CN201340405Y - Macromolecule resistive-type humidity sensitive element with hyperbranched structure - Google Patents
Macromolecule resistive-type humidity sensitive element with hyperbranched structure Download PDFInfo
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- CN201340405Y CN201340405Y CNU2008201677584U CN200820167758U CN201340405Y CN 201340405 Y CN201340405 Y CN 201340405Y CN U2008201677584 U CNU2008201677584 U CN U2008201677584U CN 200820167758 U CN200820167758 U CN 200820167758U CN 201340405 Y CN201340405 Y CN 201340405Y
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- humidity sensitive
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Abstract
The utility model discloses a macromolecule resistive-type humidity sensitive element with a hyperbranched structure, which takes ceramic as a substrate. The substrate is provided with a plurality of pairs of interdigital gold electrodes; and macromolecule quaternary ammonium salt humidity-sensitive thin films are coated on the ceramic substrate and the interdigital gold electrodes. The humidity sensitive element has the characteristics of moderate impedance value, high sensitivity, good linearity, quick response, excellent resilience, strong stability, detection at room temperature and the like in a wide humidity range, particularly in a lower humidity environment, and can be widely applied in industrial and agricultural production process and accurate measurement and control on the environmental temperature during warehousing and atmospheric environmental monitoring.
Description
Technical field
The utility model relates to a kind of high molecule electric resistance type humidity sensitive element with dissaving structure.
Background technology
Humidity plays crucial effect in human being's production and life, humidity sensor then is to detect the most frequently used of humidity and effective method.Present commercial humidity sensor mainly contains inorganic ceramic semi-conductor type and organic polymer type.And the polymer electrolyte humidity sensor is good with its response characteristic, and measurement range is wide, good stability, but room temperature detect, be easy to integratedly, advantage such as miniaturization is produced in batches, and is cheap has become the main flow of humidity sensor.Wherein the macromolecule resistance type humidity sensor preparation is very easy, functional, and is easy to realize in the system of being integrated in the measurement and the control of humidity, is one of emphasis of humidity sensor research and development.Yet, this class sensor adopts traditional linear macromolecule electrolyte as sensitive material, they are hanging down under the wet environment because ion migration difficulty, conductivity is low, cause its too high in resistance to be difficult to measure, measure low wet environment to it and bring big difficulty, also hindered it to a certain extent and further applied.For this reason, need carry out modification, improve its electric conductivity under low wet environment, adapt to and measure the low humidity environment requirement with it for macromolecule humidity sensitive material.
Summary of the invention
The purpose of this utility model provides a kind of in whole humidity range, and it is moderate, highly sensitive particularly to have resistance value under low wet environment, the linearity is good, and response is fast, and recovery is good, stability is strong, but the high molecule electric resistance type humidity sensitive element that room temperature detects with dissaving structure.
The high molecule electric resistance type humidity sensitive element of dissaving structure of the present utility model has ceramic matrix, have many at ceramic matrix photomask surface and evaporation to interdigital gold electrode, on interdigital gold electrode, be connected with lead-in wire, be coated with the wet humidity sensitive thin film of high molecular quaternary at ceramic matrix and interdigital gold electrode surfaces.
Have the method for making of the high molecule electric resistance type humidity sensitive element of dissaving structure, may further comprise the steps:
1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
2) in 100 milliliters of there-necked flasks after the deoxygenation that dewaters is handled, add the hyperbranched compound H20 that 10～20 grams have structure (I) successively, 10～20 gram succinic anhydrides, 0.1～0.4 gram SnCl
2, 30～60 milliliters of dioxane, logical argon gas 30 minutes is warming up to 100 ℃～150 ℃ then, and stirring reaction is 24～48 hours under argon shield, obtains transparent thick liquid, called after H20-COOH;
3) in 250 milliliters of there-necked flasks after the deoxygenation that dewaters is handled, add 20～30 gram 3-dimethylamino-1-propyl alcohol successively, 30～40 gram bromination of n-butane, 60～100 milliliters of acetone, stir, logical argon gas 30 minutes is warming up to 30～60 ℃ then, stirring reaction is 24～48 hours under argon shield, obtain white precipitate, vacuum filtration, with washing with acetone for several times, vacuum drying is spent the night under the room temperature, called after OH-N+;
4) in 50 milliliters of there-necked flasks after the deoxygenation that dewaters is handled, add 10～20 gram H20-COOH successively, 10～20 gram OH-N+, 0.1～0.2 gram p-toluenesulfonic acid is warming up to 120～160 ℃, logical argon gas reaction 3～6 hours, vacuumize then, continue reaction 3～6 hours down at 120～160 ℃, after reaction finishes, system is reduced under the room temperature, and use ethanol dilution, in ether, precipitate vacuum filtration, vacuum drying is spent the night under the room temperature, called after H20-N+;
5) H20-N+ is dissolved in the alcohol solvent, be mixed with the solution that concentration is 5～80 mg/ml, at room temperature left standstill 6～12 hours, obtain precursor solution, adopt dip coater that the ceramic interdigital gold electrode of step 1) be impregnated in the precursor solution 0.5～2 minute, after lifting taking-up, dry oven dry under 70～90 ℃ of temperature.
The interdigital width of the interdigital gold electrode of above-mentioned potsherd matrix surface is 20～200 μ m, and interdigital gap is 20～200 μ m.
The beneficial effects of the utility model are:
1) the dissaving structure molecular end has a large amount of functional groups, is easy to realize terminal groups modification, gives its various functions.And it also has fine solubility and excellent advantages such as filming performance, be introduced in the macromolecule, the preparation have dissaving structure macromolecule quaternary amine humidity sensitive thin film, it has fine solubility and film forming, and its end has a large amount of quaternary ammoniated unit, can obviously improve its ionic conductivity, helps reducing resistance, especially the resistance under low wet environment solves the low too high problem that is difficult to measure of wet environment impedance.
2) because the hyper-branched polymer humidity sensitive thin film has unique aggregated structure, help ion motion and charge transfer, thereby can improve its conductive capability under low wet environment, make humidity-sensitive element have lower impedance, can be used for measuring humidity under the low wet environment;
3) hyper-branched polymer quaternary amine humidity sensitive thin film, a large amount of ionic groups are positioned at the end of super branched molecule, are beneficial to the absorption and the desorption of hydrone in the environment, thereby make it have moisture absorption faster and dehumidification response speed, and the response time is shorter;
4) the high molecule electric resistance type quaternary amine humidity sensitive thin film of dissaving structure has identical ionic group with typical line style macromolecule quaternary amine, this sense wet basis is rolled into a ball and can be caused humidity sensitive thin film to have very high wet-sensitive sensitivity in the humidity range of broad, and response linearity is good under semilog coordinate;
5) the synthetic preparation process of humidity sensitive thin film is simple, and cost of material is cheap, is suitable for producing in batches;
6) adopt the method for dip-coating to prepare element, simple and easy to do, the element high conformity, the yield rate height is suitable for producing in batches;
7) to have a volume little for humidity-sensitive element of the present utility model, low cost, advantage such as easy to use.Interdigital width is 20～200 μ m, and interdigital gap is the interdigital gold electrode structure of 20～200 μ m, and ceramic matrix can improve the contact of humidity sensitive thin film and electrode matrix, the stability of raising element.This humidity-sensitive element can be widely used in the industrial and agricultural production process, and storage is accurately measured and control for ambient humidity during atmosphere environment supervision.
Description of drawings
Fig. 1 is the structural representation of humidity-sensitive element of the present utility model;
Fig. 2 is the building-up process synoptic diagram with macromolecule humidity sensitive thin film of dissaving structure;
Fig. 3 is H20, H20-COOH and the wet quick resonse characteristic with macromolecule quaternary amine electric resistance type humidity sensitive element of dissaving structure;
Fig. 4 is the response time curve with high molecule electric resistance type humidity sensitive element of dissaving structure;
Fig. 5 is the humidity hysteresis curve with high molecule electric resistance type humidity sensitive element of dissaving structure.
Embodiment
Further specify the utility model below in conjunction with drawings and Examples.
With reference to Fig. 1, high molecule electric resistance type humidity sensitive element with dissaving structure has ceramic matrix 1 to be had many to interdigital gold electrode 2 at ceramic matrix photomask surface and evaporation, on interdigital gold electrode, be connected with lead-in wire 4, be coated with humidity sensitive thin film 3 at ceramic matrix and interdigital gold electrode surfaces, humidity sensitive thin film 3 is for having the high molecular quaternary humidity-sensitive material of dissaving structure.
The interdigital interdigital width of said potsherd matrix surface is 20～200 μ m, and interdigital gap is 20～200 μ m.
Embodiment 1:
1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
2) in 100 milliliters of there-necked flasks after the deoxygenation that dewaters is handled, add the hyperbranched compound H20 that 10 grams have structure (I) successively, 10 gram succinic anhydrides, 0.2 gram SnCl
2, 30 milliliters of dioxane, logical argon gas 30 minutes is warming up to 120 ℃ then, and stirring reaction is 36 hours under argon shield, obtains transparent thick liquid, called after H20-COOH.
3) in 250 milliliters of there-necked flasks after the deoxygenation that dewaters is handled, add 20 gram 3-dimethylamino-1-propyl alcohol successively, 30 gram bromination of n-butane; 80 milliliters of acetone; stir, logical argon gas 30 minutes is warming up to 40 ℃ then; stirring reaction is 36 hours under argon shield; obtain a large amount of white precipitates, vacuum filtration, with washing with acetone for several times; vacuum drying is spent the night under the room temperature, called after OH-N+.
4) in 50 milliliters of there-necked flasks after the deoxygenation that dewaters is handled, add 10 gram H20-COOH successively, 10 gram OH-N+, 0.1 the gram p-toluenesulfonic acid is warming up to 120 ℃, logical argon gas reaction 3 hours, vacuumize then, continue reaction 3 hours down at 120 ℃, after reaction finishes, system is reduced under the room temperature, and use ethanol dilution, in ether, precipitate vacuum filtration, vacuum drying is spent the night under the room temperature, called after H20-N+.
5) H20-N+ is dissolved in the alcohol solvent, be mixed with the solution that concentration is 5 mg/ml, at room temperature left standstill 6 hours, obtain precursor solution, adopt dip coater that the ceramic interdigital gold electrode of step 1) be impregnated in the precursor solution 1 minute, after lifting taking-up, dry oven dry is 1 hour under 70 ℃ of temperature, obtains having the high molecular quaternary electric resistance type humidity sensitive element of dissaving structure.
Embodiment 2:
1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
2) in 100 milliliters of there-necked flasks after the deoxygenation that dewaters is handled, add the hyperbranched compound H20 that 12 grams have structure (I) successively, 12 gram succinic anhydrides, 0.24 gram SnCl
2, 30 milliliters of dioxane, logical argon gas 30 minutes is warming up to 120 ℃ then, and stirring reaction is 36 hours under argon shield, obtains transparent thick liquid, called after H20-COOH.
3) in 250 milliliters of there-necked flasks after the deoxygenation that dewaters is handled, add 26 gram 3-dimethylamino-1-propyl alcohol successively, 34 gram bromination of n-butane; 80 milliliters of acetone; stir, logical argon gas 30 minutes is warming up to 40 ℃ then; stirring reaction is 36 hours under argon shield; obtain a large amount of white precipitates, vacuum filtration, with washing with acetone for several times; vacuum drying is spent the night under the room temperature, called after OH-N+.
4) in 50 milliliters of there-necked flasks after the deoxygenation that dewaters is handled, add 10 gram H20-COOH successively, 10 gram OH-N+, 0.2 the gram p-toluenesulfonic acid is warming up to 140 ℃, logical argon gas reaction 4 hours, vacuumize then, continue reaction 4 hours down at 140 ℃, after reaction finishes, system is reduced under the room temperature, and use ethanol dilution, in ether, precipitate vacuum filtration, vacuum drying is spent the night under the room temperature, called after H20-N+.
5) H20-N+ is dissolved in the alcohol solvent, be mixed with the solution that concentration is 40 mg/ml, at room temperature left standstill 6 hours, obtain precursor solution, adopt dip coater that the ceramic interdigital gold electrode of step 1) be impregnated in the precursor solution 1 minute, after lifting taking-up, dry oven dry is 1 hour under 70 ℃ of temperature, obtains having the high molecular quaternary electric resistance type humidity sensitive element of dissaving structure.
Embodiment 3:
1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
2) in 100 milliliters of there-necked flasks after the deoxygenation that dewaters is handled, add the hyperbranched compound H20 that 20 grams have structure (I) successively, 20 gram succinic anhydrides, 0.4 gram SnCl
2, 60 milliliters of dioxane, logical argon gas 30 minutes is warming up to 120 ℃ then, and stirring reaction is 48 hours under argon shield, obtains transparent thick liquid, called after H20-COOH.
3) in 250 milliliters of there-necked flasks after the deoxygenation that dewaters is handled, add 30 gram 3-dimethylamino-1-propyl alcohol successively, 40 gram bromination of n-butane; 100 milliliters of acetone; stir, logical argon gas 30 minutes is warming up to 60 ℃ then; stirring reaction is 36 hours under argon shield; obtain a large amount of white precipitates, vacuum filtration, with washing with acetone for several times; vacuum drying is spent the night under the room temperature, called after OH-N+.
4) in 50 milliliters of there-necked flasks after the deoxygenation that dewaters is handled, add 20 gram H20-COOH successively, 20 gram OH-N+, 0.2 the gram p-toluenesulfonic acid is warming up to 160 ℃, logical argon gas reaction 3 hours, vacuumize then, continue reaction 3 hours down at 160 ℃, after reaction finishes, system is reduced under the room temperature, and use ethanol dilution, in ether, precipitate vacuum filtration, vacuum drying is spent the night under the room temperature, called after H20-N+.
5) H20-N+ is dissolved in the alcohol solvent, be mixed with the solution that concentration is 80 mg/ml, at room temperature left standstill 6 hours, obtain precursor solution, adopt dip coater that the ceramic interdigital gold electrode of step 1) be impregnated in the precursor solution 1 minute, after lifting taking-up, dry oven dry is 1 hour under 80 ℃ of temperature, obtains having the high molecular quaternary electric resistance type humidity sensitive element of dissaving structure.
As seen from Figure 3, the hyperbranched compound H20-COOH impedance under the higher levels of humidity environment that has carboxyl after dissaving structure compound H 20 and the modification is all very high, when being lower than 60%RH, impedance is too high and be difficult to measure, wet quick response characteristic is very poor, and the macromolecule quaternary amine electric resistance type humidity sensitive element with dissaving structure of the utility model preparation has very high sensitivity in the humidity range of broad, especially in that to be lower than under the low wet environment of 20%RH impedance also lower, be easy to measure, and under semilog coordinate, have good response linearity, embody well wet quick response characteristic;
As seen from Figure 4, the macromolecule quaternary amine electric resistance type humidity sensitive element with dissaving structure of the utility model preparation has than response speed faster, and moisture absorption and dehumidification time are all shorter, are respectively 9.2s and 9.8s;
Figure 5 shows that the humidity hysteresis curve of the macromolecule quaternary amine electric resistance type humidity sensitive element with dissaving structure, by the figure finding, nanofiber composite humidity sensor humidity hysteresis is less, only is 1.4%RH.
Claims (2)
1. the high molecule electric resistance type humidity sensitive element that has dissaving structure, it is characterized in that: it has ceramic matrix (1), have many at ceramic matrix photomask surface and evaporation to interdigital gold electrode (2), on interdigital gold electrode, be connected with lead-in wire (4), be coated with high molecular quaternary humidity sensitive thin film (3) at ceramic matrix and interdigital gold electrode surfaces.
2. the high molecule electric resistance type humidity sensitive element with dissaving structure according to claim 1, the interdigital width that it is characterized in that the interdigital gold electrode of potsherd matrix surface are 20～200 μ m, and interdigital gap is 20～200 μ m.
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| CNU2008201677584U CN201340405Y (en) | 2008-11-24 | 2008-11-24 | Macromolecule resistive-type humidity sensitive element with hyperbranched structure |
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| CNU2008201677584U CN201340405Y (en) | 2008-11-24 | 2008-11-24 | Macromolecule resistive-type humidity sensitive element with hyperbranched structure |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101408522B (en) * | 2008-11-24 | 2011-12-21 | 浙江大学 | Manufacturing method of high molecule electric resistance type humidity sensitive element with super-branched structure |
| CN104502420A (en) * | 2014-10-01 | 2015-04-08 | 浙江大学 | Humidity-sensitive composite membrane, preparation method of humidity-sensitive composite membrane and humidity sensor |
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2008
- 2008-11-24 CN CNU2008201677584U patent/CN201340405Y/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101408522B (en) * | 2008-11-24 | 2011-12-21 | 浙江大学 | Manufacturing method of high molecule electric resistance type humidity sensitive element with super-branched structure |
| CN104502420A (en) * | 2014-10-01 | 2015-04-08 | 浙江大学 | Humidity-sensitive composite membrane, preparation method of humidity-sensitive composite membrane and humidity sensor |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20091104 Termination date: 20111124 |