CN105891266A - Preparation method of humidity sensing material - Google Patents

Preparation method of humidity sensing material Download PDF

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Publication number
CN105891266A
CN105891266A CN201610186972.3A CN201610186972A CN105891266A CN 105891266 A CN105891266 A CN 105891266A CN 201610186972 A CN201610186972 A CN 201610186972A CN 105891266 A CN105891266 A CN 105891266A
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CN
China
Prior art keywords
solution
humidity sensor
preparation
humidity
sensor material
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CN201610186972.3A
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Chinese (zh)
Inventor
包磊
肖学良
包松
包宇洲
周思佳
汪亮
汪理
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Individual
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Priority to CN201610186972.3A priority Critical patent/CN105891266A/en
Priority to PCT/CN2016/096220 priority patent/WO2017166601A1/en
Publication of CN105891266A publication Critical patent/CN105891266A/en
Pending legal-status Critical Current

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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
    • G01N27/02Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • 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
    • G01N27/02Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/048Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance for determining moisture content of the material

Abstract

The invention discloses a preparation method of a humidity sensing material. The humidity sensing material based on lithium bromide/polyvinyl alcohol/barium titanate is prepared by using a mixed solution of barium acetate, ethanol, acetic acid, deionized water, butyl titanate, polyvinylpyrrolidone, polyvinyl alcohol and lithium bromide. The humidity sensing material is the composite material. The humidity response range is widened, and the relative humidity becomes 98% from 10%. A ceramic-based humidity response material is added, and therefore the response time of original pure lithium chloride series humidity response is shortened; conductive fiber filaments replaces original metal wires, the pin part of the humidity sensing material is softened, and the sensor can be more easily woven into fabric and put into clothes.

Description

A kind of preparation method of humidity sensor material
Technical field
The present invention relates to humidity sensor technical field, in particular, relate to the preparation method of a kind of humidity sensor material.
Background technology
In textile garment field, humiture is the important indicator affecting wearer's comfort level.Particularly when apparel applications is in Aero-Space, wearable electronic, deep ocean work etc., the humidity controlled between health and clothes in microenvironment is particularly important, because under the uncontrollable damp condition of staff, there is sensor senses and make clothes make humidity regulation, the intelligent of clothing can be made to greatly improve, and the range of application of clothing is the most more flexible.
Lithium chloride is to disclose most materials being applied to humidity sensor, such as CN2055247U, CN85200517U, CN101178372B, CN102269693B, CN102967631A, CN104483453A, CN1024725829A, CN203188087U, CN204496297U etc., patent disclosed in such, it is all the change utilizing lithium chloride that the sensitivity of humidity causes resistance, and obtains humidity value in surrounding air.It addition, also graphene nano wall humidity sensor (CN204359739U), Ceramic Humidity Sensor (CN102435636A) etc..But so far, humidity sensor is all the module being made into bulk, and the fibrous humidity sensor inweaving clothes have not been reported.
Summary of the invention
Technical task to be solved by this invention is, it is provided that the preparation method of a kind of humidity sensor material, solves the flexible problem that existing humidity sensor can not inweave in cloth textile.
The present invention solves the technical scheme of the problems referred to above: provides the preparation method of a kind of humidity sensor material, comprises the steps:
S1, by Barium acetate: ethanol: acetic acid: deionized water is by weight (1.5~2): (4~6): (3~5): 1 stirring mixing;It is subsequently adding the butyl titanate that weight ratio is (1.5~2.5), stirring mixing;Adding the polyvinylpyrrolidone that weight ratio is (3~3.5), stirring is mixed to get solution A;
Adding weight ratio in S2, described solution A is 1: the polyvinyl alcohol of (0.3~0.5) and lithium bromide mixed solution, and stirring is mixed to get solution B;Wherein, this polyvinyl alcohol is (0.3~0.5) with the weight ratio of lithium bromide mixed solution with described solution A: 1;
S3, gained solution B are injected in mould, insert in baking oven and solidify, and condition of cure is the temperature environment of 40~60 DEG C, and hardening time is 2~5 hours, remove mould and obtain idiosome after solidification;
S4, described idiosome is inserted in 150 DEG C~200 DEG C of environment 3~5 hours, form humidity sensor material.
In the preparation method of the humidity sensor material of present invention offer, in described step S2, described polyvinyl alcohol is 0.4: 1 with the weight ratio of lithium bromide mixed solution with described solution A.
In the preparation method of the humidity sensor material of present invention offer, in described step S3, described mould has at least two aperture, inserts a compliant conductive fiber in each described aperture, the one end making this compliant conductive fiber is immersed in solution B, and the other end is positioned at outside mould.
In the preparation method of the humidity sensor material of present invention offer, described compliant conductive fiber also included pre-treatment step before inserting aperture, described pre-treatment step includes: is placed in hydrogen peroxide dipping and removes the charged ion on surface, is subsequently placed in cleaning and dipping in distilled water.
In the preparation method of the humidity sensor material of present invention offer, idiosome and the junction of described compliant conductive fiber, use stannum or indium electric welding to strengthen binding strength.
Implement the present invention, have the advantages that
(1) humidity sensor material is composite, and humidity response range broadens, from relative humidity 10% to 98%;
(2) the wet responsive materials of ceramic base adds, and improves the response time of the original purely lithium chloride wet response of series;
(3) conductive fiber long filament replaces original tinsel so that the pin portions flexibility of humidity sensor material, it is easier to inweave in fabric by such sensor, accomplish in clothing.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, the accompanying drawing used required in embodiment or description of the prior art will be briefly described below.It should be evident that the accompanying drawing in describing below is only some embodiments of the present invention, for those skilled in the art, on the premise of without paying creative work, it is also possible to obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the flow chart of the preparation method of humidity sensor material;
Fig. 2 is the process route chart of the preferred embodiment of the preparation method of humidity sensor material;
Fig. 3 is that humidity sensor material is along with the detection device of the change of humidity;
Fig. 4 is the relative impedances rate of change that humidity sensor material produces along with the change of humidity.
Detailed description of the invention
Below in conjunction with embodiment, the technical scheme in the embodiment of the present invention is clearly and completely described.
Humidity sensor prepared by prior art has that response speed is slow, the feature such as wet sense region little (20%RH to 70%), the most also lacks the humidity sensor of flexible fiber shape.
The main innovation point of the present invention is, it is provided that the preparation method of a kind of humidity sensor material, prepares humidity sensor material based on lithium bromide/polyvinyl alcohol/Barium metatitanate., and humidity response range broadens, and the response time of wet response shortens significantly.
Fig. 1 shows the flow chart of the preparation method of humidity sensor material, as it is shown in figure 1, the preparation method of the humidity sensor material of the present invention, comprises the steps:
S1, by Barium acetate: ethanol: acetic acid: deionized water is by weight (1.5~2): (4~6): (3~5): 1 stirring mixing;It is subsequently adding the butyl titanate that weight ratio is (1.5~2.5), stirring mixing;Adding the polyvinylpyrrolidone that weight ratio is (3~3.5), stirring is mixed to get solution A;
Adding weight ratio in S2, described solution A is 1: the polyvinyl alcohol of (0.3~0.5) and lithium bromide mixed solution, and stirring is mixed to get solution B;Wherein, this polyvinyl alcohol is (0.3~0.5) with the weight ratio of lithium bromide mixed solution with described solution A: 1;
S3, gained solution B are injected in mould, insert in baking oven and solidify, and condition of cure is the temperature environment of 40~60 DEG C, and hardening time is 2~5 hours, remove mould and obtain idiosome after solidification;
S4, described idiosome is inserted in 150 DEG C~200 DEG C of environment 3 hours, form humidity sensor material.
Preferably, in step S2, polyvinyl alcohol is 0.4: 1 with the weight ratio of lithium bromide mixed solution with solution A.In step S3, mould has at least two aperture, inserts a compliant conductive fiber so that one end of this compliant conductive fiber is immersed in solution, and the other end is positioned at outside mould in each aperture.
Embodiment
The preparation method of the humidity sensor material of the present embodiment, comprises the steps:
(1) by weight proportion by Barium acetate: ethanol: acetic acid: deionized water is equal to (1.5~2): (4~6): (3~5): 1 wiring solution-forming, mix and blend 1 hour, add the butyl titanate that weight ratio is (1.5~2.5), continue to stir half an hour, add the polyvinylpyrrolidone that weight ratio is (3~3.5), stir two hours, obtain solution A.Adding weight ratio is 1:(0.3~0.5) polyvinyl alcohol and lithium bromide mixed solution, stirring is mixed to get solution B, and wherein, this mixed solution is (0.3~0.5) with the weight ratio of solution A: 1;Fig. 2 shows the process route chart of the preferred embodiment of the preparation method of humidity sensor material, as shown in Figure 2, being injected by last mixed solution 1 in a spherical module 2 (a diameter of 5~10mm), this spherical die 2 has two parallel apertures, such as Fig. 2 (a).Prepare two compliant conductive fibers 3 (the most silver-plated nylon yarn or ultra-fine copper wire, 70~120 daniers), at a temperature of 30 DEG C, it is positioned in hydrogen peroxide 1~5 minute, remove the charged ion of fiber surface, then two fibers are placed in distilled water cleaning and dipping 10~20 minutes, the most again two threads are respectively placed in the aperture of mould, two fiber parts in spherical die can not contact, as shown in schematic diagram 2 (b).
(2) being inserted by the spherical die containing solution and conductive fiber in the baking oven of 40~60 DEG C, solvent volatilizees, and solution solidifies, and becomes the spherical sensors containing two conductive fibers, as shown in schematic diagram 2 (c).General 2 to 5 hours of this setting time.
(3) spherical sensors is inserted in 150 DEG C~200 DEG C of environment 3~5 hours so that polyvinylpyrrolidone slowly decomposes, and forms porous Barium metatitanate ./polyvinyl alcohol/lithium bromide composite.If this sphere material is the highest with the bond strength of conductive fiber, with stannum or indium in the position electric welding that both combine once binding strength can be strengthened.
(4) Fig. 3 shows that humidity sensor material is along with the detection device of the change of humidity, as shown in Figure 3, the humidity sensor of fibre morphology is connected with 2K Ω rheostat, add 10V power supply, tester impedance response-return curve is along with the situation of change of relative humidity, result shows that response-turnaround time is all in 1 second, Fig. 4 shows the relative impedances rate of change that humidity sensor material produces along with the change of humidity, as shown in Fig. 4, this fibre moisture sensing material can respond between relative humidity 10% to 98%, humidity response range broadens, as can be seen here, this fibre moisture sensor not only has quickly response process, and there is high sensitivity.
Specified otherwise, above technical scheme is needed to be merely to illustrate the present invention rather than limit the scope of the present invention.Additionally, after having read present disclosure, the present invention can be made change or amendment by those skilled in the art, and these equivalent form of values are equally within the application appended claims limited range.

Claims (5)

1. the preparation method of a humidity sensor material, it is characterised in that comprise the steps:
S1, by Barium acetate: ethanol: acetic acid: deionized water is by weight (1.5~2): (4~6): (3~5): 1 stirring mixing;Being subsequently adding the butyl titanate that weight ratio is (1.5~2.5), stirring is mixed Close;Adding the polyvinylpyrrolidone that weight ratio is (3~3.5), stirring is mixed to get solution A;
Adding weight ratio in S2, described solution A is 1: the polyvinyl alcohol of (0.3~0.5) and lithium bromide Mixed solution, stirring is mixed to get solution B;Wherein, this polyvinyl alcohol and lithium bromide mixed solution and institute The weight ratio stating solution A is (0.3~0.5): 1;
S3, gained solution B are injected in mould, insert in baking oven and solidify, and condition of cure is 40~60 DEG C Temperature environment, hardening time is 2~5 hours, removes mould and obtain idiosome after solidification;
S4, described idiosome is inserted in 150 DEG C~200 DEG C of environment 3~5 hours, form humidity sensor material Material.
The preparation method of humidity sensor material the most according to claim 1, it is characterised in that described In step S2, described polyvinyl alcohol is 0.4: 1 with the weight ratio of lithium bromide mixed solution with described solution A.
The preparation method of humidity sensor material the most according to claim 1, it is characterised in that described In step S3, described mould has at least two aperture, inserts a flexibility and lead in each described aperture Electricity fiber so that one end of this compliant conductive fiber is immersed in solution B, and the other end is positioned at outside mould.
The preparation method of humidity sensor material the most according to claim 3, it is characterised in that described Compliant conductive fiber also included pre-treatment step before inserting aperture, and described pre-treatment step includes: put Remove the charged ion on surface in hydrogen peroxide dipping, be subsequently placed in cleaning and dipping in distilled water.
The preparation method of humidity sensor material the most according to claim 4, it is characterised in that idiosome With the junction of described compliant conductive fiber, use stannum or indium electric welding to strengthen binding strength.
CN201610186972.3A 2016-03-29 2016-03-29 Preparation method of humidity sensing material Pending CN105891266A (en)

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CN201610186972.3A CN105891266A (en) 2016-03-29 2016-03-29 Preparation method of humidity sensing material
PCT/CN2016/096220 WO2017166601A1 (en) 2016-03-29 2016-08-22 Preparation method for humidity-sensing material

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CN108693218A (en) * 2018-03-23 2018-10-23 天津大学 A kind of intelligent aggregate perceiving hydraulic structure inner aqueous information
CN109881365A (en) * 2019-02-18 2019-06-14 青岛海赛尔新材料科技有限公司 Graphene alginate composite nano fiber and its preparation method and application

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CN109881365A (en) * 2019-02-18 2019-06-14 青岛海赛尔新材料科技有限公司 Graphene alginate composite nano fiber and its preparation method and application
CN109881365B (en) * 2019-02-18 2020-07-03 青岛海赛尔新材料科技有限公司 Graphene alginate composite nanofiber and preparation method and application thereof

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