CN117362647A - Polyion liquid material containing hydrophobic component, low-humidity sensor using polyion liquid material as sensing material and preparation method of low-humidity sensor - Google Patents
Polyion liquid material containing hydrophobic component, low-humidity sensor using polyion liquid material as sensing material and preparation method of low-humidity sensor Download PDFInfo
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- 229920000831 ionic polymer Polymers 0.000 title claims abstract description 98
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 61
- 239000011344 liquid material Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000011540 sensing material Substances 0.000 title abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000178 monomer Substances 0.000 claims abstract description 21
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 18
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 17
- 239000010439 graphite Substances 0.000 claims abstract description 17
- 239000000919 ceramic Substances 0.000 claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 15
- WEERVPDNCOGWJF-UHFFFAOYSA-N 1,4-bis(ethenyl)benzene Chemical compound C=CC1=CC=C(C=C)C=C1 WEERVPDNCOGWJF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 86
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 51
- 239000012705 liquid precursor Substances 0.000 claims description 42
- 239000000463 material Substances 0.000 claims description 26
- 238000009210 therapy by ultrasound Methods 0.000 claims description 21
- 239000002608 ionic liquid Substances 0.000 claims description 20
- 239000002904 solvent Substances 0.000 claims description 16
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 14
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 claims description 14
- 230000001678 irradiating effect Effects 0.000 claims description 14
- 239000003999 initiator Substances 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 10
- 150000002500 ions Chemical class 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 244000028419 Styrax benzoin Species 0.000 claims description 7
- 235000000126 Styrax benzoin Nutrition 0.000 claims description 7
- 235000008411 Sumatra benzointree Nutrition 0.000 claims description 7
- 230000032683 aging Effects 0.000 claims description 7
- 229960002130 benzoin Drugs 0.000 claims description 7
- 235000019382 gum benzoic Nutrition 0.000 claims description 7
- 239000006193 liquid solution Substances 0.000 claims description 7
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 230000004044 response Effects 0.000 abstract description 16
- 238000011084 recovery Methods 0.000 abstract description 10
- 230000035945 sensitivity Effects 0.000 abstract description 6
- 229920000642 polymer Polymers 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 230000005284 excitation Effects 0.000 abstract description 2
- 238000004132 cross linking Methods 0.000 description 12
- 238000006116 polymerization reaction Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 230000008859 change Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229920006037 cross link polymer Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 125000002883 imidazolyl group Chemical group 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 229910003471 inorganic composite material Inorganic materials 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000003380 quartz crystal microbalance Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000010897 surface acoustic wave method Methods 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/121—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid for determining moisture content, e.g. humidity, of the fluid
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
- C08G75/02—Polythioethers
- C08G75/04—Polythioethers from mercapto compounds or metallic derivatives thereof
- C08G75/045—Polythioethers from mercapto compounds or metallic derivatives thereof from mercapto compounds and unsaturated compounds
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/126—Composition of the body, e.g. the composition of its sensitive layer comprising organic polymers
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Abstract
A polyion liquid material containing a hydrophobic component, a low-humidity sensor with low-humidity sensing characteristics by taking the polyion liquid material as a sensing material and a preparation method of the sensor belong to the technical field of humidity sensors. The low-humidity sensor provided by the invention consists of a ceramic substrate with graphite carbon interdigital electrodes on the surface, and a sensing layer which is dripped on the ceramic substrate and the graphite carbon interdigital electrodes. The invention prepares the polyion liquid material by adopting alkene-sulfhydryl click chemical reaction under ultraviolet light excitation, and further obtains the polyion liquid material containing hydrophobic components by introducing paradivinylbenzene monomers. The prepared low-humidity sensor based on the polyionic liquid material containing the hydrophobic component has excellent humidity-sensitive characteristics under a low humidity range, including high sensitivity, high stability, small wet hysteresis and quick response recovery characteristics, and solves the problems of low sensitivity, slow recovery and poor stability when most polymer-based humidity sensors detect low humidity.
Description
Technical Field
The invention belongs to the technical field of humidity sensors, and particularly relates to a polyion liquid material containing a hydrophobic component, a low-humidity sensor with low-humidity sensing characteristics by taking the polyion liquid material as a sensing material, and a preparation method of the sensor.
Background
Humidity is a main parameter for measuring the dryness and humidity of air, and is indispensible from the daily life of human beings. The humidity sensor has wide application in the fields of meteorological environment monitoring, industrial production, agricultural planting, aerospace, medical treatment and the like. The rapid and high-sensitivity accurate monitoring of low humidity is particularly important today when the interconnection of everything and intelligent manufacturing are rapidly developed.
There are many methods currently used to detect low humidity, including spectroscopy, quartz crystal microbalance, and surface acoustic wave methods. These methods can be applied to a certain extent to detect low humidity, but still have problems of long time consumption, high cost and complicated operation. The impedance type humidity sensor has the advantages of simple and convenient preparation, low cost and small volume, and is a technology with great application prospect in the field of low humidity detection. At present, polymer composite electrolyte, carbon-based composite material and inorganic composite material are attempted to be applied to a low humidity sensor, but the sensor has the defects of low response value, large wet hysteresis, poor stability and the like. Therefore, the novel low-humidity sensitive material is designed, the response value of the low-humidity sensor is improved, the wet hysteresis is reduced, the stability of the element is enhanced, and the low-humidity sensor with excellent performance is obtained.
Disclosure of Invention
The invention aims to provide a polyionic liquid material containing a hydrophobic component, a low-humidity sensor with low-humidity sensing characteristics by using the polyionic liquid material as a sensing material and a preparation method of the sensor. The invention prepares the polyion liquid material by adopting alkene-sulfhydryl click chemical reaction under ultraviolet light excitation, and further obtains the polyion liquid material containing hydrophobic components by introducing paradivinylbenzene monomers.
The polyionic liquid material containing the hydrophobic component is prepared by the following steps (if not specified, the solution of the invention is methanol solution):
(1) 34.8-69.1 mg of ionic liquid 1-allyl-3-vinyl imidazole chloride salt is dissolved in methanol solvent to prepare 90-110 mg/mL of ionic liquid solution;
(2) Ultrasonic treatment is carried out on the solution obtained in the step (1) for 2-5 min, and an ion liquid solution with uniform dispersion is obtained;
(3) Adding 95-105 mg of polymerized monomer pentaerythritol tetra-3-mercaptopropionate into the solution obtained in the step (2);
(4) Adding 0.5-59.1 mg of hydrophobic material monomer p-divinylbenzene into the mixed solution obtained in the step (3);
(5) Adding a methanol solvent into the solution obtained in the step (4), wherein the total dosage of the methanol solvent in the step (1) and the step (5) is 900-1100 mu L; then ultrasonic treatment is carried out for 2-5 min to obtain a mixture solution which is uniformly dispersed;
(6) Adding 1.5-2.5 mg of benzoin dimethyl ether serving as an ultraviolet curing initiator into the mixture solution obtained in the step (5) to obtain a polyion liquid precursor solution;
(7) Carrying out ultrasonic treatment on the polyion liquid precursor solution obtained in the step (6) for 2-5 min to obtain a polyion liquid precursor solution with uniform dispersion;
(8) And (3) placing the polyion liquid precursor solution obtained in the step (7) into a CL-1000 ultraviolet cross-linking irradiation instrument, and irradiating for 20-40 min under 365nm ultraviolet light, thereby obtaining the polyion liquid material containing the hydrophobic component.
The low-humidity sensor with the low-humidity sensing characteristic consists of a ceramic substrate with graphite carbon interdigital electrodes on the surface and a humidity-sensitive material sensitive layer which is dripped on the ceramic substrate and the graphite carbon interdigital electrodes; the pair number of the graphite carbon interdigital electrodes is 2-5 pairs, the length of the electrodes is 5-10 mm, the width of the electrodes is 3-7 mm, the thickness of the electrodes is 0.2-1 mm, and the electrode spacing is 0.2-1 mm. The moisture sensitive material sensitive layer absorbs water molecules after contacting with water molecules in the air, the impedance value of the moisture sensitive material sensitive layer on the surface of the graphite carbon interdigital electrode changes, and the response value of the sensor (the test voltage applied to the two ends of the interdigital electrode is 1 volt and 1000 hertz alternating voltage) can be obtained by comparing the change of the impedance value of the moisture sensitive material sensitive layer on the surface of the interdigital electrode measured by the impedance analyzer before and after moisture absorption of the low humidity sensor. The response value is calculated by dividing the resistance value of the sensor in the initial relative humidity (5%) test environment by its resistance value in the highest relative humidity (35%) test environment. The wet hysteresis is the maximum relative humidity difference of the humidity sensor at the same resistance value between an adsorption curve of 5% -35% relative humidity and a desorption curve of 35% -5% relative humidity, which are drawn through the test relation of the relative humidity and the resistance value.
The low humidity sensor is an impedance type humidity sensor, and output signals of the low humidity sensor are impedance signals which are obtained through testing by an impedance analyzer.
The invention relates to a preparation method of a low humidity sensor with low humidity sensing characteristics, which comprises the following steps:
(1) Transferring 2-5 mu L of the uniformly dispersed polyion liquid precursor solution obtained in the step (7), and dripping the polyion liquid precursor solution onto a ceramic substrate with graphite carbon interdigital electrodes on the surface, so that the ceramic substrate is covered with the graphite carbon interdigital electrodes to obtain a moisture-sensitive material sensitive film with the thickness of 10-20 mu m;
(2) Placing the device obtained in the step (1) in a CL-1000 ultraviolet cross-linking irradiation instrument, and irradiating for 20-40 min under 365nm ultraviolet light;
(3) Aging the device obtained in the step (2) at 20-30 ℃ and 75-95% relative humidity for 1-4 hours, thereby obtaining the impedance type low humidity sensor based on the polyion liquid material containing the hydrophobic component.
The invention has the advantages that:
1) The raw materials and the ceramic substrate with the graphite carbon interdigital electrode can be purchased from the market, and the ceramic substrate is low in raw material cost, high in yield, good in structural consistency and suitable for mass production.
2) The low-humidity sensor prepared by the invention has simple manufacturing process and small volume and is suitable for industrial mass production.
3) The low-humidity sensor based on the polyion liquid material containing the hydrophobic component, which is prepared by the invention, has excellent humidity-sensitive characteristics (including high sensitivity, high stability, small wet hysteresis and quick response recovery characteristics) in a low humidity range, and solves the problems of low response value, slow recovery and poor stability when most polymer-based humidity sensors detect low humidity.
4) The invention utilizes the high hydrophilicity and high ionic conductivity of the polyionic liquid material to generate ion migration in a humidity environment so as to improve the sensitivity characteristic of the device; meanwhile, a hydrophobic component is introduced into a polymer network to form a cross-linked polymer network with staggered hydrophilic and hydrophobic groups, so that the formation of continuous water molecule layers in a temperature sensitive layer is limited, the water molecule adsorption quantity of the sensitive layer in unit time is reduced, and the physical desorption characteristic of the element is improved; meanwhile, the content of ionic liquid in the polyionic liquid is reduced by introducing the hydrophobic component, so that the content of chloride ions in unit volume in the humidity-sensitive material is reduced, the number of free ions in the sensitive layer after water molecules are adsorbed is reduced, the impedance value of the element can be recovered more quickly, and the recovery characteristic of the humidity sensor is improved.
5) The preparation method of the polyion liquid material containing the hydrophobic component is easy to regulate and control the hydrophilic and hydrophobic characteristics of the polyion liquid material containing the hydrophobic component, and the composition and structure of the polyion liquid material and the sensing performance of the humidity sensor prepared by the polyion liquid material can be regulated and controlled by controlling the amount of p-divinylbenzene added into the polyion liquid precursor.
Drawings
FIG. 1 is an infrared absorption spectrum of a polyionic liquid material containing a hydrophobic component prepared in example 3;
FIG. 2 is a frequency characteristic curve of an impedance type low humidity sensor based on a polyionic liquid material containing a hydrophobic component prepared in example 3 at low humidity;
FIG. 3 is a graph showing the humidity sensitivity characteristics of the impedance low humidity sensor prepared in examples 1-5 based on a polyionic liquid material containing a hydrophobic component at low humidity;
FIG. 4 is a graph of the wet hysteresis of a resistive low humidity sensor based on a polyionic liquid material containing a hydrophobic component prepared in example 3 at low humidity;
FIG. 5 is a response recovery curve for a low humidity sensor of impedance type based on a polyionic liquid material containing a hydrophobic component prepared in example 3;
fig. 6 is a graph of the reproducibility of multiple measurements of a low humidity sensor based on a polyionic liquid material containing a hydrophobic component prepared in example 3.
Detailed Description
Example 1
(1) Dissolving 69.1mg of ionic liquid in 658 mu L of methanol solvent to prepare 105mg/mL of ionic liquid solution, wherein the ionic liquid is 1-allyl-3-vinylimidazole chloride;
(2) Ultrasonic treatment is carried out on the solution obtained in the step (1) for 2.5min, so as to obtain an ion liquid solution with uniform dispersion;
(3) Adding 100mg of a polymerization monomer into the solution in the step (2), wherein the polymerization monomer is pentaerythritol tetra-3-mercaptopropionate;
(4) Adding 0.5mg of hydrophobic material into the mixed solution in the step (3), wherein the monomer of the hydrophobic material is p-divinylbenzene;
(5) Adding 292 mu L of methanol solvent into the solution obtained in the step (4), and carrying out ultrasonic treatment on the solution for 2.5min to obtain a uniformly dispersed mixture solution;
(6) Adding 2.1mg of ultraviolet light curing initiator into the mixed solution in the step (5), wherein the ultraviolet light curing initiator is benzoin dimethyl ether, so as to obtain polyion liquid precursor solution;
(7) Ultrasonic treatment is carried out on the polyion liquid precursor solution obtained in the step (6) for 2.5min, so as to obtain 950 mu L of uniformly dispersed precursor solution;
(8) Transferring 948 mu L of the uniformly dispersed polyion liquid precursor solution obtained in the step (7) into a CL-1000 ultraviolet cross-linking irradiation instrument, and irradiating with 365nm ultraviolet light for 25min to obtain a polyion liquid material containing a hydrophobic component;
(9) Transferring 2 mu L of the uniformly dispersed polyion liquid precursor solution obtained in the step (7), and dripping the polyion liquid precursor solution onto a ceramic substrate with 3 pairs of graphite carbon interdigital electrodes on the surface, wherein the interdigital electrodes are 7mm long, 5mm wide and 0.6mm thick, and the interdigital electrode spacing is 0.5mm, so as to obtain a moisture-sensitive material sensitive film with the thickness of 10 mu m;
(10) Placing the device obtained in the step (9) in a CL-1000 ultraviolet cross-linking irradiation instrument, and irradiating 365nm ultraviolet light for 25min;
(11) Aging the device obtained in the step (10) at 25 ℃ and 95% relative humidity for 1 hour, thereby obtaining the impedance type low humidity sensor based on the polyionic liquid material containing the hydrophobic component.
Example 2
(1) 61.1mg of ionic liquid is dissolved in 611 mu L of methanol solvent to prepare 100mg/mL of ionic liquid solution, wherein the ionic liquid is 1-allyl-3-vinylimidazole chloride;
(2) Carrying out ultrasonic treatment on the solution obtained in the step (1) for 3min to obtain an ion liquid solution with uniform dispersion;
(3) Adding 100mg of a polymerization monomer into the solution in the step (2), wherein the polymerization monomer is pentaerythritol tetra-3-mercaptopropionate;
(4) Adding 14.8mg of hydrophobic material into the mixed solution in the step (3), wherein the monomer of the hydrophobic material is p-divinylbenzene;
(5) Adding 439 mu L of methanol solvent into the solution obtained in the step (4), and carrying out ultrasonic treatment on the solution for 3min to obtain a uniformly dispersed mixture solution;
(6) Adding 2.1mg of ultraviolet light curing initiator into the mixed solution in the step (5), wherein the ultraviolet light curing initiator is benzoin dimethyl ether, so as to obtain polyion liquid precursor solution;
(7) Carrying out ultrasonic treatment on the polyion liquid precursor solution obtained in the step (6) for 3min to obtain 1050 mu L of uniformly dispersed polyion liquid precursor solution;
(8) Transferring 1048 mu L of the uniformly dispersed polyion liquid precursor solution obtained in the step (7) into a CL-1000 ultraviolet crosslinking irradiation instrument, and irradiating with 365nm ultraviolet light for 30min to obtain a polyion liquid material containing a hydrophobic component;
(9) Transferring 2 mu L of the uniformly dispersed polyion liquid precursor solution obtained in the step (7), and dripping the polyion liquid precursor solution onto a ceramic substrate with 3 pairs of graphite carbon interdigital electrodes on the surface, wherein the interdigital electrodes are 7mm long, 5mm wide and 0.6mm thick, and the interdigital electrode spacing is 0.5mm, so as to obtain a moisture-sensitive material sensitive film with the thickness of 10 mu m;
(10) Placing the device obtained in the step (9) in a CL-1000 ultraviolet cross-linking irradiation instrument, and irradiating 365nm ultraviolet light for 35min;
(11) Aging the device obtained in the step (10) at 25 ℃ and 75% relative humidity for 3 hours, thereby obtaining the impedance type low humidity sensor based on the polyionic liquid material containing the hydrophobic component.
Example 3
(1) 52.2mg of ionic liquid is dissolved in 522 mu L of methanol solvent to prepare 100mg/mL of ionic liquid solution, wherein the ionic liquid is 1-allyl-3-vinylimidazole chloride;
(2) Carrying out ultrasonic treatment on the solution obtained in the step (1) for 3min to obtain an ion liquid solution with uniform dispersion;
(3) Adding 100mg of a polymerization monomer into the solution in the step (2), wherein the polymerization monomer is pentaerythritol tetra-3-mercaptopropionate;
(4) 29.8mg of hydrophobic material is added into the mixed solution in the step (3), and the monomer of the hydrophobic material is p-divinylbenzene;
(5) Adding 478 mu L of methanol solvent into the solution obtained in the step (4), and carrying out ultrasonic treatment on the solution for 3min to obtain a mixture solution with uniform dispersion;
(6) Adding 2.1mg of ultraviolet light curing initiator into the mixed solution in the step (5), wherein the ultraviolet light curing initiator is benzoin dimethyl ether, so as to obtain polyion liquid precursor solution;
(7) Carrying out ultrasonic treatment on the polyion liquid precursor solution obtained in the step (6) for 3min to obtain 1000 mu L of uniformly dispersed polyion liquid precursor solution;
(8) Transferring 998 mu L of the uniformly dispersed polyion liquid precursor solution obtained in the step (7) into a CL-1000 ultraviolet crosslinking irradiation instrument, and irradiating with 365nm ultraviolet light for 30min to obtain a polyion liquid material containing a hydrophobic component;
(9) Transferring 2 mu L of the uniformly dispersed polyion liquid precursor solution obtained in the step (7), and dripping the polyion liquid precursor solution onto a ceramic substrate with 3 pairs of graphite carbon interdigital electrodes on the surface, wherein the interdigital electrodes are 7mm long, 5mm wide and 0.6mm thick, and the interdigital electrode spacing is 0.5mm, so as to obtain a moisture sensitive material sensitive film with the thickness of 10 mu m;
(10) Placing the device obtained in the step (9) in a CL-1000 ultraviolet cross-linking irradiation instrument, and irradiating 365nm ultraviolet light for 30min;
(11) Aging the device obtained in the step (10) at 25 ℃ and 85% relative humidity for 2 hours, thereby obtaining the impedance type low humidity sensor based on the polyionic liquid material containing the hydrophobic component.
Example 4
(1) 43.7mg of ionic liquid is dissolved in 486 mu L of methanol solvent to prepare 90mg/mL of ionic liquid solution, and the ionic liquid is 1-allyl-3-vinylimidazole chloride;
(2) Ultrasonic treatment is carried out on the solution obtained in the step (1) for 4min, so as to obtain an ion liquid solution with uniform dispersion;
(3) Adding 100mg of a polymerization monomer into the solution in the step (2), wherein the polymerization monomer is pentaerythritol tetra-3-mercaptopropionate;
(4) Adding 44.4mg of hydrophobic material into the mixed solution in the step (3), wherein the monomer of the hydrophobic material is p-divinylbenzene;
(5) Adding 614 mu L of methanol solvent into the solution obtained in the step (4), and carrying out ultrasonic treatment on the solution for 4min to obtain a uniformly dispersed mixture solution;
(6) Adding 2.1mg of ultraviolet light curing initiator into the mixed solution in the step (5), wherein the ultraviolet light curing initiator is benzoin dimethyl ether, so as to obtain polyion liquid precursor solution;
(7) Carrying out ultrasonic treatment on the polyion liquid precursor solution obtained in the step (6) for 3min to obtain 1100 mu L of uniformly dispersed polyion liquid precursor solution;
(8) Transferring 1098 mu L of the uniformly dispersed polyion liquid precursor solution obtained in the step (7) into a CL-1000 ultraviolet cross-linking irradiation instrument, and irradiating with 365nm ultraviolet light for 40min to obtain a polyion liquid material containing a hydrophobic component;
(9) Transferring 2 mu L of the uniformly dispersed polyion liquid precursor solution obtained in the step (7), and dripping the polyion liquid precursor solution onto a ceramic substrate with 3 pairs of graphite carbon interdigital electrodes on the surface, wherein the interdigital electrodes are 7mm long, 5mm wide and 0.6mm thick, and the interdigital electrode spacing is 0.5mm, so as to obtain a moisture sensitive material sensitive film with the thickness of 10 mu m;
(10) Placing the device obtained in the step (9) in a CL-1000 ultraviolet cross-linking irradiation instrument, and irradiating 365nm ultraviolet light for 40min;
(11) Aging the device obtained in the step (10) at 25 ℃ and 85% relative humidity for 2 hours, thereby obtaining the impedance type low humidity sensor based on the polyionic liquid material containing the hydrophobic component.
Example 5
(1) 34.8mg of ionic liquid is dissolved in 316 mu L of methanol solvent to prepare 110mg/mL of ionic liquid solution, wherein the ionic liquid is 1-allyl-3-vinylimidazole chloride;
(2) Ultrasonic treatment is carried out on the solution obtained in the step (1) for 5min, so as to obtain an ion liquid solution with uniform dispersion;
(3) Adding 100mg of a polymerization monomer into the solution in the step (2), wherein the polymerization monomer is pentaerythritol tetra-3-mercaptopropionate;
(4) Adding 59.1mg of hydrophobic material into the mixed solution in the step (3), wherein the monomer of the hydrophobic material is p-divinylbenzene;
(5) Adding 584 mu L of methanol solvent into the solution obtained in the step (4), and carrying out ultrasonic treatment on the solution for 5min to obtain a uniformly dispersed mixture solution;
(6) Adding 2.1mg of ultraviolet light curing initiator into the mixed solution in the step (5), wherein the ultraviolet light curing initiator is benzoin dimethyl ether, so as to obtain polyion liquid precursor solution;
(7) Carrying out ultrasonic treatment on the polyion liquid precursor solution obtained in the step (6) for 5min to obtain 900 mu L of uniformly dispersed polyion liquid precursor solution;
(8) Transferring 898 mu L of the uniformly dispersed polyion liquid precursor solution obtained in the step (7) into a CL-1000 ultraviolet cross-linking irradiation instrument, and irradiating 365nm ultraviolet light for 20min to obtain a polyion liquid material containing a hydrophobic component;
(9) Transferring 2 mu L of the uniformly dispersed polyion liquid precursor solution obtained in the step (7), and dripping the polyion liquid precursor solution onto a ceramic substrate with 3 pairs of graphite carbon interdigital electrodes on the surface, wherein the interdigital electrodes are 7mm long, 5mm wide and 0.6mm thick, and the interdigital electrode spacing is 0.5mm, so as to obtain a moisture sensitive material sensitive film with the thickness of 10 mu m;
(10) Placing the device obtained in the step (9) in a CL-1000 ultraviolet cross-linking irradiation instrument, and irradiating 365nm ultraviolet light for 20min;
(11) Aging the device obtained in the step (10) at 25 ℃ and 85% relative humidity for 2 hours, thereby obtaining the impedance type low humidity sensor based on the polyionic liquid material containing the hydrophobic component.
The fourier infrared spectrum of the polyionic liquid material containing the hydrophobic component prepared in example 3 is shown in fig. 1. The characteristic peak of the carbon-carbon double bond is 3140cm -1 The characteristic peak of the carbon-oxygen double bond is 1643cm -1 Characteristic peaks for mercapto groups appear at 2967, 640 and 1256cm -1 At the position, skeleton vibration peaks and telescopic vibration of imidazole ring are respectively appeared at 1568 cm and 1172cm -1 At 808cm -1 The peak at the position is a characteristic peak generated by flexural vibration of hydrocarbon bonds on the benzene ring. The characteristic peaks of the prepared polyion liquid material containing the hydrophobic component are attributed to the characteristic peaks of the ion liquid and the characteristic peaks of the paradivinylbenzene, which shows that the polyion liquid material containing the hydrophobic component is successfully prepared.
The frequency characteristic curve of the impedance type low humidity sensor based on the polyionic liquid material containing the hydrophobic component prepared in example 3 in the range of 5 to 35% relative humidity is shown in fig. 2. For an impedance type low humidity sensor based on a polyionic liquid material containing a hydrophobic component, when the test frequency exceeds 10kHz, the response value is less than 10.0; when the test frequency is lower than 100Hz, the sensor impedance value is unstable, so 1kHz is selected as the optimal operating frequency.
The humidity sensitivity curves of the impedance type low humidity sensors based on the polyionic liquid material containing the hydrophobic component prepared in examples 1 to 5 at low humidity are shown in fig. 3. The response values of the 5 low humidity sensors in the relative humidity range of 5-35% are 232.2, 105.7, 48.0, 5.3 and 2.0 respectively, which shows that the impedance type low humidity sensor based on the polyionic liquid material containing the hydrophobic component has good response to low humidity. It is also described that the humidity-sensitive characteristics of the low humidity sensor can be effectively adjusted by adjusting the proportion of the hydrophobic component in the humidity-sensitive material in the present invention.
The wet hysteresis curve of the impedance type low humidity sensor based on the polyionic liquid material containing the hydrophobic component prepared in example 3 at low humidity is shown in fig. 4. The low humidity sensor has small wet hysteresis within the range of 5-35% relative humidity, and the low humidity sensor has 0.2% relative humidity.
The response recovery curve of the resistive low humidity sensor based on the polyionic liquid material containing the hydrophobic component prepared in example 3 between 11% and 33% relative humidity is shown in fig. 5. The response and recovery times of the sensor in the test were 1 second and 10 seconds, respectively, further illustrating that the resistive low humidity sensor based on the polyionic liquid material containing the hydrophobic component has good response recovery characteristics in low humidity measurements.
The multi-response recovery curve of the resistive low humidity sensor based on the polyionic liquid material containing the hydrophobic component prepared in example 3 between 11% and 33% relative humidity is shown in fig. 6. The sensor response value does not change significantly in the 5-cycle test, and the element baseline does not change significantly, further illustrating that the impedance type low humidity sensor based on the polyionic liquid material containing the hydrophobic component has good stability in low humidity measurement.
Claims (4)
1. A polyionic liquid material containing a hydrophobic component is prepared by the method comprising the following steps:
(1) 34.8-69.1 mg of ionic liquid 1-allyl-3-vinyl imidazole chloride salt is dissolved in methanol solvent to prepare 90-110 mg/mL of ionic liquid solution;
(2) Ultrasonic treatment is carried out on the solution obtained in the step (1) for 2-5 min, and an ion liquid solution with uniform dispersion is obtained;
(3) Adding 95-105 mg of polymerized monomer pentaerythritol tetra-3-mercaptopropionate into the solution obtained in the step (2);
(4) Adding 0.5-59.1 mg of hydrophobic material monomer p-divinylbenzene into the mixed solution obtained in the step (3);
(5) Adding a methanol solvent into the solution obtained in the step (4), wherein the total dosage of the methanol solvent in the step (1) and the step (5) is 900-1100 mu L; then ultrasonic treatment is carried out for 2-5 min to obtain a mixture solution which is uniformly dispersed;
(6) Adding 1.5-2.5 mg of benzoin dimethyl ether serving as an ultraviolet curing initiator into the mixture solution obtained in the step (5) to obtain a polyion liquid precursor solution;
(7) Carrying out ultrasonic treatment on the polyion liquid precursor solution obtained in the step (6) for 2-5 min to obtain a polyion liquid precursor solution with uniform dispersion;
(8) And (3) irradiating the polyion liquid precursor solution obtained in the step (7) for 20-40 min under 365nm ultraviolet light, so as to obtain the polyion liquid material containing the hydrophobic component.
2. A preparation method of a low humidity sensor with low humidity sensing characteristics comprises the following steps:
(1) Transferring 2-5 mu L of the uniformly dispersed polyion liquid precursor solution obtained in the step (7) of the claim 1, and dripping the polyion liquid precursor solution on a ceramic substrate with graphite carbon interdigital electrodes on the surface, so that the ceramic substrate is covered with the graphite carbon interdigital electrodes to obtain a moisture-sensitive material sensitive film with the thickness of 10-20 mu m;
(2) Irradiating the device obtained in the step (1) for 20-40 min under 365nm ultraviolet light;
(3) Aging the device obtained in the step (2) at 20-30 ℃ and 75-95% relative humidity for 1-4 hours, thereby obtaining the low humidity sensor based on the polyion liquid material containing the hydrophobic component.
3. A method of manufacturing a low humidity sensor having low humidity sensing characteristics as claimed in claim 2, wherein: the pair number of the graphite carbon interdigital electrodes is 2-5 pairs, the length of the electrodes is 5-10 mm, the width of the electrodes is 3-7 mm, the thickness of the electrodes is 0.2-1 mm, and the electrode spacing is 0.2-1 mm.
4. A low humidity sensor having low humidity sensing characteristics, characterized by: is prepared by the method of claim 2 or 3.
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