CN101078705A - Polymer grafted carbon black composite resistance type thin film humidity sensor and its production method - Google Patents
Polymer grafted carbon black composite resistance type thin film humidity sensor and its production method Download PDFInfo
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- CN101078705A CN101078705A CN 200710069737 CN200710069737A CN101078705A CN 101078705 A CN101078705 A CN 101078705A CN 200710069737 CN200710069737 CN 200710069737 CN 200710069737 A CN200710069737 A CN 200710069737A CN 101078705 A CN101078705 A CN 101078705A
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- 239000006229 carbon black Substances 0.000 title claims abstract description 49
- 229920000642 polymer Polymers 0.000 title claims abstract description 31
- 239000010409 thin film Substances 0.000 title claims description 22
- 239000002131 composite material Substances 0.000 title claims description 20
- 238000004519 manufacturing process Methods 0.000 title abstract 3
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000002241 glass-ceramic Substances 0.000 claims abstract description 5
- 230000008569 process Effects 0.000 claims abstract description 5
- 239000000758 substrate Substances 0.000 claims abstract description 4
- 239000003738 black carbon Substances 0.000 claims description 25
- 229920000075 poly(4-vinylpyridine) Polymers 0.000 claims description 24
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 23
- 239000010931 gold Substances 0.000 claims description 23
- 229910052737 gold Inorganic materials 0.000 claims description 23
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 150000001722 carbon compounds Chemical class 0.000 claims description 18
- -1 4-hydroxyl-2,2,6,6-tetramethyl pyridine nitroxyl free radical Chemical class 0.000 claims description 17
- 239000011521 glass Substances 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 16
- 239000011159 matrix material Substances 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 10
- 239000012298 atmosphere Substances 0.000 claims description 9
- 239000002243 precursor Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 238000012662 bulk polymerization Methods 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000007669 thermal treatment Methods 0.000 claims description 6
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 5
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 5
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 5
- 230000000977 initiatory effect Effects 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000004062 sedimentation Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 2
- 238000001259 photo etching Methods 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 5
- 238000005259 measurement Methods 0.000 abstract description 4
- 238000004132 cross linking Methods 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 238000005576 amination reaction Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 12
- 230000004044 response Effects 0.000 description 10
- 239000002245 particle Substances 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- ULTHEAFYOOPTTB-UHFFFAOYSA-N 1,4-dibromobutane Chemical compound BrCCCCBr ULTHEAFYOOPTTB-UHFFFAOYSA-N 0.000 description 3
- 238000006424 Flood reaction Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000006210 lotion Substances 0.000 description 3
- 230000010355 oscillation Effects 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000012271 agricultural production Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001412 amines Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920000307 polymer substrate Polymers 0.000 description 1
- 238000004393 prognosis Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
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Abstract
The invention discloses a resistance film humidity sensor with the combination of polymer and graft carbon black and the fabricating method. Glass ceramic is used as the substrate and on it there are multiple pairs of interdigital golden electrodes. Combination humidity film obtained by graft carbon black of poly 4-vinypyridine with cross-linking quaternary amination is coated on surfaces of glass ceramic and interdigital golden electrodes. The invention is provided with simple preparing process and low cost. It is suitable for mass production. Prepared humidity sensor is provided with high sensitivity, good linearity, good water resistance, measuring in room temperature so on in the humidity range of 0-98%RH, especially in circumstance with middle-low humidity (less than 30%RH). It can be applied in production process of industry and agriculture, storage and accurate measurement and control for circumstance humidity, especially the circumstance humidity with low than 30%RH, when air circumstance is monitored.
Description
Technical field
The present invention relates to a kind of polymer grafted carbon black composite resistance type thin film humidity sensor and preparation method thereof.
Background technology
Hygroscopy and control is for environmental monitoring and protection, weather prognosis, and industrial and agricultural production, material is stored, and life staying idle at home environment optimization etc. all plays crucial effect.And humidity sensor is the most frequently used and effective instrument that detects humidity, and its research and application have crucial meaning.Than traditional stupalith humidity sensor, it is good that the macromolecular material humidity sensor has response characteristic, and measurement range is wide, good stability, but the room temperature detection is easy to integrated, miniaturization is produced in batches, lower-price characteristic, the present important directions that has become the humidity sensor research and development.Wherein macromolecule resistance type humidity sensor is little owing to volume, and can be fine compatible with the modern integrated circuits technology, and development is to use the wider novel humidity sensor of a class at present rapidly.The high molecule sensitivity material easily dissolves loss under the high humidity environment but there is also, and causes responding variation, and stability is bad; And low wet environment is down because resistance is too high-leveled and difficult with problems such as mensuration.
Summary of the invention
The purpose of this invention is to provide and a kind ofly have highly sensitively at wide humidity range, the linearity is good, responds fast polymer graft black carbon laminated film electric resistance type humidity sensitive element and preparation method thereof.
Polymer carbon black composite resistance type thin film humidity sensor of the present invention, has the devitrified glass matrix, have many to interdigital gold electrode at the devitrified glass matrix surface, on interdigital gold electrode, be connected with lead-in wire, be coated with humidity sensitive thin film at devitrified glass sheet matrix and interdigital gold electrode surfaces, humidity sensitive thin film is the crosslinked quaternary ammoniated compound that obtains of carbon black process of poly 4 vinyl pyridine grafting.
The method for making of polymer grafted carbon black composite resistance type thin film humidity sensor may further comprise the steps:
1) clean surface photoetching and evaporation have the glass-ceramic substrate of interdigital gold electrode, dry for standby;
2) at 4-hydroxyl-2,2,6,6-tetramethyl pyridine nitroxyl free radical exists down, with the benzoyl peroxide is initiating agent, causes the 4-vinylpridine bulk polymerization, reacts 15～40h in 90～125 ℃ under argon gas atmosphere, products therefrom obtains the polymkeric substance of nitroxyl free radical end-blocking through precipitation, vacuum drying;
3) with the polymer dissolution of nitroxyl free radical end-blocking at N, in the dinethylformamide, add carbon black, the mass ratio of carbon black and polymkeric substance is 1: 6～24, under argon atmospher, react 2～15h in 90～125 ℃, use ether sedimentation then, after filtration, washing and vacuum drying, obtain poly 4 vinyl pyridine graft black carbon compound;
4) with poly 4 vinyl pyridine graft black carbon compound and 1, the 4-dibromobutane is scattered in N, in the N-dimethyl formamide, 4-vinylpridine unit and 1 in the poly 4 vinyl pyridine graft black carbon compound, the mol ratio of 4-dibromobutane is 1: 0.5～2, be mixed with the solution that complex concentration is 5～30 mg/ml, stir 4～12h, get precursor solution at 30 ℃ of following magnetic;
5) adopt dip coater that the interdigital gold electrode of the devitrified glass of step 1) be impregnated in the precursor solution 0.5～5 minute, lift taking-up after, thermal treatment is 2～12 hours under 80～140 ℃ of temperature, makes polymer grafted carbon black composite resistance type thin film humidity sensor.
The interdigital width of the said interdigital gold electrode of method for making of above-mentioned polymer grafted carbon black composite resistance type thin film humidity sensor is 20～200 μ m, and interdigital gap is 20～200 μ m.
Advantage of the present invention is:
1) the prepared compound humidity-sensitive material of polymer graft black carbon, be by in the presence of nitroxyl free radical, carry out the 4-vinylpridine bulk polymerization, nitroxyl free radical is introduced the end group of poly 4 vinyl pyridine, and by thermal cracking formation free radical, caught by carbon black, thereby polymer graft is arrived black carbon surface, rather than with both simple physics blend.Therefore can obviously improve the dispersiveness of carbon black in polymeric matrix in the compound substance, reduce the agglomeration of carbon black particle, make the humidity-sensitive element of preparation have the consistance that high response sensitivity is become reconciled humidity;
2) adopt the polymer graft black carbon compound as humidity sensing film, the carbon black particle that has good intrinsic conductivity by introducing, can be so that humidity sensing film also has higher electric conductivity under low wet environment, thereby it is low because of ion mobility under low humidity to solve common macromolecule resistance type humidity sensor, too high in resistance, be difficult to measure, can not detect the problem of low humidity ambient humidity;
3) adopt poly 4 vinyl pyridine and carbon black graft, be beneficial to the dispersion of carbon black particle, and polymkeric substance strengthens in quaternary ammoniated back hydroscopicity, making humidity sensing film change in the different humidity lower volume increases, cause that the carbon black particle spacing strengthens, the resistance variations scope broadens, and response sensitivity improves;
4) adopting crosslinked quaternary ammoniated poly 4 vinyl pyridine and carbon black graft compound is humidity sensing film, can be easily by regulating the ratio of carbon black and polymkeric substance, change the contribution under different humidity of carbon black particle electronic conduction and these two kinds of electrical conduction mechanisms of quaternary ammoniated poly 4 vinyl pyridine ionic conduction to the humidity response, acquisition has the proper resistor value, under low humidity based on the carbon black particle conduction, ionic conduction is main under the high humidity, can test the humidity-sensitive element of low wet environment;
5) adopting the polymer graft black carbon compound as humidity sensing film, wherein is the electronic conduction particle with the carbon black, and poly 4 vinyl pyridine is a polymer substrate, and provides the ionic conduction ability after quaternary ammoniated.By regulating the ratio of carbon black and polymkeric substance, and the excess effusion value of composite conducting material, change the contribution to the humidity response under different humidity of two kinds of electrical conduction mechanisms, obtain to have the proper resistor value, based on the carbon black particle conduction, ionic conduction is main humidity sensing film under the high humidity under low humidity;
6) by humidity-sensitive element is heat-treated, carry out crosslinked quaternary ammonium reaction, make humidity sensing film have cross-linked structure, thereby can effectively improve the stability and the water tolerance of polymer graft black carbon compound humidity sensing film; Thermal treatment simultaneously also can be eliminated high boiling solvent remaining in the humidity sensing film, reduces its influence for the humidity sensing film pattern, improves the stability of humidity-sensitive element;
7) polymer graft black carbon is scattered in N, in the organic solvents such as dinethylformamide, the preparation precursor solution carries out precrosslink, can obviously improve the dispersiveness of carbon black in solvent, simultaneously also help improving the stability of precursor solution, thereby improve the consistance and the yield rate of humidity-sensitive element;
8) adopt dip-coating method to prepare element, simple and easy to do, the element high conformity, the yield rate height is suitable for producing in batches;
9) to have a volume little for humidity-sensitive element of the present invention, low cost, advantage such as easy to use.Interdigital width is 20～200 μ m, and interdigital gap is that the electrode structure of 20～200 μ m can make humidity-sensitive element resistance reduce, and sensing range is widened, and response sensitivity improves, and also can improve its stability simultaneously.This humidity-sensitive element can be widely used in the industrial and agricultural production process, and storage for ambient humidity, especially is lower than the accurate measurement and the control of the low humidity ambient humidity of 30%RH during atmosphere environment supervision.
Description of drawings
Fig. 1 is the structural representation of humidity-sensitive element of the present invention;
Fig. 2 is the typical response family curve with humidity-sensitive element of different polymkeric substance and carbon black mass ratio of the present invention;
Fig. 3 is the typical response family curve with humidity-sensitive element of different crosslinking times of the present invention.
Embodiment
Further specify the present invention below in conjunction with drawings and Examples.
With reference to Fig. 1, polymer grafted carbon black composite resistance type thin film humidity sensor has devitrified glass matrix 1, have many to interdigital gold electrode 2 at the devitrified glass matrix surface, on interdigital gold electrode, be connected with lead-in wire 4, be coated with humidity sensitive thin film 3 at devitrified glass sheet matrix and interdigital gold electrode surfaces, humidity sensitive thin film 3 is the crosslinked quaternary ammoniated compound that obtains of carbon black process of poly 4 vinyl pyridine grafting.
The interdigital gold electrode of said microcrystalline glass matrix surface has 8～16 pairs, and the interdigital width of interdigital gold electrode is 20～200 μ m, and interdigital gap is 20～200 μ m.
Embodiment 1:
1) glass-ceramic substrate of interdigital gold electrode is arranged with absolute ethyl alcohol and acetone soaking and washing photomask surface and evaporation, dry for standby;
2) at 4-hydroxyl-2,2,6,6-tetramethyl pyridine nitroxyl free radical exists down, with the benzoyl peroxide initiating agent, causes the 4-vinylpridine bulk polymerization, 125 ℃ were reacted 15 hours under argon gas atmosphere, products therefrom is through precipitation, filtration washing, and vacuum drying obtains the polymkeric substance of nitroxyl free radical end-blocking;
3) with the polymer dissolution of nitroxyl free radical end-blocking at N, in the dinethylformamide, add carbon black, the mass ratio of carbon black and polymkeric substance is 1: 6,125 ℃ of reaction 2h under argon gas atmosphere, use ether sedimentation then, after filtration, washing and vacuum drying, make poly 4 vinyl pyridine graft black carbon compound.
4) with poly 4 vinyl pyridine graft black carbon compound and 1,4-dibromobutane sonic oscillation is scattered in N, in the dinethylformamide, 4-vinylpridine unit and 1 in the poly 4 vinyl pyridine graft black carbon compound, both mol ratios of 4-dibromobutane are 1: 0.5, be mixed with the solution that complex concentration is 5 mg/ml, stir 4h, get precursor solution at 30 ℃ of following magnetic.
5) after the employing dip coater floods 0.5 minute with the interdigital gold electrode of devitrified glass in lotion, lift taking-up,, make the polymer carbon black composite resistance type thin film humidity sensor at 80 ℃ of thermal treatment 12h.
Embodiment 2:
1) electrode cleans with embodiment 1
2) at 4-hydroxyl-2,2,6,6-tetramethyl pyridine nitroxyl free radical exists down, with the benzoyl peroxide initiating agent, cause the 4-vinylpridine bulk polymerization, 90 ℃ of reaction 40h under argon gas atmosphere, products therefrom is through precipitation, filtration washing, and vacuum drying obtains the polymkeric substance of nitroxyl free radical end-blocking;
3) just the polymer dissolution of nitroxyl free radical end-blocking at N, in the dinethylformamide, add carbon black, the mass ratio of carbon black and polymkeric substance is 1: 24,90 ℃ of reaction 15h under argon gas atmosphere, use ether sedimentation then, after filtration, washing and vacuum drying, make poly 4 vinyl pyridine graft black carbon compound.
4) with poly 4 vinyl pyridine graft black carbon compound and 1,4-dibromobutane sonic oscillation is scattered in N, in the dinethylformamide, 4-vinylpridine unit and 1 in the poly 4 vinyl pyridine graft black carbon compound, both mol ratios of 4-dibromobutane are 1: 2, being mixed with complex concentration is 30 mg/ml, stirs 12h at 30 ℃ of following magnetic, gets precursor solution.
5) after the employing dip coater floods 5 minutes with the interdigital gold electrode of devitrified glass in lotion, lift taking-up,, make the polymer carbon black composite resistance type thin film humidity sensor at 140 ℃ of thermal treatment 2h.
Embodiment 3:
1) electrode cleans with embodiment 1
2) at 4-hydroxyl-2,2,6,6-tetramethyl pyridine nitroxyl free radical exists down, with the benzoyl peroxide initiating agent, causes the 4-vinylpridine bulk polymerization, 125 ℃ were reacted 29 hours under argon gas atmosphere, products therefrom is through precipitation, filtration washing, and vacuum drying obtains the polymkeric substance of nitroxyl free radical end-blocking;
3) will obtain the polymer dissolution of nitroxyl free radical end-blocking at N, in the dinethylformamide, add carbon black, the mass ratio of carbon black and polymkeric substance is 1: 9,125 ℃ of reaction 12h under argon gas atmosphere, use ether sedimentation then, after filtration, washing and vacuum drying, make poly 4 vinyl pyridine graft black carbon compound.
4) with poly 4 vinyl pyridine graft black carbon compound and 1,4-dibromobutane sonic oscillation is scattered in N, in the dinethylformamide, 4-vinylpridine unit and 1 in the poly 4 vinyl pyridine graft black carbon compound, both mol ratios of 4-dibromobutane are 1: 2, be mixed with the solution that complex concentration is 27 mg/ml, stir 12h, get precursor solution at 30 ℃ of following magnetic.
5) after the employing dip coater floods 1 minute with the interdigital gold electrode of devitrified glass in lotion, lift taking-up,, make the polymer carbon black composite resistance type thin film humidity sensor at 110 ℃ of thermal treatment 12h.
Fig. 2 was respectively 1: 6 for polymkeric substance and carbon black mass ratio, 1: 9,1: 15, the response characteristic of 1: 24 polymer graft black carbon composite humidity sensor, as seen from the figure, the composite humidity sensor of poly 4 vinyl pyridine graft black carbon increases with the carbon black compositely proportional, can effectively reduce under the low humidity (＜30%RH) resistance value, thus make things convenient for the low humidity moisture measurement.
Fig. 3 is the humidity response characteristic of the polymer graft black carbon composite humidity sensor of different crosslinked quaternary ammoniated time preparations, as seen from the figure, at wide humidity range (in 0～98%RH), film humidity-sensitive element of the present invention, particularly crosslinked quaternary amine turns to the humidity-sensitive element of 6h, have highly sensitive, the characteristic that the linearity is good.
Claims (4)
1. polymer grafted carbon black composite resistance type thin film humidity sensor, it is characterized in that: it has devitrified glass matrix (1), have many to interdigital gold electrode (2) at the devitrified glass matrix surface, on interdigital gold electrode, be connected with lead-in wire (4), be coated with humidity sensitive thin film (3) at devitrified glass sheet matrix and interdigital gold electrode surfaces, humidity sensitive thin film (3) is the crosslinked quaternary ammoniated compound that obtains of carbon black process of poly 4 vinyl pyridine grafting.
2. polymer grafted carbon black composite resistance type thin film humidity sensor according to claim 1, it is characterized in that: the interdigital gold electrode of microcrystalline glass matrix surface has 8～16 pairs, the interdigital width of interdigital gold electrode is 20～200 μ m, and interdigital gap is 20～200 μ m.
3. the method for making of polymer grafted carbon black composite resistance type thin film humidity sensor according to claim 1 is characterized in that may further comprise the steps:
1) clean surface photoetching and evaporation have the glass-ceramic substrate of interdigital gold electrode, dry for standby;
2) at 4-hydroxyl-2,2,6,6-tetramethyl pyridine nitroxyl free radical exists down, with the benzoyl peroxide is initiating agent, causes the 4-vinylpridine bulk polymerization, reacts 15～40h in 90～125 ℃ under argon gas atmosphere, products therefrom obtains the polymkeric substance of nitroxyl free radical end-blocking through precipitation, vacuum drying;
3) with the polymer dissolution of nitroxyl free radical end-blocking at N, in the dinethylformamide, add carbon black, the mass ratio of carbon black and polymkeric substance is 1: 6～24, under argon atmospher, react 2～15h in 90～125 ℃, use ether sedimentation then, after filtration, washing and vacuum drying, obtain poly 4 vinyl pyridine graft black carbon compound;
4) with poly 4 vinyl pyridine graft black carbon compound and 1, the 4-dibromobutane is scattered in N, in the N-dimethyl formamide, 4-vinylpridine unit and 1 in the poly 4 vinyl pyridine graft black carbon compound, the mol ratio of 4-dibromobutane is 1: 0.5～2, be mixed with the solution that complex concentration is 5～30 mg/ml, stir 4～12h, get precursor solution at 30 ℃ of following magnetic;
5) adopt dip coater that the interdigital gold electrode of the devitrified glass of step 1) be impregnated in the precursor solution 0.5～5 minute, lift taking-up after, thermal treatment is 2～12 hours under 80～140 ℃ of temperature, makes polymer grafted carbon black composite resistance type thin film humidity sensor.
4. the method for making of polymer grafted carbon black composite resistance type thin film humidity sensor according to claim 3, the interdigital width that it is characterized in that said interdigital gold electrode is 20～200 μ m, interdigital gap is 20～200 μ m.
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| CN115382402A (en) * | 2021-05-24 | 2022-11-25 | 天津工业大学 | Preparation method of composite membrane material |
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| CN115382402A (en) * | 2021-05-24 | 2022-11-25 | 天津工业大学 | Preparation method of composite membrane material |
| CN115382402B (en) * | 2021-05-24 | 2024-02-02 | 天津工业大学 | Preparation method of composite membrane material |
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