CN107894448A - A kind of light of boron doped titanic oxide helps gas sensor and preparation method and application - Google Patents
A kind of light of boron doped titanic oxide helps gas sensor and preparation method and application Download PDFInfo
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- CN107894448A CN107894448A CN201711097068.6A CN201711097068A CN107894448A CN 107894448 A CN107894448 A CN 107894448A CN 201711097068 A CN201711097068 A CN 201711097068A CN 107894448 A CN107894448 A CN 107894448A
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- boron doped
- titanic oxide
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating 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
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
Abstract
The invention discloses a kind of light of boron doped titanic oxide to help gas sensor and preparation method and application, and methods described is to TiO by way of boron-doping2It is modified and is used to preparing light and help gas sensor, this method mild condition is easily operated, the B/TiO of preparation2Gas sensor shows preferable H under action of ultraviolet light2With CO response performance, and good stability and repeatability are shown, help lend some impetus to the practical application that semiconductor light helps gas sensor.
Description
Technical field
The invention belongs to gas sensor technology field, and in particular to a kind of light of boron doped titanic oxide helps gas sensor
And preparation method and application.
Background technology
With industrial expansion, environmental problem is also increasingly severe, therefore to the gas such as poisonous, harmful, inflammable in air
Monitoring ever more important.Gas sensor has been widely used for industrial production, household safe, environment measuring, health care, stone
The fields such as oiling work.Metal oxide semiconductor have high sensitivity, response time are short, cost is relatively low, simple processing, without poison ring
The advantages that guarantor, thus it is most widely used.At present, it is mainly n or the metal oxide of p-type using more gas sensitive, such as：
TiO2, ZnO, SnO2, WO3Deng.But there is also some problems during use：Less stable, selectivity is relatively low, work temperature
Degree is higher, and power consumption is larger, safety problem be present, and service life is not grown, intelligent more low.Therefore need to develop new air-sensitive
Sensor.Because semi-conducting material has light absorbs, photoconductive characteristic in itself, can be sent out under the illumination condition of certain wavelength
The third contact of a total solar or lunar eclipse response produce light induced electron, so use up excite improve Metal Oxide Gas Sensors sensitivity be one brand-new
Thinking.TiO2Not only there is good ultraviolet catalytic activity, and there is good gas-sensitive property for specific gas, therefore
By to TiO2Material is modified, and improves sensitivity, the research of repeatability and stability has certain realistic meaning.
H2As a kind of clean energy resource, there is inflammable and explosive property, it produces, stored, using in the presence of very big safety
Problem；CO is not only inflammable and explosive, and in industry and indoor environment, easily human body is caused greatly to injure.H2It is equal with CO
It is colourless, tasteless gas, therefore to H2It is particularly important with CO monitoring.To TiO by way of element doping2Introduce impurity
Energy level, can effectively it improve to H2, CO air-sensitive response, repeatability and stability.
The content of the invention
For insufficient existing for above-mentioned existing gas sensitive, it is an object of the invention to provide a kind of preparation method it is simple,
The light of gentle, the quick easy boron doped titanic oxide of reaction condition helps the preparation method and application of gas sensor, party's legal system
The high sensitivity of standby gas sensor, light helps air-sensitive performance stable, reproducible, has preferable application prospect.
To achieve these goals, the present invention uses following technical scheme：
A kind of light of boron doped titanic oxide helps the preparation method of gas sensor：Under agitation, by H3BO3Solution adds dropwise
Enter in isopropyl titanate, dried after stirring, resulting material is calcined to obtain B/TiO2Powder, method is then covered by B/ by drop
TiO2Powder is coated in golden interdigital electrode piece surface, and then roasting obtains the light of boron doped titanic oxide and helps gas sensor.
The H3BO3Amount ratio with isopropyl titanate is 1 g: 5-6.5 mL, preferably 1 g: 5.83 mL.
For the stirring condition to stir 8-12 h at room temperature, the drying condition is 90-110 DEG C.
The temperature of the material calcining is 400-600 DEG C.
The present invention is by B/TiO2The light that powder prepares boron doped titanic oxide helps comprising the following steps that for gas sensor：Successively
Golden interdigital electrode piece 20-30min is washed using deionized water, EtOH Sonicate, is dried for standby；Weigh B/TiO2Powder is in medicine bottle
In, and instill ethylene glycol ultrasonic disperse and obtain gas sensitive, the B/TiO2The amount ratio of powder and ethylene glycol is 30mg: 1
ML, then pipette 45-50 μ L gas sensitives using liquid-transfering gun and drop in golden interdigital electrode piece surface, treat its uniform drawout after
70-80 DEG C of drying, finally, golden interdigital electrode piece is placed in Muffle furnace, 1-1.5h is calcined after being warming up to 400-600 DEG C, natural
Taken out after cooling, the light for obtaining boron doped titanic oxide helps gas sensor.
Further, the heating rate is 1 DEG C/min.
Present invention also offers the application that the light of the boron doped titanic oxide helps gas sensor, the gas sensor is in purple
Under outer illumination, room temperature can be to H2, CO show the response of preferable air-sensitive.
The present invention effect and be advantageous in that：With pure TiO2Gas sensor is compared, B/TiO of the invention2Light helps air-sensitive
Element just has the response of more preferable air-sensitive, light helps air-sensitive performance stable, reproducible under ultraviolet light under room temperature condition.
The present invention is by way of element B doping to TiO2It is modified, its preparation method is simple, mild condition, easily operated, especially
To H2Air-sensitive response, the TiO of boron-doping of the present invention2It is more readily available electronics.The present invention helps gas sensor beneficial to actual light
Application and preparation, and the preparation to other gas sensitives also provides new thinking and direction.
Brief description of the drawings
Fig. 1 is TiO prepared by embodiment 12、B/TiO2The XRD spectra of material；
Fig. 2 is TiO prepared by embodiment 12、B/TiO2The DRS spectrograms of material；
Fig. 3 is TiO prepared by embodiment 12、B/TiO2The TEM spectrograms of material；
Fig. 4 is TiO prepared by embodiment 12Gas sensor and B/TiO2Gas sensor is at room temperature to H in nitrogen atmosphere2It is ultraviolet
Light helps air-sensitive response performance to compare；
Fig. 5 is the TiO of the gained of embodiment 12Gas sensor and B/TiO2Gas sensor is at room temperature to CO purple in nitrogen atmosphere
Outer light helps air-sensitive response performance to compare.
Embodiment
To enable the features described above of the present invention and advantage to become apparent, below in conjunction with the drawings and specific embodiments to this
Invention is described in further detail, but the present invention is not limited thereto.
A kind of light of boron doped titanic oxide helps the preparation method of gas sensor
1）Under agitation, by H3BO3Solution is added dropwise in isopropyl titanate, the H3BO3With the dosage of isopropyl titanate
Obtained than for 1 g: 5-6.5 mL, stirring 8-12 h at room temperature after 90-110 DEG C of drying, resulting material in 400-600 DEG C of calcining
B/TiO2Powder；
2）Golden interdigital electrode piece 20-30min is washed using deionized water, EtOH Sonicate successively, is dried for standby；
3）Weigh 30mg B/TiO2Powder instills 1 mL ethylene glycol ultrasonic disperses and obtains gas sensitive in medicine bottle, then makes
50 μ L gas sensitives are pipetted with liquid-transfering gun and drop in golden interdigital electrode piece surface, treat that its uniform drawout is dried after 70-80 DEG C, most
Afterwards, golden interdigital electrode piece is placed in Muffle furnace, is warming up to 400-600 DEG C（Heating rate is 1 DEG C/min）After be calcined 1-1.5h,
Taken out after natural cooling, the light for obtaining boron doped titanic oxide helps gas sensor.
Embodiment 1
TiO2And B/TiO2The preparation of gas sensor
Prepare B/TiO2Material：Take 1.24g H3BO3In 100ml beakers, 50ml deionized water dissolvings are added, are being stirred continuously
Under 7ml isopropyl titanate is added dropwise, stir 12h, 100 DEG C of bakings 12h, 500 DEG C of roasting 1h at room temperature.
Prepare TiO2Material：Take 50ml deionized waters that 7ml titanium is added dropwise in the case where being stirred continuously in 100ml beakers
Isopropyl propionate, 100 DEG C of bakings 12h, 500 DEG C of roasting 1h.
Deionized water, ethanol are first used, each ultrasonic 20min washs golden interdigital electrode piece, is dried for standby.
30mg TiO is weighed respectively2、B/TiO2Powder is respectively dropped into 1ml ethylene glycol in two 1.5ml medicine bottle,
Ultrasonic disperse 1h, pipette 50 μ L using liquid-transfering gun and drop on the electrode slice cleaned up, treat its uniform drawout after 80 DEG C of bakings
It is dry, finally, electrode slice is placed in Muffle furnace and heated up（Heating rate is 1 DEG C/min）1h is calcined to 500 DEG C, treats natural cooling
Further taken out after to room temperature, that is, obtain required gas sensor.
The test of air-sensitive performance
TiO obtained by embodiment 12、B/TiO2The light of gas sensor helps air-sensitive response test in JF02E type air-sensitive test systems
（Kunming Gui Yanjin peaks scientific ＆ technical corporation）Tested with reference to the device of designed, designed.Gas sensor is placed in a stainless steel
The sealed gas chamber of 100ml capacity（On have a quartz window）In tested, by four 365nm ultraviolet fluorescent lamps（4W, Philips
TL/05）Light source is provided.With high-purity N2As background gas, various concentrations under test gas is passed through into air chamber, controls the total flow to be
250ml/min.Response of the gas sensor for various gases is represented with resistance variations, the resistance of gas sensor passes through JF02E
Type air-sensitive test system is tested（Kunming Gui Yanjin peaks scientific ＆ technical corporation）, operating voltage 8.5V.Gas sensor loads air chamber
Afterwards, carry out pre-treatment, be first heated to 200 DEG C, certain time purged in background gas, with remove the water of adsorption and its
His gas, then it is down to room temperature switching gas test.
In this way, the gas sensor of the preparation of embodiment 1 is have rated respectively to H2Air-sensitive performance is helped with CO light, it is tied
Fruit sees Fig. 4-Fig. 5.
It will be seen from figure 1 that the TiO synthesized according to example 12And B/TiO2, through X ' Pert HighScore software analysis
XRD spectra：TiO2A diffraction maximum 30.81 ° (121) be present, the peak is the characteristic peak of brockite, is corresponding to other peaks
The characteristic peak of anatase, illustrate the TiO prepared2It is main to contain a small amount of brockite in Detitanium-ore-type, and B/TiO214.56 °,
There are two B in 27.77 ° (310)2O3Diffraction maximum, and brockite (121) diffraction maximum disappears substantially, illustrates to mix the TiO after B2
Crystal formation changed.
B/TiO is can be seen that from Fig. 2 UV-Vis DRS collection of illustrative plates2Absorbing wavelength slightly towards long wave length direction move
Dynamic, there occurs red shift, big change does not occur for band gap width.
Fig. 3 TEM map analysis result is consistent with XRD analysis result, there is a small amount of B during doping2O3In the presence of.
It can be seen that from Fig. 4 air-sensitive result figures and be passed through H2When, TiO2The resistance of gas sensor rises, H2Show to obtain electronics
Behavior, and B/TiO2The resistance of gas sensor is on a declining curve, H2Electron behavior is shown, response is higher, illustrates to mix B's
TiO2Be advantageous to H2The electron in its adsorption.
From fig. 5, it can be seen that B/TiO2CO response sensitivity is significantly improved, and repeatability and stability are preferable.
This illustrates by way of being adulterated element B to TiO2It is modified, room temperature can be effectively improved under action of ultraviolet light to H2With
CO air-sensitive response, and preparation method is simple and easy, in terms of this can is beneficial to the preparation that actual light helps gas sensor, and
Preparation to other gas sensitives also provides new thinking and direction.
Embodiment 2
A kind of light of boron doped titanic oxide helps the preparation method of gas sensor
1）Under agitation, by H3BO3Solution is added dropwise in isopropyl titanate, the H3BO3With the dosage of isopropyl titanate
Than for 1 g: 6 mL, stirring 12 h at room temperature B/TiO is obtained after 100 DEG C of drying, resulting material in 500 DEG C of calcinings2Powder；
2）Golden interdigital electrode piece 25min is washed using deionized water, EtOH Sonicate successively, is dried for standby；
3）Weigh 30mg B/TiO2Powder instills 1 mL ethylene glycol ultrasonic disperses and obtains gas sensitive in medicine bottle, then makes
50 μ L gas sensitives are pipetted with liquid-transfering gun and drop in golden interdigital electrode piece surface, treat that its uniform drawout is dried after 80 DEG C, finally,
Golden interdigital electrode piece is placed in Muffle furnace, is warming up to 500 DEG C（Heating rate is 1 DEG C/min）After be calcined 1h, after natural cooling
Take out, the light for obtaining boron doped titanic oxide helps gas sensor.
Embodiment 3
A kind of light of boron doped titanic oxide helps the preparation method of gas sensor
1）Under agitation, by H3BO3Solution is added dropwise in isopropyl titanate, the H3BO3With the dosage of isopropyl titanate
Than for 1 g: 5mL, stirring 8 h at room temperature B/TiO is obtained after 110 DEG C of drying, resulting material in 400 DEG C of calcinings2Powder；
2）Golden interdigital electrode piece 20min is washed using deionized water, EtOH Sonicate successively, is dried for standby；
3）Weigh 30mg B/TiO2Powder instills 1 mL ethylene glycol ultrasonic disperses and obtains gas sensitive in medicine bottle, then makes
50 μ L gas sensitives are pipetted with liquid-transfering gun and drop in golden interdigital electrode piece surface, treat that its uniform drawout is dried after 70 DEG C, finally,
Golden interdigital electrode piece is placed in Muffle furnace, is warming up to 400 DEG C（Heating rate is 1 DEG C/min）After be calcined 1.5h, natural cooling
After take out, the light for obtaining boron doped titanic oxide helps gas sensor.
Embodiment 4
A kind of light of boron doped titanic oxide helps the preparation method of gas sensor
1）Under agitation, by H3BO3Solution is added dropwise in isopropyl titanate, the H3BO3With the dosage of isopropyl titanate
Than for 1 g: 6.5 mL, stirring 10 h at room temperature B/TiO is obtained after 90 DEG C of drying, resulting material in 600 DEG C of calcinings2Powder；
2）Golden interdigital electrode piece 30min is washed using deionized water, EtOH Sonicate successively, is dried for standby；
3）Weigh 30mg B/TiO2Powder instills 1 mL ethylene glycol ultrasonic disperses and obtains gas sensitive in medicine bottle, then makes
50 μ L gas sensitives are pipetted with liquid-transfering gun and drop in golden interdigital electrode piece surface, treat that its uniform drawout is dried after 75 DEG C, finally,
Golden interdigital electrode piece is placed in Muffle furnace, is warming up to 600 DEG C（Heating rate is 1 DEG C/min）After be calcined 1.5h, natural cooling
After take out, the light for obtaining boron doped titanic oxide helps gas sensor.
Claims (10)
1. a kind of light of boron doped titanic oxide helps the preparation method of gas sensor, it is characterised in that：Under agitation, will
H3BO3Solution is added dropwise in isopropyl titanate, is dried after stirring, and resulting material is calcined to obtain B/TiO2Powder, Ran Houtong
Cross drop and cover method by B/TiO2Powder is coated in golden interdigital electrode piece surface, and then roasting obtains the light of boron doped titanic oxide and helps gas
Quick element.
2. a kind of light of boron doped titanic oxide according to claim 1 helps the preparation method of gas sensor, its feature exists
In：The H3BO3Amount ratio with isopropyl titanate is 1 g: 5-6.5 mL.
3. a kind of light of boron doped titanic oxide according to claim 2 helps the preparation method of gas sensor, its feature exists
In：The H3BO3Amount ratio with isopropyl titanate is 1 g: 5.83 mL.
4. a kind of light of boron doped titanic oxide according to claim 1 helps the preparation method of gas sensor, its feature exists
In：For the stirring condition to stir 8-12 h at room temperature, the drying condition is 90-110 DEG C.
5. a kind of light of boron doped titanic oxide according to claim 1 helps the preparation method of gas sensor, its feature exists
In：The temperature of the material calcining is 400-600 DEG C.
6. a kind of light of boron doped titanic oxide according to claim 1 helps the preparation method of gas sensor, its feature exists
In：By B/TiO2The light that powder prepares boron doped titanic oxide helps comprising the following steps that for gas sensor：Deionization is used successively
Water, EtOH Sonicate wash golden interdigital electrode piece 20-30min, are dried for standby；Weigh B/TiO2Powder instills second in vessel
Glycol ultrasonic disperse obtains gas sensitive, the B/TiO2The amount ratio of powder and ethylene glycol is 30mg: 1 mL, then using shifting
Liquid rifle pipettes 45-50 μ L gas sensitives and drops in golden interdigital electrode piece surface, treats that its uniform drawout is dried after 70-80 DEG C, most
Afterwards, golden interdigital electrode piece is placed in Muffle furnace, 1-1.5h is calcined after being warming up to 400-600 DEG C, takes out, obtains after natural cooling
The light of boron doped titanic oxide helps gas sensor.
7. a kind of light of boron doped titanic oxide according to claim 6 helps the preparation method of gas sensor, its feature exists
In：The heating rate is 1 DEG C/min.
8. the light such as the boron doped titanic oxide that any preparation methods of claim 1-7 obtain helps gas sensor.
9. the light such as the boron doped titanic oxide that any preparation methods of claim 1-7 obtain helps the application of gas sensor, it is special
Sign is：It is used under room temperature and ultraviolet light conditions produce particular volume air-sensitive response.
10. the light of boron doped titanic oxide according to claim 9 helps the application of gas sensor, it is characterised in that：It is described
Specific gas be H2Or CO.
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| CN108452788A (en) * | 2018-05-09 | 2018-08-28 | 同济大学 | The preparation method and application of interstitial boron doped titanium dioxide photocatalytic material |
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| CN109187664A (en) * | 2018-09-20 | 2019-01-11 | 电子科技大学 | Enhanced self energizing gas sensor of a kind of external force trigger-type response and preparation method thereof |
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