CN103529080A - Preparation method of film-type gas sensor - Google Patents
Preparation method of film-type gas sensor Download PDFInfo
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- CN103529080A CN103529080A CN201310488778.7A CN201310488778A CN103529080A CN 103529080 A CN103529080 A CN 103529080A CN 201310488778 A CN201310488778 A CN 201310488778A CN 103529080 A CN103529080 A CN 103529080A
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Abstract
The invention provides a preparation method of a film-type gas sensor, which comprises the following steps: (1) preparing an iron nitrate/nickel nitrate mixed solution according to the stoichiometric proportion of NiFe2O4; (2) completely precipitating Fe<3+> and Ni<2+> by using stronger ammonia water as a precipitating agent; (3) transferring the mixed solution into a reaction kettle, and keeping the temperature at 220 DEG C for 6-10 hours to generate NiFe2O4 nano powder; (4) washing the obtained powder with deionized water to a neutral state, adding a right amount of PAA (polyacrylic acid), and stirring at 70 DEG C for 1 hour to generate NiFe2O4/PAA magnetic nano composite powder; (5) preparing the magnetic nano composite powder into a suspension, dripping on an interdigital electrode substrate, and drying under the action of an alternating magnetic field; (6) putting the dried interdigital electrode in a resistance furnace, keeping at the temperature of 200 DEG C for 1 hour, and keeping at the temperature of 400-600 DEG C for 1 hour; and (7) repeating the step (5) and the step (6) 4-10 times to obtain the macroporous-structure film-type gas sensor. The method can obtain the low-temperature high-sensitivity macroporous film gas sensor by utilizing the alternating magnetic field.
Description
Technical field
The preparation method who the present invention relates to a kind of thin film type gas-sensitive element, belongs to sensor technical field.
Background technology
Gas sensor is identification gaseous species the device that is changed into electric signal, is the ideal probe of gasometry or half-quantitative detection, leakage alarm, control.The shortcoming such as at present,, although thick film firing type semi-conductor electricity resistive gas sensor is widely used, it exists, and working temperature is high, poor selectivity, serviceable life are short.Along with the continuous progress of science and technology, gas sensor is also towards trend development microminiaturized, integrated, multifunction.In addition thin-film material surface is long-pending very large with the ratio of volume, has significant surface effect, so the filming of gas sensitive has become the developing direction of gas sensor.Because gas is mainly, at material surface, absorption and desorption occur, the air-sensitive performance of air-sensitive film and nano particle and membrane structure have much relations, so the contact area of increase and gas to be measured is the key that determines air-sensitive film air-sensitive performance.
Except dense film, also there is the film of certain factor of porosity, this class film is divided into two classes substantially.The one, the particle of film forming itself has certain factor of porosity, forms through hole to a certain degree after film forming in whole film; Another kind is by the mutual lapping of regular particle with certain length-diameter ratio, makes the film forming have certain factor of porosity.These two kinds of films and traditional film have had fundamental difference, can increase in theory the contact area with gas to be measured, improve sensitivity.But unsatisfactory in practical application, because the concentration of gas to be measured is generally all less, formed partial pressure is also lower, seems that power is limited in the process of permeating in film; The factor of porosity of film itself is limited simultaneously, and the infiltration of gas to be measured is existed to larger resistance.Gas to be measured permeates the top layer that is confined to equally film in film.Want to change this situation, the film that obtains the patterned array structure of macroporsity is crucial.
Adopt at present magnetic nano-particle to prepare the approach that magnetic ordered nano-structure is a kind of patterned array structure of the acquisition macroporsity with good prospect.There are in this respect imprint lithography and self-assembly method.Based on imprint lithography, obtain ordered nano-structure and obtained good achievement and practical, but the technological process of expensive equipment, complexity and lower resolution are its bottlenecks further developing of restriction.Utilize various self-assembling techniques to obtain the extensive concern that ordered nano-structure has been subject to various countries researchists.Studying many is template-mediated construction from part and evaporating solvent construction from part.Template can effectively be got rid of the agglomeration that the magnetic interaction of magnetic material self causes, but how to utilize with design template, is the difficult point of research always, and template is commonly used to prepare magnetic Nano one dimension oldered array structure.In evaporating solvent construction from part, interparticle repulsion and irreversible cohesion should be within limits, but magnetic Nano structured material is often because the interaction of self magnetic dipole produces reunion, be difficult to obtain stable ordered nano magnetic texure material by the method for chemosynthesis, dull sequential holes structure is also barely satisfactory aspect the magnetic property of adjusting material simultaneously.The method that therefore, can effectively obtain magnetic nano-particle array structure becomes the key of preparation macroporsity air-sensitive film sensor.
Summary of the invention
The object of this invention is to provide a kind of preparation method that can meet the demand, highly sensitive thin film type gas-sensitive element.Its technical scheme is:
A preparation method for thin film type gas-sensitive element, is characterized in that adopting following steps: (1) is according to NiFe
2o
4stoichiometric proportion, the mixed solution of preparation ferric nitrate and nickel nitrate; (2) adopting strong aqua is precipitation agent, dropwise joins in mixed solution, until mixed solution pH value is 11-12, by Fe
3+and Ni
2+precipitate completely; (3) mixed solution is moved into polytetrafluoroethyllining lining reactor, at 220 ℃, be incubated 6-10 hour, generate NiFe
2o
4nano-powder; (4) gained powder is used after 1M salt acid soak, then added heat abstraction HCl; Then extremely neutral with deionized water washing residue, then the NiFe that adds step (3) to obtain
2o
4the PAA of nano-powder quality 10-40%, 70 ℃ are stirred 1 hour, generate NiFe
2o
4/ PAA magnetic nano composite powder, then clean 2-3 time with absolute ethyl alcohol; (5) magnetic nano composite powder after cleaning is made to mass concentration and be not more than 1% suspending liquid, drop on interdigital electrode substrate, dry under the effect of the alternating magnetic field that is 0.05-0.2T at magnetic induction density; (6) dried interdigital electrode is put into resistance furnace, first 200 ℃ are incubated one hour, then are incubated one hour at 400-600 ℃; (7) repeatedly carry out step (5) and step (6) 4-10 time, obtain the thin film type gas-sensitive element of macroporous structure.
The preparation method of described a kind of thin film type gas-sensitive element, in step (5), the modes of emplacement of interdigital electrode substrate is parallel to magnetic line of force direction, and action of alternating magnetic field is to drop bone dry.
The preparation method of described a kind of thin film type gas-sensitive element, in step (5), the modes of emplacement of interdigital electrode substrate is perpendicular to magnetic line of force direction, and action of alternating magnetic field is to drop bone dry.
The preparation method of described a kind of thin film type gas-sensitive element, in step (7), a step of every repetition (5), interdigital electrode substrate will turn 90 ° at substrate place plane internal rotation.
Compared with prior art, its advantage is in the present invention:
1. alternating magnetic field is introduced to the implementation procedure of the pattern structure of magnetic nano-particle, utilized the self reinforcement effect of the AC magnetic field magnetic line of force, make in the situation that less magnetic field intensity obtains good effect.
2. utilize the alternating magnetic field mode of action flexibly, the different pattern structure of realizing in colloid solidification process, and obtain different pattern structures by controlling the magnetic line of force, thus obtain the macropore film gas sensor of various structure.
Accompanying drawing explanation
Fig. 1 is that interdigital electrode substrate parallel of the present invention is in the array structure of the individual layer air-sensitive film of magnetic line of force direction formation.
Fig. 2 is that interdigital electrode substrate of the present invention is perpendicular to the array structure of the individual layer air-sensitive film of magnetic line of force direction formation.
Embodiment
Embodiment 1, and concrete steps are:
(1) according to NiFe
2o
4stoichiometric proportion, the mixed solution of preparation ferric nitrate and nickel nitrate, concentration is that 0.005M(is with Ni
2+concentration calculate);
(2) adopting strong aqua is precipitation agent, dropwise joins in mixed solution, until pH is 11, by Fe
3+and Ni
2+precipitate completely;
(3) mixed solution is moved into polytetrafluoroethyllining lining reactor, at 220 ℃, be incubated 6 hours, generate NiFe
2o
4nano-powder;
(4) gained powder is used after 1M salt acid soak, added heat abstraction HCl; Then extremely neutral with deionized water washing residue, then the NiFe that adds step (3) to obtain
2o
4the PAA of nano-powder quality 10%, 70 ℃ are stirred 1 hour, generate NiFe
2o
4/ PAA magnetic nano composite powder, then clean 2 times with absolute ethyl alcohol, remove not compound PAA;
(5) magnetic nano composite powder after cleaning being made to mass concentration is 0.5% suspending liquid, drops on interdigital electrode substrate, and dry under the effect of the alternating magnetic field that is 0.05T at magnetic induction density, wherein interdigital electrode substrate parallel is in the magnetic line of force;
(6) dried interdigital electrode is put into resistance furnace, heating rate is 2 ℃/min to 200 ℃, is rapidly heated to 400 ℃ after being incubated one hour again, is incubated one hour;
(7) repeatedly carry out step (5) and step (6) 4 times, every repetition once, interdigital electrode substrate all turns 90 ° at substrate place plane internal rotation, finally obtains the thin film type gas-sensitive element of macroporous structure.
Object of the present invention is tested to the gas sensing property of gas sensor to acetone gas at WS-30A Testing system of gas-sensor built, test voltage Vc=0,2,4,5V, gas concentration is 200ppm.Test findings shows: its sensitivity is respectively 1.7,7.8,5.4,4.3, shows that this thin film type gas-sensitive element has good susceptibility at low temperatures.
Embodiment 2, and its concrete steps are:
(1) according to NiFe
2o
4stoichiometric proportion, the mixed solution of preparation ferric nitrate and nickel nitrate, concentration is that 0.005M(is with Ni
2+concentration calculate);
(2) adopting strong aqua is precipitation agent, dropwise joins in mixed solution, until pH is 12, by Fe
3+and Ni
2+precipitate completely;
(3) mixed solution is moved into polytetrafluoroethyllining lining reactor, at 220 ℃, be incubated 10 hours, generate NiFe
2o
4nano-powder;
(4) gained powder is used after 1M salt acid soak, added heat abstraction HCl; Then extremely neutral with deionized water washing residue, then the NiFe that adds step (3) to obtain
2o
4the PAA of nano-powder quality 30%, stirs 1 hour at 70 ℃, generates NiFe
2o
4/ PAA magnetic nano composite powder; With absolute ethyl alcohol, clean 3 times again, remove not compound PAA;
(5) magnetic nano composite powder after cleaning being made to mass concentration is 1% suspending liquid, drops on interdigital electrode substrate, and dry under the effect of the alternating magnetic field that is 0.2T at magnetic induction density, wherein interdigital electrode substrate is perpendicular to the magnetic line of force;
(6) dried interdigital electrode is put into resistance furnace, heating rate is 2 ℃/min to 200 ℃, is rapidly heated to 600 ℃ after being incubated one hour, is incubated one hour;
(7) repeatedly carry out step (5) and step (6) 10 times, every repetition once, interdigital electrode substrate all turns 90 ° at substrate place plane internal rotation, finally obtains the thin film type gas-sensitive element of macroporous structure.
Object of the present invention is tested to the gas sensing property of gas sensor to acetone gas at WS-30A Testing system of gas-sensor built, test voltage Vc=0,2,4,5V, gas concentration is 200ppm.Test findings shows: its sensitivity is respectively 1.7,7.8,5.4,4.3, shows that this thin film type gas-sensitive element has good susceptibility at low temperatures.
Embodiment 3, and its concrete steps are:
(1) according to NiFe
2o
4stoichiometric proportion, the mixed solution of preparation ferric nitrate and nickel nitrate, concentration is that 0.005M(is with Ni
2+concentration calculate);
(2) adopting strong aqua is precipitation agent, dropwise joins in mixed solution, until pH is 11, by Fe
3+and Ni
2+precipitate completely;
(3) mixed solution is moved into polytetrafluoroethyllining lining reactor, at 220 ℃, be incubated 8 hours, generate NiFe
2o
4nano-powder;
(4) gained powder is used after 1M salt acid soak, added heat abstraction HCl; Then extremely neutral with deionized water washing residue, then the NiFe that adds step (3) to obtain
2o
4the PAA of nano-powder quality 20%, 70 ℃ are stirred 1 hour, generate NiFe
2o
4/ PAA magnetic nano composite powder, then clean 3 times with absolute ethyl alcohol, remove not compound PAA;
(5) magnetic nano composite powder after cleaning being made to mass concentration is 1% suspending liquid, drops on interdigital electrode substrate, and dry under the effect of the alternating magnetic field that is 0.15T at magnetic induction density, wherein interdigital electrode substrate is perpendicular to the magnetic line of force;
(6) dried interdigital electrode is put into resistance furnace, heating rate is 2 ℃/min to 200 ℃, is rapidly heated to 500 ℃ after being incubated one hour, is incubated one hour;
(7) repeatedly carry out step (5) and step (6) 6 times, every repetition once, every repetition once, interdigital electrode substrate all turns 90 ° at substrate place plane internal rotation, finally obtains the thin film type gas-sensitive element of macroporous structure.
Object of the present invention is tested to the gas sensing property of gas sensor to acetone gas at WS-30A Testing system of gas-sensor built, test voltage Vc=0,2,4,5V, gas concentration is 200ppm.Test findings shows: its sensitivity is respectively 1.7,7.8,5.4,4.3, shows that this thin film type gas-sensitive element has good susceptibility at low temperatures.
Embodiment 4, and its concrete steps are:
(1) according to NiFe
2o
4stoichiometric proportion, the mixed solution of preparation ferric nitrate and nickel nitrate, concentration is that 0.005M(is with Ni
2+concentration calculate);
(2) adopting strong aqua is precipitation agent, dropwise joins in mixed solution, until pH is 12, by Fe
3+and Ni
2+precipitate completely;
(3) mixed solution is moved into polytetrafluoroethyllining lining reactor, at 220 ℃, be incubated 8 hours, generate NiFe
2o
4nano-powder;
(4) gained powder is used after 1M salt acid soak, added heat abstraction HCl; Then extremely neutral with deionized water washing residue, then the NiFe that adds step (3) to obtain
2o
4the PAA of nano-powder quality 10%, 70 ℃ are stirred 1 hour, generate NiFe
2o
4/ PAA magnetic nano composite powder, then clean 3 times with absolute ethyl alcohol, remove not compound PAA;
(5) magnetic nano composite powder after cleaning being made to mass concentration is 1% suspending liquid, drops on interdigital electrode substrate, and dry under the effect of the alternating magnetic field that is 0.2T at magnetic induction density, wherein interdigital electrode substrate parallel is in the magnetic line of force;
(6) dried interdigital electrode is put into resistance furnace, heating rate is 2 ℃/min to 200 ℃, is rapidly heated to 600 ℃ after being incubated one hour again, is incubated one hour;
(7) repeatedly carry out step (5) and step (6) 8 times, every repetition once, interdigital electrode substrate all turns 90 ° at substrate place plane internal rotation, finally obtains the thin film type gas-sensitive element of macroporous structure.
Object of the present invention is tested to the gas sensing property of gas sensor to acetone gas at WS-30A Testing system of gas-sensor built, test voltage Vc=0,2,4,5V, gas concentration is 200ppm.Test findings shows: its sensitivity is respectively 1.7,7.8,5.4,4.3, shows that this thin film type gas-sensitive element has good susceptibility at low temperatures.
Claims (4)
1. a preparation method for thin film type gas-sensitive element, is characterized in that adopting following steps: (1) is according to NiFe
2o
4stoichiometric proportion, the mixed solution of preparation ferric nitrate and nickel nitrate; (2) adopting strong aqua is precipitation agent, dropwise joins in mixed solution, until mixed solution pH value is 11-12, by Fe
3+and Ni
2+precipitate completely; (3) mixed solution is moved into polytetrafluoroethyllining lining reactor, at 220 ℃, be incubated 6-10 hour, generate NiFe
2o
4nano-powder; (4) gained powder is used after 1M salt acid soak, then added heat abstraction HCl; Then extremely neutral with deionized water washing residue, then the NiFe that adds step (3) to obtain
2o
4the PAA of nano-powder quality 10-40%, stirs 1 hour at 70 ℃, generates NiFe
2o
4/ PAA magnetic nano composite powder, then clean 2-3 time with absolute ethyl alcohol; (5) magnetic nano composite powder after cleaning is made to mass concentration and be not more than 1% suspending liquid, drop on interdigital electrode substrate, dry under the effect of the alternating magnetic field that is 0.05-0.2T at magnetic induction density; (6) dried interdigital electrode is put into resistance furnace, first 200 ℃ are incubated one hour, then are incubated one hour at 400-600 ℃; (7) repeatedly carry out step (5) and step (6) 4-10 time, obtain the thin film type gas-sensitive element of macroporous structure.
2. the preparation method of a kind of thin film type gas-sensitive element as claimed in claim 1, is characterized in that: in step (5), the modes of emplacement of interdigital electrode substrate is parallel to magnetic line of force direction, and action of alternating magnetic field is to drop bone dry.
3. the preparation method of a kind of thin film type gas-sensitive element as claimed in claim 1, is characterized in that: in step (5), the modes of emplacement of interdigital electrode substrate is perpendicular to magnetic line of force direction, and action of alternating magnetic field is to drop bone dry.
4. the preparation method of a kind of thin film type gas-sensitive element as claimed in claim 1, is characterized in that: in step (7), and a step of every repetition (5), interdigital electrode substrate will turn 90 ° at substrate place plane internal rotation.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105702475A (en) * | 2016-02-03 | 2016-06-22 | 三峡大学 | Super capacitor negative electrode material nickel ferrite and preparation method therefor |
| CN109900757A (en) * | 2016-05-19 | 2019-06-18 | 广东海洋大学 | A kind of aptamer sensor and preparation method thereof |
| CN111175349A (en) * | 2020-01-03 | 2020-05-19 | 上海交通大学 | Method for controllably constructing high-performance gas-sensitive/humidity-sensitive sensor |
| CN114397331A (en) * | 2021-12-28 | 2022-04-26 | 郑州美克盛世电子科技有限公司 | Preparation method of gas-sensitive material for high-response and high-selectivity acetone sensor |
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| CN1743387A (en) * | 2005-04-07 | 2006-03-08 | 东华大学 | Method for preparing carbon nanotube magnetic compositematerial modified by iron oxide red |
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2013
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105702475A (en) * | 2016-02-03 | 2016-06-22 | 三峡大学 | Super capacitor negative electrode material nickel ferrite and preparation method therefor |
| CN105702475B (en) * | 2016-02-03 | 2018-04-10 | 三峡大学 | A kind of super capacitor anode material nickel ferrite based magnetic loaded and preparation method thereof |
| CN109900757A (en) * | 2016-05-19 | 2019-06-18 | 广东海洋大学 | A kind of aptamer sensor and preparation method thereof |
| CN111175349A (en) * | 2020-01-03 | 2020-05-19 | 上海交通大学 | Method for controllably constructing high-performance gas-sensitive/humidity-sensitive sensor |
| CN114397331A (en) * | 2021-12-28 | 2022-04-26 | 郑州美克盛世电子科技有限公司 | Preparation method of gas-sensitive material for high-response and high-selectivity acetone sensor |
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