CN109704394B - Preparation method of doped tin dioxide powder and doped tin dioxide powder obtained by method - Google Patents
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 157
- 239000000843 powder Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 12
- 150000003839 salts Chemical class 0.000 claims abstract description 22
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 21
- 230000009467 reduction Effects 0.000 claims abstract description 21
- 239000011259 mixed solution Substances 0.000 claims abstract description 19
- 239000011812 mixed powder Substances 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 9
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims description 11
- 239000006185 dispersion Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract description 3
- 229910021626 Tin(II) chloride Inorganic materials 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 34
- 239000000463 material Substances 0.000 description 15
- 230000035945 sensitivity Effects 0.000 description 15
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 12
- 238000001514 detection method Methods 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 239000012279 sodium borohydride Substances 0.000 description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 230000007774 longterm Effects 0.000 description 5
- 230000002829 reductive effect Effects 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 101710134784 Agnoprotein Proteins 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910006406 SnO 2 At Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses a preparation method of doped tin dioxide powder and the doped tin dioxide powder obtained by the method, wherein the preparation method comprises the following steps: a dispersing step: dissolving tin dioxide powder in a solvent, and adding a reducing agent and soluble metal salt to obtain a mixed solution; a primary reduction step: stirring and dispersing the mixed solution, standing and settling for at least 12h, then preserving heat for 1-3h under the condition that the temperature is 50-80 ℃, then raising the temperature to 180-650 ℃ and preserving heat for 1-2h, raising the temperature to 550-650 ℃ and preserving heat for 3-6h, and obtaining mixed powder after cooling; and (3) secondary reduction: grinding the mixed powder in gas H 2 Calcining under the condition of (1) to obtain doped tin dioxide powder; the method takes tin dioxide as a raw material, solves the problem of instability of a reaction process caused by taking tin salt as a raw material in the prior art, can be generally suitable for doping various types of metals, and obtains the doped tin dioxide powder with wide application.
Description
Technical Field
The invention relates to a preparation method of doped tin dioxide powder and the doped tin dioxide powder obtained by the method, belonging to the technical field of functional powder material processing.
Background
Tin dioxide is an important oxide semiconductor material, has a rutile crystal structure, and has been widely applied to solar cells, electrothermal materials, transparent conductive electrode materials, gas-sensitive materials and the like. SnO due to the presence of oxygen vacancies or metal interstitial atoms 2 Semiconductor materials, typically of N-type conductivity, when gases in the ambient atmosphere adsorb to such SnO 2 At the surface of the oxide thin film, the resistance of the oxide thin film changes due to charge transfer. Based on this principle, tin dioxide can be used to detect changes in organic volatile gases (VOC gases) in ambient gases.
Characteristic parameters of the gas sensor include sensitivity, selectivity, time characteristics, stability and reliability. The direct use of undoped tin dioxide as a gas sensitive material presents several problems: firstly, the undoped tin dioxide powder has fewer surface active sites, has low sensitivity when reacting with gas in the environment atmosphere, affects circuit detection, and can detect resistance value change only with higher resolution, thereby greatly increasing the overall power consumption of the device and being not beneficial to portable design; multiple experiments prove that undoped tin dioxide powder is at high temperature for a long time, crystal particles continuously grow, the resistance value of the gas-sensitive material is continuously increased, and the long-term stability is poor; the problem of poor selectivity of the semiconductor metal oxide type gas sensor generally exists, and the main problem lies in that tin dioxide is a common sensitive material and can adsorb various reductive or oxidative gases.
Therefore, when tin dioxide is used as a gas sensitive material, the tin dioxide is subjected to a doping treatment.
Disclosure of Invention
In order to overcome the defects of the prior art, the first object of the invention is to provide a preparation method of doped tin dioxide powder, which takes tin dioxide as a raw material, solves the problem of instability of a reaction process caused by taking tin salt as a raw material in the prior art, can be generally suitable for doping various types of metals, selects different doped metals aiming at different detection objects, and has wide application of the obtained doped tin dioxide powder.
The second purpose of the invention is to provide the doped tin dioxide powder obtained by the preparation method, and the doped tin dioxide powder can obviously improve the sensitivity of the gas sensitive material, effectively inhibit the growth of tin dioxide crystal particles and ensure the long-term stability of the sensor.
The first purpose of the invention can be achieved by adopting the following technical scheme: a preparation method of doped tin dioxide powder comprises the following steps:
a dispersing step: dissolving tin dioxide powder in a solvent, and adding a reducing agent and soluble metal salt to obtain a mixed solution;
a primary reduction step: stirring and dispersing the mixed solution, standing and settling for at least 12h, preserving heat for 1-3h at the temperature of 50-80 ℃, then heating to 180-650 ℃ for 1-2h, then heating to 550-650 ℃ for 3-6h, and cooling to obtain mixed powder;
and (3) secondary reduction: grinding the mixed powder in gas H 2 Calcining at the temperature of 280-400 ℃ for 3-6h to obtain the doped tin dioxide powder.
Further, in the dispersing step, the powder particle diameter of the tin dioxide powder is 25-500 nm.
Furthermore, in the dispersion step, the mass ratio of the tin dioxide powder to the solvent is 1 (3-5).
Further, in the dispersing step, the solvent is an ether solvent.
Further, in the dispersion step, the mass ratio of the reducing agent to the tin dioxide powder is (7-12): 100.
Further, in the dispersing step, the reducing agent is sodium borohydride.
Further, in the dispersing step, the soluble metal salt comprises soluble Pd 2+ Salt, soluble Sb 3+ Salt and soluble Ag + At least one of salts.
Further, in the dispersing step, the soluble metal salt is Pd (NO) 3 ) 2 、Sb(NO 3 ) 3 And AgNO 3 At least one of (1).
Further, in the dispersing step, the amount of the soluble metal salt added is 0.5-2% wt of the mixed solution.
Further, in the primary reduction step, the rotation speed of stirring and dispersing is 300-500rpm, and the time is 4-8 h.
Further, a primary reduction step: stirring and dispersing the mixed solution, standing and settling for at least 12h at 20 ℃, preserving heat for 2h at 70 ℃, then heating to 250 ℃, preserving heat for 1.5h, then heating to 600 ℃, preserving heat for 4h, and cooling to obtain mixed powder;
further, a secondary reduction step: grinding the mixed powder in gas H 2 Calcining at 350 ℃ for 4 hours to obtain the doped tin dioxide powder.
The second purpose of the invention can be achieved by adopting the following technical scheme: the doped tin dioxide powder is prepared by the preparation method.
The formulation design principle of the invention is as follows: the invention directly adopts the existing tin dioxide to directly carry out doping treatment, uniformly mixes the tin dioxide powder and doped metal salt through physical dispersion, attaches the metal salt to the surface of the nano tin dioxide powder by using a standing impregnation method, leads metal ions to form effective bond energy contact with tin dioxide crystals under reasonable temperature parameters, reduces the metal ions into metal atoms under the action of a reducing agent, and finally carries out secondary reduction under the action of hydrogen to lead the surface of the tin dioxide crystals to form metal atoms with high catalytic action, thus finishing the doping process.
Compared with the prior art, the invention has the beneficial effects that:
1. the preparation method overcomes the technical defects that the particle size and the doping effect of tin dioxide particles are difficult to control when tin salt is used as a raw material in the prior art, and the uniformity of the tin dioxide particles has great influence on the consistency of the product performance;
2. the preparation method has the advantages of simple doping effect reaction operation, short flow time consumption and high preparation efficiency, and can be applied to mass industrial production;
3. the preparation method of the invention can be suitable for doping different metals, different doping metals are selected for different detection objects, the selectivity of different sensors to a certain specific gas is realized, and the doped tin dioxide powder has wide application;
4. the doped tin dioxide powder prepared by the preparation method provided by the invention has the advantages that the sensitivity of the gas sensitive material is greatly improved, the long-term stability is greatly improved, the initial resistance value of the material end is effectively controlled, the initial resistance value of the material end is in a reasonable range, and the circuit resolution is facilitated.
Drawings
FIG. 1 is a graphical representation of sensitivity detection data;
FIG. 2 is a graphical representation of long term stability test data;
FIG. 3 is a graphical representation of gas selective detection data.
Detailed Description
The invention will be further described with reference to the accompanying drawings and the detailed description below:
a preparation method of doped tin dioxide powder comprises the following steps:
a dispersing step: dissolving tin dioxide powder in ether solvent, wherein the particle diameter of the tin dioxide powder is 25-500nm, the mass ratio of the tin dioxide powder to the ether solvent is 1 (3-5), and adding sodium borohydride and soluble metal salt, wherein the soluble metal salt comprises soluble Pd 2+ Salt, soluble Sb 3+ Salt and soluble Ag + At least one of the salts, the adding amount of the soluble metal salt is 0.5-2 wt% of the mixed solution, and the mass ratio of the sodium borohydride to the tin dioxide powder is (7-12):100, so as to obtain the mixed solution;
a primary reduction step: stirring and dispersing the mixed solution at the rotation speed of 300-500rpm for 4-8h, standing and settling for at least 12h at the temperature of 20 ℃, keeping the temperature for 1-3h at the temperature of 50-80 ℃ to completely volatilize the solvent, then heating to 180-300 ℃ for keeping the temperature for 1-2h, then heating to 550-650 ℃ for keeping the temperature for 3-6h, and cooling to obtain mixed powder;
and (3) secondary reduction: grinding the mixed powder in gas H 2 Calcining at the temperature of 280-400 ℃ for 3-6h to obtain the doped tin dioxide powder.
The obtained doped tin dioxide powder can be used as a gas sensitive material of a gas sensor.
Example 1:
a preparation method of doped tin dioxide powder comprises the following steps:
a dispersing step: dissolving 10g of tin dioxide powder in 50mL of diethyl ether, wherein the particle diameter of the tin dioxide powder is 100nm, and adding 1g of sodium borohydride and 0.1g of Pd (NO) 3 ) 2 、0.08g Sb(NO 3 ) 3 And 0.15g Ag NO 3 Obtaining a mixed solution;
a primary reduction step: stirring and dispersing the mixed solution at the rotation speed of 350rpm for 4.5h, standing and settling for at least 12h at the temperature of 20 ℃, preserving heat for 2h at the temperature of 60 ℃ to completely volatilize the solvent, then heating to 200 ℃, preserving heat for 1.8h, heating to 580 ℃, preserving heat for 4h, and cooling to obtain mixed powder;
and (3) secondary reduction: grinding the mixed powder in gas H 2 Calcining at 300 ℃ for 5 hours to obtain the doped tin dioxide powder.
Example 2:
a preparation method of doped tin dioxide powder comprises the following steps:
a dispersing step: taking 8g of tin dioxide powder, dissolving in 45mL of diethyl ether, wherein the particle diameter of the tin dioxide powder is 100nm, and adding 0.8g of sodium borohydride and 0.08g of Pd (NO) 3 ) 2 、0.08g Sb(NO 3 ) 3 And 0.08g AgNO 3 Obtaining a mixed solution;
a primary reduction step: stirring and dispersing the mixed solution, keeping the stirring and dispersing speed at 350rpm for 5h, standing and settling for at least 12h at 20 ℃, keeping the temperature at 70 ℃ for 2h to completely volatilize the solvent, then heating to 250 ℃ and keeping the temperature for 1.5h, then heating to 600 ℃ and keeping the temperature for 4h, and cooling to obtain mixed powder;
and (3) secondary reduction: grinding the mixed powder in gas H 2 Calcining at 350 ℃ for 4 hours to obtain the doped tin dioxide powder.
Example 3:
a preparation method of doped tin dioxide powder comprises the following steps:
a dispersing step: taking 12g of tin dioxide powder, dissolving in 65mL of diethyl ether, wherein the particle diameter of the tin dioxide powder is 100nm, and adding 1.42g of sodium borohydride and 0.18g of Pd (NO) 3 ) 2 、0.15g Sb(NO 3 ) 3 And 0.2g AgNO 3 Obtaining a mixed solution;
a primary reduction step: stirring and dispersing the mixed solution at the rotation speed of 350rpm for 7.5h, standing and settling for at least 12h at the temperature of 20 ℃, preserving heat for 2h at the temperature of 75 ℃ to completely volatilize the solvent, then heating to 250 ℃ and preserving heat for 2h, heating to 550 ℃ and preserving heat for 5.5h, and cooling to obtain mixed powder;
and (3) secondary reduction: grinding the mixed powder in gas H 2 Calcining at 350 ℃ for 5.5 hours to obtain the doped tin dioxide powder.
The doped tin dioxide powder obtained in the example 1 is used for preparing a VOC gas sensor, and then detection is carried out:
1. and (3) sensitivity detection:
the experimental steps are as follows:
1) placing the VOC gas sensor subjected to 12-hour power-on aging in a sealed box;
2) starting to collect data after the power-on state is stable for 30s, and collecting one data point every 2 s;
3) 10ppm of ethanol gas is introduced, an American Huarui PGM-7340VOC detector is used as a gas concentration standard, data is recorded and collated as shown in figure 1, and data of a sensor prepared in example 1 is compared with data of a sensor prepared from undoped tin dioxide powder, such as a broken line (R).
As can be seen from the data in fig. 1, the sensitivity of the sensor prepared using example 1 to ethanol gas was greatly improved. The resistance of the sensor prepared using example 1 was reduced from 546K Ω to 35K Ω in a 10ppm ethanol gas atmosphere, and the sensitivity was 15.6; the resistance of the sensor using undoped tin oxide dropped from 608K Ω to 397K Ω with a sensitivity of 1.5.
2. And (3) detecting the long-term stability:
the experimental steps are as follows: placing a VOC gas sensor in a well-ventilated indoor environment, electrifying, reading resistance data once at intervals of 2h, continuously testing for 2 months, and collating the data as shown in figure 2, wherein the data of the sensor prepared in the embodiment 1 is shown as a broken line I and the data of the sensor prepared by using undoped tin dioxide powder is compared with the data of the sensor prepared by using the undoped tin dioxide powder, such as a broken line II.
It can be seen that the resistance of the sensor prepared using example 1 fluctuates between 580-620K Ω, and the resistance of the sensor prepared using undoped tin dioxide powder continues to increase from 630K Ω to 1989K Ω.
3. Detecting an initial resistance value:
the experimental steps are as follows: experiments were carried out using example 1 and a sensor made from undoped powder having the same tin dioxide content as in example 1 as a comparative example, and 9 replicates were sampled. And respectively electrifying and aging for 24h, and detecting the initial resistance values, wherein the data is shown in the table 1 and the unit of K omega.
Table 1 initial resistance data (K Ω)
| | Sample | 1 | |
|
|
|
|
|
|
|
| Examples | 356 | 366 | 378 | 351 | 349 | 361 | 354 | 363 | 372 | |
| Comparative example | 654 | 612 | 635 | 660 | 618 | 632 | 651 | 624 | 636 |
Description of the data: as can be seen from the data in the table, the initial resistance of the gas sensitive material end of example 1 is reduced, and is more suitable for circuit resolution.
4. And (3) gas selective detection:
the experimental steps are as follows: the sensor prepared in example 1 was tested for a variety of gases including methane, ethanol and hydrogen at 10ppm concentrations, and the data is shown in figure 3. The broken line is a test of hydrogen; broken line II is the test of ethanol; and testing methane. As can be seen from fig. 3, the sensor prepared in example 1 had the highest sensitivity to hydrogen, the resistance decreased from 595K Ω to 29K Ω, and the sensitivity was 20.5; secondly, the resistance value of the sensitivity to methane is reduced from 571K omega to 258K omega, and the sensitivity is 2.2; the sensitivity to ethanol is the worst, the resistance value is reduced from 577K omega to 320K omega, and the sensitivity is 1.8. Therefore, the sensor manufactured in example 1 has a certain selectivity to hydrogen, and the sensor can be used as a semiconductor type hydrogen sensor by performing a certain treatment on a circuit after calibration.
Various other changes and modifications to the above-described embodiments and concepts will become apparent to those skilled in the art from the above description, and all such changes and modifications are intended to be included within the scope of the present invention as defined in the appended claims.
Claims (7)
1. A preparation method of doped tin dioxide powder is characterized by comprising the following steps:
a dispersing step: dissolving tin dioxide powder in a solvent, and adding a reducing agent and soluble metal salt to obtain a mixed solution; the soluble metal salt comprises soluble Pd 2+ Salt, soluble Sb 3+ Salt and soluble Ag + A composition in salt; wherein the mass ratio of the reducing agent to the tin dioxide powder is (7-12) to 100; the adding amount of the soluble metal salt is 0.5-2% wt of the mixed solution;
a primary reduction step: stirring and dispersing the mixed solution, standing and settling for at least 12h, then preserving heat for 1-3h under the condition that the temperature is 50-80 ℃, then raising the temperature to 180-650 ℃ and preserving heat for 1-2h, raising the temperature to 550-650 ℃ and preserving heat for 3-6h, and obtaining mixed powder after cooling;
and (3) secondary reduction: grinding the mixed powder in gas H 2 Calcining at the temperature of 280-400 ℃ for 3-6h to obtain the doped tin dioxide powder.
2. The method of claim 1, wherein in the dispersing step, the tin dioxide powder has a particle size of 25-500 nm.
3. The method according to claim 1, wherein in the dispersing step, the mass ratio of the tin dioxide powder to the solvent is 1 (3-5).
4. The method according to claim 1, wherein the stirring dispersion speed is 300-500rpm for 4-8h in the first reduction step.
5. The method for preparing doped tin dioxide powder according to claim 1, wherein the primary reduction step comprises: stirring and dispersing the mixed solution, standing and settling for at least 12h at 20 ℃, then preserving heat for 2h at the temperature of 70 ℃, then raising the temperature to 250 ℃, preserving heat for 1.5h, raising the temperature to 600 ℃, preserving heat for 4h, and cooling to obtain mixed powder.
6. The method for preparing doped tin dioxide powder according to claim 1, wherein the secondary reduction step comprises: grinding the mixed powder in gas H 2 Calcining at 350 ℃ for 4 hours to obtain the doped tin dioxide powder.
7. Doped tin dioxide powder, characterized in that it is prepared by the preparation method according to claim 1.
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| WO2013002919A1 (en) * | 2011-06-28 | 2013-01-03 | 3M Innovative Properties Company | Tin dioxide nanopartcles and method for making the same |
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