CN1996004A - Coating type ammonia sensor nano film and method for preparing same - Google Patents
Coating type ammonia sensor nano film and method for preparing same Download PDFInfo
- Publication number
- CN1996004A CN1996004A CN 200610124333 CN200610124333A CN1996004A CN 1996004 A CN1996004 A CN 1996004A CN 200610124333 CN200610124333 CN 200610124333 CN 200610124333 A CN200610124333 A CN 200610124333A CN 1996004 A CN1996004 A CN 1996004A
- Authority
- CN
- China
- Prior art keywords
- indium
- gas sensor
- ammonia gas
- nano
- film according
- 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.)
- Granted
Links
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The coating type alkaline air sensor nanometer thin film forms with weight ratio of(100-90)(0-10) of indium trioxide, metatitanic acid, with the working process starting from adding alkaline water into the solution of InCl3 .4H2O stirring till the deposit of indium hydroxide, centrifugation, filtering, cleaning and drying to get dry gel by adding metatitanic acid after solution of the indium hydroxide with hydrolytic decomposition and glacial acetic acid volatilization, sintering, cooling to get the titan mixed indium oxide particle and grinding, getting the clear liquid after ultrasonic settlement, centrifugation, getting indium trioxide powder. It is simple, with good response and optional feature, high sensitivity, low monitoring limit, quick recovery of response, good stability and low working temperature.
Description
Technical Field
The invention relates to a film coated on a sensor, in particular to a coating type ammonia gas sensor nano film, and also relates to a preparation method for preparing the nano film, belonging to the technical field of film materials.
Background
Although ammonia exists in the atmosphere at low concentration, ammonia with lower concentration still has adverse effects on people and the environment, has strong stimulation effect on the mouth, nasal membranes and upper respiratory tract, and also has strong corrosion effect on substances in the environment under certain conditions, so that the rapid and accurate determination of the content of the ammonia provides a basis for the treatment of the air environment, which is very necessary. The currently recommended national monitoring method is a nano-grade reagent spectrophotometry, which has relatively high sensitivity but slightly poor selectivity and is not suitable for field monitoring.
Currently based on In2O3The semiconductor ammonia gas sensor made of the material has been reported In the literature, and the In is known from the existing literature report2O3A problem with micro-sensors made for gas sensitive materials is that In is2O3Poor selectivity to ammonia and low sensitivity (this is because In2O3Large and non-uniform particle), In2O3The preparation method and the manufacturing technology of the sensitive film can directly influence the gas-sensitive performance of the sensitive film, the manufacturing of the sensitive film mostly adopts a relatively complex physical method, and the sensitive film manufactured by the physical method is not stable and is difficult to develop and apply so far.
Disclosure of Invention
The first purpose of the invention is to provide a coating type ammonia gas sensor nano-film which has good responsiveness, selectivity, high detection sensitivity and good stability.
The second purpose of the invention is to provide a preparation method of the coating type ammonia gas sensor nano-film with the functions,
the first purpose of the invention is implemented by the following technical scheme:
the coating type ammonia gas sensor nano film comprises the following components in percentage by mass: indium trioxide and butyl titanate (100-90) to (0-10).
The preferable formula of the coating type ammonia gas sensor nano film is as follows according to the mass ratio of the materials: indium trioxide to butyl titanate 99: 1.
The second purpose of the invention is implemented by the following technical scheme:
a manufacturing process of a coating type ammonia gas sensor nano film comprises the following steps:
(1) analytically pure crystalline InCl3·4H2O is prepared into a solution with the concentration of 0.2-0.3 mol/L, and the concentration is controlledSlowly dripping ammonia water with the concentration of 0.9-1.1 mol/L under the condition of preparing a certain stirring speed, stopping adding the ammonia water when the solution is alkaline, and continuously stirring to ensure that the generated indium hydroxide particles are relatively uniform and prevent the indium hydroxide particles from coagulating; the stirring speed is not too fast, otherwise the solution can splash, and too slow can cause the local alkalinity of the solution to be too high, so that uneven coagulation is generated.
The chemical reaction equation of the step is as follows:
In3++OH-→In(OH)3↓
(2) centrifuging at a centrifugal speed of 8000-12000 rpm, filtering, and washing indium hydroxide with deionized water to remove chloride ions in the indium hydroxide, wherein the chloride ions have negative influence on the performance of the gas sensor;
(3) putting the indium hydroxide which is repeatedly cleaned into a vacuum drying oven at the temperature of 110-120 ℃ for vacuum drying for 5-10 hours, and removing water in the indium hydroxide as much as possible;
(4) dissolving indium hydroxide fully by glacial acetic acid, dropwise adding butyl titanate, then adding a small amount of water to hydrolyze the indium hydroxide, and slowly volatilizing the glacial acetic acid at normal temperature to form dry gel; wherein the dosage of the indium hydroxide is about 1g/5ml, and the indium hydroxide reacts with acetate to generate the indium acetate. When a small amount of water is added, indium acetate can be hydrolyzed;
the chemical reaction equation of the step is as follows:
(5) the xerogel is put in a muffle furnace to be calcined for 1 hour at 550 ℃, and after natural cooling, the titanium-doped nano indium oxide particles are obtained, and are fully ground to be more uniform (the powder is easy to generate sintering phenomenon during calcination); the powder calcined at 550 ℃ for one hour is the most sensitive to gases.
The chemical reaction equation of the step is as follows:
2In(OH)3→In2O3+3H2O
(6) carrying out ultrasonic treatment on the titanium-doped powder in n-amyl alcohol for 15-17 min, centrifuging for 10-15 min under the condition that the centrifugation speed is 10000 (+ -500) rpm, removing supernatant, and completely volatilizing the n-amyl alcohol in the supernatant at room temperature to obtain nano indium trioxide powder with finer particles (50-100 nm); the powder is treated by ultrasonic in n-amyl alcohol, some powder sintered in one piece is dispersed, the centrifugal rotating speed can centrifuge off particles with the particle size larger than 100nm, the particles in the supernatant are all indium trioxide particles with the particle size smaller than 100nm, and if the centrifugal time is shorter than 10 minutes, the large particles can not be completely precipitated.
In the manufacturing process of the coating type ammonia gas sensor nano film, the certain stirring speed in the step (1) is 400-500 r/min, and the stirring time is 2.8-3.1 hours.
In step (1), the addition of ammonia is stopped when the solution is more basic, wherein the more basic is PH 8.
In the step (2), the cleaning criteria for cleaning indium hydroxide with deionized water are: the chloride ion in the solution is less than 10-5mol/L, washing supernatant to make 0.01MAGNO not3Become turbid (Ksp)AgCl＝1.69*10-10)。
In the step (4), the mass ratio of the butyl titanate added dropwise is 1%, wherein titanium is doped for the purpose of improving selectivity.
The manufacturing process of the film of the coating type ammonia gas sensor comprises the following steps of: indium trioxide and butyl titanate (100-90) to (0-10).
The manufacturing process of the film of the coating type ammonia gas sensor comprises the following steps of: indium oxide and butyl titanate are mixed together at a ratio of 99: 1.
Compared with the prior art, the invention has the advantages that: (1) the cost is low, the manufacture is simple, and the operation is stable and practical; (2) the nano-scale coating type ammonia gas sensor film has the characteristics of good responsiveness, selectivity, high detection sensitivity, low monitoring lower limit, quick response-recovery, good stability and low working temperature.
Detailed Description
Example 1:
the invention provides a manufacturing process of a film of a coating type ammonia gas sensor, which comprises the following steps:
(1) analytically pure crystalline InCl3·4H2O is prepared into a solution with the concentration of 0.25mol/L, ammonia water with the concentration of 1mol/L is slowly dripped under the condition of controlling the speed of 400 revolutions/minute, when the PH is 8, the ammonia water addition is stopped, and the stirring is continued for three hours to ensure that the indium hydroxide is uniformly precipitated.
(2) Centrifuging at a centrifugal speed of 10000 rpm, filtering, and washing with deionized water to obtain solution with chloride ion content of less than 10-5mol/L。
(3) The indium hydroxide which is repeatedly cleaned is placed in a vacuum drying oven at 120 ℃ for vacuum drying for 10 hours.
(4) Indium hydroxide was dissolved sufficiently in 1g/mL glacial acetic acid, 1% (mass ratio) of butyl titanate was added dropwise, then a small amount of water was added to hydrolyze the mixture, and then glacial acetic acid was slowly volatilized at room temperature to form a dry gel.
(5) And (3) calcining the dry gel in a muffle furnace for one hour at 550 ℃, naturally cooling to obtain titanium-doped nano indium oxide particles, and fully grinding to make the particles more uniform.
(6) And (3) carrying out ultrasonic treatment on the titanium doped powder in n-amyl alcohol for 15min, centrifuging for 15min at the centrifugation speed of 10000 r, transferring supernatant, and completely volatilizing n-amyl alcohol in the supernatant at room temperature to obtain the nano indium trioxide powder with finer particles (50-100 nm).
Example 2:
the invention provides a manufacturing process of a film of a coating type ammonia gas sensor, which comprises the following steps:
(1) analytically pure crystalline InCl3·4H2O is prepared into a solution with the concentration of 0.2mol/L, ammonia water with the concentration of 0.9mol/L is slowly dripped under the condition of controlling the speed of 450 revolutions/minute, when the PH is 8, the ammonia water addition is stopped, and the stirring is continued for 2.8 hours to ensure that the indium hydroxide is uniformly precipitated.
(2) Centrifuging at 9500 rpm, filtering, and washing with deionized water to obtain solution with chloride ion content of less than 10-5mol/L。
(3) The indium hydroxide which is repeatedly cleaned is placed in a vacuum drying oven at 110 ℃ for vacuum drying for 5 hours.
(4) Indium hydroxide was dissolved sufficiently in 1g/mL glacial acetic acid, 1% (mass ratio) of butyl titanate was added dropwise, then a small amount of water was addedto hydrolyze the mixture, and then glacial acetic acid was slowly volatilized at room temperature to form a dry gel.
(5) And (3) calcining the dry gel in a muffle furnace for one hour at 550 ℃, naturally cooling to obtain titanium-doped nano indium oxide particles, and fully grinding to make the particles more uniform.
(6) And (3) carrying out ultrasonic treatment on the powder in n-amyl alcohol for 16min, centrifuging for 10min at the centrifugation speed of 9500 r/min, transferring supernatant, and completely volatilizing the n-amyl alcohol in the supernatant at room temperature to obtain the nano indium trioxide powder with finer particles.
Example 3:
the invention provides a manufacturing process of a film of a coating type ammonia gas sensor, which comprises the following steps:
(1) analytically pure crystalline InCl3·4H2O is prepared into a solution with the concentration of 0.3mol/L, ammonia water with the concentration of 1.1mol/L is slowly dripped under the condition of controlling the speed of 500 revolutions/minute, when the PH is 8, the ammonia water addition is stopped, and the stirring is continued for 3.1 hours to ensure that the indium hydroxide is uniformly precipitated.
(2) Centrifuging at 10500 rpm, filtering, and washing with deionized waterHas a chloride ion of less than 10-5mol/L。
(3) The indium hydroxide which is repeatedly cleaned is placed in a vacuum drying oven at 115 ℃ for vacuum drying for 8 hours.
(4) Indium hydroxide was dissolved sufficiently in 1g/mL glacial acetic acid, 1% (mass ratio) of butyl titanate was added dropwise, then a small amount of water was added to hydrolyze the mixture, and then glacial acetic acid was slowly volatilized at room temperature to form a dry gel.
(5) And (3) calcining the dry gel in a muffle furnace for one hour at 550 ℃, naturally cooling to obtain titanium-doped nano indium oxide particles, and fully grinding to make the particles more uniform.
(6) And (3) carrying out ultrasonic treatment on the powder in n-amyl alcohol for 17min, centrifuging for 12min at the centrifugation speed of 10500 r/min, transferring supernatant, and completely volatilizing n-amyl alcohol in the supernatant at room temperature to obtain the nano indium trioxide powder with finer particles.
The present invention is not limited to the above embodiments, and can be implemented as long as the embodiments mentioned in the specification.
Claims (9)
1. The coating type ammonia gas sensor nano film comprises the following components in percentage by mass: indium trioxide and butyl titanate (100-90) to (0-10).
2. The coated ammonia gas sensor nano-film according to claim 1, which is prepared by the following formula according to the mass ratio: indium trioxide to butyl titanate 99: 1.
3. A manufacturing process of a coating type ammonia gas sensor nano film comprises the following steps:
(1) analytically pure crystalline InCl3·4H2O is prepared into a solution with the concentration of 0.2-0.3 mol/L, ammonia water with the concentration of 0.9-1.1 mol/L is slowly dripped under the condition of controlling a certain stirring speed, when the solution is alkaline, the ammonia water is stopped to be added, and the stirring is continued to ensure that the indium hydroxide is uniformly precipitated;
(2) centrifuging at 10000 (+ -500) rpm, filtering, and washing with deionized water;
(3) putting the indium hydroxide which is repeatedly cleaned into a vacuum drying oven at the temperature of 110-120 ℃ for vacuum drying for 5-10 hours, and removing water in the indium hydroxide as much as possible;
(4) dissolving indium hydroxide fully by glacial acetic acid, dropwise adding butyl titanate, then adding a small amount of water to hydrolyze the indium hydroxide, and slowly volatilizing the glacial acetic acid at normal temperature to form dry gel;
(5) calcining the xerogel in a muffle furnace at 550 ℃ for 1 hour, naturally cooling to obtain titanium-doped nano indium oxide particles, and fully grinding to make the particles more uniform;
(6) and (3) carrying out ultrasonic treatment on the titanium-doped powder in n-amyl alcohol for 15-17 min, centrifuging for 10-15 min under the condition that the centrifugation speed is 10000 (+ -500) rpm, removing supernatant, and completely volatilizing the n-amyl alcohol in the supernatant at room temperature to obtain the nano indium trioxide powder with finer particles.
4. The process for preparing the coated ammonia gas sensor nano-film according to claim 3, wherein the step
(1) The stirring speed is 400-500 r/min, and the stirring time is 2.8-3.1 hours.
5. The process for preparing a coated ammonia gas sensor nano-film according to claim 3, wherein the alkalinity in the step (1) is PH 8.
6. The process for preparing a coated ammonia gas sensor nano-film according to claim 3, wherein the cleaning standard in the step (2) is to make the chloride ions in the solution less than 10-5mol/L。
7. The process for preparing a coated ammonia gas sensor nano-film according to claim 3, wherein the mass ratio of the butyl titanate dripped in the step (4) is 1%.
8. The process for preparing the coated ammonia gas sensor nano film according to the claim 3, 4, 5, 6 or 7, wherein the formula comprises the following components in percentage by mass: indium trioxide and butyl titanate (100-90) to (0-10).
9. The process for preparing the coated ammonia gas sensor nano film according to claim 8, wherein the formula comprises the following components in percentage by mass: indium oxide and butyl titanate are mixed together at a ratio of 99: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101243330A CN100465635C (en) | 2006-12-21 | 2006-12-21 | Coating type ammonia sensor nano film and method for preparing same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101243330A CN100465635C (en) | 2006-12-21 | 2006-12-21 | Coating type ammonia sensor nano film and method for preparing same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1996004A true CN1996004A (en) | 2007-07-11 |
| CN100465635C CN100465635C (en) | 2009-03-04 |
Family
ID=38251147
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006101243330A Expired - Fee Related CN100465635C (en) | 2006-12-21 | 2006-12-21 | Coating type ammonia sensor nano film and method for preparing same |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100465635C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107153083A (en) * | 2017-05-22 | 2017-09-12 | 江苏时瑞电子科技有限公司 | A kind of preparation method of gas containing nitrogen oxide sensor |
| CN112968122A (en) * | 2021-04-02 | 2021-06-15 | 福建晶烯新材料科技有限公司 | Method for manufacturing transparent P-type semiconductor nano film for refrigeration |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4743881A (en) * | 1985-05-08 | 1988-05-10 | Motorola, Inc. | Ceramic temperature sensor |
| DE4445359A1 (en) * | 1994-12-20 | 1996-06-27 | Bosch Gmbh Robert | Sensor for the detection of flammable gases |
| JP2981467B1 (en) * | 1998-09-28 | 1999-11-22 | 岡谷電機産業株式会社 | Ozone sensor manufacturing method |
| KR100474845B1 (en) * | 2002-03-22 | 2005-03-09 | 삼성코닝 주식회사 | Tin oxide powder, manufacturing method thereof, and manufacturing method of high density indium tin oxide target using the same |
| CN100401548C (en) * | 2003-12-11 | 2008-07-09 | 上海大学 | Method for making ferric oxide/stannic oxide bilaminar membrane alcohol sensitive element |
| CN1775693A (en) * | 2005-11-22 | 2006-05-24 | 华东理工大学 | Method for preparing tin-doped indium oxide nano powder |
-
2006
- 2006-12-21 CN CNB2006101243330A patent/CN100465635C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107153083A (en) * | 2017-05-22 | 2017-09-12 | 江苏时瑞电子科技有限公司 | A kind of preparation method of gas containing nitrogen oxide sensor |
| CN112968122A (en) * | 2021-04-02 | 2021-06-15 | 福建晶烯新材料科技有限公司 | Method for manufacturing transparent P-type semiconductor nano film for refrigeration |
| CN112968122B (en) * | 2021-04-02 | 2023-07-18 | 福建晶烯新材料科技有限公司 | Manufacturing method of transparent P-type semiconductor nano film for refrigeration |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100465635C (en) | 2009-03-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103785852B (en) | A kind of nanometer silver-nano micro crystal cellulose complex and preparation method and application | |
| CN106085156A (en) | A kind of wash resistant anti static antibacterial coating and preparation method thereof | |
| TW200408614A (en) | Method for producing ceramic dispersion composition | |
| CN108918633A (en) | Pd-SnO2Nanocomposite preparation and the application in hydrogen gas sensor | |
| CN104910656A (en) | Method for preparing super-hydrophobic silicon dioxide powder and super-hydrophobic coating from composite silicon source | |
| CN110296973B (en) | SiO2@ Ag @ ZrO2 multilayer core-shell structure nano material and preparation method and application thereof | |
| CN105753040B (en) | Nanometer In for acetone gas sensor2O3The preparation method of powder | |
| WO2017152745A1 (en) | Lanthanum-doped formaldehyde-sensitive material and preparation method therefor, and formaldehyde sensor | |
| CN107570194B (en) | Fe/Co-Nx/TiO 2 photocatalyst and preparation method and application thereof | |
| CN110694607A (en) | Preparation method and application of activated carbon silicon dioxide/zinc oxide composite photocatalyst | |
| JP5510521B2 (en) | Photocatalyst particle dispersion and process for producing the same | |
| CN1996004A (en) | Coating type ammonia sensor nano film and method for preparing same | |
| CN110455873B (en) | Method for improving performance of MoS2 gas sensor by adopting W doping | |
| CN105158295A (en) | Preparation method of titanium dioxide-graphene composite humidity-sensitive material | |
| CN102507657A (en) | Method for preparing high-sensitivity bismuth-doped tin dioxide sensing material | |
| CN110487772A (en) | A kind of three-dimensional S nO2/ Ag NPs Raman enhances substrate and the preparation method and application thereof | |
| CN109540970A (en) | One kind being based on novel ZnO nano column/SnO2Thin film detector and preparation method | |
| CN111217387B (en) | Three-dimensional flower-like hydroxyl zinc fluoride material, preparation method thereof and application thereof in gas-sensitive detection | |
| CN104310306B (en) | High sensitivity wine sensitive gas sensor and preparation method thereof, mesoporous SnO2The preparation method of material | |
| CN105486720B (en) | A kind of H2The preparation method of S gas sensing materials | |
| CN101055782A (en) | A making method for novel biological compatible magnetic fluorescence nano particle | |
| CN106970067B (en) | Mesoporous TiO 22Preparation and application methods of surface-enhanced Raman scattering active substrate | |
| CN110026227B (en) | Chromium-doped titanium dioxide nanotube-amino modified graphene oxide composite material and preparation method and application thereof | |
| CN109553128A (en) | Rutile titanium dioxide is nanocrystalline, preparation method and application | |
| CN106084923A (en) | A kind of preparation method of aqueous deodorization inorganic coating |
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 | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20090304 Termination date: 20121221 |