CN105129842B - Preparation method of high-activity SnO2 nanocrystal responding to visible light - Google Patents
Preparation method of high-activity SnO2 nanocrystal responding to visible light Download PDFInfo
- Publication number
- CN105129842B CN105129842B CN201510577536.4A CN201510577536A CN105129842B CN 105129842 B CN105129842 B CN 105129842B CN 201510577536 A CN201510577536 A CN 201510577536A CN 105129842 B CN105129842 B CN 105129842B
- Authority
- CN
- China
- Prior art keywords
- nanocrystal
- sno
- sno2
- visible light
- 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
Landscapes
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of high-activity SnO2 nanocrystal responding to visible light. The method comprises the steps of dissolving two types of tin salts such as SnCl4.5H2O and SnCl2.2H2O in deionized water, so as to be uniformly mixed; then adjusting the pH value of mixed liquor with hydrochloric acid and ammonia water, so that the pH value is enabled to be between 0 and 14; finally, performing a hydrothermal reaction for 1 to 120 hours under the condition of the temperature of 100 to 300 DEG C, and filtering and drying a product, so as to obtain the SnO2 nanocrystal. According to the preparation method, the SnO2 nanocrystal is synthesized by adopting a hydrothermal method, and the synthetic method has the advantages of simplicity, environmental friendliness, low temperature, no need of calcination and the like, and the SnO2 nanocrystal obtained by adopting the method has the advantages of high purity, uniform and controllable particle size and high activity, and has strong visible light response and photoresponse adjustability and can be used in the field of energy and environmental protection of visible light-induced photocatalysts, solar cells and the like.
Description
Technical field
The invention belongs to visible light catalyst and solaode equal energy source field of environment protection, and in particular to a kind of visible ray rings
The high activity SnO for answering2The preparation method of nanocrystal.
Background technology
SnO2It is one of important semiconductor material with wide forbidden band, in solar energy conversion, photocatalysis, nesa coating, air-sensitive
Sensor equal energy source field of environment protection is all widely used.It is 3.65ev yet with its energy gap, only in ultraviolet light range
There is response, and UV energy only accounts for 4% of sunshine gross energy or so, so accounting for visible ray of the gross energy up to 43% can not be by
Which makes full use of；When exciting additionally, due to light, produced electronics is very easy to compound with hole so that its photo-quantum efficiency is very
It is low.Based on two above major defect, people are constantly to SnO2It is modified and develops the nano material of novel visible response.
Based on the consideration for developing visible light-responded high efficiency catalysis material, each research of world wide in the last few years is little
Group is to SnO2Nano material is modified and continually develops new catalysis material, and its progress is concentrated mainly on following
Aspect：1、SnO2Crystal morphology Growth Control：Crystal with high activity face is synthesized to improve its performance by control；2、
SnO2Crystal doping is adjusted can band：By the doping of various ions reducing its bandwidth；3rd, surfactant is to SnO2Plane of crystal
Modified and dye sensitization；4th, noble metal decorated SnO2Crystal；5th, using Graphene or other quasiconductors and SnO2Crystal carries out different
Matter is combined.Research is for expansion SnO above2Photoresponse serve positive effect from ultra-violet (UV) band to visible region, but its
Material preparation technology is more complicated, as substantial amounts of surfactant or noble metal will be used in such as preparation process, thus
It is relatively costly, and the material such as dye sensitizing agent under arms during efficiency, activity, photoetch and stability etc. exists and asks
Topic, it is important to which these technologies still do not solve SnO at present2Photoresponse does not also reach black TiO in the weaker shortcoming in visual field2
Visible light-responded ability.Therefore find a cheap, stable, preferable SnO of effect2The preparation method of nanocrystal becomes
When previous important problem.
The content of the invention
Present invention is primarily targeted at overcoming prior art to visible light-responded weaker shortcoming, there is provided a kind of technique letter
List, energy-conserving and environment-protective, visible light-responded strong high activity SnO2The preparation method of nanocrystal.
The present invention is achieved by the following technical programs：A kind of visible light-responded high activity SnO2Nanocrystal
Preparation method, it is characterised in that：The divalent salts of the quaternary salts of stannum and stannum are dissolved in into mix homogeneously in deionized water, rubbing for the two is made
Your concentration ratio is 1:0.01～0.01:1；Hydrochloric acid and ammonia is adopted to adjust the pH value of mixed liquor again so as in 0～14 model
Enclose；Last to carry out hydro-thermal reaction 1～120 hour under conditions of temperature is for 100～300 DEG C, product is dry through being filtered dry, you can
To SnO2Nanocrystal.
The quaternary salts of the stannum are：Na2SnO3·4H2O or SnCl4·5H2O；The divalent salts of stannum are：SnCl2·2H2O or
SnSO4。
Above-mentioned SnO2Nanocrystal is cubic facies pattern, and its particle size is 3～5 nanometers.
Relative to prior art, the invention has the advantages that and beneficial effect：
（1）The present invention synthesizes SnO using hydro-thermal method2Nanocrystal, synthetic method are simple, do not use any surface activity
Agent, has the advantages that environmental friendliness, low temperature compared with other methods, is not required to calcining and can directly obtain product in the solution；
（2）Gained SnO of the invention2Nanocrystal, granule are less, size uniform, and activity is higher, with stronger visible ray
Response and photoresponse adjustability.
Description of the drawings
Fig. 1 is the SnO prepared by experimental example of the present invention 1 ~ 62The XRD figure of nanocrystal；
Fig. 2 is the SnO prepared by the embodiment of the present invention 12The transmission electron microscope photo of nanocrystal.
Specific embodiment
For further illustrating the present invention for reaching technological means and effect that predetermined goal of the invention is taken, below in conjunction with
Preferred embodiment, to as follows according to the detailed description of the invention：
Embodiment 1
By SnCl4·5H2O and SnCl2·2H2O is dissolved in deionized water, is uniformly mixed, and distinguishes the two concentration
For 0.3mol/L, 0.003mol/L, concentration ratio are 1:0.01;The pH value that mixed liquor is adjusted with hydrochloric acid is 0；Finally at 100 DEG C
Hydrothermal condition under react 120 hours, product filtration drying is obtained even size distribution, and size is about the SnO of 3-5nm2
Nanocrystal.As shown in curve 1 in Fig. 1, all diffraction maximums can be with the Tetragonal SnO of bottom2The base peak phase of nanocrystal
Correspondence, it can thus be appreciated that gained SnO2For pure cubic facies pattern structure, the TEM photos of such as Fig. 2, it can be seen that SnO2Crystalline size point
Cloth is uniform, and size is about 3-5nm.
Embodiment 2
By Na2SnO34H2O and SnCl22H2O is dissolved in deionized water, is uniformly mixed, and is respectively the two concentration
0.003mol/L, 0.3mol/L, concentration ratio are 0.01:1;The pH value that mixed liquor is adjusted with ammonia is 14；Finally at 300 DEG C
Hydrothermal condition under react 1 hour, product filtration drying is obtained even size distribution, and size is about the SnO of 3-5nm2Receive
Meter Jing Ti.As shown in curve 2 in Fig. 1, all diffraction maximums can be with the Tetragonal SnO of bottom2The base peak of nanocrystal is relative
Should, it can thus be appreciated that gained SnO2For pure cubic facies pattern structure.
Embodiment 3
By SnCl4·5H2O and SnSO4It is dissolved in deionized water, is uniformly mixed, is respectively the two concentration
0.21mol/L, 0.09mol/L, concentration ratio are 0.7:0.3;The pH value that mixed liquor is adjusted with ammonia is 12；Finally at 200 DEG C
Hydrothermal condition under react 48 hours, product filtration drying is obtained even size distribution, and size is about the SnO of 3-5nm2Receive
Meter Jing Ti.As shown in curve 3 in Fig. 1, all diffraction maximums can be with the Tetragonal SnO of bottom2The base peak of nanocrystal is relative
Should, it can thus be appreciated that gained SnO2For pure cubic facies pattern structure.
Embodiment 4
By Na2SnO3·4H2O and SnSO4It is dissolved in deionized water, is uniformly mixed, is respectively the two concentration
0.15mol/L, 0.15mol/L, concentration ratio are 0.5:0.5;The pH value that mixed liquor is adjusted with ammonia is 10；Finally at 150 DEG C
Hydrothermal condition under react 72 hours, product filtration drying is obtained even size distribution, and size is about the SnO of 3-5nm2Receive
Meter Jing Ti.As shown in curve 4 in Fig. 1, all diffraction maximums can be with the Tetragonal SnO of bottom2The base peak of nanocrystal is relative
Should, it can thus be appreciated that gained SnO2For pure cubic facies pattern structure.
Embodiment 5
By SnCl4·5H2O and SnCl2·2H2O is dissolved in deionized water, is uniformly mixed, and is respectively the two concentration
0.09mol/L, 0.21mol/L, concentration ratio are 0.3:0.7;The pH value that mixed liquor is adjusted with hydrochloric acid is 4；Finally at 250 DEG C
React 24 hours under hydrothermal condition, product filtration drying is obtained even size distribution, size is about the SnO of 3-5nm2Nanometer
Crystal.As shown in curve 5 in Fig. 1, all diffraction maximums can be with the Tetragonal SnO of bottom2The base peak of nanocrystal is corresponding,
It can thus be appreciated that gained SnO2For pure cubic facies pattern structure.
Embodiment 6
By Na2SnO3·4H2O and SnSO4It is dissolved in deionized water, is uniformly mixed, is respectively the two concentration
0.03mol/L, 0.27mol/L, concentration ratio are 0.1:0.9;The pH value that mixed liquor is adjusted with hydrochloric acid is 6；Finally at 120 DEG C
React 96 hours under hydrothermal condition, product filtration drying is obtained even size distribution, size is about the SnO of 3-5nm2Nanometer
Crystal.As shown in curve 6 in Fig. 1, all diffraction maximums can be with the Tetragonal SnO of bottom2The base peak of nanocrystal is corresponding,
It can thus be appreciated that gained SnO2For pure cubic facies pattern structure.
Above example be obtained product XRD test be to carry out in 2200 VPC of Rigaku D/MAX, TEM be
Carry out in JEM-2010HR transmission electron microscopes.
Presently preferred embodiments of the present invention is the foregoing is only, the present invention, all originals in the present invention is not limited to
Then with spirit within any modification, equivalent and the improvement made etc., be included within protection scope of the present invention.
Claims (1)
1. a kind of visible light-responded high activity SnO2The preparation method of nanocrystal, it is characterised in that：By SnCl4·5H2O and
SnCl2·2H2O is dissolved in deionized water, is uniformly mixed, and makes the two concentration be respectively 0.3mol/L, 0.003mol/L, dense
Degree is than being 1:0.01;The pH value that mixed liquor is adjusted with hydrochloric acid is 0；It is last to react 120 hours under 100 DEG C of hydrothermal condition, produce
Thing filtration drying is obtained even size distribution, SnO of the size for 3-5nm2Nanocrystal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510577536.4A CN105129842B (en) | 2015-09-12 | 2015-09-12 | Preparation method of high-activity SnO2 nanocrystal responding to visible light |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510577536.4A CN105129842B (en) | 2015-09-12 | 2015-09-12 | Preparation method of high-activity SnO2 nanocrystal responding to visible light |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105129842A CN105129842A (en) | 2015-12-09 |
| CN105129842B true CN105129842B (en) | 2017-03-22 |
Family
ID=54715505
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510577536.4A Expired - Fee Related CN105129842B (en) | 2015-09-12 | 2015-09-12 | Preparation method of high-activity SnO2 nanocrystal responding to visible light |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105129842B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105776323B (en) * | 2016-02-26 | 2018-08-14 | 西南石油大学 | A method of it prepares with visible light-responded tin dioxide quantal-point |
| CN106268750B (en) * | 2016-10-14 | 2019-05-28 | 山东大学 | A kind of visible-light response type Photoreduction Activity of Isolated SnO2-XThe preparation method of nano particle |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100365170C (en) * | 2005-12-01 | 2008-01-30 | 华中师范大学 | SnO2 monodisperse nano monocrystal with square structure and synthesis method thereof |
| CN101209856B (en) * | 2007-12-21 | 2011-09-28 | 中国科学院长春应用化学研究所 | Method for synthesizing tin oxide nanocrystalline by mould plate method combined with hydrothermal condition |
| WO2014183265A1 (en) * | 2013-05-14 | 2014-11-20 | Essilor International (Compagnie Generale D'optique) | Fluorine-doped stannic oxide colloids and method for preparing same |
| CN103263906A (en) * | 2013-05-16 | 2013-08-28 | 陕西科技大学 | Nanocrystal tin oxide photocatalyst and preparation method thereof |
| CN103508484B (en) * | 2013-09-30 | 2015-03-25 | 西北大学 | Infrared low-emissivity nanocrystalline thin-film material SnO2 and preparation method thereof |
-
2015
- 2015-09-12 CN CN201510577536.4A patent/CN105129842B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN105129842A (en) | 2015-12-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhu et al. | Fabrication and photocatalytic activity enhanced mechanism of direct Z-scheme g-C3N4/Ag2WO4 photocatalyst | |
| CN108147462A (en) | A kind of tungsten trioxide nano-rod and its preparation with photocatalysis performance | |
| CN102674451A (en) | Preparation method of {001} face exposed titanium dioxide nanocrystals | |
| CN106215942B (en) | A kind of controllable synthesis method for the plate-like zinc oxide being doped with transition metal or rare earth metal | |
| CN108502922B (en) | Anatase titanium dioxide microsphere and preparation method thereof | |
| Yao et al. | Biomimetic Bi2WO6 with hierarchical structures from butterfly wings for visible light absorption | |
| CN110368962A (en) | A kind of BiOI/WO3Preparation method, product and the application of hetero-junctions efficient photoelectricity treater catalysis electrode | |
| CN105129842B (en) | Preparation method of high-activity SnO2 nanocrystal responding to visible light | |
| CN110465285B (en) | BiVO4Preparation method and application of @ carbon nano-dot composite photocatalytic material | |
| CN105478153A (en) | CeVO4 / Ag / g-C3N4 composite photocatalyst and preparation method thereof | |
| CN113877586B (en) | Preparation method and application of cerium-iron bimetallic composite oxide with hierarchical structure and controllable morphology | |
| Xiao et al. | Multiple layered macroporous SnO2 film for applications to photoelectrochemistry and morphology control of iron oxide nanocrystals | |
| CN108654663B (en) | Boron-nitrogen co-doped single crystal mesoporous TiO prepared by mixed nitrate molten salt method2Method for catalyzing materials | |
| CN109437292A (en) | A kind of ultra-thin two-dimension titanium dioxide nanoplate efficiently synthesized and preparation method | |
| CN111151233B (en) | Oxygen-deficient TiO2Normal temperature and pressure water phase preparation method | |
| CN110394175B (en) | Method for preparing copper-doped mesoporous titanium dioxide by template method and application | |
| CN105948106B (en) | A kind of preparation method of narrow band gap tin ash semiconductor nano material | |
| CN108525651A (en) | A kind of reduction titanium dioxide process with highlight catalytic active | |
| CN110075903B (en) | Preparation method of C, N co-doped nano titanium dioxide | |
| CN103861631A (en) | Preparation method of nitrogen-doped titanium dioxide nanoribbon visible light photocatalyst | |
| CN103060872A (en) | Method for preparing lignin sulfonate-doped nano-zinc oxide composite film by electrochemical deposition method | |
| CN103754929B (en) | Preparation method for TiO2/InVO4 composite porous micro-sphere | |
| CN109939745A (en) | A kind of nano-titanium dioxide/wood flour composite material and its preparation method and application | |
| CN108067277B (en) | High nitrogen content single crystal TiO2Preparation method of mesoporous material | |
| CN109289880A (en) | A kind of BiOI (100)/BiOI (001) is the same as phase homojunction and preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: 333001 Tao Yang Road, Jingdezhen New District, Jiangxi, No. 27 Applicant after: JINGDEZHEN CERAMIC INSTITUTE Address before: 333001 Tao Yang Road, Jingdezhen New District, Jiangxi, No. 27 Applicant before: Jingdezhen College of Ceramic Industry |
|
| COR | Change of bibliographic data | ||
| 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: 20170322 Termination date: 20200912 |