CN102248737B - Cr2O3 or NiO porous film material using WO3 as base material and method for manufacturing air-sensitive sensor - Google Patents

Cr2O3 or NiO porous film material using WO3 as base material and method for manufacturing air-sensitive sensor Download PDF

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CN102248737B
CN102248737B CN 201110093965 CN201110093965A CN102248737B CN 102248737 B CN102248737 B CN 102248737B CN 201110093965 CN201110093965 CN 201110093965 CN 201110093965 A CN201110093965 A CN 201110093965A CN 102248737 B CN102248737 B CN 102248737B
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nio
porous film
film material
sol
cr2o3
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CN102248737A (en
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高鹏
季惠明
冯婉评
曹培
周玉贵
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Tianjin University
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Abstract

The invention relates to a preparation method for a Cr2O3 or NiO porous film material using WO3 as a base material and a method for manufacturing an air-sensitive sensor. A WO3-Cr2O3 or WO3-NiO sol material is prepared by using chemical pure tungstic acid H2WO4 and analytical pure Cr(NO3)3.9H2O or Ni(NO3)2.6H2O as raw materials, 2mol/L of citric acid as a complexing agent, 30 percent of hydrogen peroxide (H2O2) as a dispersing agent and urea as a pore-forming agent. A porous film type air-sensitive sensor manufactured by a sol-gel method has the characteristics of high selectivity, high sensitivity, short response-recovery time, high stability and the like. By the methods, the sensitivity of low-concentration specific gas can be detected; and the methods are particularly suitable for the fields of breath detection, food quality detection, environment detection and the like, have obvious research and application value, have the characteristics of low energy consumption, low cost, small volume and the like and are easy to operate.

Description

With WO 3Cr for base material 2O 3Or the preparation method of the porous film material of NiO and prepare the method for gas sensor
Technical field
The invention belongs to semi-conductor gas sensitive material engineering field, relate to WO 3The preparation method of base semiconductor porous film material and this material sensors.Concrete is with WO 3Cr for base material 2O 3Or the preparation method of the porous film material of NiO and prepare the method for gas sensor.
Background technology
Along with the development of society and the raising of living standards of the people, people more and more need remove to survey the various gases that may contact in daily life and industrial production.For example in industry and public safety field, by the leakage of acetone gas in the acetone gas sensor monitoring of environmental, can make warning to the safety that might cause and the great harm of health of human body aspect; In breathing is diagnosed a disease, by the acetone concentration in the human body breath, can judge whether to suffer from type i diabetes.In the detection of driving when intoxicated, by the concentration of alcohol in driver's breath is detected, can the real-time judge driver whether drive when intoxicated.In halitosis detects, by H in the human body breath 2The concentration of S gas can conveniently detect whether suffer from halitosis.
Before this minimum gas is carried out quantitative detection method and mainly contain gas phase or liquid chromatography, solid electrolyte method, spectrophotometer method, quartz crystal micro-balance method, SAW device (SAW), LAPS (LAPS) method and Fiber Optical Sensor Based etc.But these methods detect cost costliness, preparation method's complexity of sensor.
In recent years, along with going deep into of research, people use new material, new technology has been researched and developed many new sensors.At present, the oxide semiconductor gas sensor becomes the focus that people pay close attention to just gradually.Its excellent performance not only depends on the chemical composition of material, more depends on microstructure and the preparation technology of material.Wherein with WO 3Be the semiconductor sensitive material of base, by selecting different alloys and preparation method etc., have excellent performance especially, obtained using widely in a lot of fields.
Summary of the invention
The invention provides a kind of preparation with WO 3Cr for base material 2O 3Or the porous film material of NiO and prepare the method for gas sensor with this material.The present invention passes through sol-gel process earlier with WO 3-Cr 2O 3Or WO 3The raw material of-NiO sensitive material is made colloidal sol, adopts the impregnation technology method to form the porous film type sensitive material, makes the heater-type semiconductor transducer then, to realize the Sensitive Detection to specific gas to be measured.Gas sensor of the present invention has selectively good, highly sensitive, characteristics such as the response-recovery time fast, good stability, solve current gas sensor poor selectivity, the low problem of sensitivity, expanded this type of gas sensor greatly in each Application for Field.
Technology of the present invention is achieved in that
A kind of with WO 3Cr for base material 2O 3Or the preparation method of the porous film material of NiO, step is as follows:
A) raw material adopts chemical pure wolframic acid H 2WO 4With analytically pure Cr (NO 3) 39H 2O or Ni (NO 3) 26H 2O; Be complexing agent, 30% hydrogen peroxide (H with the 2mol/L citric acid 2O 2) be that dispersant, urea are pore creating material; In the beaker of 50mL, take by weighing 3.7479g (0.015mol) H 2WO 4And 0.5g urea places beaker, and taking by weighing molar percentage is the Cr (NO of 0.1-10% 3) 39H 2O or Ni (NO 3) 26H 2O places different beakers, and adds 12.5mL deionized water and 20mL H 2O 2Stir the ultrasonic dispersion in back, obtain WO 3-Cr 2O 3Or WO 3-NiO solution;
B) under constantly stirring, to above-mentioned WO 3-Cr 2O 3Or WO 3Dropwise add 2mol/L citric acid 5-10mL in the-NiO solution, dropwise add 3mol/L ammoniacal liquor adjusting pH value again and be 3-5, to guarantee the stability of colloidal sol; Afterwards mixed solution is placed heating environment, temperature is controlled at 70-100 ℃, and constantly stirs with agitator, fully mixes, and obtains WO 3-Cr 2O 3Or WO 3-NiO sol material.
C) painting method that adopts dipping to lift is with WO 3-Cr 2O 3Or WO 3-NiO sol material is coated to the Al that is printed on electrode 2O 3On the earthenware, carry out 150-200 ℃ of drying down, repeat above-mentioned steps 3-6 time;
D) earthenware is put into the sintering furnace sintering, be warmed up to 500 ℃-700 ℃ heat treatment 1-2 hour.The cooling back obtains porous film material.
Adopt the method for preparing gas sensor of porous film material, step is as follows:
A) to WO 3-Cr 2O 3Porous membrane or WO 3-NiO porous film material is warmed up to 500 ℃-700 ℃ again behind the employing sintering and handled 1-2 hour.To WO 3-Cr 2O 3Porous membrane adopts the mode that is taken out in the air cooling rapidly under this temperature from stove to handle porous membrane; To WO 3-NiO film adopts with 2 ℃ of/minute speed controls and is cooled to the porous membrane that 200 ℃ of modes of slowly cooling off are handled coating;
B) after being welded on the earthenware that obtains on the pedestal, and in pipe, put on the nickel filament heater strip, obtain WO 3-Cr 2O 3Or WO 3-NiO film-type sensor.
Obtain WO 3-Cr 2O 3Porous membrane or WO 3-NiO porous film material sensor as shown in Figure 1.
Adopt the present invention with WO 3Cr for base material 2O 3Or NiO is sensitive material, and by the porous film type gas sensor of sol-gel process preparation, it is selectively good, highly sensitive to have, and the response-recovery time is fast, characteristics such as good stability.The present invention can realize the Sensitive Detection to the low concentration specific gas, is particularly suitable in breathing detection, and food quality detects, fields such as environment measuring, and research is remarkable with using value, can and have energy consumption and cost is low, volume is little, characteristics such as simple to operate.
Description of drawings
Fig. 1: the WO of preparation 3Base film type sensor photo;
Fig. 2: preparation WO 3-Cr 2O 3The SEM surface topography map of porous film material;
Fig. 3: preparation WO 3The SEM surface topography map of-NiO porous film material.
Specific implementation method
Embodiment 1:
(1) in the beaker of 50mL, takes by weighing 3.7479g powder stock H 2WO 4, put into beaker, add the 12.5mL dissolved in distilled water, mix; Take by weighing 0.006g powder stock Cr (NO 3) 39H 2O and 0.5g powder stock urea are put into above-mentioned beaker, add 20mL30%H 2O 2Solution mixes the ultrasonic dispersion in back, obtains WO 3The base mixed solution.
(2) under magnetic agitation, to WO 3Base dropwise adds 2mol/L citric acid 6mL in the mixed solution, and adding 3mol/L ammoniacal liquor, to regulate pH value be 3, with the stability of assurance colloidal sol.Afterwards mixed solution is placed heating environment, temperature is controlled at 70 ℃, by magnetic stirrer 2 hours, fully mixes, and obtains Cr 2O 3Doping is 0.1% uniform and stable WO 3The base precursor sol.
(3) will be about 4mm, inner and outer diameter and be about 0.8mm, 1.2mm respectively, two ends have the Al of Au electrode and Pt silk lead-in wire 2O 3Earthenware ultrasonic cleaning, oven dry.Immerse then in the above-mentioned precursor sol, with speed slowly it is vertically lifted out liquid level, obtain sol pellicle, dry down at 150 ℃ then.After the repetition above-mentioned steps 3 times, obtain gel mould.
(4) earthenware is put into the sintering furnace sintering, with speed intensification slowly, 600 ℃ of heat treatments 1 hour.Behind the sintering, adopt the temperature insulation so far 1 hour that heats up again, the back is taken out to the mode of cooling off rapidly in the air and handles porous membrane from stove, obtain WO 3The based sensor film.The WO of preparation 3-Cr 2O 3The SEM surface topography of porous film material as shown in Figure 2.
(5) with WO 3Base film in the base of sensor, through burin-in process, forms film-type heater-type sensor together with substrate welds, carries out the test of gas-sensitive property.Under the 5V operating voltage, the sensor of this embodiment preparation is 2.08 to the sensitivity of 20ppm ethanol.
Embodiment 2:
Step of preparation process is identical with embodiment 1, and difference is to take by weighing 0.006g powder stock Cr (NO in above-mentioned (1) 3) 39H 2O changes into and takes by weighing 0.3g powder stock Cr (NO 3) 39H 2O puts into beaker; In above-mentioned (2) to WO 3Base dropwise adds 2mol/L citric acid 5mL in the mixed solution, and adding 3mol/L ammoniacal liquor, to regulate the pH value be 4, and mixed solution is placed heating environment, and temperature is controlled at 80 ℃, obtains Cr at last 2O 3Doping is 5% uniform and stable WO 3The base precursor sol; In above-mentioned (3) that earthenware is dry under 170 ℃, and repeat above-mentioned steps 4 times; In above-mentioned (4) with dried film 500 ℃ of heat treatments 1.5 hours, behind the sintering, adopt the temperature insulation so far 1.5 hours that heats up again; Gas to be measured is acetone in above-mentioned (5), and sensitivity is 8.91.
Embodiment 3:
Step of preparation process is identical with embodiment 1, and difference is to take by weighing 0.006g powder stock Cr (NO in above-mentioned (1) 3) 39H 2O changes into and takes by weighing 0.6g powder stock Cr (NO 3) 39H 2O puts into beaker; In above-mentioned (2) to WO 3Base dropwise adds 2mol/L citric acid 10mL in the mixed solution, and adding 3mol/L ammoniacal liquor, to regulate the pH value be 5, and mixed solution is placed heating environment, and temperature is controlled at 100 ℃, obtains Cr at last 2O 3Doping is 10% uniform and stable WO 3The base precursor sol; In above-mentioned (3) that earthenware is dry under 200 ℃, and repeat above-mentioned steps 6 times; In above-mentioned (4) with dried film 700 ℃ of heat treatments 2 hours, behind the sintering, adopt the temperature insulation so far 2 hours that heats up again.Gas to be measured is ammonia in above-mentioned (5), and sensitivity is 1.27.
Embodiment 4:
Step of preparation process is identical with embodiment 1, and difference is to take by weighing 0.006g powder stock Cr (NO in above-mentioned (1) 3) 39H 2O changes into and takes by weighing 0.0044g powder stock Ni (NO 3) 26H 2O puts into beaker, obtains the NiO doping at last and be 0.1% uniform and stable WO 3The base precursor sol; After in above-mentioned (4), the sintering rear film being warming up to again sintering temperature and insulation, adopt with 2 ℃ of/minute speed controls be cooled to 200 ℃ slowly the modes of cooling handle the porous membrane of coating; The WO of preparation 3The SEM surface topography of-NiO porous film material as shown in Figure 3; Gas to be measured is ethanol in above-mentioned (5), and sensitivity is 1.67.
Embodiment 5:
Step of preparation process is identical with embodiment 2, and difference is to take by weighing 0.3g powder stock Cr (NO in above-mentioned (1) 3) 39H 2O changes into and takes by weighing 0.0436g powder stock Ni (NO 3) 26H 2O puts into beaker, obtains the NiO doping at last and be 1% uniform and stable WO 3The base precursor sol; After in above-mentioned (4), the sintering rear film being warming up to again sintering temperature and insulation, adopt with 2 ℃ of/minute speed controls be cooled to 200 ℃ slowly the modes of cooling handle the porous membrane of coating; Gas to be measured is acetone in above-mentioned (5), and sensitivity is 5.83.
Embodiment 6:
Step of preparation process is identical with embodiment 3, and difference is to take by weighing 0.6g powder stock Cr (NO in above-mentioned (1) 3) 39H 2O changes into and takes by weighing 0.4362g powder stock Ni (NO 3) 26H 2O puts into beaker, obtains the NiO doping at last and be 10% uniform and stable WO 3The base precursor sol; After in above-mentioned (4), the sintering rear film being warming up to again sintering temperature and insulation, adopt with 2 ℃ of/minute speed controls be cooled to 200 ℃ slowly the modes of cooling handle the porous membrane of coating; Gas to be measured is ammonia in above-mentioned (5), and sensitivity is 1.10.
Annotate: sensitivity (S) is defined as the ratio of the resistance value Ra of sensor in air atmosphere and resistance value Rg in gas atmosphere to be measured.
All material, method and technology of preparing that the present invention discloses and proposes, those skilled in the art can be by using for reference this paper content, links such as appropriate change raw material and process route realize, although method of the present invention and technology of preparing are described by preferred embodiment, person skilled obviously can change or reconfigure method as herein described and technology path in not break away from content of the present invention, spirit and scope, realizes final result.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.

Claims (2)

1. one kind with WO 3Cr for base material 2O 3Or the preparation method of the porous film material of NiO, it is characterized in that step is as follows:
A) raw material adopts chemical pure wolframic acid H 2WO 4With analytically pure Cr (NO 3) 39H 2O or Ni (NO 3) 26H 2O; Be complexing agent, 30% hydrogen peroxide (H with the 2mol/L citric acid 2O 2) be that dispersant, urea are pore creating material; In the beaker of 50mL, take by weighing 3.7479g (0.015mol) H 2WO 4And 0.5g urea places beaker, and taking by weighing molar percentage is the Cr (NO of 0.1-10% 3) 39H 2O or Ni (NO 3) 26H 2O places beaker, and adds 12.5mL deionized water and 20mL H 2O 2Stir the ultrasonic dispersion in back, obtain WO 3-Cr 2O 3Or WO 3-NiO solution;
B) under constantly stirring, to above-mentioned WO 3-Cr 2O 3Or WO 3Dropwise add 2mol/L citric acid 5-10mL in the-NiO solution, dropwise add 3mol/L ammoniacal liquor adjusting pH value again and be 3-5; Afterwards mixed solution is placed heating environment, temperature is controlled at 70-100 ℃, and constantly stirs with agitator, obtains WO 3-Cr 2O 3Or WO 3-NiO sol material;
C) painting method that adopts dipping to lift is with WO 3-Cr 2O 3Or WO 3-NiO sol material is coated to the Al that is printed on electrode 2O 3On the earthenware, carry out 150-200 ℃ of drying down, repeat above-mentioned steps 3-6 time;
D) earthenware is put into the sintering furnace sintering, be warmed up to 500 ℃-700 ℃ heat treatment 1-2 hour, cooling back obtains porous film material.
2. the porous film material of employing claim 1 prepares the method for gas sensor, it is characterized in that step is as follows:
To WO 3-Cr 2O 3Porous membrane or WO 3-NiO porous film material is warmed up to 500 ℃-700 ℃ again behind the employing sintering and handled 1-2 hour; To WO 3-Cr 2O 3Porous membrane adopts the mode that is taken out in the air cooling rapidly under this temperature from stove to handle porous membrane; To WO 3-NiO film adopts with 2 ℃ of/minute speed controls and is cooled to the porous membrane that 200 ℃ of modes of slowly cooling off are handled coating; After being welded on the earthenware that obtains on the pedestal, and in pipe, put on the nickel filament heater strip, obtain WO 3-Cr 2O 3Or WO 3-NiO film-type sensor.
CN 201110093965 2011-04-14 2011-04-14 Cr2O3 or NiO porous film material using WO3 as base material and method for manufacturing air-sensitive sensor Expired - Fee Related CN102248737B (en)

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