CN106040016A - Preparation method of reusable organic gas detection film - Google Patents
Preparation method of reusable organic gas detection film Download PDFInfo
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- CN106040016A CN106040016A CN201610375172.6A CN201610375172A CN106040016A CN 106040016 A CN106040016 A CN 106040016A CN 201610375172 A CN201610375172 A CN 201610375172A CN 106040016 A CN106040016 A CN 106040016A
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- 238000001514 detection method Methods 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 230000008021 deposition Effects 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims description 31
- 239000010408 film Substances 0.000 claims description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 239000010409 thin film Substances 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- 239000002033 PVDF binder Substances 0.000 claims description 4
- 150000001768 cations Chemical class 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 239000004745 nonwoven fabric Substances 0.000 claims description 4
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 4
- 238000004062 sedimentation Methods 0.000 claims description 4
- 239000011592 zinc chloride Substances 0.000 claims description 4
- 125000000129 anionic group Chemical group 0.000 claims description 3
- 239000001117 sulphuric acid Substances 0.000 claims description 3
- 235000011149 sulphuric acid Nutrition 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical group Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- MEYZYGMYMLNUHJ-UHFFFAOYSA-N tunicamycin Natural products CC(C)CCCCCCCCCC=CC(=O)NC1C(O)C(O)C(CC(O)C2OC(C(O)C2O)N3C=CC(=O)NC3=O)OC1OC4OC(CO)C(O)C(O)C4NC(=O)C MEYZYGMYMLNUHJ-UHFFFAOYSA-N 0.000 claims description 2
- 241000521257 Hydrops Species 0.000 claims 1
- 206010030113 Oedema Diseases 0.000 claims 1
- -1 moon Ion Chemical class 0.000 claims 1
- 238000000151 deposition Methods 0.000 abstract description 28
- 238000000034 method Methods 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 4
- 230000004044 response Effects 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 239000012855 volatile organic compound Substances 0.000 description 8
- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 description 7
- 229960003351 prussian blue Drugs 0.000 description 7
- 239000013225 prussian blue Substances 0.000 description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 4
- 238000002386 leaching Methods 0.000 description 4
- 238000010408 sweeping Methods 0.000 description 4
- 238000004040 coloring Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 238000001338 self-assembly Methods 0.000 description 3
- 241001062009 Indigofera Species 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 206010010071 Coma Diseases 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000133 brain stem Anatomy 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000036461 convulsion Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/022—Metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0069—Inorganic membrane manufacture by deposition from the liquid phase, e.g. electrochemical deposition
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
- B01D69/105—Support pretreatment
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/783—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour for analysing gases
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N2021/775—Indicator and selective membrane
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Biochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Plasma & Fusion (AREA)
- Electrochemistry (AREA)
- Manufacturing & Machinery (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention relates to a preparation method of a reusable organic gas detection film. The preparation method comprises the specific following steps that deposition solutions A and B are prepared; film deposition is conducted on a supporting body, and the supporting body is immersed in the deposition solution A and is taken out after a period of time; then, the supporting body is immersed into deionized water and is taken out after a period of time; the supporting body is immersed into the deposition solution B and is taken out after a period of time; finally, the supporting body is immersed into deionized water and is taken out after a period of time to complete deposition of a layer of film. The prepared film can be used for detecting multiple organic volatile substances, is high in response speed and produces different color responses to different types of volatile substances, and the color of the film in the environment containing no volatile substance can be rapidly recovered. The film preparation method is simple in process and low in cost and has a good large-scale production prospect.
Description
Technical field
The present invention relates to the preparation method of the organic gas detection thin film of a kind of repeatable utilization.Prepared thin film is permissible
It is used for detecting multiple organic volatile such as ethanol, acetone, N-N-dimethylformamide etc., detects speed, have the most of the same race
Machine volatile matter has different colours to respond, and thin film color can be recovered rapidly under without organic volatile environment.
Background technology
Since 18 beginnings of the century, Prussian blue since Germany is found that, the Prussian blue similar thing also thing followed
Flourish growth is got up, and its various character are widely studied by people institute.And some transition in some Prussian blue similar thing
Metal ion is owing to the change of coordination environment is it is possible that metachromatism.Along with the development of science and technology, people are more and more heavier
Green and health depending on living environment.And wherein human body can be caused harm greatly by volatile organic matter (VOCs), by
Gradually having obtained everybody concern, in life and production, the content of VOCs also has the clear and definite regulation upper limit.
The harm of volatile organic matter (VOCs) is it is obvious that when in room, VOC concentration exceedes finite concentration, in the short time
Interior people feel headache, Nausea and vomiting, limbs fatigue;Can twitch time serious, go into a coma, hypomnesis.The liver of VOC harm people
Dirty, kidney, brain and nervous system.In room, VOC pollutes and has caused various countries to pay attention to.VOC method of testing is generally divided into two kinds: one
Planting is the PID detection method quickly going out data, and one is gas chromatography.Two kinds of method instruments are costly.And operate and need
Want professional.Therefore, develop a kind of detection material easy and simple to handle, cheap, reusable and there is great reality
Border meaning and wide application prospect.
Summary of the invention
It is an object of the invention to overcome the defect of prior art, it is provided that the gas organism detection of a kind of repeatable utilization is thin
The method of film.The VOC's such as the method simplicity is controlled, it is adaptable to the acetone produced in various commercial production and interior decoration, methanol
Detection.With large batch of, this film can be prepared, there is good large-scale production prospect.
The technical scheme is that the preparation method of the organic gas detection thin film of a kind of repeatable utilization, it is concrete
Step is as follows:
Step 1: deposition liquid A, the preparation of B;Anionic donor is deposited liquid A with acid solution mixed preparing, cation is supplied
Body deposits liquid B with acid solution mixed preparing;Wherein acid used by deposition liquid A and deposition liquid B is identical, and has identical concentration;Institute
Stating anionic donor is K4Fe(CN)6、K3Fe(CN)6Or K3[Co(CN)6One in];Described cation donor is FeCl3、
ZnCl2Or CoCl2In one;Described acid is the one in hydrochloric acid, sulphuric acid or nitric acid;
Step 2: deposit film on supporter;Supporter is submerged in deposition liquid A, takes out after a period of time;To support again
Body is submerged in deionized water, takes out after a period of time;Then supporter is submerged in deposition liquid B, takes out after a period of time;
Finally again supporter is submerged in deionized water, takes out after a period of time, complete the deposition of a tunic;
Step 3: repeat step 2, deposits and is naturally dried by prepared thin film after terminating or dry, obtain repeatable utilization
Organic gas detection thin film.
In preferred deposition liquid A and deposition liquid B, the concentration of zwitterion is 0.001-0.1M;The concentration of acid is 0.01-
0.5M。
The most above-mentioned supporter is the one in aluminium oxide ceramics, PVDF non-woven fabrics or ITO electro-conductive glass.
In preferred steps 2, ambient temperature (being also deposition liquid A and the temperature of deposition liquid B) controls at 15-35 DEG C;At deposition liquid
In A and deposition liquid B, sedimentation time is 1-10min;The submergence deionized time is 10-60s.
According to the requirement of prepared film, the number of times being typically repeated step 2 is 50-200 time.
Beneficial effect:
The present invention is preparation technology based on the Prussian blue similar thing modified membrane of LBL self-assembly.Utilize Prussian blue similar
Active force between thing and supporter for combining, can on perforated substrate on directly deposition last layer Prussian blue similar
Thing.Owing to utilizing the reaction between zwitterion to synthesize Prussian blue similar thing, electrostatic force can be relied on, by controlling
The number of times of cycle alternation dipping controls thickness.If film is the thinnest will not see obvious color changeable effect, film is the thickest will postpone
Coloring Time.Simultaneously because it is deposited as, adsorption process, sedimentation time and ambient temperature be upper to deposition, general on supporter
Shandong scholar's indigo plant thickness has impact.If film is the thinnest will not see obvious color changeable effect, film is the thickest will postpone Coloring Time.General
Shandong scholar's indigo plant thickness increases along with the increase of frequency of depositing, sedimentation time and ambient temperature.The inventive method is simple, economy also
And go for the production of high-volume film.
Accompanying drawing explanation
Fig. 1 is that at 25 DEG C, LBL self-assembly number of times is the surface sweeping electricity of the organic gas detection thin film of the repeatable utilization of 100
The phenogram of mirror (SEM).
Fig. 2 is that at 15 DEG C, LBL self-assembly number of times is the surface sweeping electricity of the organic gas detection thin film of the repeatable utilization of 200
The phenogram of mirror (SEM).
Detailed description of the invention
Embodiment 1
1) K of same concentrations is prepared3Co(CN)6Aqueous hydrochloric acid solution and CoCl2Aqueous hydrochloric acid solution, K3Co(CN)6With
CoCl2The concentration of solution is 0.01M, and the concentration of hydrochloric acid is 0.1M, PVDF non-woven fabrics is cut into sizeable shape as propping up
Support body;
2) ambient temperature controls to be submerged into by supporter in deposition liquid A at 25 DEG C to take out after 5min;Again by supporter submergence
Enter in deionized water and take out after 10s;Then supporter is submerged in deposition liquid B and takes out after 5min;Last again by supporter leaching
Submerge and deionized water takes out after 10s.More than operation repeats 100 times.The film prepared is dried.Prepared repeatable utilization
The phenogram of surface sweeping Electronic Speculum (SEM) of organic gas detection thin film as it is shown in figure 1, can be seen that from figure membrane granule size is equal
Even, film growth is finer and close.
Embodiment 2
1) K of same concentrations is prepared3Fe(CN)6Aqueous solution of nitric acid and CoCl2Aqueous solution of nitric acid, K3Fe(CN)6With
CoCl2The concentration of solution is 0.05M, and the concentration of nitric acid is 0.01M, by ITO electro-conductive glass supporter respectively with acetone, ethanol and
Deionized water ultrasonic cleaning ten minutes.
2) ambient temperature controls to be submerged into by supporter in deposition liquid A at 25 DEG C to take out after 10min;Again by supporter submergence
Enter in deionized water and take out after 10s;Then supporter is submerged in deposition liquid B and takes out after 10min;Last again by supporter leaching
Submerge and deionized water takes out after 10s.More than operation repeats 80 times.The film prepared is dried.
Embodiment 3
1) K of same concentrations is prepared3Co(CN)6Aqueous sulfuric acid and ZnCl2Aqueous sulfuric acid, K3Co(CN)6With
ZnCl2The concentration of solution is 0.1M, and the concentration of sulphuric acid is 0.5M, by ITO electro-conductive glass supporter respectively with acetone, and ethanol and going
Ionized water ultrasonic cleaning ten minutes.
2) ambient temperature controls to be submerged into by supporter in deposition liquid A at 35 DEG C to take out after 1min;Again by supporter submergence
Enter in deionized water and take out after 30s;Then supporter is submerged in deposition liquid B and takes out after 1min;Last again by supporter leaching
Submerge and deionized water takes out after 30s.More than operation repeats 50 times.The film prepared is dried.
Embodiment 4
1) K of same concentrations is prepared3Co(CN)6Aqueous hydrochloric acid solution and FeCl3Aqueous hydrochloric acid solution, K3Co(CN)6With
FeCl3The concentration of solution is 0.001M, and the concentration of hydrochloric acid is 0.1M, PVDF non-woven fabrics is cut into sizeable shape as propping up
Support body;
3) ambient temperature controls to be submerged into by supporter in deposition liquid A at 15 DEG C to take out after 2min;Again by supporter submergence
Enter in deionized water and take out after 60s;Then supporter is submerged in deposition liquid B and takes out after 2min;Last again by supporter leaching
Submerge and deionized water takes out after 60s.More than operation repeats 200 times.The film prepared is dried.Prepared repeatable utilization
The phenogram of surface sweeping Electronic Speculum (SEM) of organic gas detection thin film as in figure 2 it is shown, can be seen that from figure membrane granule size is equal
Even, film growth is finer and close.
The specifically used method of the gas sensing film prepared by embodiment 1-4 is as follows:
Based on above embodiment, by prepared film, it is cut into sizeable shape, puts into different types of volatilization
Property Organic substance atmosphere in, observe color change state and response time, experimental result is shown in Table one..After this gas sensing film variable color, put back to
Can recover original state in air voluntarily, be a reusable gas sensing film, the time recovering original state sees
Table two.
Table one thin film is Coloring Time under different organic volatile atmosphere
Example 1 | Example 2 | Example 3 | Example 4 | |
Methanol | 6min | 7min | 8min | 9min |
Acetonitrile | 8min | 9min | 10min | 12min |
Acetone | 5min | 5min | 8min | 7min |
Ethanol | 3min | 3min | 5min | 4min |
DMF | 10min | 11min | 13min | 16min |
DMSO | 12min | 13min | 15min | 18min |
True qualities required time is recovered after table two thin film variable color
Example 1 | Example 2 | Example 3 | Example 4 | |
Methanol | 3min | 2min | 2min | 3min |
Acetonitrile | 3min | 2.5min | 3min | 2min |
Acetone | 3.5min | 3min | 4min | 4.5min |
Ethanol | 2min | 1.5min | 2.5min | 2min |
DMF | 8min | 6min | 7min | 7min |
DMSO | 9min | 7min | 8min | 9min |
Claims (5)
1. a preparation method for the organic gas detection thin film of repeatable utilization, it specifically comprises the following steps that
Step 1: deposition liquid A, the preparation of B;Anionic donor and acid solution mixed preparing are deposited liquid A, by cation donor with
Acid solution mixed preparing deposition liquid B;Wherein acid used by deposition liquid A and deposition liquid B is identical, and has identical concentration;Described the moon
Ion donor is K4Fe(CN)6、K3Fe(CN)6Or K3[Co(CN)6One in];Described cation donor is FeCl3、ZnCl2Or
CoCl2In one;Described acid is the one in hydrochloric acid, sulphuric acid or nitric acid;
Step 2: deposit film on supporter;Supporter is submerged in deposition liquid A, takes out after a period of time;Again supporter is soaked
Submerge in deionized water, take out after a period of time;Then supporter is submerged in deposition liquid B, takes out after a period of time;Finally
Again supporter is submerged in deionized water, takes out after a period of time, complete the deposition of a tunic;
Step 3: repeat step 2, deposits and is naturally dried by prepared thin film after terminating or dry, obtain the organic of repeatable utilization
Gas detecting thin film.
Preparation method the most according to claim 1, it is characterised in that the concentration of zwitterion in deposition liquid A and deposition liquid B
It is 0.001-0.1M;The concentration of acid is 0.01-0.5M.
Preparation method the most according to claim 1, it is characterised in that the supporter described in step 2 be aluminium oxide ceramics,
One in PVDF non-woven fabrics or ITO electro-conductive glass.
Preparation method the most according to claim 1, it is characterised in that in step 2, ambient temperature controls at 15-35 DEG C;Heavy
In hydrops A and deposition liquid B, sedimentation time is 1-10min;The submergence deionized time is 10-60s.
Preparation method the most according to claim 1, it is characterised in that the number of times repeating step 2 is 50-200 time.
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CN110384990A (en) * | 2018-04-19 | 2019-10-29 | 北京化工大学 | A kind of three-dimensional netted flexible sensing film of functionalized nano-fiber and its preparation method and application |
CN110384990B (en) * | 2018-04-19 | 2021-01-12 | 北京化工大学 | Functionalized nanofiber three-dimensional mesh flexible sensing film and preparation method and application thereof |
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