CN105403598B - A kind of sensing material and preparation method thereof converted to N-type based on adjustable P - Google Patents

A kind of sensing material and preparation method thereof converted to N-type based on adjustable P Download PDF

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CN105403598B
CN105403598B CN201510919509.0A CN201510919509A CN105403598B CN 105403598 B CN105403598 B CN 105403598B CN 201510919509 A CN201510919509 A CN 201510919509A CN 105403598 B CN105403598 B CN 105403598B
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sensing material
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adjustable
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CN105403598A (en
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邵绍峰
江凡
傅瑞雪
王世敏
雷雅婷
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Nanjing University of Information Science and Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/12Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
    • G01N27/125Composition of the body, e.g. the composition of its sensitive layer
    • G01N27/127Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00Compounds of tin
    • C01G19/02Oxides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM

Abstract

The invention discloses a kind of sensing materials and preparation method thereof converted to N-type based on adjustable P.Sensing material and the integrated high-performance sensors of device are prepared with in-situ synthesis, the novel sensing material of thickness and aperture controllably is prepared by steam hydrothermal synthesis method.Content by regulating and controlling calcination temperature and dopant realizes the controlledly synthesis that p-type is converted to N-type performance.This method is by regulating and controlling calcination temperature and platinum content.Roasting process can the nano-structural ordered property of Effective Regulation, nanocrystalline grain size and component ratio.The sensing capabilities that sensing material may be implemented by regulating and controlling calcination temperature by the present invention are changed from p-type to N-type, and the sensing response time can be controlled in 25 seconds or so under room temperature, and sensing material has good sensitivity and selectivity to trace toluene.

Description

A kind of sensing material and preparation method thereof converted to N-type based on adjustable P
Technical field
The invention belongs to new gas senser element, more particularly to a kind of sensing material converted to N-type based on adjustable P and Preparation method.
Background technology
In recent years, not only in scientific domain but also in daily life, for example, food security, biological medicine and The status of urban safety etc., sensor of chemical gas is more and more important.Currently, the research emphasis of gas sensor mainly collects In detection poisonous and harmful substance.In numerous poisonous and harmful substances, toluene has irritation effect to the skin of the mankind, And the nervous system of human body can be injured.Therefore, publilc health and environment are defended in the instant accurate detection of toluene trace Life is most important.
Now, the means of testing for detecting trace toluene includes mainly electrochemical process, optic test method and chemical-electrical Hinder method of testing.In this three classes method, metal oxide base chemoresistive sensors are because its manufacturing cost is low, simple for process, reading The features such as facilitating is taken to become most potential a kind of sensor.The sensing material of various different types of structure such as nanometer Grain, nano wire, nanoneedle and nanoscale film have been attempted in the real work for being applied to detection toluene.It is above-mentioned Ordered nano hole base sensing arrangement has high-specific surface area, high activity near-surface region, abundant surface in different types of structure Active sites and extremely strong gas sorption ability, bringing up it has the potentiality for promoting sensing capabilities.However, existing sensor Operating temperature will be higher than 200 DEG C, and respond tunable performance deviation, up to the present there are no about under room temperature The performance of sensing material is reported from p-type to the invention of the adjustable conversion of N-type.
Invention content
The present invention is directed to the problem of existing sensing material and deficiency, and sensing material and device one are prepared with in-situ synthesis The high-performance sensors of body prepare the novel sensing material of thickness and aperture controllably by steam hydrothermal synthesis method.Pass through The content of regulation and control calcination temperature and dopant realizes the controlledly synthesis that p-type is converted to N-type performance.The present invention provides a kind of bases In the sensing material and preparation method thereof that adjustable P is converted to N-type, this method is by regulating and controlling calcination temperature and platinum content.Roasting Process can the nano-structural ordered property of Effective Regulation, nanocrystalline grain size and component ratio.The present invention is by regulating and controlling calcination temperature The sensing capabilities of sensing material may be implemented from p-type to N-type to be changed, under room temperature the sensing response time can be controlled in 25 seconds left sides The right side, and sensing material has good sensitivity and selectivity to trace toluene.
This hair develops a kind of method using steam hydro-thermal and prepares high-crystallinity ordered nano Porous materials, and this method can be with The highly crystalline of metal oxide is realized in low temperature, also, low temperature goes mano-porous material after template agent removing that can still keep high Spend the nanometer hole wall of crystallization.By using above-mentioned synthetic method, and the mode of precious metal doping is combined to prepare novel sensing material Material.Contained by regulating and controlling the difference of different calcination temperatures and noble metal be found that during sensing capabilities detection There is a kind of controllable conversion of p-type to N-type in amount, sensing material.Before this, if it is a small number of in relation to p-type to the sensing capabilities of N-type Controllable conversion, and turning for performance is mainly realized by the operating temperature of the concentration and sensor that regulate and control under test gas It changes.For example, the scientific workers such as Huang have found to modify SnO by regulating and controlling the concentration ZnO of under test gas2Sensor can realize N- The conversion of P-N;Wang etc. is reported senses material by the concentration ZnO nanotube/for changing senor operating temperature and under test gas The conversion of N-P may be implemented in material;The scientific workers such as Dai are by establishing the theoretical model of under test gas concentration and operating temperature Realize nano-pore Fe2O3The controllable conversion of sensing material P-N.However, up to the present there are no about realizing under room temperature The report and invention that P is converted to N-type sensing capabilities.
For achieving the above object, the present invention uses following technical scheme:
A kind of sensing material and preparation method thereof converted to N-type based on adjustable P, is included the following steps:
A. the configuration of sol solution:It is 1 to take mass ratio:100-4:100 precious metal salt and pink salt, it is pink salt to be dissolved in quality 20-40 times of polar solvent in, it is the surfactant between 0.3-0.5 times of pink salt that quality, which is then added, and matter is added Amount is 1-2 times of a certain amount of concentrated acid of pink salt quality, matches to obtain required sol solution;
B. the preparation of gelatinous sensor material:By sol solution obtained by step (a) using spin-coating method in blank interdigital electrode Plated film is carried out to get the device of sensing material is coated with, the relative humidity inside sol evenning machine is controlled in spin coating process and is controlled in 20- Between 50%;It is dry in 30-60 DEG C of temperature range that the device of sensing material will be coated with, drying time control 2h-12h it Between, obtain gelatinous sensor material;
C. the regulation and control of humidity:The supersaturated solution for allocating metal salt, puts it into closed container, it is ensured that under room temperature Relative humidity in closed container is put between 75%-95%, then by the device for being coated with gelatinous sensor material obtained by step (b) Enter in closed container, it is ensured that the relative humidity in container reaches stable;
D. the preparation of laminated film:The closed container of step (c) mask placement device is put into air dry oven and adjusts temperature Between 105-145 DEG C, start calculating reacting time, reaction time 36- when the temperature of air dry oven reaches stable 120h.After reaction, senser element taking-up is cooled to room temperature.One step of this method prepares ordered nano hole SnO2Sense material Material;
E. the roasting of laminated film:Step d is prepared into gained ordered nano hole SnO2Sensing material carries out different temperatures Roasting, calcination temperature is between 200-400 DEG C;
F. sensing capabilities detect:Under room temperature, the sensor for step (e) being prepared to gained carries out VOCs gas detections, Regulate and control the concentration of gas between 10ppm-200ppm, carries out within every two minutes an atmosphere and exchange.Regulate and control reproducibility in gas Atmosphere is toluene/argon gas, ethyl alcohol/argon gas, acetone/argon gas, isopropanol/argon gas, the mixed gas such as ether/argon gas, oxidisability gas Body is dry air.
Wherein, precious metal salt is PtCl in step (a)4;Pink salt is anhydrous stannic chloride;Polar solvent be ethyl alcohol, n-butanol, Isopropanol, preferably n-butanol;Surfactant is F127, P123, P103, preferably P103;Concentrated acid is concentrated hydrochloric acid, concentrated nitric acid, dense Sulfuric acid, the preferably concentrated sulfuric acid.
Spin-coating method uses spin speed for 2500-4500rpm in step (b), preferably 4000rpm, and each spin-coating time is 30-60s, preferably time are 45sec;The interior cavity humidity that controls of sol evenning machine is 20-50%, and preferably 35%, spin coating number of repetition is 5 It is secondary.
Metal salt supersaturated solution in step (c), metal salt NaCl, KCl, CuSO4, preferably NaCl.
Sensing material performance detection in step (f), 200 DEG C of roasting samples show p-type sensing capabilities under room temperature, 400 DEG C of roasting samples show N-type sensing capabilities under room temperature;When calcination temperature is less than 400 DEG C, sensing material is shown as P-type sensing characteristics, when calcination temperature is higher than in 400 DEG C, sensing material shows as N-type sensing characteristics.
The present invention has the following advantages compared with prior art:
1, the sensing of the gas sensor for the ordered nano crystalline substance tin oxide sensing material that the adjustable p-type of the present invention is converted to N-type It has excellent performance, to low concentration VOCs gas response times and recovery time close to 20sec.
2, the present invention prepares high-performance sensing material using in-situ synthesis, simplifies preparation process, reduces the production cost, And the repeatability of sensing material is strong, the nano-particles size for forming sense film is small, and average grain size is with calcination temperature Increase and increase, but when calcination temperature is less than 400 DEG C, average grain size is less than 5nm, material specific surface area is big;Low temperature roasts When burning, tin oxide nano particle forms high-quality p-n layer with metal oxide containing precious metals, and sensing capabilities are changed into p-type by N-type;Work as roasting When temperature is higher than 400 DEG C, the pore structure of sensing material is stable and order is good, the generation of surfaces externally and internally therewith, to activate The adsorption capacity of grain surface promotes surface reaction activity, improves sensitivity and shortens the response time, sensing capabilities are turned by p-type Become N-type, and room temperature condition stable working state, eliminate the problems of energy consumption of traditional sensors part, effectively reduces system Standby and use cost.
Description of the drawings
Fig. 1 is small angle X-ray diffraction (SAXRD) figure of the sensing material prepared in the embodiment of the present invention 1;
Fig. 2 is the high-resolution-ration transmission electric-lens (HRTEM) of sensing material after the 200 DEG C of roastings prepared in the embodiment of the present invention 1 Figure;
Fig. 3 is the high-resolution-ration transmission electric-lens (HRTEM) of sensing material after the 400 DEG C of roastings prepared in the embodiment of the present invention 1 Figure;
Fig. 4 is the VOCs sensing capabilities figures of the senser element prepared in the embodiment of the present invention 1, and the concentration of VOCs is respectively 10,20,40,80,120,160,180,200ppm.
Specific implementation mode
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
In glove box, 0.004g platinum chlorides and 0.12g anhydrous stannic chlorides are weighed, is dissolved in 2.5g anhydrous normal butyl alcohols, 0.024g polymer Ps 103 are added, add the 0.18g concentrated sulfuric acids, magnetic agitation is uniformly mixed and obtains clear solution, is stirred overnight. Start sol evenning machine, sensing substrate devices are fixed in sol evenning machine cavity, pipette 100l sol solutions every time using pipettor, are controlled Humidity in cavity processed is 30%, and spin speed 3500rpm, spin-coating time 40sec, spin coating are repeated 5 times.Film will be coated with The device of material dry 2h under the conditions of 60 DEG C obtains gel rubber material.Sodium chloride supersaturated solution is allocated, supersaturated solution is put Enter in closed container, it is ensured that the relative humidity in closed container is stablized 75% or so under room temperature, then will be coated with gel biography The device of sense material is put into closed container.When the relative humidity in container reaches stable, closed container is put into air blast and is done It is 105 DEG C that temperature is adjusted in dry case, starts calculating reacting time when the temperature of air dry oven reaches stable, the reaction time is 120h.After reaction, senser element taking-up is cooled to room temperature.Ordered nano crystalline substance SnO is prepared in situ out in this method2Sense material Material.Gained sensing material is roasted under different calcination temperatures, calcination temperature is 200 DEG C -400 DEG C.Under room temperature will Roasting gained ordered nano crystalline substance SnO2Sensing material carries out VOCs gas detections, regulates and controls the concentration of gas between 10ppm-200ppm Between, exchange atmosphere within every two minutes.Reducing atmosphere be toluene/argon gas, ethyl alcohol/argon gas, acetone/argon gas, isopropanol/argon gas, The mixed gas such as ether/argon gas, oxidizing gas are dry air.Test result shows that sensing material has Gao Ling to VOCs Sensitivity and selectivity is good.And 200 DEG C of roasting samples show p-type sensing capabilities, 400 DEG C of roasting sample room temperatures under room temperature Under the conditions of show N-type sensing capabilities.When calcination temperature is less than 400 DEG C, sensing material shows as p-type sensing characteristics, works as roasting It burns temperature to be higher than when 400 DEG C, sensing material shows as N-type sensing characteristics.
Fig. 1 is the small angle X-ray diffraction figure of ordered nano crystalline substance SnO 2 thin film material, as can be seen from Figure 1 with roasting The structural order of thin-film material obtained by the raising of temperature shows incremental trend;Fig. 2 is the height of 200 DEG C of roasting thin-film materials Resolved transmittance electron microscope, the figure show that there is tin oxide grain good crystallinity, nanocrystal average-size to be less than 3nm; Fig. 3 is the high-resolution-ration transmission electric-lens figure of 400 DEG C of roasting thin-film materials, which shows that tin oxide grain has good crystallization Degree, nanocrystal average-size are less than 4nm;Fig. 4 be senser element air-sensitive performance test chart, sensitivity with VOCs concentration from 10ppm-200ppm is stepped up, and the response time of sensor and recovery time are both less than 20sec.
Embodiment 2
In glove box, 0.004g platinum chlorides and 0.12g anhydrous stannic chlorides are weighed, is dissolved in 3.6g anhydrous normal butyl alcohols, 0.036g polymer Ps 103 are added, add the 0.2g concentrated sulfuric acids, magnetic agitation is uniformly mixed and obtains clear solution, is stirred overnight. Start sol evenning machine, sensing substrate devices are fixed in sol evenning machine cavity, pipette 100l sol solutions every time using pipettor, are controlled Humidity in cavity processed is 20%, and spin speed 3500rpm, spin-coating time 40sec, spin coating are repeated 5 times.Film will be coated with The device of material dry 8h under the conditions of 40 DEG C obtains gel rubber material.Potassium chloride supersaturated solution is allocated, supersaturated solution is put Enter in closed container, it is ensured that the relative humidity in closed container is stablized 85% or so under room temperature, then will be coated with gel biography The device of sense material is put into closed container.When the relative humidity in container reaches stable, closed container is put into air blast and is done It is 125 DEG C that temperature is adjusted in dry case, starts calculating reacting time when the temperature of air dry oven reaches stable, the reaction time is 72h.After reaction, senser element taking-up is cooled to room temperature.Ordered nano crystalline substance SnO is prepared in situ out in this method2Sense material Material.Gained sensing material is roasted under different calcination temperatures, calcination temperature is 200 DEG C -400 DEG C.
Embodiment 3
In glove box, 0.002g platinum chlorides and 0.12g anhydrous stannic chlorides are weighed, is dissolved in 4.8g anhydrous normal butyl alcohols, 0.06g polymer Ps 103 are added, add the 0.24ml concentrated sulfuric acids, magnetic agitation is uniformly mixed and obtains clear solution, is stirred overnight. Start sol evenning machine, sensing substrate devices are fixed in sol evenning machine cavity, pipette 100l sol solutions every time using pipettor, are controlled Humidity in cavity processed is 50%, and spin speed 4000rpm, spin-coating time 30sec, spin coating are repeated 5 times.Film will be coated with The device of material dry 12h under the conditions of 30 DEG C obtains gel rubber material.Copper sulphate supersaturated solution is allocated, supersaturated solution is put Enter in closed container, it is ensured that the relative humidity in closed container is stablized 95% or so under room temperature, then will be coated with gel biography The device of sense material is put into closed container.When the relative humidity in container reaches stable, closed container is put into air blast and is done It is 145 DEG C that temperature is adjusted in dry case, starts calculating reacting time when the temperature of air dry oven reaches stable, the reaction time is 36h.After reaction, senser element taking-up is cooled to room temperature.Ordered nano crystalline substance SnO is prepared in situ out in this method2Sense material Material.Gained sensing material is roasted under different calcination temperatures, calcination temperature is 200 DEG C -400 DEG C.
Embodiment 4
0.003g platinum chlorides and 0.1g anhydrous stannic chlorides are weighed, is dissolved in 3.0g isopropanols, 0.035g polymer is added P123, adds 0.1g concentrated nitric acids, and magnetic agitation is uniformly mixed and obtains clear solution, is stirred overnight.Start sol evenning machine, will sense Interdigital electrode is fixed in sol evenning machine cavity, pipettes 100l sol solutions every time using pipettor, and the humidity in control chamber body is 30%, spin speed 2500rpm, spin-coating time 60sec, spin coating are repeated 5 times.The device of thin-film material will be coated in 30 DEG C of items Dry 12h obtains gel rubber material under part.Potassium chloride supersaturated solution is allocated, supersaturated solution is put into closed container, it is ensured that Relative humidity in closed container is stablized 85% or so under room temperature, then the device for being coated with gelatinous sensor material is put into close It closes in container.When the relative humidity in container reaches stable, it is 145 that closed container, which is put into air dry oven, and adjusts temperature DEG C, start calculating reacting time, reaction time 36h when the temperature of air dry oven reaches stable.After reaction, it will pass Inductor component taking-up is cooled to room temperature.Ordered nano crystalline substance SnO is prepared in situ out in this method2Sensing material.Gained sensing material is existed It is roasted under different calcination temperatures, calcination temperature is 200 DEG C -400 DEG C.
Embodiment 5
0.003g platinum chlorides and 0.1g anhydrous stannic chlorides are weighed, is dissolved in 3.5g absolute ethyl alcohols, 0.04g polymer is added F127, adds 0.1g concentrated hydrochloric acids, and magnetic agitation is uniformly mixed and obtains clear solution, is stirred overnight.Start sol evenning machine, will sense Interdigital electrode is fixed in sol evenning machine cavity, pipettes 100l sol solutions every time using pipettor, and the humidity in control chamber body is 30%, spin speed 2500rpm, spin-coating time 60sec, spin coating are repeated 5 times.The device of thin-film material will be coated in 60 DEG C of items Dry 2h obtains gel rubber material under part.Copper sulphate supersaturated solution is allocated, supersaturated solution is put into closed container, it is ensured that room Relative humidity in closed container is stablized 95% or so under the conditions of temperature, then the device for being coated with gelatinous sensor material is put into closed In container.When the relative humidity in container reaches stable, it is 145 that closed container, which is put into air dry oven, and adjusts temperature DEG C, start calculating reacting time, reaction time 36h when the temperature of air dry oven reaches stable.After reaction, it will pass Inductor component taking-up is cooled to room temperature.Ordered nano crystalline substance SnO is prepared in situ out in this method2Sensing material.Gained sensing material is existed It is roasted under different calcination temperatures, calcination temperature is 200 DEG C -400 DEG C.
The preparation method of the present invention fully simplifies synthesis step, and composite sensing material is directly prepared by in-situ synthesis. During synthesis, by configuring clear sol solution, passing through dry aging, it is opposite in synthesis by adequately regulating and controlling Humidity effectively obtains quantum scale titanium oxide/polymer composites.The repeatability of sensing material is strong, forms sense film Nano-particles size it is small, average grain size increases with the increase of calcination temperature, but when calcination temperature be less than 400 DEG C when, Average grain size is less than 5nm, and material specific surface area is big;When low-temperature bake, tin oxide nano particle and metal oxide containing precious metals shape At high-quality p-n layer, sensing capabilities are changed into p-type by N-type;When calcination temperature is higher than 400 DEG C, the pore structure of sensing material is stablized And order is good, the generation of surfaces externally and internally therewith, to activate the adsorption capacity of grain surface, promotes surface reaction activity, It improves sensitivity and shortens the response time, sensing capabilities are changed into N-type, and room temperature condition stable working state by p-type, eliminate The problems of energy consumption of traditional sensors part effectively reduces preparation and use cost.Compared with existing sensor, prepare It is simple for process, to the of less demanding of equipment, cost reduction, it is easier to large-scale production.

Claims (8)

1. a kind of sensing material converted to N-type based on adjustable P, which is characterized in that the preparation of the sensing material includes following Step:
A. the configuration of sol solution:Precious metal salt and pink salt are taken, is dissolved in polar solvent, surfactant is then added, and add Enter concentrated acid, matches to obtain required sol solution;Precious metal salt is PtCl4, pink salt is anhydrous stannic chloride, surfactant F127, P123, P103;The mass ratio of precious metal salt and pink salt is 1:100-4:100;
B. the preparation of gelatinous sensor material:Sol solution obtained by step a is plated using spin-coating method in blank interdigital electrode Film to get being coated with the device of sensing material, the relative humidity control in spin coating process inside control sol evenning machine 20-50% it Between;The device for being coated with sensing material is dry in 30-60 DEG C of temperature range, and drying time controls between 2h-12h, obtains Gelatinous sensor material;
C. the regulation and control of humidity:The supersaturated solution for allocating metal salt, puts it into closed container, it is ensured that closed under room temperature Relative humidity in container is between 75%-95%, then the device that gelatinous sensor material is coated with obtained by step b is put into closed In container, it is ensured that the relative humidity in container reaches stable;
D. the preparation of laminated film:It is 105- that the closed container of step c mask placement devices, which is put into air dry oven, and adjusts temperature Between 145 DEG C, start calculating reacting time, reaction time 36-120h when the temperature of air dry oven reaches stable;Reaction After, senser element taking-up is cooled to room temperature, a step prepares ordered nano hole SnO2Sensing material;
E. the roasting of laminated film:Step d is prepared into gained ordered nano hole SnO2Sensing material carries out the roasting of different temperatures, Calcination temperature is between 200-400 DEG C;
F. sensing capabilities detect:Under room temperature, the sensing material that step e is prepared to gained carries out VOCs gas detections, regulation and control The concentration of gas carries out an atmosphere for every two minutes and exchanges between 10ppm-200ppm;Sensing material performance detection, 200 DEG C roasting sample shows p-type sensing capabilities under room temperature, and 400 DEG C of roasting samples show N-type sensitivities under room temperature Energy;When calcination temperature is less than 400 DEG C, sensing material shows as p-type sensing characteristics, when calcination temperature is higher than in 400 DEG C, passes Sense material shows as N-type sensing characteristics.
2. the sensing material according to claim 1 converted to N-type based on adjustable P, which is characterized in that polarity in step a Solvent is ethyl alcohol, n-butanol, isopropanol;Concentrated acid is concentrated hydrochloric acid, concentrated nitric acid, the concentrated sulfuric acid.
3. the sensing material according to claim 2 converted to N-type based on adjustable P, which is characterized in that polarity in step a Solvent is n-butanol;Surfactant is P103;Concentrated acid is the concentrated sulfuric acid.
4. the sensing material according to claim 1 converted to N-type based on adjustable P, which is characterized in that surface in step a 0.3-0.5 times that quality is pink salt quality is added in activating agent;1-2 times that quality is pink salt quality is added in concentrated acid.
5. the sensing material according to claim 1 converted to N-type based on adjustable P, which is characterized in that spin coating in step b Method uses spin speed for 2500-4500rpm;Each spin-coating time is 30-60s;Control cavity humidity is 20- in sol evenning machine 50%;Spin coating number of repetition is 5 times.
6. the sensing material according to claim 5 converted to N-type based on adjustable P, which is characterized in that spin coating in step b Method uses spin speed for 4000rpm, and each spin-coating time is 45s;Control cavity humidity is 35% in sol evenning machine.
7. the sensing material according to claim 1 converted to N-type based on adjustable P, which is characterized in that metal in step c Salt supersaturated solution, metal salt NaCl, KCl, CuSO4
8. the sensing material according to claim 7 converted to N-type based on adjustable P, which is characterized in that metal in step c Salt supersaturated solution, metal salt NaCl.
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敏感功能材料的气敏机理及二氧化锡在传感器中给的应用研究;王广健等;《功能材料》;20030430;第34卷(第4期);全文 *

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