CN107164837A - A kind of preparation method of ZnO nano fibre air-sensitive material - Google Patents
A kind of preparation method of ZnO nano fibre air-sensitive material Download PDFInfo
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- CN107164837A CN107164837A CN201710373081.3A CN201710373081A CN107164837A CN 107164837 A CN107164837 A CN 107164837A CN 201710373081 A CN201710373081 A CN 201710373081A CN 107164837 A CN107164837 A CN 107164837A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention provides a kind of preparation method of ZnO nano fibre air-sensitive material, first PVA is added in deionized water, is swelled, add sodium alginate, citric acid, glucose, heating and thermal insulation obtains matrix liquid, adds C4H6O4Zn·2H2O、La(NO3)3·6H2O、Ce(NO3)3·6H2Absolute ethyl alcohol is added dropwise in O, heating and thermal insulation while stirring, obtains spinning solution, then electrostatic spinning, will collect gained fiber and be placed in sintering in vacuum tube furnace, and produce.The ZnO nano fibre air-sensitive material of the present invention is to acetone and H2S has higher sensitivity, and response and recovery time are very fast.
Description
Technical field
The invention belongs to gas sensor technology field, and in particular to a kind of preparation side of ZnO nano fibre air-sensitive material
Method.
Background technology
In recent years, during use, transport and production leakage accident often occurs for gas, and can cause and one be
The blast of row, fire, and these gases are largely that tool is poisonous and harmful and inflammable and explosive, and these gases are mainly scientific and technological water
It is flat develop, industrial progress and it is production-scale progressively expand, product category is continuously increased generation, also can
Serious pollution is caused to air, or makes one poisoning etc., these gases have many potential danger, gently then endanger the wealth of the mankind
Production safety, the heavy then personal safety of the harm mankind.Simultaneously with the continuous improvement of living standard, liquefied gas and natural gas oneself through general
Store-through is in daily life.But, fire, the poisoning even event such as blast are caused due to liquefied gas and natural gas leakage
Increasingly increase.Mankind itself's judgement quantitative to toxic and harmful gas is limited, when human body is not felt also
Wait, danger is with regard to oneself through there occurs.It whether there is poisonous and harmful gas in environment accordingly, it would be desirable to detect, this is accomplished by accurate measurement
The equipment and instrument of gas concentration and gaseous species.
ZnO is a kind of broad stopband, direct band gap group Ⅱ-Ⅵ compound semiconductor, and its energy gap is 3.37eV, in room
Under temperature, its exciton binding energy, with performances such as excellent electricity, optics, piezoelectricity and air-sensitives, is widely used up to 60meV
In many key areas.
The content of the invention
The technical problem of solution：It is an object of the invention to provide a kind of preparation method of ZnO nano fibre air-sensitive material,
Gained gas sensitive is to acetone and H2S has higher sensitivity.
Technical scheme：A kind of preparation method of ZnO nano fibre air-sensitive material, comprises the following steps：
Step 1, in parts by weight, by PVA 8-12 parts add in 100 parts of deionized water, be swelled, add sodium alginate 0.5-
1.2 parts, 0.2-0.5 parts of citric acid, 0.1-0.6 parts of glucose, be heated to 80-90 DEG C, be incubated 4-6h, obtain matrix liquid；
Step 2, in parts by weight, by C4H6O4Zn·2H210-20 parts of O, La (NO3)3·6H23-5 parts of O, Ce (NO3)3·
6H21-4 parts of O is added in step 1 gained matrix liquid, is heated to 50-60 DEG C, is incubated 30-40min, anhydrous second is added dropwise while stirring
2-8 parts of alcohol, obtains spinning solution；
Step 3, step 2 gained spinning solution is subjected to electrostatic spinning, collects fiber；
Step 4, step 3 gained fiber is placed in vacuum tube furnace and sintered, produced.
Further, 0.1-0.3 parts of surfactant sodium dodecyl base benzene sulfonic acid sodium salt is additionally added in step 1.
Further, condition is swelled in step 1 for 30-40 DEG C, 12-24h.
Further, mixing speed is 100-200rpm in step 2.
Further, in step 3 voltage of electrostatic spinning be 8-12kV, receive distance be 10-15cm.
Further, in step 4 sintering temperature be 600-650 DEG C, the time be 2-4h.
Beneficial effect：The ZnO nano fibre air-sensitive material of the present invention is to acetone and H2S has higher sensitivity, rings
Should be very fast with recovery time.
Embodiment
Embodiment 1
A kind of preparation method of ZnO nano fibre air-sensitive material, comprises the following steps：
Step 1, in parts by weight, by PVA 8 parts add in 100 parts of deionized water, be swelled, add 0.5 part of sodium alginate, lemon
Lemon acid 0.2 part, 0.1 part of glucose, are heated to 80 DEG C, are incubated 6h, obtain matrix liquid；
Step 2, in parts by weight, by C4H6O4Zn·2H210 parts of O, La (NO3)3·6H23 parts of O, Ce (NO3)3·6H21 part of O
Add in step 1 gained matrix liquid, be heated to 50 DEG C, be incubated 40min, 2 parts of absolute ethyl alcohol is added dropwise while stirring, spinning is obtained
Liquid；
Step 3, step 2 gained spinning solution is subjected to electrostatic spinning, collects fiber；
Step 4, step 3 gained fiber is placed in vacuum tube furnace and sintered, produced.
Wherein, 0.1 part of surfactant sodium dodecyl base benzene sulfonic acid sodium salt is additionally added in step 1, condition is swelled for 30 DEG C, 24h.
Mixing speed is 100rpm in step 2.
In step 3 voltage of electrostatic spinning be 8kV, receive distance be 15cm.
In step 4 sintering temperature be 600 DEG C, the time be 4h.
Gained gas sensitive is in 200-450 DEG C of working range, to the sensitivity of 1000ppm acetone steams at 300 DEG C
Maximum is reached, up to 45 Ra/Rg；In 250-450 DEG C of working range, to 10ppm H2S sensitivity reaches at 400 DEG C
Maximum, up to 13 Ra/Rg.
Embodiment 2
A kind of preparation method of ZnO nano fibre air-sensitive material, comprises the following steps：
Step 1, in parts by weight, by PVA 9 parts add in 100 parts of deionized water, be swelled, add 0.7 part of sodium alginate, lemon
Lemon acid 0.3 part, 0.2 part of glucose, are heated to 85 DEG C, are incubated 6h, obtain matrix liquid；
Step 2, in parts by weight, by C4H6O4Zn·2H213 parts of O, La (NO3)3·6H24 parts of O, Ce (NO3)3·6H22 parts of O
Add in step 1 gained matrix liquid, be heated to 55 DEG C, be incubated 40min, 4 parts of absolute ethyl alcohol is added dropwise while stirring, spinning is obtained
Liquid；
Step 3, step 2 gained spinning solution is subjected to electrostatic spinning, collects fiber；
Step 4, step 3 gained fiber is placed in vacuum tube furnace and sintered, produced.
Wherein, 0.2 part of surfactant sodium dodecyl base benzene sulfonic acid sodium salt is additionally added in step 1, condition is swelled for 35 DEG C, 20h.
Mixing speed is 150rpm in step 2.
In step 3 voltage of electrostatic spinning be 10kV, receive distance be 15cm.
In step 4 sintering temperature be 600 DEG C, the time be 4h.
Gained gas sensitive is in 200-450 DEG C of working range, to the sensitivity of 1000ppm acetone steams at 300 DEG C
Maximum is reached, up to 47 Ra/Rg；In 250-450 DEG C of working range, to 10ppm H2S sensitivity reaches at 400 DEG C
Maximum, up to 12 Ra/Rg.
Embodiment 3
A kind of preparation method of ZnO nano fibre air-sensitive material, comprises the following steps：
Step 1, in parts by weight, by PVA 10 parts add in 100 parts of deionized water, be swelled, add 0.9 part of sodium alginate,
0.4 part of citric acid, 0.3 part of glucose, are heated to 80 DEG C, are incubated 6h, obtain matrix liquid；
Step 2, in parts by weight, by C4H6O4Zn·2H217 parts of O, La (NO3)3·6H24 parts of O, Ce (NO3)3·6H23 parts of O
Add in step 1 gained matrix liquid, be heated to 50 DEG C, be incubated 40min, 2 parts of absolute ethyl alcohol is added dropwise while stirring, spinning is obtained
Liquid；
Step 3, step 2 gained spinning solution is subjected to electrostatic spinning, collects fiber；
Step 4, step 3 gained fiber is placed in vacuum tube furnace and sintered, produced.
Wherein, 0.2 part of surfactant sodium dodecyl base benzene sulfonic acid sodium salt is additionally added in step 1, condition is swelled for 30 DEG C, 24h.
Mixing speed is 100rpm in step 2.
In step 3 voltage of electrostatic spinning be 8kV, receive distance be 15cm.
In step 4 sintering temperature be 600 DEG C, the time be 4h.
Gained gas sensitive is in 200-450 DEG C of working range, to the sensitivity of 1000ppm acetone steams at 300 DEG C
Maximum is reached, up to 42 Ra/Rg；In 250-450 DEG C of working range, to 10ppm H2S sensitivity reaches at 400 DEG C
Maximum, up to 15 Ra/Rg.
Embodiment 4
A kind of preparation method of ZnO nano fibre air-sensitive material, comprises the following steps：
Step 1, in parts by weight, by PVA 12 parts add in 100 parts of deionized water, be swelled, add 1.2 parts of sodium alginate,
0.5 part of citric acid, 0.6 part of glucose, are heated to 90 DEG C, are incubated 4h, obtain matrix liquid；
Step 2, in parts by weight, by C4H6O4Zn·2H220 parts of O, La (NO3)3·6H25 parts of O, Ce (NO3)3·6H24 parts of O
Add in step 1 gained matrix liquid, be heated to 60 DEG C, be incubated 30min, 2 parts of absolute ethyl alcohol is added dropwise while stirring, spinning is obtained
Liquid；
Step 3, step 2 gained spinning solution is subjected to electrostatic spinning, collects fiber；
Step 4, step 3 gained fiber is placed in vacuum tube furnace and sintered, produced.
Wherein, 0.3 part of surfactant sodium dodecyl base benzene sulfonic acid sodium salt is additionally added in step 1, condition is swelled for 40 DEG C, 12h.
Mixing speed is 200rpm in step 2.
In step 3 voltage of electrostatic spinning be 12kV, receive distance be 10cm.
In step 4 sintering temperature be 650 DEG C, the time be 2h.
Gained gas sensitive is in 200-450 DEG C of working range, to the sensitivity of 1000ppm acetone steams at 300 DEG C
Maximum is reached, up to 46 Ra/Rg；In 250-450 DEG C of working range, to 10ppm H2S sensitivity reaches at 400 DEG C
Maximum, up to 17 Ra/Rg.
Claims (6)
1. a kind of preparation method of ZnO nano fibre air-sensitive material, it is characterised in that：Comprise the following steps：
Step 1, in parts by weight, by PVA 8-12 parts add in 100 parts of deionized water, be swelled, add sodium alginate 0.5-
1.2 parts, 0.2-0.5 parts of citric acid, 0.1-0.6 parts of glucose, be heated to 80-90 DEG C, be incubated 4-6h, obtain matrix liquid；
Step 2, in parts by weight, by C4H6O4Zn·2H210-20 parts of O, La (NO3)3·6H23-5 parts of O, Ce (NO3)3·6H2O
1-4 parts add in step 1 gained matrix liquid, are heated to 50-60 DEG C, are incubated 30-40min, and absolute ethyl alcohol 2-8 is added dropwise while stirring
Part, obtain spinning solution；
Step 3, step 2 gained spinning solution is subjected to electrostatic spinning, collects fiber；
Step 4, step 3 gained fiber is placed in vacuum tube furnace and sintered, produced.
2. the preparation method of ZnO nano fibre air-sensitive material according to claim 1, it is characterised in that：Also add in step 1
Enter 0.1-0.3 parts of surfactant sodium dodecyl base benzene sulfonic acid sodium salt.
3. the preparation method of ZnO nano fibre air-sensitive material according to claim 1, it is characterised in that：It is swelled in step 1
Condition is 30-40 DEG C, 12-24h.
4. the preparation method of ZnO nano fibre air-sensitive material according to claim 1, it is characterised in that：Stirred in step 2
Speed is 100-200rpm.
5. the preparation method of ZnO nano fibre air-sensitive material according to claim 1, it is characterised in that：Electrostatic in step 3
The voltage of spinning be 8-12kV, receive distance be 10-15cm.
6. the preparation method of ZnO nano fibre air-sensitive material according to claim 1, it is characterised in that：Sintered in step 4
Temperature is 600-650 DEG C, the time is 2-4h.
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| CN201710373081.3A CN107164837A (en) | 2017-05-24 | 2017-05-24 | A kind of preparation method of ZnO nano fibre air-sensitive material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108771976A (en) * | 2018-07-04 | 2018-11-09 | 南京林业大学 | A method of the antibacterial filtering PM2.5 of tunica fibrosa and degradating organic dye are prepared based on electrostatic spinning |
| CN110498440A (en) * | 2019-07-11 | 2019-11-26 | 江苏大学 | A kind of zinc oxide air-sensitive membrane material, preparation method and applications |
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| JPH07294470A (en) * | 1994-04-28 | 1995-11-10 | Sogo Keibi Hosho Co Ltd | Semiconductor fiber gas sensor |
| CN101266225A (en) * | 2008-04-28 | 2008-09-17 | 吉林大学 | Electric spinning method for preparing high performance ceramic base nanometer fibre gas-sensitive sensor |
| CN102331443A (en) * | 2011-07-13 | 2012-01-25 | 东华大学 | Acetone gas sensor and manufacturing method thereof |
| CN103011257A (en) * | 2013-01-05 | 2013-04-03 | 青岛大学 | Preparation method of P-type zinc oxide micro/nano fibers |
| CN106501456A (en) * | 2016-11-10 | 2017-03-15 | 合肥铭志环境技术有限责任公司 | A kind of have supersensitive composite nano fiber gas sensitive and preparation method thereof |
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2017
- 2017-05-24 CN CN201710373081.3A patent/CN107164837A/en active Pending
Patent Citations (5)
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|---|---|---|---|---|
| JPH07294470A (en) * | 1994-04-28 | 1995-11-10 | Sogo Keibi Hosho Co Ltd | Semiconductor fiber gas sensor |
| CN101266225A (en) * | 2008-04-28 | 2008-09-17 | 吉林大学 | Electric spinning method for preparing high performance ceramic base nanometer fibre gas-sensitive sensor |
| CN102331443A (en) * | 2011-07-13 | 2012-01-25 | 东华大学 | Acetone gas sensor and manufacturing method thereof |
| CN103011257A (en) * | 2013-01-05 | 2013-04-03 | 青岛大学 | Preparation method of P-type zinc oxide micro/nano fibers |
| CN106501456A (en) * | 2016-11-10 | 2017-03-15 | 合肥铭志环境技术有限责任公司 | A kind of have supersensitive composite nano fiber gas sensitive and preparation method thereof |
Non-Patent Citations (2)
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| 万桂新等: "Ce掺杂ZnO纳米纤维的气敏特性研究", 《兰州交通大学学报》 * |
| 牛新书等: "掺杂稀土氧化物的ZnO材料的制备及气敏性能", 《稀土》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108771976A (en) * | 2018-07-04 | 2018-11-09 | 南京林业大学 | A method of the antibacterial filtering PM2.5 of tunica fibrosa and degradating organic dye are prepared based on electrostatic spinning |
| CN110498440A (en) * | 2019-07-11 | 2019-11-26 | 江苏大学 | A kind of zinc oxide air-sensitive membrane material, preparation method and applications |
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Application publication date: 20170915 |