying basin dry 12h, is then put into again in drying baker, after processing 2h at 100 DEG C, take out that to be placed again in drying basin standby.
Carry out alcohol gas-sensitive experiment: 1 debugging air-sensitive test system, connecting test sample; 2 inject a certain amount of ethanol in test chamber so that it is in test chamber, fully volatilization mixes with air, record change in resistance; 3 inject air, alcohol gas in releasing system to test system, record change in resistance; 4 are repeatedly performed inflation deflation cycles experiment, the testing element gas sensing property to variable concentrations (81.6ppm, 163.2ppm, 244.8ppm, 326.4ppm, 408ppm) ethanol.
Carry out air-sensitive selectivity test: 1 debugging air-sensitive test system, connecting test sample; 2 inject 4ul ethanol in test chamber so that it is in test chamber, fully volatilization mixes with air, records change in resistance; 3 inject air, alcohol gas in releasing system in test chamber, record change in resistance; 4 inject 4ul acetone in test chamber so that it is in test chamber, fully volatilization mixes with air, records change in resistance; It is inflated deflation cycles experiment, the testing element air-sensitive selectivity to ethanol and acetone for more than 5 time. Test result shows, the element air-sensitive response value S to 4ul ethanoleth=195.1, the element air-sensitive response value S to 4ul acetoneace=129.7��
Embodiment 2
The preparation of a kind of Sn mixed ZnO semiconductor material and air-sensitive method of testing, it is characterized in that, concrete steps including following: 1) weigh Zn powder (analytical pure) 0.28g and Sn powder (analytical pure) 0.12g(Zn:Sn=7:3), put into porcelain boat;2) surface being placed horizontally in porcelain boat by electrode microscope slide preset in drying basin and gas sensor mixed powder, fixes with copper wire and puts into tube furnace quartz ampoule middle section; 3) heating process is warming up to 630 DEG C with the speed of 18 DEG C/min, is incubated 20min; 4) in heating process, Ar throughput is set as 80sccm, O2Throughput is set as 0sccm, and in insulating process, Ar throughput is set as 120sccm, O2Throughput is set as 8sccm; 5) insulation closes diamond heating program after terminating, and takes out sample air cooling to room temperature;
The preparation method of gas sensor is, first sheet glass is put in beaker, carry out ultrasonic cleaning, dry up standby after cleaning, both are sufficiently stirred for according to the ratio of 3.5g:1ml by argentum powder and conducting resinl and are mixed into starchiness, as binding agent, copper wire is fixed on sheet glass with it, elargol is dried in atmosphere, whole element is placed in drying basin dry 10h, is then put into again in drying baker, after processing 1.5h at 150 DEG C, take out that to be placed again in drying basin standby.
Alcohol gas-sensitive is tested: 1 debugging air-sensitive test system, connecting test sample; 2 inject a certain amount of ethanol in test chamber so that it is in test chamber, fully volatilization mixes with air, record change in resistance; 3 inject air, alcohol gas in releasing system to test system, record change in resistance; 4 are repeatedly performed inflation deflation cycles experiment, the testing element gas sensing property to variable concentrations (81.6ppm, 163.2ppm, 244.8ppm, 326.4ppm, 408ppm) ethanol.
Air-sensitive selectivity test: 1 debugging air-sensitive test system, connecting test sample; 2 inject 4ul ethanol in test chamber so that it is in test chamber, fully volatilization mixes with air, records change in resistance; 3 inject air, alcohol gas in releasing system in test chamber, record change in resistance; 4 inject 4ul acetone in test chamber so that it is in test chamber, fully volatilization mixes with air, records change in resistance; It is inflated deflation cycles experiment, the testing element air-sensitive selectivity to ethanol and acetone for more than 5 time. Test result shows, the element air-sensitive response value S to 4ul ethanoleth=213.2, the element air-sensitive response value S to 4ul acetoneace=132.8��
Claims (7)
1. the preparation method of a Sn mixed ZnO semiconductor material, it is characterised in that include following preparation process: 1) adopt the method for preset electrode to prepare gas sensor; 2) CVD chemical vapour deposition technique is adopted to prepare Sn doping zinc oxide nanometer structure on gas sensor, first Zn powder is mixed with the stirring of Sn powder, by staggered relatively in porcelain boat to mixed powder and gas sensor, porcelain boat is put in heating furnace, behind the heating rate of 13��18 DEG C/min to 630 DEG C��650 DEG C, insulation 10��20min, is Ar gas atmosphere in heating process; It is Ar gas, O at insulating process2The mixed atmosphere of gas; 3) take out porcelain boat after insulation, after room temperature air cooling, obtain Sn mixed ZnO semiconductor material; The mass ratio of described Zn powder and Sn powder is 4:1��7:3.
2. the preparation method of a kind of Sn mixed ZnO semiconductor material according to claim 1, it is characterised in that described Ar gas, O2Respectively, in heating process, Ar throughput is set as 80��100sccm, O to the control flow of gas2Throughput is set as 0sccm; In insulating process, Ar throughput is set as 100��120sccm, O2Throughput is set as 8��10sccm.
3. the preparation method of a kind of Sn mixed ZnO semiconductor material according to claim 1, it is characterized in that, the preparation method of described gas sensor is, first sheet glass is put in beaker, carry out ultrasonic cleaning, dry up standby after cleaning, both are sufficiently stirred for according to the ratio of 3��3.5g:1ml by argentum powder and conducting resinl and are mixed into starchiness, as binding agent, copper wire is fixed on sheet glass with mixed paste mixture, elargol is dried in atmosphere, whole element is placed in drying basin and dries 10��12h, then more whole element is inserted in drying baker, process at 100 DEG C��150 DEG C and take out that to be placed again in drying basin standby after 1.5��2h.
4. the Sn mixed ZnO semiconductor material that preparation method described in claim 1 prepares, it is characterised in that the organizational structure of described semi-conducting material is the mixing network structure of size 40��100nm nanoneedle and 200��500nm nanometer rods.
5. semi-conducting material according to claim 4, it is characterised in that the gas sensing property response value S of described semi-conducting material is material ratio of resistance and resistance in atmosphere in test gas, and when alcohol concentration is 326ppm, S value is more than 250.
6. the application of the Sn mixed ZnO semiconductor material that preparation method described in claim 1 prepares, it is characterised in that described Sn mixed ZnO semiconductor materials application is in gas sensor.
7. the application of semi-conducting material according to claim 6, it is characterised in that ethanol and acetone are detected and monitor by described semi-conducting material at ambient temperature.
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| CN101251508A (en) * | 2008-04-01 | 2008-08-27 | 重庆大学 | Method for manufacturing gas sensor for testing hydrogen |
| CN103236352A (en) * | 2013-04-23 | 2013-08-07 | 上海大学 | Preparation method of ZnO sol compounded Sn doping ZnO thick films |
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| CN101328609B (en) * | 2008-04-11 | 2010-12-08 | 北京科技大学 | Method for preparing tin doping zinc oxide nanowire by vapor deposition |
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| CN102442787B (en) * | 2011-09-23 | 2013-09-04 | 青岛海信电器股份有限公司 | Nano air-sensitive thin film and preparation method thereof |
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| CN101251508A (en) * | 2008-04-01 | 2008-08-27 | 重庆大学 | Method for manufacturing gas sensor for testing hydrogen |
| CN103236352A (en) * | 2013-04-23 | 2013-08-07 | 上海大学 | Preparation method of ZnO sol compounded Sn doping ZnO thick films |
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