CN101462764B - Preparation of stannic oxide nano-rod - Google Patents
Preparation of stannic oxide nano-rod Download PDFInfo
- Publication number
- CN101462764B CN101462764B CN2009100449274A CN200910044927A CN101462764B CN 101462764 B CN101462764 B CN 101462764B CN 2009100449274 A CN2009100449274 A CN 2009100449274A CN 200910044927 A CN200910044927 A CN 200910044927A CN 101462764 B CN101462764 B CN 101462764B
- Authority
- CN
- China
- Prior art keywords
- reactor
- length
- preparation
- tin dioxide
- liquid mixture
- 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
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims description 14
- 239000002073 nanorod Substances 0.000 title abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002485 combustion reaction Methods 0.000 claims abstract description 11
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 6
- 239000010935 stainless steel Substances 0.000 claims abstract description 6
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims abstract description 5
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 5
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims abstract description 5
- 239000006200 vaporizer Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 238000009834 vaporization Methods 0.000 claims description 6
- 230000008016 vaporization Effects 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 230000001939 inductive effect Effects 0.000 claims description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- 239000008246 gaseous mixture Substances 0.000 claims 3
- 238000000034 method Methods 0.000 abstract description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 9
- 239000007789 gas Substances 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 239000000758 substrate Substances 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 abstract 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 abstract 1
- 230000006698 induction Effects 0.000 abstract 1
- 238000002347 injection Methods 0.000 abstract 1
- 239000007924 injection Substances 0.000 abstract 1
- 230000005540 biological transmission Effects 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Images
Classifications
-
- 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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
Landscapes
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention relates to a method for preparing tin dioxide nanorods, which comprises the following steps: tin tetrachloride, ferric trichloride and ethanol are uniformly mixed and added by an injection pump into an evaporator to react with preheated air; the mixed air enters a stainless steel tube reactor which is adjustable in length from a burner arranged at the top of a combustion reactor to undergo a hydrolysis reaction at 1,500 to 2,500 DEGC to grow in an oriented way under the induction of the iron element to form a tin dioxide rod structure finally; and tail gases are discharged from the top of the combustion reactor, collected and passed through a hydrogen chloride absorption tower to be discharged completely. The method for preparing a tin dioxide nanorod structure does not require any substrate and is simple in equipment and process, low in period, high in yield, suitable for continuous large-scale production and easy to implement industrially.
Description
Technical field
The present invention relates to a kind of preparation method of nanometer tin dioxide rod, especially serialization mass-producing ground preparation nanometer tin dioxide rod.
Background technology
In recent years, the research of oxide compound one dimension Nano structure becomes the hot subject of physics, material, chemical field.The oxide compound one dimension Nano structure has excellent physics and chemical property, simultaneously be easy to make up nano-device again to form suitability for industrialized production, they have broad application prospects in Laser Devices, nanoelectronics, nanophotonics and following integrated circuit (IC) design of new generation.In traditional field, tindioxide is a kind of conductor oxidate material of excellent property, and it has wide band gap (3.6eV), low resistivity (10
-4-10
-6Ω cm) rare high light transmittance and in other semi-conductors, thereby be ideal electrode of solar battery and sensor material.Now, field-effect transistor, highly sensitive chemical sensor, high power lithium battery and the sun power dye cell etc. made with the tin oxide nano rod of beginning have caused international concern.At present; the synthetic method of nanometer tin dioxide rod shape structure mainly comprises hydrothermal method, heat deposition method, molten-salt growth method, template etc.; advantages such as that though aforesaid method has are simple to operate, controllability is strong, complicated aftertreatment technology, high energy consumption and little output have greatly limited the production of the continuous mass-producing of nanometer tin dioxide rod shape material.Therefore, the method for developing a kind of continuous large-scale production nanometer tin dioxide rod has broad application prospects.
Summary of the invention
The object of the present invention is to provide the preparation method of the continuous mass-producing of a kind of nanometer tin dioxide rod, to overcome the above-mentioned defective of existing in prior technology.
Design of the present invention is such:
With SnCl
4, FeCl
3Ethanolic soln add vaporizer through syringe pump because ethanol and SnCl
4Boiling point be respectively 78.4 ℃ and 114.4 ℃, FeCl in addition
3Content is few, the formation mixing steam so solution is vaporized fully.This mixing steam enters the high-speed jet stainless steel reactor by the burner of pipe core after with air mixed, promptly enters into the annular flame inside that combustion of hydrogen forms after the burner ejection, and part ethanol is also ignited simultaneously.Two stages of doped element iron in the flame process can influence particulate and form and pattern: at first, in the starting stage of flame, formation, sintering and growth velocity that the initial cluster of influence is crossed by the doped element Tie Tong influence nascent particulate size; In the follow-up phase of flame, along with gas temperature reduces, doped element iron begins to influence the formation of crystalline structure, thereby has suppressed the growth of (100) faces.The formation of final club shaped structure can be thought the result of particle in rear half stage annealing reformation and edge (001) planar orientation growth.Can increase the residence time of particle in flame by the length that prolongs stainless steel reactor, and then strengthen this process, obtain the higher nanometer tin dioxide rod shape structure of productive rate.
Preparation method of the present invention is characterized in that, comprises the steps:
Tin tetrachloride, iron trichloride and ethanol uniform mixing are obtained liquid mixture, utilize syringe pump to add the air mixed of vaporizer vaporization with preheating, enter length-adjustable reactor (can be stainless steel) by the pipe core that is arranged on combustion reactor top burner, in reactor, carry out abundant hydrolysis reaction, and oriented growth forms the nano bar-shape structure under the inducing action of ferro element, and temperature of reaction is 1000～2000 ℃; The final club shaped structure tindioxide that generates can discharge from the combustion reactor top and collect, and tail gas then passes through emptying behind the HCl absorption tower.The length of gained club shaped structure tindioxide is 100～400nm, and wide is 20～80nm, and length-to-diameter ratio is 5～20, and is better dispersed.
Control the length and the length-to-diameter ratio of synthetic nanometer tin dioxide rod by the adjustment of following processing parameter:
The ethanolic soln mass concentration of tin tetrachloride and iron trichloride is 10～20%, and the mol ratio of tin and iron is 10: 1～100: 1, and the air input of pipe core and the ratio of above-mentioned solution feed amount are 1～2m
3/ h: 2～5ml/min;
The length of stainless steel tube reactor was directly proportional with the residence time of particle in flame, and its length can be 20cm～80cm;
Tin tetrachloride, iron trichloride and alcoholic acid mixing solutions, utilizing syringe pump to add temperature range is 200～300 ℃ vaporizer vaporization.
Adopt method of the present invention to prepare the tindioxide club shaped structure, apparatus and process is simple, does not need any substrate, short output height of cycle, and large-scale production continuously is easy to industrializing implementation.And resulting structures homogeneous and controllable, crystallinity are good, have utmost point application prospects.
Description of drawings
Fig. 1 is the Production Flow Chart synoptic diagram of the embodiment of the invention;
Fig. 2 is the electromicroscopic photograph of the embodiment of the invention 1 product;
Fig. 3 is the electromicroscopic photograph of the embodiment of the invention 2 products.
Embodiment
To help to understand the present invention by the following description of the embodiments, but not limit content of the present invention.
Embodiment 1
The schema of the continuous large-scale preparation method of nanometer tin dioxide rod as shown in Figure 1, SnCl
4And FeCl
3The ethanol solution of (mol ratio of Sn: Fe is 10: 1) (massfraction is 18%) utilizes syringe pump to add the same air mixed of vaporizer, and feeding rate is 2ml/min, and air flow quantity is 1.5m
3/ h, preheating temperature is 250 ℃, evaporator temperature is controlled at 250 ℃, vaporization is after the burner pipe core enters reactor, reactor length is 50cm, because the length of reactor was directly proportional with the residence time of particle in flame, the length of this reactor can be adjusted between 20cm～80cm.The too short purpose that prolongs the length of flame that do not have of reactor length, long meeting causes the excessive sintering of particle, and agglomeration is serious, therefore selects above-mentioned length range to operate.The hydrolysis reaction of presoma carries out in the combustion chamber, and hydrolysising reacting temperature is 1500 ℃, and oriented growth generates club shaped structure under the inducing action of ferro element, discharges from the combustion reactor top and collects, emptying behind the tail gas process HCl absorption tower.For preventing condensation in the mixing steam transmission course, 250 ℃ of the whole constant temperature of vaporizer and transmission pipeline.The mean diameter of products therefrom is 40nm, and length is 300nm, and length-to-diameter ratio is about 10, and its electromicroscopic photograph as shown in Figure 2.
Embodiment 2
The schema of the continuous large-scale preparation method of nanometer tin dioxide rod as shown in Figure 1, SnCl
4And FeCl
3The ethanol solution of (mol ratio of Sn: Fe is 100: 1) (massfraction is 20%) utilizes syringe pump to add the same air mixed of vaporizer, and feeding rate is 5ml/min, and air flow quantity is 1.5m
3/ h, preheating temperature is 300 ℃, evaporator temperature is controlled at 300 ℃, vaporization is after the burner pipe core enters combustion reactor, reactor length is 30cm, because the length of reactor was directly proportional with the residence time of particle in flame, the length of this reactor can be adjusted between 20cm～80cm.The hydrolysis of presoma is carried out in the combustion chamber, and hydrolysising reacting temperature is 2500 ℃, and oriented growth finally generates club shaped structure under the inducing action of ferro element, discharges from the combustion reactor top and collects, emptying behind the tail gas process HCl absorption tower.For preventing condensation in the mixing steam transmission course, 300 ℃ of the whole constant temperature of vaporizer and transmission pipeline.The mean diameter of products therefrom is 50nm, and length is 250nm, and length-to-diameter ratio is about 5, and its electromicroscopic photograph as shown in Figure 3.
Claims (6)
1. the continuous preparation method of a nanometer tin dioxide rod is characterized in that, comprises the steps: at first, and tin tetrachloride, iron trichloride and ethanol uniform mixing are obtained liquid mixture; Then, utilize syringe pump that described liquid mixture is added the vaporizer vaporization and obtains gaseous mixture with the air mixed of preheating, described gaseous mixture enters length-adjustable reactor by the pipe core that is arranged on the burner on the combustion reactor, in described reactor, carry out abundant hydrolysis reaction, and oriented growth forms the nano bar-shape structure under the ferro element inducing action of described iron trichloride, and described hydrolysising reacting temperature is 1500～2500 ℃; Finally obtain nanometer tin dioxide rod.
2. preparation method according to claim 1, it is characterized in that, the mass concentration of described liquid mixture is 10～20%, and wherein the mol ratio of tin element and ferro element is 10: 1～100: 1, and the air input of described pipe core and the inlet amount ratio of described liquid mixture are 1～2m
3/ h:2～5ml/min.
3. preparation method according to claim 1 is characterized in that, the length of described reactor was directly proportional with particle residence time of high-temperature zone in flame of described gaseous mixture, and the length of described reactor is 20～80cm.
4. preparation method according to claim 1 is characterized in that, the temperature range of vaporization operation is 200～300 ℃ in the described vaporizer.
5. preparation method according to claim 1 is characterized in that, the length of described nanometer tin dioxide rod is 100～400nm, and width is 20～80nm, and length-to-diameter ratio is 5～20.
6. preparation method according to claim 1 is characterized in that described reactor is a stainless steel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100449274A CN101462764B (en) | 2009-01-06 | 2009-01-06 | Preparation of stannic oxide nano-rod |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100449274A CN101462764B (en) | 2009-01-06 | 2009-01-06 | Preparation of stannic oxide nano-rod |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101462764A CN101462764A (en) | 2009-06-24 |
| CN101462764B true CN101462764B (en) | 2011-02-09 |
Family
ID=40803590
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100449274A Expired - Fee Related CN101462764B (en) | 2009-01-06 | 2009-01-06 | Preparation of stannic oxide nano-rod |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101462764B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043712B (en) * | 2013-01-15 | 2014-05-21 | 华东理工大学 | Method for preparing precious metal gold particle catalytically-grown stannic oxide nanowire |
-
2009
- 2009-01-06 CN CN2009100449274A patent/CN101462764B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN101462764A (en) | 2009-06-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101456580B (en) | Method for preparing stannic oxide nano wire | |
| CN108502918B (en) | Synthesis method of inorganic perovskite nanowire | |
| Wang et al. | Synthesis of TiO2 nanoparticles by premixed stagnation swirl flames | |
| CN101954480B (en) | Method for preparing carbon-coated core-shell nanoparticles continuously | |
| CN104973615B (en) | Microwave burning preparation method of nano gadolinium oxide powder | |
| Guo et al. | Synthesis of ZnO nanoparticles with a novel combustion method and their C2H5OH gas sensing properties | |
| CN100369803C (en) | Method and apparatus for preparing fumed nano oxide | |
| CN102658105B (en) | Continuous preparation method of titanium dioxide with high visible light absorptivity | |
| CN103359773B (en) | A kind of preparation method of zinc oxide nano rod | |
| CN103043712B (en) | Method for preparing precious metal gold particle catalytically-grown stannic oxide nanowire | |
| CN103706350A (en) | In2O3/ZnO heterostructure nanotube as well as preparation method and application thereof | |
| CN108126728B (en) | Preparation method of g-C3N4/g-C3N4 metal-free isomeric structure, obtained product and application | |
| CN101412542A (en) | Method for preparing perovskite type LaFe0.5Mn0.5O3 by geoceric acid solution combustion method | |
| CN101462764B (en) | Preparation of stannic oxide nano-rod | |
| CN104556006A (en) | Equipment and process for industrially producing graphene by microwaves | |
| CN102515177B (en) | Preparation method of stannic oxide/silica composite nano-particle | |
| CN108608006A (en) | A kind of preparation method and system of silver copper oxide composite powder | |
| CN104556009A (en) | Equipment for industrially producing graphene by microwaves | |
| CN100376483C (en) | Prepn process of nanometer tin dioxide particle with homogenous particle size | |
| Habibi et al. | Shape and size-controlled fabrication of ZnO nanostructures using novel templates | |
| CN101498034A (en) | Preparation of transient metal doped nano zinc oxide crystal whisker | |
| CN207243476U (en) | Electronic-grade polycrystalline silicon reduction furnace | |
| CN101215002B (en) | Process for preparing titanium dioxide of core-shell structure | |
| CN102863018A (en) | Preparation method of nanometer tin dioxide particles | |
| CN101734720A (en) | Method for preparing vanadium dioxide ultrafine powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110209 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |