CN103529085B - Resistance type humidity sensitive material and preparation method thereof - Google Patents
Resistance type humidity sensitive material and preparation method thereof Download PDFInfo
- Publication number
- CN103529085B CN103529085B CN201310480287.8A CN201310480287A CN103529085B CN 103529085 B CN103529085 B CN 103529085B CN 201310480287 A CN201310480287 A CN 201310480287A CN 103529085 B CN103529085 B CN 103529085B
- Authority
- CN
- China
- Prior art keywords
- sensitive material
- zinc
- humidity sensitive
- hours
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The present invention relates to a kind of resistance type humidity sensitive material and preparation method thereof, humidity sensitive material is by ZnO and Fe203The nano composite oxide of composition, its preparation method is: be respectively prepared stable aqueous solution with zinc salt soluble in water and iron salt for initiation material, the above solution of preparation is mixed under proper condition, precipitation is slowly generated by regulating solution ph, aged, filter, washing, dry and grind after, make nano-powder material by high-temperature calcination.Preparation technology is simple for this humidity sensitive material, safety non-toxic, it is suitable for industrialized production and is prone to life-time service, response and the recovery of rapid sensitive can be made in relative humidity 7% one 92% scope, the humidity sensor made of this sensitive material, has highly sensitive, response rapidly and the feature such as good stability.
Description
Technical field
The present invention relates to a kind of humidity sensitive material, resistance type humidity sensitive material being especially made up of and preparation method thereof ZnO and Fe203.Belong to field of sensing technologies.
Background technology
Humidity indicates that the physical quantity of air drying degree.At a certain temperature, the steam contained in the air of certain volume is many, then air is more moist.Air dry and wet degree is called humidity, conventional absolute humidity, relative humidity, compares the physical quantitys such as humidity, mixing ratio, saturation deficit and dew point and represents.The monitoring of humidity is all particularly significant to many production processes.Damp condition is had strict requirement by production and storage such as products such as fiber, paper, photographic film, optical glass, hot pressing part, electronic component, Precision Machinery Elements and cigarette, tea, cookiess；Additionally, chamber crop cultivation, corn and fruit storage, chicken farm and pig farm etc. are also required for humid control.The productive life activity decision of people is had important guiding reference significance by humidity data.Relevant moisture measurement, just on the books as far back as 16th century.Many ancient measuring methods, are still widely adopted so far such as psychrometer, hair hygrometer and dew point instrument etc..Modern industrial technology requires high accuracy, highly reliable and measure humidity continuously, thus occur in that miscellaneous dew cell successively.As: 2011104432123 disclose a kind of electric resistance type humidity sensitive element and preparation method thereof, 2012102131624 preparation methoies disclosing a kind of zinc oxide humidity-sensitive material, 2012103665633 disclose a kind of moisture sensor based on potassium tantalite sensitive membrane and preparation method thereof etc..The insufficient sensitivity that the subject matter that the development of current humidity sensor faces is humidity-sensitive material is high poor with long-time stability, thus, preparation high sensitivity, the quickly humidity-sensitive material of response and high stability are significant to the raising of humidity sensor performance.
Summary of the invention
It is an object of the invention to provide a kind of resistance type humidity sensitive material and preparation method thereof.The humidity sensor made 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 Fe2O3The nano-powder of composition, preparation method is: be respectively prepared stable aqueous solution with zinc salt soluble in water and iron salt for initiation material, the above solution of preparation is mixed under proper condition, precipitation is slowly generated by regulating solution ph, aged, filter, washing, dry and grind after, make nano-powder material by high-temperature calcination.Wherein zinc salt is the mixture of one or more of the anhydride of zinc chloride, zinc sulfate, zinc nitrate, zinc perchlorate, zinc dihydrogen phosphate and zinc acetate or hydrate；Iron salt is the mixture of one or more of the anhydride of iron chloride, ferric perchlorate, iron sulfate and ferric nitrate or hydrate.
The optimum humidity sensitive material of the present invention is made by following technique.Zinc salt and iron salt is weighed respectively by the amount that the atomic ratio of Zn and Fe is 30～45:100, and it is dissolved in etc. in the aqueous hydrochloric acid solution of mass fraction 5%～10% of weight respectively, mix after two solution are separately heated to 40 DEG C, keep temperature and be stirred continuously down, it is slowly added dropwise the ammonia of mass fraction 15-25%, dripping quantity is the 1/5～1/3 of mixed liquor weight, rate of addition is that two seconds l drip, after being added dropwise to complete, it is cooled to room temperature, continue stirring 1 hour, stand 5 hours, will precipitation filtration under diminished pressure with deionized water wash twice, dry 2 hours in 105 DEG C, after being fully ground, high temperature box type resistance furnace is warming up to 390 DEG C with the speed less than 4 DEG C per minute, and calcine 5 hours at this temperature, namely obtain by ZnO and Fe2O3The nano-powder material of composition.
Prepared powder body material is carried out granularity and component analysis, when powder body material particle diameter is less than 60nm, and when the mass percent of ZnO is 12%-20%, there is highly sensitive, response rapidly and the feature such as good stability as humidity sensitive material.
Present invention have the advantage that
(1) gained humidity sensitive material can make response and the recovery of rapid sensitive within the scope of relative humidity 7%-92%；
(2) gained sensitive material is metal composite oxide, safety non-toxic, it is easy to long-term preservation and use；
(3) preparation technology of the present invention is simple, and raw material is easy to get, and operating condition is gentle, is suitable for industrialized production.
Accompanying drawing explanation
Fig. 1 is the resonse characteristic of the humidity sensor made by embodiment 1 gained humidity sensitive material.
Fig. 2 is the resonse characteristic of the humidity sensor made by embodiment 2 gained humidity sensitive material.
Fig. 3 is the resonse characteristic of the humidity sensor made by embodiment 3 gained humidity sensitive material.
Fig. 4 is the resonse characteristic of the humidity sensor made by embodiment 4 gained humidity sensitive material.
Fig. 5 is the resonse characteristic of the humidity sensor made by embodiment 5 gained humidity sensitive material.
Detailed description of the invention
Embodiment 1
Two water zinc chloride and Iron trichloride hexahydrates are weighed respectively by the amount that the atomic ratio of Zn and Fe is 35:100, and it is dissolved in etc. in the aqueous hydrochloric acid solution of mass fraction 6% of weight respectively, mix after two solution are separately heated to 40 DEG C, keep temperature and be stirred continuously down, it is slowly added dropwise the ammonia of mass fraction 20%, dripping quantity is the l/3 of mixed liquor weight, rate of addition be two seconds 1, after being added dropwise to complete, it is cooled to room temperature, continue stirring l hour, stand 5 hours, will precipitation filtration under diminished pressure with deionized water wash twice, dry 2 hours in 105 DEG C, after being fully ground, high temperature box type resistance furnace is warming up to 390 DEG C with the speed less than 4 DEG C per minute, and calcine 5 hours at this temperature, namely the nano-powder material being made up of ZnO and Fe203 is obtained.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is less than 55nm；It is carried out component analysis, and the mass percent recording ZnO is 14.05%.
Application: making thin film 3 microns thick as humidity sensitive material using this powder body material in gold interdigital electrode, the resonse characteristic of this sensor is shown in Fig. 1.
Embodiment 2
Four water zinc sulphates and nine water ferric perchlorate are weighed respectively by the amount that the atomic ratio of Zn and Fe is 40:100, and it is dissolved in etc. in the aqueous hydrochloric acid solution of mass fraction 9% of weight respectively, mix after two solution are separately heated to 40 DEG C, keep temperature and be stirred continuously down, it is slowly added dropwise the ammonia of mass fraction 22%, dripping quantity is the l/4 of mixed liquor weight, rate of addition be two seconds 1, after being added dropwise to complete, it is cooled to room temperature, continue stirring l hour, stand 5 hours, will precipitation filtration under diminished pressure with deionized water wash twice, dry 2 hours in 105 DEG C, after being fully ground, high temperature box type resistance furnace is warming up to 390 DEG C with the speed less than 4 DEG C per minute, and calcine 5 hours at this temperature, namely obtain by ZnO and Fe2O3The nano-powder material of composition.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is less than 60nm；It is carried out component analysis, and the mass percent recording ZnO is 16.39%.
Application: making thin film 2.8 microns thick as humidity sensitive material using this powder body material in gold interdigital electrode, the resonse characteristic of this sensor is shown in Fig. 2.
Embodiment 3
Zinc nitrate hexahydrate and anhydrous ironic sulfate is weighed respectively by the amount that the atomic ratio of Zn and Fe is 30:100, and it is dissolved in etc. in the aqueous hydrochloric acid solution of mass fraction 7% of weight respectively, mix after two solution are separately heated to 40 DEG C, keep temperature and be stirred continuously down, it is slowly added dropwise the ammonia of mass fraction 18%, dripping quantity is the 1/3 of mixed liquor weight, rate of addition be two seconds 1, after being added dropwise to complete, it is cooled to room temperature, continue stirring 1 hour, stand 5 hours, will precipitation filtration under diminished pressure with deionized water wash twice, dry 2 hours in 105 DEG C, after being fully ground, high temperature box type resistance furnace is warming up to 390 DEG C with the speed less than 4 DEG C per minute, and calcine 5 hours at this temperature, namely obtain by ZnO and Fe2O3The nano-powder material of composition.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is less than 50nm；It is carried out component analysis, and the mass percent recording ZnO is 13.54%.
Application: making thin film 4 microns thick as humidity sensitive material using this powder body material in gold interdigital electrode, the resonse characteristic of this sensor is shown in Fig. 3.
Embodiment 4
Perchlorate hexahydrate's zinc and nine water ferric nitrates are weighed respectively by the amount that the atomic ratio of Zn and Fe is 45:100, and it is dissolved in etc. in the aqueous hydrochloric acid solution of mass fraction 8% of weight respectively, mix after two solution are separately heated to 40 DEG C, keep temperature and be stirred continuously down, it is slowly added dropwise the ammonia of mass fraction 24%, dripping quantity is the l/5 of mixed liquor weight, rate of addition be two seconds 1, after being added dropwise to complete, it is cooled to room temperature, continue stirring 1 hour, stand 5 hours, will precipitation filtration under diminished pressure with deionized water wash twice, dry 2 hours in 105 DEG C, after being fully ground, high temperature box type resistance furnace is warming up to 390 DEG C with the speed less than 4 DEG C per minute, and calcine 5 hours at this temperature, namely the nano-powder material being made up of ZnO and Fe203 is obtained.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is less than 60nm；It is carried out component analysis, and the mass percent recording ZnO is 19.08%.
Application: making thin film 2.5 microns thick as humidity sensitive material using this powder body material in gold interdigital electrode, the resonse characteristic of this sensor is shown in Fig. 4.
Embodiment 5
Zinc dihydrogen phosphate is weighed respectively by the amount that the atomic ratio of Zn and Fe is 42:100, zinc acetate dihydrate, iron chloride and ferric nitrate, and it is dissolved in etc. in the aqueous hydrochloric acid solution of mass fraction 7% of weight respectively, mix after two solution are separately heated to 40 DEG C, keep temperature and be stirred continuously down, it is slowly added dropwise the ammonia of mass fraction 20%, dripping quantity is the 1/4 of mixed liquor weight, rate of addition be two seconds 1, after being added dropwise to complete, it is cooled to room temperature, continue stirring 1 hour, stand 5 hours, will precipitation filtration under diminished pressure with deionized water wash twice, dry 2 hours in 105 DEG C, after being fully ground, high temperature box type resistance furnace is warming up to 390 DEG C with the speed less than 4 DEG C per minute, and calcine 5 hours at this temperature, namely obtain by ZnO and Fe2O3The nano-powder material of composition.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is less than 55nm；It is carried out component analysis, and the mass percent recording ZnO is 17.72%.
Application: making thin film 3 microns thick as humidity sensitive material using this powder body material in gold interdigital electrode, the resonse characteristic of this sensor is shown in Fig. 5.
Claims (4)
1. resistance type humidity sensitive material, is characterized in that by ZnO and Fe2O3The nano composite oxide of composition, wherein the mass percent of ZnO is 12%-20%；nullIts preparation method is: weigh zinc salt soluble in water and iron salt respectively by the amount that the atomic ratio of Zn and Fe is 30-45: 100，And be dissolved in respectively etc. in the aqueous hydrochloric acid solution of mass fraction 5%-10% of weight，Mix after two solution are separately heated to 40 DEG C，Keep temperature and be stirred continuously down，It is slowly added dropwise the ammonia of mass fraction 15%-25%，Dripping quantity is the 1/5-1/3 of mixed liquor weight，Rate of addition be two seconds 1，After being added dropwise to complete，It is cooled to room temperature，Continue stirring 1 hour，Stand 5 hours，Will precipitation filtration under diminished pressure with deionized water wash twice，Dry 2 hours in 105 DEG C，After being fully ground，High temperature box type resistance furnace is warming up to 390 DEG C with the speed less than 4 DEG C per minute，And calcine 5 hours at this temperature，Namely obtain by ZnO and Fe2O3The resistance type humidity sensitive material of composition.
null2. the preparation method that electric resistance moisture is sensitive，It is characterized in that weighing zinc salt soluble in water and iron salt respectively by the amount that the atomic ratio of Zn and Fe is 30-45: 100，And be dissolved in respectively etc. in the aqueous hydrochloric acid solution of mass fraction 5%-10% of weight，Mix after two solution are separately heated to 40 DEG C，Keep temperature and be stirred continuously down，It is slowly added dropwise the ammonia of mass fraction 15%-25%，Dripping quantity is the 1/5-1/3 of mixed liquor weight，Rate of addition be two seconds 1，After being added dropwise to complete，It is cooled to room temperature，Continue stirring 1 hour，Stand 5 hours，Will precipitation filtration under diminished pressure with deionized water wash twice，Dry 2 hours in 105 DEG C，After being fully ground，High temperature box type resistance furnace is warming up to 390 DEG C with the speed less than 4 DEG C per minute，And calcine 5 hours at this temperature，Namely obtain by ZnO and Fe2O3The resistance type humidity sensitive material of composition.
3. resistance type humidity sensitive material according to claim 1, is characterized in that described zinc salt is the mixture of one or more of the anhydride of zinc chloride, zinc sulfate, zinc nitrate, zinc perchlorate, zinc dihydrogen phosphate and zinc acetate or hydrate；Iron salt is the mixture of one or more of the anhydride of iron chloride, ferric perchlorate, iron sulfate and ferric nitrate or hydrate.
4. resistance type humidity sensitive material according to claim 1, is characterized in that the particle diameter of described humidity sensitive material is less than 60nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310480287.8A CN103529085B (en) | 2013-10-04 | 2013-10-04 | Resistance type humidity sensitive material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310480287.8A CN103529085B (en) | 2013-10-04 | 2013-10-04 | Resistance type humidity sensitive material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103529085A CN103529085A (en) | 2014-01-22 |
| CN103529085B true CN103529085B (en) | 2016-07-06 |
Family
ID=49931268
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310480287.8A Expired - Fee Related CN103529085B (en) | 2013-10-04 | 2013-10-04 | Resistance type humidity sensitive material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103529085B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109030484B (en) * | 2018-08-30 | 2021-02-05 | 湘潭大学 | Colorimetric humidity sensor |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6214507B1 (en) * | 1998-08-11 | 2001-04-10 | Xerox Corporation | Toner compositions |
| CN101251521A (en) * | 2008-04-10 | 2008-08-27 | 北京联合大学生物化学工程学院 | Nanometer sensitive material of organic chlorine agriculture chemicals |
| CN102879521A (en) * | 2011-07-11 | 2013-01-16 | 北京联合大学生物化学工程学院 | Nano-sensitive material for monitoring hexachlorocyclohexanes |
| CN103149330A (en) * | 2013-02-20 | 2013-06-12 | 北京联合大学生物化学工程学院 | Nano sensitive material for acetone |
| CN103245657A (en) * | 2013-05-27 | 2013-08-14 | 北京联合大学生物化学工程学院 | Nano sensitive material for acrylic acid |
-
2013
- 2013-10-04 CN CN201310480287.8A patent/CN103529085B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6214507B1 (en) * | 1998-08-11 | 2001-04-10 | Xerox Corporation | Toner compositions |
| CN101251521A (en) * | 2008-04-10 | 2008-08-27 | 北京联合大学生物化学工程学院 | Nanometer sensitive material of organic chlorine agriculture chemicals |
| CN102879521A (en) * | 2011-07-11 | 2013-01-16 | 北京联合大学生物化学工程学院 | Nano-sensitive material for monitoring hexachlorocyclohexanes |
| CN103149330A (en) * | 2013-02-20 | 2013-06-12 | 北京联合大学生物化学工程学院 | Nano sensitive material for acetone |
| CN103245657A (en) * | 2013-05-27 | 2013-08-14 | 北京联合大学生物化学工程学院 | Nano sensitive material for acrylic acid |
Non-Patent Citations (2)
| Title |
|---|
| A. Avila-García等.Ac response to humidity and propane of sprayed Fe-Zn oxide films.《REVISTA MEXICANA DE FÍ * |
| SICA》.2009,第55卷(第4期),第249页摘要，第2节第1段. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103529085A (en) | 2014-01-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103529085B (en) | Resistance type humidity sensitive material and preparation method thereof | |
| CN105388187B (en) | The test method of the semiconductor gas sensor of controlled humidity | |
| Thomas et al. | The continuous measurement of photosynthesis, respiration, and transpiration of alfalfa and wheat growing under field conditions | |
| CN205909848U (en) | Trendy full -automatic demarcation temperature and humidity sensor system | |
| CN107976434B (en) | The sensitive material of formaldehyde in air, benzene and trimethylamine is measured simultaneously | |
| CN102636407A (en) | Tobacco physical humectation performance testing method | |
| CN103792227A (en) | Nano composite oxide sensitive material for formaldehyde and benzene | |
| CN105668613A (en) | Fe-doped stannic oxide flower-like nanosphere material with ultrasensitive respiratory sensing performance | |
| CN103712882A (en) | Method and system for measuring humidity of high-temperature high-pressure high-humidity gas | |
| CN110045055B (en) | High-selectivity sensitive material of trimethylamine and hydrogen sulfide | |
| CN103512927B (en) | A kind of humidity sensitive material and preparation method thereof | |
| CN105973840A (en) | Method for quickly detecting fermented grain physicochemical indexes of Maotai-flavor liquor | |
| CN107817278A (en) | The preparation method of new cerium dopping acetone gas-sensitive sensing element | |
| CN103558265A (en) | Automatic testing system with gas sensitive element | |
| CN101251521B (en) | Nanometer sensitive material of organic chlorine agriculture chemicals | |
| CN107817273A (en) | The preparation method of aluminium, Ti doped Zinc oxide-base acetone gas sensor | |
| CN103760055B (en) | The method of testing of silver content in a kind of silver paste | |
| CN110927001A (en) | Humidity sensitive element and preparation process thereof | |
| CN108802116A (en) | A kind of preparation method of acetone gas sensitive material | |
| CN105445133A (en) | Quartz crystal microbalance sensor for detecting trimethylamine gas as well as preparation method and application thereof | |
| CN110672591B (en) | Low-temperature response sensitive material for formaldehyde and trimethylamine in air | |
| CN104267022A (en) | Cross sensitive material of ammonia and benzene in air and preparation method of cross sensitive material | |
| CN102809628B (en) | Nano-sensitive material for trimethylamine | |
| CN101545893A (en) | Nanometer sensitive material of pyrethroid pesticide | |
| CN110082399A (en) | A kind of fast non-destructive detection method of fresh tobacco leaves total reducing sugar |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160706 Termination date: 20181004 |