CN103529085A - Resistance type humidity sensitive material and preparation method thereof - Google Patents
Resistance type humidity sensitive material and preparation method thereof Download PDFInfo
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- CN103529085A CN103529085A CN201310480287.8A CN201310480287A CN103529085A CN 103529085 A CN103529085 A CN 103529085A CN 201310480287 A CN201310480287 A CN 201310480287A CN 103529085 A CN103529085 A CN 103529085A
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Abstract
The invention relates to a resistance type humidity sensitive material and a preparation method thereof. The humidity sensitive material is nano composite oxide consisting of ZnO and Fe2O3. The preparation method comprises the following steps: preparing aqueous solutions respectively from zinc salt and iron salt which are soluble in water and serve as starting materials; mixing the prepared solutions under a proper condition; slowly producing precipitate by adjusting the pH value of the solution; ageing, filtering, washing, drying and grinding; and calcining at high temperature to prepare a nanopowder material. The humidity sensitive material is simple in preparation process, safe and non-toxic, suitable for industrialized production and can be easily used for a long time, can respond quickly and sensitively in the relative humidity range of 7% to 92%, and has the characteristics of high sensitivity, quick response, high stability and the like.
Description
Technical field
The present invention relates to a kind of humidity sensitive material, resistance-type humidity sensitive material especially being formed by ZnO and Fe203 and preparation method thereof.Belong to field of sensing technologies.
Background technology
Humidity means the physical quantity of air drying degree.At a certain temperature, the steam containing in the air of certain volume is many, and air is moister.The dry wet degree of air is called humidity, and the physical quantitys such as conventional absolute humidity, relative humidity, comparison humidity, mixing ratio, saturation deficit and dew point represent.The monitoring of humidity is all very important to many production runes.As the production of the products such as fiber, paper, sensitive film, optical glass, hot pressing part, electronic component, Precision Machinery Elements and cigarette, tea, biscuit and storage damp condition is had to strict requirement; In addition, chamber crop cultivation, cereal and fruit storage, chicken farm and pig farm etc. also all need humidity to control.Humidity data has important guiding reference significance to people's productive life activity decision-making.Relevant moisture measurement, just on the books as far back as 16th century.Many ancient measuring methods, as wet-and-dry bulb thermometer, hair hygrometer and dew point instrument etc. are still widely adopted so far.Modern industrial technology requires high precision, highly reliable and measure continuously humidity, thereby has occurred successively miscellaneous humidity-sensitive element.As: 2011104432123 disclose a kind of electric resistance type humidity sensitive element and preparation method thereof, 2012102131624 disclose a kind of preparation method of zinc paste humidity-sensitive material, and 2012103665633 disclose a kind of moisture sensor based on potassium tantalate sensitive membrane and preparation method thereof etc.The subject matter that at present humidity sensor development faces is that the insufficient sensitivity of humidity-sensitive material is high and long-time stability are poor, thereby, preparation high sensitivity, fast respond and the humidity-sensitive material of high stability significant to the raising of humidity sensor performance.
Summary of the invention
The object of this invention is to provide a kind of resistance-type humidity sensitive material and preparation method thereof.The humidity sensor of making of this sensitive material, has highly sensitive, response rapidly and the feature such as good stability.
Resistance-type humidity sensitive material of the present invention is by ZnO and Fe
2o
3the nano-powder forming, preparation method is: take zinc salt soluble in water and molysite makes respectively stable aqueous solution as initiation material, the above solution of preparation is mixed under proper condition, by regulator solution pH value, slowly generate precipitation, after ageing, filtration, washing, oven dry and grinding, by high-temperature calcination, make nano-powder material.Wherein zinc salt is one or more potpourri of the anhydride of zinc chloride, zinc sulfate, zinc nitrate, zinc perchlorate, zinc dihydrogen phosphate and zinc acetate or hydrate; Molysite is one or more potpourri of the anhydride of iron chloride, ferric perchlorate, iron sulfate and ferric nitrate or hydrate.
Optimum humidity sensitive material of the present invention is made by following technique.The amount that is 30～45:100 by the atomic ratio of Zn and Fe takes respectively zinc salt and molysite, and be dissolved in respectively etc. in the aqueous hydrochloric acid solution of massfraction 5%～10% of weight, after being heated to respectively to 40 ℃, mix two solution, keep under temperature continuous stirring, slowly drip the ammoniacal liquor of massfraction 15-25%, dripping quantity is 1/5～1/3 of mixed liquor weight, rate of addition be two second l drip, after being added dropwise to complete, be cooled to room temperature, continue to stir 1 hour, standing 5 hours, to precipitate filtration under diminished pressure and use deionized water washed twice, in 105 ℃, dry 2 hours, after fully grinding, in high temperature box type resistance furnace, with per minute, be no more than the speed of 4 ℃ and be warming up to 390 ℃, and this temperature lower calcination 5 hours, obtain by ZnO and Fe
2o
3the nano-powder material forming.
The powder body material making is carried out to granularity and constituent analysis, and when powder body material particle diameter is no more than 60nm, and the mass percent of ZnO is while being 12%-20%, as humidity sensitive material, has highly sensitive, response rapidly and the feature such as good stability.
Tool of the present invention has the following advantages:
(1) gained humidity sensitive material can be made response and the recovery of rapid sensitive within the scope of relative humidity 7%-92%;
(2) gained sensitive material is composite metal oxide, and safety non-toxic is easy to long preservation and use;
(3) preparation technology of the present invention is simple, and raw material is easy to get, and operating conditions is gentle, is applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the resonse characteristic by the humidity sensor of embodiment 1 gained humidity sensitive material making.
Fig. 2 is the resonse characteristic by the humidity sensor of embodiment 2 gained humidity sensitive materials making.
Fig. 3 is the resonse characteristic by the humidity sensor of embodiment 3 gained humidity sensitive materials making.
Fig. 4 is the resonse characteristic by the humidity sensor of embodiment 4 gained humidity sensitive materials making.
Fig. 5 is the resonse characteristic by the humidity sensor of embodiment 5 gained humidity sensitive materials making.
Embodiment
Embodiment 1
The amount that is 35:100 by the atomic ratio of Zn and Fe takes respectively two water zinc chloride and Iron trichloride hexahydrates, and be dissolved in respectively etc. in the aqueous hydrochloric acid solution of massfraction 6% of weight, after being heated to respectively to 40 ℃, mix two solution, keep under temperature continuous stirring, slowly drip the ammoniacal liquor of massfraction 20%, dripping quantity is the l/3 of mixed liquor weight, rate of addition is 1 of two second, after being added dropwise to complete, be cooled to room temperature, continue to stir l hour, standing 5 hours, to precipitate filtration under diminished pressure and use deionized water washed twice, in 105 ℃, dry 2 hours, after fully grinding, in high temperature box type resistance furnace, with per minute, be no more than the speed of 4 ℃ and be warming up to 390 ℃, and this temperature lower calcination 5 hours, obtain the nano-powder material being formed by ZnO and Fe203.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is no more than 55nm; It is carried out to constituent analysis, and the mass percent that records ZnO is 14.05%.
Application: using this powder body material makes the film of 3 micron thick in golden interdigital electrode as humidity sensitive material, the resonse characteristic of this sensor is shown in Fig. 1.
Embodiment 2
The amount that is 40:100 by the atomic ratio of Zn and Fe takes respectively four water zinc sulphates and nine water ferric perchlorates, and be dissolved in respectively etc. in the aqueous hydrochloric acid solution of massfraction 9% of weight, after being heated to respectively to 40 ℃, mix two solution, keep under temperature continuous stirring, slowly drip the ammoniacal liquor of massfraction 22%, dripping quantity is the l/4 of mixed liquor weight, rate of addition is 1 of two second, after being added dropwise to complete, be cooled to room temperature, continue to stir l hour, standing 5 hours, to precipitate filtration under diminished pressure and use deionized water washed twice, in 105 ℃, dry 2 hours, after fully grinding, in high temperature box type resistance furnace, with per minute, be no more than the speed of 4 ℃ and be warming up to 390 ℃, and this temperature lower calcination 5 hours, obtain by ZnO and Fe
2o
3the nano-powder material forming.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is no more than 60nm; It is carried out to constituent analysis, and the mass percent that records ZnO is 16.39%.
Application: using this powder body material makes the film of 2.8 micron thick in golden interdigital electrode as humidity sensitive material, the resonse characteristic of this sensor is shown in Fig. 2.
Embodiment 3
The amount that is 30:100 by the atomic ratio of Zn and Fe takes respectively zinc nitrate hexahydrate and anhydrous ironic sulfate, and be dissolved in respectively etc. in the aqueous hydrochloric acid solution of massfraction 7% of weight, after being heated to respectively to 40 ℃, mix two solution, keep under temperature continuous stirring, slowly drip the ammoniacal liquor of massfraction 18%, dripping quantity is 1/3 of mixed liquor weight, rate of addition is 1 of two second, after being added dropwise to complete, be cooled to room temperature, continue to stir 1 hour, standing 5 hours, to precipitate filtration under diminished pressure and use deionized water washed twice, in 105 ℃, dry 2 hours, after fully grinding, in high temperature box type resistance furnace, with per minute, be no more than the speed of 4 ℃ and be warming up to 390 ℃, and this temperature lower calcination 5 hours, obtain by ZnO and Fe
2o
3the nano-powder material forming.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is no more than 50nm; It is carried out to constituent analysis, and the mass percent that records ZnO is 13.54%.
Application: using this powder body material makes the film of 4 micron thick in golden interdigital electrode as humidity sensitive material, the resonse characteristic of this sensor is shown in Fig. 3.
Embodiment 4
The amount that is 45:100 by the atomic ratio of Zn and Fe takes respectively perchlorate hexahydrate's zinc and nine water ferric nitrates, and be dissolved in respectively etc. in the aqueous hydrochloric acid solution of massfraction 8% of weight, after being heated to respectively to 40 ℃, mix two solution, keep under temperature continuous stirring, slowly drip the ammoniacal liquor of massfraction 24%, dripping quantity is the l/5 of mixed liquor weight, rate of addition is 1 of two second, after being added dropwise to complete, be cooled to room temperature, continue to stir 1 hour, standing 5 hours, to precipitate filtration under diminished pressure and use deionized water washed twice, in 105 ℃, dry 2 hours, after fully grinding, in high temperature box type resistance furnace, with per minute, be no more than the speed of 4 ℃ and be warming up to 390 ℃, and this temperature lower calcination 5 hours, obtain the nano-powder material being formed by ZnO and Fe203.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is no more than 60nm; It is carried out to constituent analysis, and the mass percent that records ZnO is 19.08%.
Application: using this powder body material makes the film of 2.5 micron thick in golden interdigital electrode as humidity sensitive material, the resonse characteristic of this sensor is shown in Fig. 4.
Embodiment 5
The amount that is 42:100 by the atomic ratio of Zn and Fe takes respectively zinc dihydrogen phosphate, zinc acetate dihydrate, iron chloride and ferric nitrate, and be dissolved in respectively etc. in the aqueous hydrochloric acid solution of massfraction 7% of weight, after being heated to respectively to 40 ℃, mix two solution, keep under temperature continuous stirring, slowly drip the ammoniacal liquor of massfraction 20%, dripping quantity is 1/4 of mixed liquor weight, rate of addition is 1 of two second, after being added dropwise to complete, be cooled to room temperature, continue to stir 1 hour, standing 5 hours, to precipitate filtration under diminished pressure and use deionized water washed twice, in 105 ℃, dry 2 hours, after fully grinding, in high temperature box type resistance furnace, with per minute, be no more than the speed of 4 ℃ and be warming up to 390 ℃, and this temperature lower calcination 5 hours, obtain by ZnO and Fe
2o
3the nano-powder material forming.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is no more than 55nm; It is carried out to constituent analysis, and the mass percent that records ZnO is 17.72%.
Application: using this powder body material makes the film of 3 micron thick in golden interdigital electrode as humidity sensitive material, the resonse characteristic of this sensor is shown in Fig. 5.
Claims (3)
1. resistance-type humidity sensitive material and preparation method thereof, is characterized in that by ZnO and Fe
2o
3the nano composite oxide forming, wherein the mass percent of ZnO is 12%-20%, its preparation method is: the amount that is 30-45:100 by the atomic ratio of Zn and Fe takes respectively zinc salt soluble in water and molysite, and be dissolved in respectively etc. in the aqueous hydrochloric acid solution of massfraction 5%-10% of weight, after being heated to respectively to 40 ℃, mix two solution, keep under temperature continuous stirring, slowly drip the ammoniacal liquor of massfraction 15%-25%, dripping quantity is the 1/5-1/3 of mixed liquor weight, rate of addition is 1 of two second, after being added dropwise to complete, be cooled to room temperature, continue to stir 1 hour, standing 5 hours, to precipitate filtration under diminished pressure and use deionized water washed twice, in 105 ℃, dry 2 hours, after fully grinding, in high temperature box type resistance furnace, with per minute, be no more than the speed of 4 ℃ and be warming up to 390 ℃, and this temperature lower calcination 5 hours, obtain by ZnO and Fe
2o
3the resistance-type humidity sensitive material forming.
2. resistance-type humidity sensitive material according to claim 1 and preparation method thereof, is characterized in that described zinc salt is one or more potpourri of the anhydride of zinc chloride, zinc sulfate, zinc nitrate, zinc perchlorate, zinc dihydrogen phosphate and zinc acetate or hydrate; Molysite is one or more potpourri of the anhydride of iron chloride, ferric perchlorate, iron sulfate and ferric nitrate or hydrate.
3. according to resistance-type humidity sensitive material described in claim l and preparation method thereof, it is characterized in that the particle diameter of described humidity sensitive material is no more than 60nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107884451A (en) * | 2017-11-07 | 2018-04-06 | 潘柏霖 | A kind of device that can quickly, accurately detect ambient humidity |
| CN108490037A (en) * | 2018-02-09 | 2018-09-04 | 梧州井儿铺贸易有限公司 | A kind of printer that can show humidity |
| CN109030484A (en) * | 2018-08-30 | 2018-12-18 | 湘潭大学 | A kind of colorimetric humidity sensitive material and preparation method thereof and a kind of colorimetric humidity sensor |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107884451A (en) * | 2017-11-07 | 2018-04-06 | 潘柏霖 | A kind of device that can quickly, accurately detect ambient humidity |
| CN107884451B (en) * | 2017-11-07 | 2020-07-14 | 中创新海(天津)认证服务有限公司 | Device capable of rapidly and accurately detecting environment humidity |
| CN108490037A (en) * | 2018-02-09 | 2018-09-04 | 梧州井儿铺贸易有限公司 | A kind of printer that can show humidity |
| CN109030484A (en) * | 2018-08-30 | 2018-12-18 | 湘潭大学 | A kind of colorimetric humidity sensitive material and preparation method thereof and a kind of colorimetric humidity sensor |
| CN109030484B (en) * | 2018-08-30 | 2021-02-05 | 湘潭大学 | Colorimetric humidity sensor |
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| CN103529085B (en) | 2016-07-06 |
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