CN107525825A - It is prepared by a kind of gas sensor based on screen printing technique - Google Patents

It is prepared by a kind of gas sensor based on screen printing technique Download PDF

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Publication number
CN107525825A
CN107525825A CN201610443934.1A CN201610443934A CN107525825A CN 107525825 A CN107525825 A CN 107525825A CN 201610443934 A CN201610443934 A CN 201610443934A CN 107525825 A CN107525825 A CN 107525825A
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China
Prior art keywords
preparation
humidity sensor
cuo
graphene
ink
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CN201610443934.1A
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Chinese (zh)
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刘君
潘鹏
杨正春
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Tianjin University of Technology
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Tianjin University of Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B41PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41MPRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M1/00Inking and printing with a printer's forme
    • B41M1/12Stencil printing; Silk-screen printing

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)

Abstract

As a kind of special gas sensor, it has been widely used humidity sensor in the fields such as environment, safety, meteorology and medical treatment tool.In order to better meet and solve the problems, such as humidity sensor demand in the application and exist, the development of sensor of high sensitivity, strong selectivity, fast-response speed and high stability receives much concern.The present invention is prepared for cupric oxide nano piece (CuO), cupric oxide nano piece multi-walled carbon nanotube (CuO MWCNTs) and cupric oxide nano piece graphene (CuO Graphene) composite using simple in-situ oxidation reducing process, go forward side by side the ratio of a step section material, additive and solvent, the printing ink for silk-screen printing is prepared, screen process press double-deck chromatography on flexible pet film (PET) is finally used, prints out the humidity sensor for Humidity Detection.The humidity sensor has the advantages that low detection limit, high sensitivity, stability are good, in the practical application in future, has certain application prospect.

Description

It is prepared by a kind of gas sensor based on screen printing technique
Technical field
The humidity sensor prepared the present invention relates to a kind of preparation method of humidity sensor and with this preparation method, especially It is a kind of simplified fabrication schedule, the advantages that low process safety compliance detection limit, high sensitivity, stability are good can be lifted, in the future Practical application in, there is certain application prospect.
Background technology
In air institute it is steam-laden it is how many be called humidity, the humidity in environment and daily life, industrial production, The existence growth of animals and plants has relation closely.The seizure and extraction of humidity information are always all by the extensive pass of people Note.Different biology, plant or things, there is different requirements to the ambient humidity residing for it.It is all kinds of in order to preferably make Things can develop according to the direction of human demand, it is necessary to the humidity environment for making it meet to adapt to, so the detection and control of humidity System, has very important significance to industrial or agricultural, animal husbandry, forestry, building trade, food electronics industry etc..
The material and sensing principle prepared according to sensor, the species of humidity sensor is a lot, can be generally divided into electrolysis Matter humidity sensor, semiconductive ceramic humidity sensor and high molecule humidity sensor three major types.Electrolyte humidity sensors are sent out Exhibition is earliest, but because vapor easily reacts with sensitive material, so as to corrode and aging sensor, so its development and Application surface is narrower;High molecule humidity sensor[6]The latest, but it is (high sensitivity, stability with the excellent properties of uniqueness for starting Good, fast response time etc.) and larger application market, gradually substitute other types sensor, occupy principle market.Profit of the invention Be prepared for the printing ink suitable for silk-screen printing with simple in-situ oxidation reducing process, using screen process press on PET it is double Layer chromatography, prints out the humidity sensor for Humidity Detection.The humidity sensor has low detection limit, high sensitivity, steady The advantages that qualitative good, in the practical application in future, there is certain application prospect.
The content of the invention
The purpose of the present invention is to be directed to presently, there are problem, there is provided a kind of cost is low, preparation method is simple, detection limit The good humidity sensor of low, high sensitivity, stability.
The preparation method of this humidity sensor, it is characterized in that:
1. first being allocated existing silver ink, suitable ink viscosity is mixed, passes through screen process press Pre-rendered good silver-colored interdigital electrode is printed in PET base material.
2. in-situ oxidation reducing process is used to prepare with CuO nano particles and graphene, the composite of multi-walled carbon nanotube.
3. the composite prepared is fully dissolved, and formulated viscosity is to 180-190cP.
4. using screen printing technique by the composite ink prepared to the silver electrode prepared, and true 100 DEG C of drying in empty van.
Composite is made according to above technical scheme, by screen printing technique make humidity sensor have with The advantages of lower:
1. ink prepares material and can bought on the market, ink preparation process meets energy-conservation and subtracted to not needing hot environment Row's demand;
2. small, preparation process is polluted compared with the preparation methods such as traditional etching, sputtering using silk-screen printing production technology Middle environmental condition is easily controlled, and suitable for batch production.
3. production equipment and environmental requirement be not high, production cost is relatively low.
Brief description of the drawings
Fig. 1 is the Nano Silver interdigital electrode of the sensor.
Fig. 2-Fig. 4 is the curve that humidity sensor resistance changes with humidity under the different composite material.Wherein Fig. 2 CuO materials Expect humidity sensor resistance with moisture curve;Fig. 3 is that CuO-MWCNts material humidity sensors resistance changes song with humidity Line;Fig. 4 is CuO-Graphene material humidity sensor resistance with moisture curve.
Fig. 5-Fig. 7 is humidity sensor resistance stability measurement figure under the different composite material.Fig. 5 surveys for CuO stability Spirogram;Fig. 6 is CuO-MWCNts stability measurement figures;Fig. 7 is CuO-Graphene stability measurement figures.
Embodiment
1. print out Nano Silver interdigital electrode on an insulating substrate by screen printing technique first.Comprise the following steps that (1) draw electrode and make web plate;(2) silver ink proportioning is optimized;(3) alcohol washes screen process press is used;(4) with water and Washes of absolute alcohol dries PET base to be printed;(5) printing silver, which is inserted, refers to electrode.
2. sheet CuO powder synthesizes:Manufacturing process is as follows:(1) copper sulphate 5g is taken, magnetic agitation is dissolved completely in 100 millis Rise in water, obtain copper-bath;(2) by 3.2 grams of sodium hydroxide powder, it is dissolved in 50 milliliters of water, magnetic agitation dissolving Afterwards, sodium hydroxide solution is obtained, measures its PH as 12.(3) sodium hydroxide solution obtained in step (2) is added slowly to solution (1) in, magnetic force heating stirring, temperature control at 80 DEG C, reaction 8 hours after, obtain dark solution, by vacuum filtration 100 DEG C After drying, cupric oxide solid is obtained, after grinding, obtains cupric oxide solid powder.
3. other composite materials powder synthesize:CuO-MWCNTs composites make:Synthesize, need relative to CuO powder Acidification is done to the MWCNTs of addition before making:3g carbon nanotube powders are taken, and import the concentrated sulfuric acid that volume ratio is 3: 1 In concentrated nitric acid mixed acid, after ultrasonic disperse 5 hours, acid solution is diluted with water, and black is arrived with using vacuum filtration method Powder.Then the MWCNTs 0.1g and the NaOH solid powders of equal quality added according to method shown in second step after acidifying. CuO-Graphene composites make:Graphene oxide is obtained using Hummer methods, preparation process is:Take graphite solid powder Last 2.5g is simultaneously dissolved in the 60ml concentrated sulfuric acid, and solution is placed in into agitating and heating in oil bath and adds 8g potassium permanganate;At 100 degree Lower heating, and be slowly added to 300 milliliters deionized water and 10 milliliters of hydrogen peroxide, allow its reaction 10 hours after, centrifugal drying, Obtain graphene oxide.Graphene oxide is added in 50 milliliters of water, and mixed solution is placed in reactor, 250 degree add Heat 10 hours, obtains graphene, takes graphene 0.5g and according to method shown in the 2nd step, CuO- is synthesized by liquid phase method Graphene composites.
4. the preparation of printing ink:The powder of above-mentioned 2,3 steps synthesis is added to be stirred by terpinol and ethyl cellulose and mixed In solution after conjunction, by magnetic agitation and carry out cell pulverization obtain viscosity be 188.3cP ink.
5. it is printed substrates to insert finger electrode using the silver prepared in step 1, the printing-ink of foregoing preparation is placed in web plate On, the parameter such as regulation print speed printing speed, print pass is printed, and the sensor produced is placed in vacuum drying chamber into 100 degree Drying one hour, after be put into hermetic bag, kept dry.
In order to examine the effect of manipulation, relative humidity test is carried out to made sensing arrangement and is verified.In experiment Required standard humidity is produced by the saturated solution method of salt.Depressed in a normal atmosphere, when experimental temperature is 25 DEG C, point LiCl, MgCl are not taken2, NaBr, NaCl, KCl, and K2SO4, saturated salt solution realize 11%, 33%, 59%, 75%, 85% and 98% relative humidity (RH), is measured using 4 half universal meters.

Claims (9)

1. a kind of preparation method of humidity sensor, it is characterised in that comprise the following steps:
1. select substrate;
2. print Nano Silver interdigital electrode in substrate surface;
3. make related nano material and its ink;
4. nano material ink is printed to interdigital electrode using screen printing technique;
5. being dried one hour for 100 degree in drying box, the preparation of humidity sensor is completed.
2. the preparation method of the humidity sensor as described in requiring right 1, it is characterised in that wherein the substrate is pet substrate.
3. the preparation method of the humidity sensor as described in requiring right 1, it is characterised in that wherein interdigital electrode uses Nano Silver Ink, disposably printed and formed by screen printing apparatus, wherein interdigital electrode number can be increased and decreased according to design.
4. the preparation method of the humidity sensor as described in requiring right 1, it is characterised in that sheet CuO and its compound nanometer The preparation of material.
A) prepared by sheet CuO nanometer sheet:(1) copper sulphate 5g is taken, magnetic agitation is dissolved completely in 100 milliliters of water, obtains sulfuric acid Copper solution;(2) by 3.2 grams of sodium hydroxide powder, it is dissolved in 50 milliliters of water, after magnetic agitation dissolving, obtains sodium hydroxide Solution, its PH is measured as 12.(3) sodium hydroxide solution obtained in step (2) is added slowly in solution (1), magnetic force heating Stirring, temperature control after reacting 8 hours, obtain dark solution at 80 DEG C, after 100 DEG C of drying of vacuum filtration, obtain black Cupric oxide solid, after grinding, obtain cupric oxide solid powder.
B) CuO-MWCNTs composites make:Synthesized relative to CuO powder, it is necessary to do acid to the MWCNTs of addition before making Change is handled:3g carbon nanotube powders are taken, and are imported in the concentrated sulfuric acid and concentrated nitric acid mixed acid that volume ratio is 3: 1, with ultrasonic disperse 5 After hour, acid solution is diluted with water, and black powder is arrived with using vacuum filtration method.Then according to a) method adds shown in step Enter the NaOH solid powders of MWCNTs 0.1g and equal quality after acidifying.
C) CuO-Graphene composites make:Graphene oxide is obtained using Hummer methods, preparation process is:Take graphite Solid powder 2.5g is simultaneously dissolved in the 60ml concentrated sulfuric acid, and solution is placed in into agitating and heating in oil bath and adds 8g potassium permanganate; Heated under 100 degree, and be slowly added to 300 milliliters deionized water and 10 milliliters of hydrogen peroxide, allow its reaction 10 hours after, from The heart is dried, and obtains graphene oxide.Graphene oxide is added in 50 milliliters of water, and mixed solution is placed in reactor, 250 degree are heated 10 hours, are obtained graphene, are taken graphene 0.5g and according to a) method shown in step, CuO- is synthesized by liquid phase method Graphene composites.
5. the preparation method of the humidity sensor as described in requiring right 1, it is characterised in that used during preparation nano material Ultrasonic disperse technology and magnetic agitation method.
6. the preparation method of the humidity sensor as described in requiring right 1, it is characterised in that CuO and its compound nanometer ink Preparation, each component content is as shown in 2,3 in specification.
7. the preparation method of the humidity sensor as described in requiring right 1, it is characterised in that adopted during preparing nanometer ink With cell pulverization technology.
8. the preparation method of the humidity sensor as described in requiring right 1, it is characterised in that preparation process temperature control is 100 Below degree Celsius.
9. the preparation method of the humidity sensor as described in requiring right 1, it is characterised in that the solvent for preparing ink process is pine Oleyl alcohol and ethyl cellulose.
CN201610443934.1A 2016-06-21 2016-06-21 It is prepared by a kind of gas sensor based on screen printing technique Pending CN107525825A (en)

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CN108802111A (en) * 2018-03-21 2018-11-13 北京旭碳新材料科技有限公司 Miniature gas-sensitive sensor and preparation method thereof
CN109304952A (en) * 2018-09-01 2019-02-05 哈尔滨工程大学 A kind of preparation method of the printable formula temperature sensor of the ionic liquid containing pyrenyl
CN110308013A (en) * 2019-06-18 2019-10-08 山西大学 A kind of mechanically recyclable automatically taking water sampling device
CN110376253A (en) * 2019-07-26 2019-10-25 华中科技大学 A kind of humidity sensor, preparation method and wet sensitive type switch trigger
CN110412487A (en) * 2019-07-31 2019-11-05 电子科技大学 A kind of textile type flexible compound type sensor and preparation method thereof
WO2021180253A1 (en) 2020-03-10 2021-09-16 Západočeská Univerzita V Plzni Humidity sensor for measurement with dc measuring signal and method of its production
CN114088778A (en) * 2021-11-17 2022-02-25 湘潭大学 High-repeatability film type PPB (pentatricopeptide repeats) formaldehyde gas sensor and preparation method thereof

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Cited By (11)

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Publication number Priority date Publication date Assignee Title
CN108802111A (en) * 2018-03-21 2018-11-13 北京旭碳新材料科技有限公司 Miniature gas-sensitive sensor and preparation method thereof
CN109304952A (en) * 2018-09-01 2019-02-05 哈尔滨工程大学 A kind of preparation method of the printable formula temperature sensor of the ionic liquid containing pyrenyl
CN110308013A (en) * 2019-06-18 2019-10-08 山西大学 A kind of mechanically recyclable automatically taking water sampling device
CN110308013B (en) * 2019-06-18 2021-07-02 山西大学 Mechanical type recoverable automatic water sampling device
CN110376253A (en) * 2019-07-26 2019-10-25 华中科技大学 A kind of humidity sensor, preparation method and wet sensitive type switch trigger
CN110376253B (en) * 2019-07-26 2020-11-24 华中科技大学 Humidity sensor, preparation method and humidity-sensitive switch trigger
CN110412487A (en) * 2019-07-31 2019-11-05 电子科技大学 A kind of textile type flexible compound type sensor and preparation method thereof
CN110412487B (en) * 2019-07-31 2021-04-20 电子科技大学 Fabric-type flexible composite sensor and manufacturing method thereof
WO2021180253A1 (en) 2020-03-10 2021-09-16 Západočeská Univerzita V Plzni Humidity sensor for measurement with dc measuring signal and method of its production
CN114088778A (en) * 2021-11-17 2022-02-25 湘潭大学 High-repeatability film type PPB (pentatricopeptide repeats) formaldehyde gas sensor and preparation method thereof
CN114088778B (en) * 2021-11-17 2023-08-29 湘潭大学 High-repeatability film type PPB-level formaldehyde gas sensor and preparation method thereof

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