CN109467127A - A kind of preparation method of more Metal Supported tungsten oxide composite nano-lines - Google Patents
A kind of preparation method of more Metal Supported tungsten oxide composite nano-lines Download PDFInfo
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- CN109467127A CN109467127A CN201811285394.4A CN201811285394A CN109467127A CN 109467127 A CN109467127 A CN 109467127A CN 201811285394 A CN201811285394 A CN 201811285394A CN 109467127 A CN109467127 A CN 109467127A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/02—Oxides; Hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
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- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
Abstract
The invention belongs to technical field of nanometer material preparation, are related to a kind of preparation method of more Metal Supported tungsten oxide composite nano-lines, prepare W first with solvent thermal technology18O49Nano-material, then noble metal precursor body is added in liquid phase environment, W is prepared using in-situ reducing noble metal precursor body18O49Surfactant, linking agent is not used in/Ag/Pt composite nano-line, and obtained surface of metal particles is completely without ligand；Preparation method is simple, has versatility, and the dosage by changing metal precursor can easily regulate and control the tenor of composite Nano linear load.
Description
Technical field:
The invention belongs to technical field of nanometer material preparation, are related to a kind of system of more Metal Supported tungsten oxide composite nano-lines
Preparation Method, especially a kind of W18O49The preparation method of/Ag/Pt composite nano-line.
Background technique:
Tungsten oxide is a kind of important transition metal oxide semiconductor material, has and prepares simple, structure easy-regulating, object
Physicochemical steady performance is widely used in the research such as sensor, photochemical catalyst, lithium ion battery, electrooptical device
Field.Tungsten oxide nano-material has very important application prospect, unique one-dimentional structure energy in the semiconductor device
Biggish surface volume ratio, higher carrier mobility speed and surface defect site abundant are enough improved, is very suitable to use
To make gas sensor.
For the detection performance for further increasing sensor, people are usually in tungsten oxide area load noble metal nano particles.
Currently, mainly using the methods of chemical reduction method or physical sputtering, example in tungsten oxide nano-material area load noble metal
If CN201610953128.9 discloses a kind of synthetic method of noble-metal-supported tungsten oxide nano for gas sensor,
The following steps are included: weighing several tungsten oxide nanos rich in oxygen defect, ultrasonic disperse stirs evenly shape into deionized water
Au bleu suspension；It measures several precious metal salt solutions and is divided into two parts, be added while stirring into blue suspension in two times
Precious metal salt solution；Mixture is transferred to centrifuge tube, centrifugation obtains the solid of supernatant liquid and bottom, discards supernatant liquid, protects
It keeps on file the solid in portion；Clean solid；Solid after cleaning is through being dried to obtain final product.The present invention utilizes the oxygen rich in oxygen defect
The reproducibility for changing tungsten itself is reduced directly carried noble metal on its surface, so that material has splendid purity without after any
Treatment process is purified, so that the present invention becomes a room temperature aqueous phase reactions process, with high security, operability
By force, the characteristics of easily promoting；Document " RuiZhou, Xiaoping Lin, Dongyang Xue, Fengyi Zong, Jianmin
Zhang, Xiaochuan Duan, Qiuhong Li, Taihong Wang, Sensors and Actuators B 2018,
260,900-907 " is reported in W18O49Sea urchin body structure surface adsorbs PdCl2, W is then obtained by roasting18O49/ Pd is compound to be received
Rice material；Document " Shibin Sun, Xueting Chang, Lihua Dong, Yidong Zhang, ZhenjiangLi,
Yanyan Qiu, J.Solid State Chem.2011,184,2190-2195 " is reported to be prepared using photochemical reduction
Ag/AgCl/W18O49The method of composite nanorod；Document " Lian Feng Zhua, Jun Cong She, Jian Yi Luo,
Shao Zhi Deng, Jun Chen, Xue Wen Ji, Ning Sheng Xu, Sensors and Actuators B, 2011,
153,354-360 " it reports and is prepared for W using sputtering method18O49/ Pt composite nano-line.Although the above method can be in W18O49Material
Expect area load noble metal, but need multi-step chemical to react and post-process or use physical sputtering equipment, prepared
Journey is not easy enough；In addition, having not yet to see report for multi-component noble-metal-supported.
Summary of the invention:
It is an object of the invention to overcome disadvantage of the existing technology, design provides a kind of in-situ chemical reduction of simplicity
Technology prepares W18O49The method of/Ag/Pt composite nano-line has the advantages such as efficient, easy, ingredient is controllable.
In order to achieve the above-mentioned object of the invention, the present invention prepares W first with solvent thermal technology18O49Nano-material, then in liquid
Noble metal precursor body is added in phase environment, prepares W using in-situ reducing noble metal precursor body18O49/ Ag/Pt composite nano-line, tool
Body includes following steps:
(1) 0.1-0.3g WCl is added in 40mL ethyl alcohol6, stirring and dissolving is packed into stainless steel cauldron, at 180 DEG C plus
Thermal response 20-30h, obtains W18O49Nano wire；
(2) W for taking step (1) to obtain18O49Nano wire 0.1g is added in 20mL deionized water, stirs 10min, is added
0.3-0.5mL concentration is the AgNO of 4mg/mL3Solution obtains reaction solution；
(3) after the reaction solution of step (2) being stirred 4h, the H that 0.5-1.5mL concentration is 4mg/mL is added2PtCl6Solution stirs
12h is mixed, precipitating is dried for 24 hours after being collected by centrifugation at 160 DEG C, and centrifugal speed 9000r/min obtains W18O49/ Ag/Pt is compound
Nano wire.
The present invention and the prior art, are not used surfactant, linking agent, and obtained surface of metal particles is not matched completely
Body；Preparation method is simple, has versatility, and the dosage by changing metal precursor can easily regulate and control composite Nano linear load
Tenor.
Detailed description of the invention:
Fig. 1 is W prepared by the embodiment of the present invention 118O49/ Ag composite nano-line transmission electron microscope photo.
Fig. 2 is W prepared by the embodiment of the present invention 118O49/ Ag composite nano-line high power transmission electron microscope photo.
Fig. 3 is W prepared by the embodiment of the present invention 218O49/ Pt composite nano-line transmission electron microscope photo.
Fig. 4 is W prepared by the embodiment of the present invention 218O49/ Pt composite nano-line high power transmission electron microscope photo.
Fig. 5 is W prepared by the embodiment of the present invention 318O49/ Ag/Pt composite nano-line transmission electron microscope photo.
Fig. 6 is W prepared by the embodiment of the present invention 318O49/ Ag/Pt composite nano-line high power transmission electron microscope photo.
Specific embodiment:
The present invention will be further described by way of example and in conjunction with the accompanying drawings.
Embodiment 1:
0.1g W is added in the present embodiment in 20mL deionized water18O49After stirring 10min, it is dense that 0.4mL is added in nano wire
Degree is the AgNO of 4mg/mL3Solution continues to stir 12h；Obtained product is collected by centrifugation, is successively washed with deionized water and ethyl alcohol
Wash three times, 160 DEG C of dry 12h to get arrive W18O49/ Ag nano wire.
The present embodiment carries out transmission electron microscope characterization to product, and result is as shown in Figure 1, sample has one-dimensional characteristic, by very
The aggregate of Donna rice noodles composition；High power transmission electron microscope characterization is carried out to product, result is as shown in Fig. 2, nano wire has
Highly crystalline, in nanowire surface it can be observed that the Ag nano particle of load.
Embodiment 2:
0.1g W is added in the present embodiment in 20mL deionized water18O49After stirring 10min, it is dense that 0.65mL is added in nano wire
Degree is the H of 4mg/mL2PtCl6Solution continues to stir 12h；Obtained product is collected by centrifugation, successively with deionized water and ethyl alcohol
Washing three times, in 160 DEG C of dry 12h to get to W18O49/ Pt nano wire.
The present embodiment carries out transmission electron microscope characterization to product, and result is as shown in Figure 1, sample has one-dimensional characteristic, by very
The aggregate of Donna rice noodles composition；High power transmission electron microscope characterization is carried out to product, result is as shown in Fig. 2, nano wire has height
Crystallinity is spent, in nanowire surface it can be observed that the Pt nano particle of load.
Embodiment 3:
0.1g W is added in the present embodiment in 20mL deionized water18O49After stirring 10min, it is dense that 0.4mL is added in nano wire
Degree is the AgNO of 4mg/mL3After reaction solution stirs 4h, the H that 1.3mL concentration is 4mg/mL is added in solution2PtCl6Solution continues to stir
12h is mixed, precipitating is after being collected by centrifugation in 160 DEG C of dry 12h to get W18O49/ Ag/Pt composite nano-line.
The present embodiment carries out transmission electron microscope characterization to product, and result is as shown in Figure 1, sample has one-dimensional characteristic, by very
The aggregate of Donna rice noodles composition；High power transmission electron microscope characterization is carried out to product, result is as shown in Fig. 2, nano wire has height
Crystallinity is spent, in nanowire surface it can be observed that Ag the and Pt nano particle of load.
Claims (1)
1. a kind of preparation method of more Metal Supported tungsten oxide composite nano-lines, it is characterised in that prepared first with solvent thermal technology
W18O49Nano-material, then noble metal precursor body is added in liquid phase environment, it is prepared using in-situ reducing noble metal precursor body
W18O49/ Ag/Pt composite nano-line specifically includes following steps:
(1) 0.1-0.3g WCl is added in 40mL ethyl alcohol6, stirring and dissolving is packed into stainless steel cauldron, in 180 DEG C of heating reactions
20-30h obtains W18O49Nano wire；
(2) W for taking step (1) to obtain18O49Nano wire 0.1g is added in 20mL deionized water, stirs 10min, and 0.3- is added
0.5mL concentration is the AgNO of 4mg/mL3Solution obtains reaction solution；
(3) after the reaction solution of step (2) being stirred 4h, the H that 0.5-1.5mL concentration is 4mg/mL is added2PtCl6Solution, stirring
12h, precipitating are dried for 24 hours after being collected by centrifugation at 160 DEG C, and centrifugal speed 9000r/min obtains W18O49/ Ag/Pt is compound to be received
Rice noodles.
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| CN201811285394.4A CN109467127A (en) | 2018-10-31 | 2018-10-31 | A kind of preparation method of more Metal Supported tungsten oxide composite nano-lines |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114392741A (en) * | 2021-12-28 | 2022-04-26 | 安徽大学 | Vacancy-rich silver-loaded tungsten oxide nanowire for improving visible light and near infrared light dynamic bacteriostasis and preparation and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101734614A (en) * | 2009-12-22 | 2010-06-16 | 上海大学 | Method for manufacturing metal oxide nano-wire/noble metal nanocrystalline composite material |
| CN101913597A (en) * | 2010-09-14 | 2010-12-15 | 武汉理工大学 | Tungsten oxide nano-wire and porous carbon nano composite structural material and preparation method thereof |
| KR20130048403A (en) * | 2011-11-02 | 2013-05-10 | 포항공과대학교 산학협력단 | Pt nanodendrites on conductive tungsten oxide nanowires and process for preparing the material |
| CN105148952A (en) * | 2015-08-27 | 2015-12-16 | 陕西科技大学 | Method for preparing spherical AgCl/W18O49 composite material |
| JP2016128803A (en) * | 2014-12-30 | 2016-07-14 | ゼネラル・エレクトリック・カンパニイ | Materials and sensors for detecting gaseous agents |
| CN106430087A (en) * | 2016-11-03 | 2017-02-22 | 中国检验检疫科学研究院 | Synthesis method of precious metal loaded tungsten oxide nanowires for gas sensor |
-
2018
- 2018-10-31 CN CN201811285394.4A patent/CN109467127A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101734614A (en) * | 2009-12-22 | 2010-06-16 | 上海大学 | Method for manufacturing metal oxide nano-wire/noble metal nanocrystalline composite material |
| CN101913597A (en) * | 2010-09-14 | 2010-12-15 | 武汉理工大学 | Tungsten oxide nano-wire and porous carbon nano composite structural material and preparation method thereof |
| KR20130048403A (en) * | 2011-11-02 | 2013-05-10 | 포항공과대학교 산학협력단 | Pt nanodendrites on conductive tungsten oxide nanowires and process for preparing the material |
| JP2016128803A (en) * | 2014-12-30 | 2016-07-14 | ゼネラル・エレクトリック・カンパニイ | Materials and sensors for detecting gaseous agents |
| CN105148952A (en) * | 2015-08-27 | 2015-12-16 | 陕西科技大学 | Method for preparing spherical AgCl/W18O49 composite material |
| CN106430087A (en) * | 2016-11-03 | 2017-02-22 | 中国检验检疫科学研究院 | Synthesis method of precious metal loaded tungsten oxide nanowires for gas sensor |
Non-Patent Citations (2)
| Title |
|---|
| LIAN FENG ZHU ET AL.: "Self-heated hydrogen gas sensors based on Pt-coatedW18O49 nanowire networks with high sensitivity, good selectivity and low power consumption", 《SENSORS AND ACTUATORS B》 * |
| YANG LIU ET AL.: "Switchable optical nonlinear properties of W18O49 nanowires by Ag nanoparticles supported", 《CHINA-PHYS. MECH. ASTRON.》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114392741A (en) * | 2021-12-28 | 2022-04-26 | 安徽大学 | Vacancy-rich silver-loaded tungsten oxide nanowire for improving visible light and near infrared light dynamic bacteriostasis and preparation and application thereof |
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