CN103149246A - Graphene film humidity sensor - Google Patents
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- CN103149246A CN103149246A CN2012103900760A CN201210390076A CN103149246A CN 103149246 A CN103149246 A CN 103149246A CN 2012103900760 A CN2012103900760 A CN 2012103900760A CN 201210390076 A CN201210390076 A CN 201210390076A CN 103149246 A CN103149246 A CN 103149246A
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Abstract
The invention relates to a humidity sensor based on nano material film. The humidity sensor comprises a flexible polymer substrate, a comb-like interdigital electrode, a graphene based humidity sensitive film, a humidity sensitive film resistor pickup circuit board, a circuit signal line and an air hole casing. The graphene based humidity sensitive film is a multilayer network film composed of a static induced self-assembly polyelectrolyte precursor and a solvent evaporation induced self-assembly graphene film, and prepared on surfaces of the flexible polymer substrate and the comb-like interdigital electrode to form a humidity sensitive film sensing element. The film resistor pickup circuit and the humidity sensitive element are electrically connected together through a contact pin mode; the humidity sensitive element and the signal pickup circuit board are fixed through screws and nuts, and arranged in air hole plastic casing; and the circuit signal line is lead out through a casing lead hole to realize functions of data acquisition, storage, display and alarm. The sensor has the characteristics of stability, reliability, low cost, high sensitivity, good repeatability, and high speed of humidity sensitive response and recovery, etc.
Description
Technical field
What the present invention relates to is a kind of nano material film sensor and preparation method thereof, specifically relates to a kind of based on the graphene film humidity sensor.
Background technology
Humidity sensor has important influence power and application background widely in sensor field, not only directly affects the basic living condition of the mankind, and on the very big impact that has of the aspects such as industrial or agricultural, biological products, medical and health, national defense construction.The development of humidity-sensitive element occupies an important position in the sensor industry, is the device that detects external environment humidity based on the humidity sensor of humidity-sensitive element, and it is converted into the moisture signal that detects is convenient to the signal processing, transmit, show, record.At present humidity sensor mainly comprises the kinds such as Electrolyte type, semiconductor ceramics type and high molecular polymer type, and electrolytes humidity sensor principle is simply with low cost, but can not prolonged application in high humidity environment; The stable performance of semiconductor ceramics class wet sensitive device, sensing range is wide, but temperature coefficient is higher, and the difficult desorption of anti-pollution not.It is comparatively extensive that the polymer electrolyte wet sensitive device is used, but exist the shortcomings such as poor and response time of long-time stability is long.Therefore, seek the important directions that novel sensitive material has become the humidity sensor development.
Along with the development of science and technology, nanometer technology has become very popular field, and its range of application is also in continuous expansion.2004, the physicist An Deliehaimu of Univ Manchester UK and Constantine Nuo Woxiaoluofu, successfully isolate Graphene in experiment from graphite, two people obtain 2010 years Nobel Prizes in physics jointly because of " in the initiative experiment of two-dimentional grapheme material ".Graphene as a kind of fully by sp
2The two dimensional crystal material that the carbon atom of hydridization consists of, thickness is only monoatomic layer (0.335nm), have the excellent performance such as high strength and pliability, light transmission and electric conductivity, high-specific surface area and high adsorption ability, cause scientist's extensive concern in fields such as high-performance nanometer electronic device, gas sensor, photoelectric device, compound substance, field emmision material and stored energies.The research and development Novel wet dependent sensor that is found to be of Graphene provides a kind of new way.Particularly Graphene has very large specific surface area, and very strong interaction is arranged between surrounding medium, and the humidity sensitive of environment, be the ideal material of making the moisture sensor sensitive membrane to external world.At present, the assembling of graphene film preparation becomes the bottleneck of its device development of restriction, and it is a kind of method that extensively adopts that solution blended process prepares film, reunites and affects uniformity of film and quality but film forming easily occurs.The method that the present invention adopts the electrostatic induction self assembly to combine with the evaporation induced self-assembly technology, at flexible polymer substrate and the graphene-based film of pectination interdigital electrode surface construction, prepared a kind of graphene film moisture sensor, had that method is simple, absorption affinity is strong, characteristics such as with low cost, fast response time, sensitivity height.
Summary of the invention
The present invention is directed to the deficiency on existing method for preparing graphene membrane, a kind of self-assembly preparation method thereof easily and effectively is provided, and made in wider humidity range, response and regeneration rate are very fast, measurable graphene film humidity sensor under room temperature, be provided with flexible polymer substrate, pectination interdigital electrode, graphene-based humidity sensitive thin film, resistance pick-up circuit plate, electrode contact pin, ventilative shell, fairlead.
The present invention is achieved by the following technical solutions, the method that adopts the electrostatic induction self assembly to combine with the evaporation induced self-assembly technology, at flexible polymer substrate and the graphene-based film of pectination interdigital electrode surface construction as the wet sensitive sensing element, be matched with one with sheet resistance pick-up circuit plate and consist of humidity sensor, change by detecting the thin-film electro resistance detection that realizes relative humidity.
Described flexible polymer substrate adopts the flexible polymer take polyimide as base material, and on it, photoetching and Evaporation preparation have pectination interdigital electrode pattern.
Described graphene-based humidity sensitive thin film is the multitiered network shape film that is made of the first conducting shell of electrostatic induction self assembly polyelectrolyte and evaporation induced self-assembly graphene film.The thickness of polyelectrolyte monofilm is used for flexible polymer substrate and the finishing of pectination interdigital electrode at 2-6nm, makes graphene film bed interface linking firm stable, difficult drop-off.
Described graphene-based humidity sensitive thin film preparation method is as follows: adopt dilute sulfuric acid and diluted sodium hydroxide solution soaking and washing to be prepared with the flexible polymer substrate of pectination interdigital electrode, immerse diallyl dimethyl ammoniumchloride (PDDA) solution of 15mg/L, carry out the self assembly of PDDA, take out after 10-15 minute and use deionized water rinsing 2-3 minute, dry up; Poly-4-styrene sulfonic acid (PSS) solution that immerses again 3mg/L carries out the self assembly of PSS, takes out after 10-15 minute and uses deionized water rinsing 2-3 minute, dries up, and operation repeats once.Then immerse diallyl dimethyl ammoniumchloride (PDDA) solution of 15mg/L, carry out the self assembly of PDDA, take out after 10-15 minute and use deionized water rinsing 2-3 minute, dry up; Adopt accurate pipettor to draw even the dripping of 0.5-1ml graphene dispersing solution and be coated in above-mentioned substrate surface, put into 50 ℃ of vacuum drying chambers and processed 5-8 hour, obtain being coated with the electric resistance type humidity sensitive element of polyelectrolyte-Graphene stratiform film.
Described diallyl dimethyl ammoniumchloride is said polycation solution, and poly-4-styrene sulfonic acid is polyanion solution.
Described graphene dispersing solution concentration is 0.5mg/ml, and particle is with negative charge.
Described pectination interdigital electrode is Cu/Ni or Cr/Au, spacing 5-200 μ m, facewidth 5-200 μ m.
Described moisture sensor spare electrode and resistance pick-up circuit plate adopt pin type mode electricity to be connected in one.
Described moisture sensor spare is fixed assembling with resistance pick-up circuit plate by screw rod and nut, and is packaged in the bleeder vent plastic casing.
Described resistance pick-up circuit signal wire is drawn by the plastic casing fairlead, can be connected with computing machine or microprocessor, realizes the measuring abilities such as data acquisition, storage, demonstration and warning.
The method that the present invention utilizes electrostatic induction self-assembling method and evaporation induced self-assembly to combine prepares the graphene film humidity sensor, provide a kind of simple and convenient, the high sensitivity humidity sensor that absorption affinity is strong, with low cost, fast response time, repeatability and good stability.
Description of drawings
Fig. 1 is that the structure of the embodiment of the present invention forms schematic diagram, and wherein 1 is bleeder vent, and 2 is shell on plastics, 3 is standing screw, and 4 is graphene-based humidity sensitive thin film, and 5 is flexible polymer substrate, 6 is the pectination interdigital electrode, 7 is the electrode contact pin, and 8 is fixing threaded hole, and 9 is resistance pick-up circuit plate, 10 is signal wire, 11 is fairlead, and 12 is the plastics lower casing, and 13 is hold-down nut.
Fig. 2 is the structural representation of wet sensitive sensing element, wherein 1 is the graphene film of evaporation induced self-assembly, 2 is diallyl dimethyl ammoniumchloride (polycation) self-assembled film, 3 are poly-4-styrene sulfonic acid (polyanion) self-assembled film, 4 is graphene-based humidity sensitive thin film, 5 is the pectination interdigital electrode, and 6 is flexible polymer substrate, and 7 is the electrode contact pin.
Fig. 3 is wet sensitive sensing element and resistance pick-up circuit plate assembling schematic diagram, and wherein 1 is moisture sensor spare, and 2 is resistance pick-up circuit plate, and 3 is standing screw, and 4 is hold-down nut, and 5 is the electrode contact pin.
Fig. 4 is preparation technology's process flow diagram of graphene film, wherein 1 is the flexible polymer substrate with the pectination interdigital electrode after dilute sulfuric acid and diluted sodium hydroxide solution immersion treatment, 2 is diallyl dimethyl ammoniumchloride solution, 3 are poly-4-styrene sulfonic acid solution, 4 is accurate pipettor, and 5 for being prepared with the sensing element of graphene-based humidity sensitive thin film.
Fig. 5 is the change curve of graphene film humidity sensor electrical response under different humidity.
The resistance that Fig. 6 is the graphene film humidity sensor under 0%, 12%, 23%, 33%, 43%, 52%, 75% humidity is switched and time response curve.
Embodiment
The invention will be further described in connection with accompanying drawing for following examples.
Referring to Fig. 1, the embodiment of the present invention is provided with flexible polymer substrate 5, pectination interdigital electrode 6, graphene-based humidity sensitive thin film 4, resistance pick-up circuit plate 9, electrode contact pin 7, ventilative shell 2 and 12, fairlead 11, fixing threaded hole 8, standing screw 3 and nut 13.
The flexible polymer substrate of making take polyimide as base material, on it, photoetching and Evaporation preparation have pectination interdigital electrode pattern.Adopt the electrostatic induction self-assembling method at flexible polymer substrate and pectination interdigital electrode surface preparation polyelectrolyte membrane layer as first conducting shell, then adopt the evaporation induced self-assembly method to prepare graphene film, consist of the humidity sensitive thin film sensing element, as shown in Figure 2, union sheet resistance pick-up circuit plate consists of humidity sensor in one.
Described wet sensitive sensing element electrode and sheet resistance pick-up circuit adopt pin type mode electricity to be connected in one, and wet sensitive sensing element and signal pickup circuit plate as shown in Figure 3, and are packaged in the bleeder vent plastic casing by screw rod and the fixing assembling of nut.
Described graphene-based humidity sensitive thin film preparation method is as follows: adopt dilute sulfuric acid and diluted sodium hydroxide solution soaking and washing to be prepared with the flexible polymer substrate of pectination interdigital electrode, immerse diallyl dimethyl ammoniumchloride (PDDA) solution of 15mg/L, carry out the self assembly of PDDA, take out after 10-15 minute and use deionized water rinsing 2-3 minute, dry up; Poly-4-styrene sulfonic acid (PSS) solution that immerses again 3mg/L carries out the self assembly of PSS, takes out after 10-15 minute and uses deionized water rinsing 2-3 minute, dries up, and repetitive operation once; Then immerse diallyl dimethyl ammoniumchloride (PDDA) solution of 15mg/L, carry out the self assembly of PDDA, take out after 10-15 minute and use deionized water rinsing 2-3 minute, dry up; Adopt accurate pipettor to draw even the dripping of 0.5-1ml graphene dispersing solution and be coated in above-mentioned substrate surface, put into 50 ℃ of vacuum drying chambers and processed 5-8 hour, so far can obtain being coated with the electric resistance type humidity sensitive element of polyelectrolyte-Graphene stratiform film.
Described resistance pick-up circuit signal wire is comprised of power lead, ground wire, output signal line, draws by the plastic casing fairlead, can be connected with computing machine or microprocessor, realizes the measuring abilities such as data acquisition, storage, demonstration and warning.
Adopting saturated salt method allotment surrounding environment relative humidity is 0%-97%, record the polyelectrolyte-variation of graphene film sensor electrical resistance under corresponding humidity environment and realize the detection of relative humidity, as shown in Figure 5, resistance variations and relative humidity have good response relation.
Allocated environment relative humidity is respectively 0%, 12%, 23%, 33%, 43%, 52%, 75%, the graphene film humidity sensor is put into the detection that different humidity environments is realized relative humidity successively, has response rapidly, high stability, highly sensitive advantage (shown in Figure 6) especially has higher sensitivity to the accurate measurement of humidity under low wet environment.
Claims (7)
1. a graphene film humidity sensor, is characterized in that being provided with flexible polymer substrate, pectination interdigital electrode, graphene-based humidity sensitive thin film, resistance pick-up circuit plate, electrode contact pin, ventilative shell, fairlead; The method that adopts the electrostatic induction self assembly to combine with the evaporation induced self-assembly technology, at flexible polymer substrate and the graphene-based film of pectination interdigital electrode surface construction as the wet sensitive sensing element, be matched with one with sheet resistance pick-up circuit plate and consist of humidity sensor, change by detecting the thin-film electro resistance detection that realizes relative humidity.
2. graphene film humidity sensor according to claim 1, is characterized in that described graphene-based humidity sensitive thin film is the multitiered network shape film that is made of the first conducting shell of electrostatic induction self assembly polyelectrolyte and evaporation induced self-assembly graphene film; The thickness of polyelectrolyte monofilm is used for flexible polymer substrate and the finishing of pectination interdigital electrode at 2-6nm, makes graphene film bed interface linking firm stable, difficult drop-off.
3. graphene film humidity sensor according to claim 1, is characterized in that described flexible polymer substrate adopts the flexible polymer take polyimide as base material, and on it, photoetching and Evaporation preparation have pectination interdigital electrode pattern.
4. graphene film humidity sensor according to claim 1, is characterized in that described wet sensitive sensing element electrode and sheet resistance pick-up circuit adopt pin type mode electricity to be connected in one.
5. graphene film humidity sensor according to claim 1, is characterized in that described wet sensitive sensing element and signal pickup circuit plate by screw rod and the fixing assembling of nut, and be packaged in the bleeder vent plastic casing.
6. graphene film humidity sensor according to claim 1, it is characterized in that described resistance pick-up circuit signal wire draws by the plastic casing fairlead, can be connected with computing machine or microprocessor, realize the measuring abilities such as data acquisition, storage, demonstration and warning.
7. graphene film humidity sensor according to claim 1 is characterized in that described graphene-based humidity sensitive thin film preparation comprises the following steps:
(1) adopt dilute sulfuric acid and diluted sodium hydroxide solution soaking and washing to be prepared with the flexible polymer substrate of pectination interdigital electrode;
(2) configuration diallyl dimethyl ammoniumchloride solution and poly-4-styrene sulfonic acid solution concentration are respectively 15mg/L and 3mg/L, and graphene dispersing solution concentration is 0.5mg/ml;
(3) soaked above-mentioned substrate 10-15 minute in diallyl dimethyl ammoniumchloride solution, take out, washed with de-ionized water 2-3 minute, dry up;
(4) soaked above-mentioned substrate 10-15 minute in poly-4-styrene sulfonic acid solution, take out, washed with de-ionized water 2-3 minute, dry up;
(5) repeating step (3) and (4) are once;
(6) soaked above-mentioned substrate 10-15 minute in diallyl dimethyl ammoniumchloride solution, take out, washed with de-ionized water 2-3 minute, dry up;
(7) adopt accurate pipettor to draw even the dripping of 0.5-1ml graphene dispersing solution and be coated in above-mentioned substrate surface, put into 50 ℃ of vacuum drying chambers and processed 5-8 hour, obtain being coated with the electric resistance type humidity sensitive element of polyelectrolyte-Graphene stratiform film.
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| CN110146555A (en) * | 2019-05-30 | 2019-08-20 | 河海大学常州校区 | A kind of humidity sensor based on redox graphene humidity sensitive thin film, method of preparation and use |
| CN110687169A (en) * | 2019-11-01 | 2020-01-14 | 电子科技大学 | Humidity-sensitive carbon nanotube/graphene/organic composite flexible material, humidity sensor and preparation method thereof |
| CN110687169B (en) * | 2019-11-01 | 2022-06-10 | 电子科技大学 | Humidity-sensitive carbon nano tube/graphene/organic composite flexible material, humidity sensor and preparation method thereof |
| CN112611787A (en) * | 2020-12-15 | 2021-04-06 | 无锡豪帮高科股份有限公司 | High-molecular resistance type humidity sensitive element and preparation method thereof |
| CN117746596A (en) * | 2023-12-19 | 2024-03-22 | 广东工业大学 | Humidity alarm device based on laser-induced graphene and processing method |
| CN117746596B (en) * | 2023-12-19 | 2024-08-20 | 广东工业大学 | Humidity alarm device based on laser-induced graphene and processing method |
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