CN111908500A - Preparation method of silver-doped tin dioxide nanosheet self-assembled flower-shaped material - Google Patents
Preparation method of silver-doped tin dioxide nanosheet self-assembled flower-shaped material Download PDFInfo
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- CN111908500A CN111908500A CN202010698412.2A CN202010698412A CN111908500A CN 111908500 A CN111908500 A CN 111908500A CN 202010698412 A CN202010698412 A CN 202010698412A CN 111908500 A CN111908500 A CN 111908500A
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 239000000463 material Substances 0.000 title claims abstract description 29
- 239000002135 nanosheet Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000011259 mixed solution Substances 0.000 claims abstract description 35
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 239000001509 sodium citrate Substances 0.000 claims abstract description 14
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 13
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims abstract description 12
- 229940038773 trisodium citrate Drugs 0.000 claims abstract description 12
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 11
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000011150 stannous chloride Nutrition 0.000 claims abstract description 10
- 239000001119 stannous chloride Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 4
- 229910052709 silver Inorganic materials 0.000 abstract description 4
- 239000004332 silver Substances 0.000 abstract description 4
- 239000007789 gas Substances 0.000 description 25
- 230000035945 sensitivity Effects 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 235000012055 fruits and vegetables Nutrition 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002057 nanoflower Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000011540 sensing material Substances 0.000 description 1
- 229910021509 tin(II) hydroxide Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Images
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-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
Abstract
The invention discloses a preparation method of a silver-doped tin dioxide nanosheet self-assembled flower-shaped material, which comprises the following steps: adding stannous chloride and trisodium citrate into a mixed solution of deionized water and ethylene glycol, stirring to obtain a mixed solution A, adding silver nitrate into the mixed solution, and stirring to obtain a mixed solution B; placing the mixed solution B in a polytetrafluoroethylene reaction kettle for hydrothermal reaction, cooling, taking out a mixture at the bottom of the reaction kettle, and performing centrifugal separation on the mixture to obtain a sample; and washing the sample by using deionized water and ethanol in sequence, and drying to obtain the silver-doped tin dioxide nanosheet self-assembled flower-shaped material. Silver is introduced into the tin dioxide, so that the conductivity of the tin dioxide is changed, and the gas-sensitive performance of the tin dioxide is enhanced, thereby realizing the detection of target gas molecules.
Description
Technical Field
The invention belongs to the technical field of gas-sensitive sensing materials, and relates to a preparation method of a silver-doped tin dioxide nanosheet self-assembled flower-shaped material.
Background
Along with the progress of science and technology, the daily emission of gas of industry and agriculture and people is gradually increased. Some of these gases are flammable and explosive, such as hydrogen, alcohol, methane, etc.; some are toxic, such as hydrogen sulfide, carbon monoxide, and the like; some of them are gases such as ethylene, etc. which accelerate the decomposition of fruits and vegetables in agricultural production. The gas sensor can detect the components and the concentration of the gas and convert the related information into a usable output signal, thereby having the functions of detecting the gas, alarming and the like. This is of great significance for production and life.
Increasing tin dioxide (SnO)2) There are various methods for the selectivity and sensitivity of gas sensors. The doping modification can change the energy band structure and provide more active centers in the gas-sensitive reaction process, preferentially adsorb target gas molecules, accelerate the reaction speed of the target gas molecules with the target gas molecules, change the conductivity of tin dioxide, and enhance the gas-sensitive performance of the tin dioxide, thereby realizing the detection of the target gas molecules. At present, tin dioxide as a gas sensitive material with the most applications has good performance, but has the defects of low sensitivity, poor selectivity, high operation temperature and the like, so that the application in practice is limited.
Disclosure of Invention
The invention aims to provide a preparation method of a silver-doped tin dioxide nanosheet self-assembled flower-shaped material, and solves the problem of low sensitivity of a gas-sensitive material in the prior art.
The invention adopts the technical scheme that a preparation method of a silver-doped tin dioxide nanosheet self-assembled flower-shaped material comprises the following steps:
step 1, adding stannous chloride and trisodium citrate into a mixed solution of deionized water and ethylene glycol, stirring to obtain a mixed solution A, adding silver nitrate into the mixed solution, and stirring to obtain a mixed solution B;
step 2, placing the mixed solution B in a polytetrafluoroethylene reaction kettle for hydrothermal reaction, cooling, taking out a mixture at the bottom of the reaction kettle, and performing centrifugal separation on the mixture to obtain a sample;
and 3, washing the sample by adopting deionized water and ethanol in sequence, and drying to obtain the silver-doped tin dioxide nanosheet self-assembled flower-shaped material.
The invention is also characterized in that:
the molar ratio of the stannous chloride to the trisodium citrate to the silver nitrate is 1:1: 0.0208-1: 1: 0.0832.
The mixing ratio of the deionized water to the ethylene glycol in the step 1 is 2: 3.
The stirring time after adding the silver nitrate in the step 1 is 1-1.5 h.
The temperature of the hydrothermal reaction in the step 2 is 180-200 ℃, and the reaction time is 18-24 h.
The invention has the beneficial effects that:
according to the preparation method of the silver-doped tin dioxide nanosheet self-assembled flower-shaped material, the tin dioxide powder is prepared by a hydrothermal method, trisodium citrate is used as a system structure regulator, silver is introduced into tin dioxide, the conductivity of tin dioxide is changed, and the gas-sensitive performance of the tin dioxide is enhanced, so that the detection of target gas molecules is realized; one-step hydrothermal method is simple to operate, and sample influence factors are reduced compared with two-step hydrothermal method; the preparation process is simple, and the product has good sensitivity and selectivity to ethanol at 350 ℃.
Drawings
FIG. 1 is an SEM image of a silver-doped tin dioxide nanosheet self-assembled flower-like material obtained by the preparation method of the present invention;
FIG. 2 is a high-power SEM image of a silver-doped tin dioxide nanosheet self-assembled flower-like material obtained by the preparation method of the present invention;
FIG. 3a is an XRD (X-ray diffraction) pattern of a silver-doped tin dioxide nanosheet self-assembled flower-shaped material obtained by the preparation method of the invention;
FIG. 3b is a partial enlarged view of an XRD pattern of the silver-doped tin dioxide nanosheet self-assembled flower-like material obtained by the preparation method of the present invention;
FIG. 4 is a gas-sensitive performance diagram of the silver-doped tin dioxide nanosheet self-assembled flower-like material obtained by the preparation method of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
A preparation method of a silver-doped tin dioxide nanosheet self-assembled flower-shaped material specifically comprises the following steps:
step 1, adding stannous chloride and trisodium citrate into a mixed solution of deionized water and ethylene glycol, stirring to obtain a mixed solution A, adding silver nitrate into the mixed solution, and stirring for 1-1.5 hours to obtain a mixed solution B; the molar ratio of stannous chloride to trisodium citrate to silver nitrate is 1: 0.0208-1: 0.0832, and the mixing ratio of deionized water to ethylene glycol is 2: 3;
SnO2can be obtained by hydrolyzing tin salt, and the specific reaction is as follows:
Sn 2++2H2O→Sn(OH)2+2H+
Sn(OH)4+2OH-→Sn(OH)6 2-
Sn(OH)6 2-→SnO2+2OH-+2H2O
wherein the sodium citrate is in SnO2The formation process of the structure plays an important role. SnO promotion of sodium citrate in reaction process2The growth of the nano-sheets is accelerated, and the self-assembly of the nano-sheets is accelerated to form a final flower-shaped structure; while silver nitrate may provide the silver element needed for doping.
Step 2, placing the mixed solution B in a polytetrafluoroethylene reaction kettle for hydrothermal reaction at the temperature of 180-200 ℃ for 18-24 h, cooling, taking out a mixture at the bottom of the reaction kettle, and placing the mixture in a centrifugal tube for centrifugal separation to obtain a sample;
and 3, washing the sample by adopting deionized water and ethanol in sequence, and drying to obtain the silver-doped tin dioxide nanosheet self-assembled flower-shaped material.
According to the preparation method of the silver-doped tin dioxide nanosheet self-assembled flower-shaped material, the tin dioxide powder is prepared by a hydrothermal method, trisodium citrate is used as a system structure regulator, silver is introduced into tin dioxide, the conductivity of tin dioxide is changed, the gas-sensitive performance of the tin dioxide is enhanced, and therefore the detection of target gas molecules is realized; one-step hydrothermal method is simple to operate, and sample influence factors are reduced compared with two-step hydrothermal method; the preparation process is simple, and the product has good sensitivity and selectivity to ethanol at 350 ℃.
Example 1
Step 1, adding 0.188g of stannous chloride and 2.45g of trisodium citrate into a mixed solution of deionized water and ethylene glycol, stirring to obtain a mixed solution A, adding 0.0035g of silver nitrate into the mixed solution, and stirring for 1 hour to obtain a mixed solution B; the mixing ratio of the deionized water to the ethylene glycol is 2: 3;
step 2, placing the mixed solution B in a polytetrafluoroethylene reaction kettle for hydrothermal reaction at the temperature of 200 ℃ for 24 hours, cooling to room temperature, taking out a mixture at the bottom of the reaction kettle, and placing the mixture in a centrifugal tube for centrifugal separation to obtain a sample;
step 3, washing the sample by using deionized water and ethanol in sequence, and drying to obtain the silver-doped tin dioxide nanosheet self-assembled flower-like material, wherein SEM images are shown in figures 1 and 2, and the SnO of the embodiment 1 is SnO2The nano material is a nano flower with the diameter of about 4.3-4.9 mu m, which is composed of a wafer with the diameter of about 1.0-1.2 mu m and the thickness of about 70-75 nm, and has clear pattern outline but larger diameter; the XRD patterns are shown in FIG. 3a and FIG. 3b, and it can be seen from the patterns that the diffraction peak and tetragonal SnO of the product2Standard card (JCPDS.41-1445) was in agreement, indicating that the product was of tetragonal rutile structure. In addition, the peak intensity of the prepared sample is higher, which indicates that the crystallinity of the sample is stronger. Since the amount of doping is relatively small and the peak of Ag is not obvious in the figure, the SnO of example 1 is used2The nano material is used as an example to enlarge and purify an XRD patternSnO2The comparison of the nano materials can see an obvious Ag peak, which proves that the Ag is successfully doped.
The WS-30A gas sensor test system is used to test the response of the silver-doped tin dioxide nanosheet self-assembled flower-like material of the present embodiment to ethanol gas at different concentrations, and the results are shown in fig. 4. The influence of the concentration of the ethanol gas on the sensitivity of the sample is tested at the working temperature of 350 ℃. As can be seen, in the range of 1ppm to 500ppm, the sample sensitivity increases with increasing gas concentration.
Example 2
Step 1, adding 0.19g of stannous chloride and 2.46g of trisodium citrate into a mixed solution of deionized water and ethylene glycol, stirring to obtain a mixed solution A, adding 0.014g of silver nitrate into the mixed solution, and stirring for 1.2h to obtain a mixed solution B; the mixing ratio of the deionized water to the ethylene glycol is 2: 3;
step 2, placing the mixed solution B in a polytetrafluoroethylene reaction kettle for hydrothermal reaction at the temperature of 190 ℃ for 20 hours, cooling to room temperature, taking out a mixture at the bottom of the reaction kettle, and placing the mixture in a centrifugal tube for centrifugal separation to obtain a sample;
and 3, washing the sample by adopting deionized water and ethanol in sequence, and drying to obtain the silver-doped tin dioxide nanosheet self-assembled flower-shaped material.
Example 3
Step 1, adding 0.2g of stannous chloride and 2.5g of trisodium citrate into a mixed solution of deionized water and ethylene glycol, stirring to obtain a mixed solution A, adding 0.007g of silver nitrate into the mixed solution, and stirring for 1.5 hours to obtain a mixed solution B; the mixing ratio of the deionized water to the ethylene glycol is 2: 3;
step 2, placing the mixed solution B in a polytetrafluoroethylene reaction kettle for hydrothermal reaction at the temperature of 180 ℃ for 18h, cooling to room temperature, taking out a mixture at the bottom of the reaction kettle, and placing the mixture in a centrifugal tube for centrifugal separation to obtain a sample;
and 3, washing the sample by adopting deionized water and ethanol in sequence, and drying to obtain the silver-doped tin dioxide nanosheet self-assembled flower-shaped material.
Claims (5)
1. A preparation method of a silver-doped tin dioxide nanosheet self-assembled flower-shaped material is characterized by comprising the following steps:
step 1, adding stannous chloride and trisodium citrate into a mixed solution of deionized water and ethylene glycol, stirring to obtain a mixed solution A, adding silver nitrate into the mixed solution, and stirring to obtain a mixed solution B;
step 2, placing the mixed solution B in a polytetrafluoroethylene reaction kettle for hydrothermal reaction, cooling, taking out a mixture at the bottom of the reaction kettle, and performing centrifugal separation on the mixture to obtain a sample;
and 3, washing the sample by adopting deionized water and ethanol in sequence, and drying to obtain the silver-doped tin dioxide nanosheet self-assembled flower-shaped material.
2. The preparation method of the silver-doped tin dioxide nanosheet self-assembled flower-like material as claimed in claim 1, wherein the molar ratio of the stannous chloride to the trisodium citrate to the silver nitrate is 1:1: 0.0208-1: 1: 0.0832.
3. The method for preparing the silver-doped tin dioxide nanosheet self-assembled flower-like material according to claim 1, wherein the mixing ratio of the deionized water to the ethylene glycol in step 1 is 2: 3.
4. The method for preparing the silver-doped tin dioxide nanosheet self-assembled flower-like material as recited in claim 1, wherein the stirring time after the silver nitrate is added in step 1 is 1h to 1.5 h.
5. The method for preparing the silver-doped tin dioxide nanosheet self-assembled flower-like material according to claim 1, wherein the hydrothermal reaction in step 2 is carried out at a temperature of 180-200 ℃ for a reaction time of 18-24 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113860360A (en) * | 2021-11-17 | 2021-12-31 | 云南锡业锡化工材料有限责任公司 | Preparation method of nano flower-ball-shaped tin dioxide |
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2020
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Non-Patent Citations (1)
| Title |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113860360A (en) * | 2021-11-17 | 2021-12-31 | 云南锡业锡化工材料有限责任公司 | Preparation method of nano flower-ball-shaped tin dioxide |
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