CN103880090A - Preparation method and application of AgFeO2 nanoparticle gas sensitive material - Google Patents
Preparation method and application of AgFeO2 nanoparticle gas sensitive material Download PDFInfo
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- CN103880090A CN103880090A CN201410117120.XA CN201410117120A CN103880090A CN 103880090 A CN103880090 A CN 103880090A CN 201410117120 A CN201410117120 A CN 201410117120A CN 103880090 A CN103880090 A CN 103880090A
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Abstract
The invention provides a preparation method and application of an AgFeO2 nanoparticle gas sensitive material. Compared with the prior art, the method has the advantages that a depth defect is introduced onto the surface of the AgFeO2 material to generate a more effective defect layer by gamma ray radiation, so that the sensitivity of a gas sensor is improved. The gas sensor for ethanol provided by the invention has the advantages of high sensitivity, high selectivity, short response time, short recovery time, high recoverability, simple process and low cost.
Description
Technical field
The invention belongs to preparation method of nano material and radiation chemistry cross-application field, be specifically related to gas sensitive preparation and Application Areas.
Background technology
Along with the development of modernization industry, environmental pollution and weather variation issue have caused the great attention of countries in the world.Obnoxious flavour wherein, not only contaminate environment and affect weather, and have generation blast, fire and make the poisoning danger of people.In order to prevent burst accident, improve living environment quality, ensure the consistence of production process condition, protection of the environments etc., must accomplish effective detection to explosive and toxic gas.Gas sensor, as detecting one of effective way of obnoxious flavour, has been subject to the mankind's extensive concern in recent years.
Particularly in recent years, due to development and the progress of nanosecond science and technology, greatly advanced preparation and the application development of Novel air dependent sensor.Many gas sensors with nanostructure are developed at present.In numerous nano-sensors, be studied SnO the most widely
2, In
2o
3, ZnO, WO
3, Co
3o
4, Fe
2o
3with semiconductor gas sensors such as CuO.
Delafossite type oxide gas sensor is seldom in the news.Delafossite type oxide compound is owing to having the special character such as structure and optics, electricity, and caused scientist's interest widely.AgFeO
2be the one in delafossite type oxide compound, up to the present, not yet have about AgFeO
2the research of gas sensor application.
Gamma rays, owing to having short wavelength and high-energy, is the short-cut method of synthetic and decorative material.It can at room temperature carry out, easy to operate; State to reactant does not limit, and can be solid, liquid or gas, is not subject to the restriction of environment.
Summary of the invention
The object of the present invention is to provide a kind of AgFeO
2the preparation method of nanoparticle gas sensitive, utilizes gamma rays irradiation, and technique is simple, cost is low.
A further object of the invention, provides AgFeO
2the application of the gas sensor that nanoparticle gas sensitive detects as ethanol.
A kind of AgFeO provided by the invention
2the preparation method of nanoparticle gas sensitive, comprises the following steps:
(1) NaOH is dissolved in distilled water, obtains solution A; By AgNO
3and Fe (NO
3)
39H
2o is dissolved in distilled water, and stirring and dissolving obtains solution B;
(2) solution A is dropwise added drop-wise in solution B and constantly and stirs, be added dropwise to complete rear stirring 30-50 minute, obtained suspension liquid is transferred in stainless steel cauldron, sealing, reacting by heating, then, reactor is taken out and naturally cools to room temperature, the product that obtains, through centrifugation, water and washing with alcohol 3-5 time, is dried 12-24 hour at 60 ℃, obtains AgFeO
2material;
(3) with radiation cobalt 60 source gamma rays to by the AgFeO of above-mentioned preparation
2material, carrying out irradiation, obtains AgFeO
2nanoparticle.
Step obtains solution A described in (1), and concentration is 1-4mol/L;
AgNO in solution B described in step (1)
3and Fe (NO
3)
39H
2the amount of substance of O is identical, AgNO in solution B
3concentration is 0.04-0.1mol/L;
In step (2), the volume ratio solution A of solution A used and solution B: solution B=1:5;
Reacting by heating described in step (2), temperature 160-200 ℃, reaction 12-24h;
The metering of the described radiation cobalt 60 source of step (3) gamma rays is 10-1000kGy;
The present invention also provides a kind of AgFeO
2the application of the gas sensor that nanoparticle gas sensitive detects as ethanol.
10-50mg AgFeO prepared by the present invention
2nanoparticle mixes with 0.5-1mL dehydrated alcohol, and ultrasonic 5-10 minute forms even mud.Mud is dripped and be coated on the vitrified pipe with a pair of gold electrode and 4 platinum lines again, make gas sensor, nichrome coil carrys out red-tape operati temperature through vitrified pipe and by changing heater voltage.
Ethanol gas dependent sensor prepared by the present invention, adopts air-sensitive test macro (WS-30A, Zhengzhou Wei Sheng Electronic Technology Co., Ltd) to carry out air-sensitive performance test, and relative humidity is 50-60%.In the time that the concentration of ethanol is 100ppm, its sensitivity reaches 36.8, and test concentrations is all the sensitivity of the gas with various such as 100ppm ethanol, methyl alcohol, acetone, ammoniacal liquor, normal hexane, Tri N-Propyl Amine, benzene.Result shows that this gas sensor is the highest to the detection sensitivity of ethanol, has very strong selectivity.
Testing method: a certain amount of test sample is dripped on the hot-plate in test box, then flashed to gas.The sensitivity of sensor is defined as S=Rg/Ra, and Rg and Ra are respectively that sensor is at test gas and airborne resistance.
The present invention compared with prior art, by gamma rays irradiation, at AgFeO
2material surface is introduced degree of depth defect, produces more effectively defect layer, the sensitivity that improves gas sensor.That the sensor of ethanol provided by the invention has is highly sensitive, selectivity good, the time of response is short, time of recovery is short, restorative good and technique is simple, cost is low advantage.
Accompanying drawing explanation
Fig. 1 is AgFeO prepared by embodiment 1
2x-ray powder diffraction (XRD) figure of nanoparticle, wherein gamma rays dosage used is respectively (a) 0kGy, (b) 100kGy, (c) 500kGy and (d) 1000kGy.
Fig. 2 is AgFeO prepared by embodiment 1
2scanning electronic microscope (SEM) figure of nanoparticle.
Fig. 3 is AgFeO prepared by embodiment 1
2transmission electron microscope (HRTEM) figure of nanoparticle.
Fig. 4 is AgFeO prepared by embodiment 3
2nanoparticle gas sensor, under differing temps, is tested the ethanol sensitivity map to 100ppm: wherein (a) 0kGy; (b) 500kGy.
Fig. 5 is embodiment 4AgFeO
2nanoparticle gas sensor, at 140 ℃, is tested the sensitivity map of the ethanol to different concns.
Fig. 6 is embodiment 5AgFeO
2nanoparticle gas sensor is at 140 ℃, and test concentrations is all the sensitivity map of the gas with various of 100ppm, wherein a) be ethanol, b) for methyl alcohol, c) for acetone, d) for ammoniacal liquor.
Fig. 7 is embodiment 6AgFeO
2nanoparticle gas sensor is at 140 ℃ of optimal working temps, and test concentrations is all the sensitivity map of the gas with various of 100ppm.
Embodiment
Embodiment 1
A kind of AgFeO
2the preparation method of nanoparticle gas sensitive, comprises the following steps:
(1) NaOH of 0.4g is dissolved in the distilled water of 5mL, obtains solution A; By the AgNO of 2mmol
3fe (NO with 2mmol
3)
39H
2o adds in the distilled water of 25mL, obtains solution B;
(2) solution A is dropwise added drop-wise in solution B and constantly and stirs, be added dropwise to complete rear stirring 30 minutes, obtained suspension liquid is transferred in stainless steel cauldron, sealing, at 180 ℃, heating, reacted after 12 hours, reactor is taken out and naturally cools to room temperature, the product obtaining, through the each washing of centrifugation, water and ethanol 3 times, is dried 12 hours at 60 ℃, obtains AgFeO
2material.
(3) be 0-500kGy radiation cobalt 60 source gamma rays to by the AgFeO of above-mentioned preparation with metering
2material, carrying out irradiation, obtains AgFeO
2nanoparticle.
A kind of AgFeO
2the application of the gas sensor that nanoparticle gas sensitive detects as ethanol.
By above-mentioned gained AgFeO
2nanoparticle mixes with several dehydrated alcohols, forms mud.Again mud is coated on the vitrified pipe with a pair of gold electrode and 4 platinum lines.Nichrome coil carrys out red-tape operati temperature through vitrified pipe and by changing heater voltage.Adopt air-sensitive test macro (WS-30A, Zhengzhou Wei Sheng Electronic Technology Co., Ltd) to carry out air-sensitive performance test, relative humidity is 50-60%.
Embodiment 2
The structure of product and morphology characterization
With the Empyrean type X-ray powder diffraction instrument of Dutch PANalytical company to embodiment 1 products therefrom (Cu target, λ=0.15406nm, 0.05 ° of sweep velocity/s) carry out the thing identification of phases, as shown in Figure 1.Contrast JCPDS standard card (21-1081), all diffraction peaks and six side's phase α-AgFeO
2fit like a glove, occur without other impurity peaks, show that the product making is the α-AgFeO of six side's phases
2, gamma rays irradiation does not change the structure of material.With scanning electron microscope and transmission electron microscope to AgFeO
2nanoparticle carries out morphology analysis, and result as shown in Figure 2,3.Show prepared α-AgFeO
2the diameter of nanoparticle is 50-100nm.
Embodiment 3
A kind of AgFeO
2the air-sensitive performance of nanoparticle gas sensor detects.
A certain amount of test sample is dripped on the hot-plate in test box, then flashed to gas.The sensitivity of sensor is defined as S=Rg/Ra, and Rg and Ra are respectively that sensor is at test gas and airborne resistance.
First, under differing temps, the ethanol sensitivity of test to 100ppm, chooses optimal working temp, as shown in Figure 4.As can be seen from Figure 4 the AgFeO, obtaining without gamma rays irradiation
2the optimal working temp of gas sensor is 180 ℃, and through 500kGy gamma rays irradiation AgFeO
2the optimal working temp of gas sensor is 140 ℃.Clearly, AgFeO after gamma rays irradiation
2the working temperature of nanoparticle gas sensor is low, and this application for gas sensor provides more favourable guarantee.
Embodiment 4
A kind of AgFeO
2the ethanol sensitivity air-sensitive performance of nanoparticle gas sensor detects.
At 140 ℃, the ethanol sensitivity of test to different concns, as shown in Figure 5.Result of study shows that the sensitivity of this sensor increases along with the increase of alcohol concn.In the time that the concentration of ethanol is 100ppm, its sensitivity reaches 36.8, and this shows that this sensor has very high sensitivity to ethanol.
Embodiment 5
A kind of AgFeO
2the air-sensitive performance selectivity of nanoparticle gas sensor detects.
At 140 ℃, respectively concentration is all to ethanol, methyl alcohol, the acetone of 100ppm, the sensitivity test of four kinds of gas with various of ammoniacal liquor, result is as shown in Figure 6.As can be seen from Figure 6,, when to this four kinds of gas detection, this gas sensor is the highest to the detection sensitivity of ethanol, is about 36.8, has very strong selectivity.
Embodiment 6
A kind of AgFeO
2the air-sensitive performance selectivity of nanoparticle gas sensor detects.
At 140 ℃, respectively concentration is all to hexanaphthene, the propylamine of 100ppm, the sensitivity test of three kinds of different organic gass of benzene, found that, this gas sensor is very low to the detection sensitivity of normal hexane, Tri N-Propyl Amine, benzene, be about 1.5 left and right, result as shown in Figure 7.As can be seen from Figure 7, this gas sensor is the highest to the detection sensitivity of ethanol, has very strong selectivity.
Claims (8)
1. an AgFeO
2the preparation method of nanoparticle gas sensitive, is characterized in that, described preparation method comprises the following steps:
(1) NaOH is dissolved in distilled water, obtains solution A; By AgNO
3and Fe (NO
3)
39H
2o is dissolved in distilled water, and stirring and dissolving obtains solution B;
(2) solution A is dropwise added drop-wise in solution B and constantly and stirs, be added dropwise to complete rear stirring 30-50 minute, obtained suspension liquid is transferred in stainless steel cauldron, sealing, reacting by heating, then, reactor is taken out and naturally cools to room temperature, the product that obtains, through centrifugation, water and washing with alcohol 3-5 time, is dried 12-24 hour at 60 ℃, obtains AgFeO
2material;
(3) with radiation cobalt 60 source gamma rays to by the AgFeO of above-mentioned preparation
2material, carrying out irradiation, obtains AgFeO
2nanoparticle.
2. preparation method according to claim 1, is characterized in that, step obtains solution A described in (1), and concentration is 1-4m
ol/L.
3. preparation method according to claim 1, is characterized in that, AgNO in solution B described in step (1)
3and Fe (NO
3)
39H
2the amount of substance of O is identical, AgNO in solution B
3concentration is 0.04-0.1mol/L.
4. preparation method according to claim 1, is characterized in that, the volume ratio solution A of solution A used and solution B: solution B=1:5 in step (2).
5. preparation method according to claim 1, is characterized in that, reacting by heating described in step (2), temperature 160-200 ℃, reaction 12-24h.
6. preparation method according to claim 1, is characterized in that, the metering of the described radiation cobalt 60 source of step (3) gamma rays is 10-1000kGy.
7. an AgFeO prepared by claim 1-6 any one
2the application of the gas sensor that nanoparticle gas sensitive detects as ethanol.
8. the application of gas sensor according to claim 7, is characterized in that, the preparation method of described gas sensor is: 10-50mg AgFeO prepared by the present invention
2nanoparticle mixes with 0.5-1mL dehydrated alcohol, and ultrasonic 5-10 minute forms even mud.Mud is dripped and be coated on the vitrified pipe with a pair of gold electrode and 4 platinum lines again, make gas sensor.
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| CN103880090B CN103880090B (en) | 2015-07-22 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109569648A (en) * | 2018-10-25 | 2019-04-05 | 湖北省晴川生态工程技术有限公司 | A kind of method of ferrous acid silver nano material catalysis organic wastewater treatment through persulfate |
| CN110161097A (en) * | 2019-06-02 | 2019-08-23 | 上海纳米技术及应用国家工程研究中心有限公司 | The preparation of the modified tin dioxide nanometer material of di-iron trioxide-silver for gas sensor and product and application |
| CN114956190A (en) * | 2021-12-30 | 2022-08-30 | 昆明理工大学 | Ferrosite type AgFeO with controllable oxygen defect 2+δ Method for producing powder material |
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| CN101289228A (en) * | 2008-06-03 | 2008-10-22 | 浙江理工大学 | Method for preparing porous zinc ferrite nano-rods |
| CN101733049A (en) * | 2008-11-14 | 2010-06-16 | 黑龙江省科学院技术物理研究所 | Method for preparing core-shell structure composite material by Gamma-ray irradiation |
| CN101774646A (en) * | 2009-01-12 | 2010-07-14 | 中国科学院过程工程研究所 | Preparation method of spinel ferrite hollow sphere with core-shell structure |
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2014
- 2014-03-26 CN CN201410117120.XA patent/CN103880090B/en not_active Expired - Fee Related
Patent Citations (3)
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| CN101289228A (en) * | 2008-06-03 | 2008-10-22 | 浙江理工大学 | Method for preparing porous zinc ferrite nano-rods |
| CN101733049A (en) * | 2008-11-14 | 2010-06-16 | 黑龙江省科学院技术物理研究所 | Method for preparing core-shell structure composite material by Gamma-ray irradiation |
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| 牛新书等: ""ZnFe2O4纳米粉体的室温固相合成及其气敏特性研究"", 《功能材料》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109569648A (en) * | 2018-10-25 | 2019-04-05 | 湖北省晴川生态工程技术有限公司 | A kind of method of ferrous acid silver nano material catalysis organic wastewater treatment through persulfate |
| CN109569648B (en) * | 2018-10-25 | 2021-05-18 | 湖北省晴川生态工程技术有限公司 | Method for treating organic wastewater by catalyzing persulfate through silver ferrite nano material |
| CN110161097A (en) * | 2019-06-02 | 2019-08-23 | 上海纳米技术及应用国家工程研究中心有限公司 | The preparation of the modified tin dioxide nanometer material of di-iron trioxide-silver for gas sensor and product and application |
| CN114956190A (en) * | 2021-12-30 | 2022-08-30 | 昆明理工大学 | Ferrosite type AgFeO with controllable oxygen defect 2+δ Method for producing powder material |
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| CN103880090B (en) | 2015-07-22 |
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