CN103498190B - The preparation method of high purity dendrite FeWO4/FeS nanometer nuclear shell nano-structure - Google Patents
The preparation method of high purity dendrite FeWO4/FeS nanometer nuclear shell nano-structure Download PDFInfo
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- CN103498190B CN103498190B CN201310422662.3A CN201310422662A CN103498190B CN 103498190 B CN103498190 B CN 103498190B CN 201310422662 A CN201310422662 A CN 201310422662A CN 103498190 B CN103498190 B CN 103498190B
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Abstract
A kind of high purity dendrite FeWO
4the preparation method of/FeS nanometer nuclear shell nano-structure, belongs to technical field of material.The present invention adopts vacuum tube furnace, with Tungsten oxide 99.999 and sulphur powder for evaporation source, by the method for thermal evaporation, under carrier gas protection; on the substrate being coated with iron film, through strictly controlling vaporization temperature, the distance between evaporation source and substrate; reaction chamber pressure, the conditions such as carrier gas stream, have synthesized dendritic FeWO
4/ FeS shell core nanostructure.Simply, processing parameter controllability is strong, with low cost for described method synthesis technique and equipment.The dendritic FeWO of gained
4kernel and the shell of/FeS shell core nanostructure are crystalline state, and branch is even with dry diameter Distribution; This dendritic shell core nanostructure is at photoconductive fiber, and sensor, the field such as semiconducter device and catalyzer has wide practical use.
Description
Technical field
The present invention relates to a kind of high purity dendrite FeWO
4the preparation method of/FeS nanometer nuclear shell nano-structure, belongs to technical field of material.
Background technology
Tungstate, due to the chemistry of its excellence and physicals, has been applied to many fields, as photoconductive fiber, humidity sensor and catalyzer etc.Wherein, iron tungstate, as a kind of p-type semiconductor, has also shown excellent magnetics and optical property.But, due to tungstate nano structure synthesis difficulty, yet there are no the report of tungstate nano structural research work.And iron sulphide synthesis is than being easier to, heating sulphur and iron just can obtain under vacuo, are generally used for oil, the industry of Sweet natural gas equal energy source as catalyzer.
Along with the development of nano material and composite science and technology, scientist finds to which results in the extensive concern of people by the excellent properties that the compound of two or more material or hydridization often can produce single composition material and do not have.Wherein, nano-heterogeneous structure is subject to people's attention due to the energy performance of strongthener or the function of expansion material.Such as, nucleocapsid structure has been widely used in the compound of the electricity of material, magnetics, optics, catalysis, mechanics and chemical property as a kind of important heterojunction structure.According to ChenGong etc., the coated iron tungstate particle of carbon prepared by thermochemical method is at 800mA
-1excellent large current discharging capability and long-term circulation ability (ChenGong has been shown under current cycle, Yu-JunBai, JunFeng, RuiTang, Yong-XinQi, NingLunandRun-HuaFan.Enhancedelectrochemicalperformanceo fFeWO
4bycoatingnitrogen-dopedcarbon.ACSappliedmaterials & interfaces, 2013,5,4209-4215), and dendritic FeWO
4/ FeS nucleocapsid structure have not been reported.Meanwhile, because the basic device forming contemporary large-scale integrated circuit generally has the electrode of more than 3 or 3, single wire nanostructure can not meet the needs of nanoelectronics to nano material and nano-device performance study.Therefore the synthesis of dendritic nano-structure is prepared in nano-device and all has great importance to practical aspect from theory.
At present, nanometer nuclear shell nano-structure generally adopts chemical method to prepare, but it is difficult to prepare branched structure.In addition, compared to the complexity of chemical reaction and restive, the physical vapor depositions such as thermal evaporation have that cost is low, preparation process simple, processing parameter controllability is strong and prepare material mostly is the features such as crystal.The present invention utilizes thermal evaporation techniques to prepare high purity dendrite FeWO first
4/ FeS nanometer nuclear shell nano-structure.Due to the constructional feature that it is dendritic, will have wide practical use in various electronic devices and components field.
Summary of the invention
The object of the invention is to propose the FeWO of a kind of high purity, dendritic, crystallization
4the preparation method of/FeS nanometer nuclear shell nano-structure, the method adopts vacuum tube furnace, with Tungsten oxide 99.999 (WO
3) and sulphur (S) as evaporation source, by the method for thermal evaporation, carrier gas protection under; on the substrate being coated with iron film, through strictly controlling vaporization temperature, the distance between evaporation source and substrate; reaction chamber pressure, the conditions such as carrier gas stream, have prepared dendritic FeWO
4/ FeS shell core nanostructure.The method have reaction conditions strictly controlled, equipment and process is simple, product yield is high, the advantage such as with low cost.Obtain dendritic FeWO
4/ FeS nanometer nuclear shell nano-structure, branch and dry equal uniform diameter, well-crystallized, their kernel is the FeWO of highly crystalline
4, shell is the FeS of highly crystalline; Kernel in nanostructure and the diameter Distribution of shell are all very even, controlled diameter.Its surface is clean, purity is high.
The dendritic FeWO that the present invention proposes
4/ FeS nanometer nuclear shell nano-structure preparation method, is characterized in that, described method synthesizes dendritic FeWO by thermal evaporation Tungsten oxide 99.999 and sulphur on the substrate being coated with iron film
4/ FeS nanometer nuclear shell nano-structure, comprises the following steps:
(1) in vacuum tube furnace, respectively WO will be housed
3the alumina ceramic crucible of powder and S powder or WO is housed
3be placed on the heating region of stove central authorities with the alumina ceramic crucible of S powder mix, in its airflow downstream distance, WO be housed
3the region placement surface that the crucible 15-25mm place temperature of powder is lower is coated with the substrate of Fe film;
(2) before heating, first whole system is vacuumized, then in system, pass into high-purity inert carrier gas, and repeatedly, with the air in removal system; Then with 10-30 DEG C/min ramp to maximum heating temperature, and be incubated a few hours; In heat-processed; carrier gas flux is kept to be that in 100-300 sccm, tube furnace, vacuum tightness is-0.01 to-0.1MPa; and whole heat-processed completes under inert carrier gas protection; last Temperature fall, to room temperature, can obtain the FeWO of high purity, dendritic, highly crystallized on substrate
4/ FeS nanometer nuclear shell nano-structure.
In above-mentioned preparation method, the evaporation source in described step (1) is commercially available analytical pure WO
3powder and sulphur powder.
In above-mentioned preparation method, in described step (1), if will WO be equipped with
3the alumina ceramic crucible of powder and S powder is placed on different heating region respectively and heats, then WO will be housed
3the alumina ceramic crucible of powder is placed on the highest heating region of the centralised temperature of stove, in its air-flow upstream or downstream distance, WO is housed
3the alumina ceramic crucible that S powder is housed is placed in the region that the crucible 5-15mm place Heating temperature of powder is lower.
In above-mentioned preparation method, in described step (1), if will WO be equipped with
3the heating region being placed on stove central authorities with the alumina ceramic crucible of S powder mix heats, then wherein WO
3the mass ratio of powder and S powder controls between 10:1 to 150:1.
In above-mentioned preparation method, on the substrate that surface is coated with Fe film in described step (1), Fe film thickness is 5-50nm.
In above-mentioned preparation method, the substrate that the middle surface of described step (1) is coated with Fe film is the one among silicon chip, gallium arsenide film, single-crystal silicon carbide sheet.
In above-mentioned preparation method, in described step (2), high-purity inert carrier gas is the one among argon gas, nitrogen.
In above-mentioned preparation method, the inert carrier gas in described step (2) is high-purity gas, and purity is at more than 99.99vol.%.
In above-mentioned preparation method, the maximum heating temperature in described step (2) is 1000-1200 DEG C.
In above-mentioned preparation method, in described step (2), under maximum heating temperature, soaking time is 1-5 hour.
This technology is adopted to prepare dendritic FeWO
4/ FeS nanometer nuclear shell nano-structure, have that equipment and process is simple, reaction conditions strictly controlled, product yield is high, the feature such as with low cost, the dendritic FeWO obtained
4/ FeS nanometer nuclear shell nano-structure branch and dry equal uniform diameter, the kernel in nucleocapsid structure and shell crystallization are all good, and along nanostructure growth orient diameter evenly, length is controlled, purity is high for kernel and shell.
Accompanying drawing explanation
Fig. 1 is the dendritic FeWO obtained by the embodiment of the present invention 1
4the stereoscan photograph of/FeS nanometer nuclear shell nano-structure
Fig. 2 is the single dendritic FeWO obtained by the embodiment of the present invention 1
4the transmission electron microscope photo of/FeS nanometer nuclear shell nano-structure
Fig. 3 is the single dendritic FeWO obtained by the embodiment of the present invention 1
4the high-resolution-ration transmission electric-lens photo of/FeS nanometer nuclear shell nano-structure
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described further.
The present invention proposes a kind of high purity dendrite FeWO
4the preparation method of/FeS nanometer nuclear shell nano-structure, is characterized in that, described method synthesizes dendritic FeWO by thermal evaporation Tungsten oxide 99.999 and sulphur on the substrate being coated with iron film
4/ FeS nanometer nuclear shell nano-structure, and comprise the steps and content:
(1) adopt evaporation source to be commercially available analytically pure WO
3powder and sulphur powder.
(2) on clean silicon chip, gallium arsenide film or single-crystal silicon carbide sheet, depositing a layer thickness by the method for magnetron sputtering coater or arc evaporation is in advance the metal Fe film that 5-50nm is thick.
(3) in vacuum tube furnace, respectively WO will be housed
3the alumina ceramic crucible of powder and S powder or WO is housed
3be placed on the heating region of stove central authorities with the alumina ceramic crucible of S powder mix, in its airflow downstream distance, WO be housed
3the region placement surface that the crucible 15-25mm place temperature of powder is lower is coated with the substrate of Fe film;
(4) in evaporation source put procedure, if will WO be equipped with
3the alumina ceramic crucible of powder and S powder is placed on different heating region respectively and heats, then WO will be housed
3the alumina ceramic crucible of powder is placed on the highest heating region of the centralised temperature of stove, in its air-flow upstream or downstream distance, WO is housed
3the alumina ceramic crucible that S powder is housed is placed in the region that the crucible 5-15mm place Heating temperature of powder is lower.
(5) in evaporation source put procedure, if will WO be equipped with
3the heating region being placed on stove central authorities with the alumina ceramic crucible of S powder mix heats, then wherein WO
3the mass ratio of powder and S powder controls between 10:1 to 150:1.
(6) before heating, first whole system is vacuumized, then in system, pass into high-purity inert carrier gas, and repeatedly, with the air in removal system; Then with 10-30 DEG C/min ramp to maximum heating temperature, and be incubated a few hours; In heat-processed; carrier gas flux is kept to be that in 100-300 sccm, tube furnace, vacuum tightness is-0.01 to-0.1MPa; and whole heat-processed completes under inert carrier gas protection; last Temperature fall, to room temperature, can obtain the FeWO of high purity, dendritic, highly crystallized on substrate
4/ FeS nanometer nuclear shell nano-structure.
(7) testing inert carrier gas used is high-purity argon gas or nitrogen, and whole experiment heat-processed completes under carrier gas protection.
(8) maximum heating temperature of testing is 1000-1200 DEG C, and soaking time is 1-5 hour.
Institute obtains dendritic FeWO
4/ FeS nanometer nuclear shell nano-structure is green film in appearance.
Under a scanning electron microscope, a large amount of dendritic nano-structure can be observed, under transmission electron microscope, then obviously can observe FeWO
4/ FeS nucleocapsid structure.High-resolution-ration transmission electric-lens analysis shows, the kernel of this nucleocapsid structure and shell well-crystallized, and kernel is monocrystalline FeWO
4, shell is monocrystalline FeS.In a word, high purity, dendritic crystallization FeWO can be obtained by this technology
4/ FeS nanometer nuclear shell nano-structure, wherein kernel is monocrystalline FeWO
4, shell is monocrystalline FeS.
Embodiment 1: 0.4g analytical pure WO will be housed
3the alumina ceramic crucible of powder is placed on the central heating zone of vacuum tube furnace, in its air-flow upstream distance, WO is housed
3the alumina ceramic crucible that 0.01g analytical pure S powder is housed is placed at the crucible 14mm place of powder, in its airflow downstream distance, WO is housed
3the crucible 14mm place placement surface of powder is coated with the silicon chip of 5nmFe film.
Before heating, first whole system is vacuumized, then in system, pass into high-purity argon gas, and repeat 2 times, with the air in removal system.Then with 15 DEG C/min ramp to 1050 DEG C, insulation 2h.In heat-processed, keep carrier gas flux to be that in 300 sccm (sccm), tube furnace, vacuum tightness is-0.04MPa, last Temperature fall, to room temperature, can obtain dendritic FeWO on substrate
4/ FeS nanometer nuclear shell nano-structure.
Synthesized nanostructure is obviously dendritic, branch and dry equal uniform diameter (see Fig. 1).Obviously can observe nucleocapsid structure under microscope, nanometer rod external diameter 120-200nm, internal diameter is 60-160nm (see Fig. 2).Kernel is the FeWO of monocrystalline
4, shell is monocrystalline FeS (see Fig. 3).
Claims (2)
1. high purity dendrite FeWO
4the preparation method of/FeS nanometer nuclear shell nano-structure, is characterized in that: described dendritic nanometer nuclear shell nano-structure kernel is monocrystalline FeWO
4, shell is monocrystalline FeS; Described method is by thermal evaporation WO
3powder and S powder synthesize dendritic FeWO on the substrate being coated with iron film
4/ FeS nanometer nuclear shell nano-structure, comprises the following steps:
(1) in vacuum tube furnace, respectively WO will be housed
3the alumina ceramic crucible of powder and S powder or WO is housed
3be placed on the heating region of stove central authorities with the alumina ceramic crucible of S powder mix, in its airflow downstream distance, WO be housed
3the region placement surface that the crucible 15-25mm place temperature of powder is lower is coated with the substrate of Fe film;
(2) before heating, first whole system is vacuumized, then in system, pass into high-purity inert carrier gas, and repeatedly, with the air in removal system; Then with 10-30 DEG C/min ramp to 1000-1200 DEG C, and be incubated 1-5 hour; In heat-processed; carrier gas flux is kept to be that in 100-300 sccm, tube furnace, vacuum tightness is-0.01 to-0.1MPa; and whole heat-processed completes under inert carrier gas protection; last Temperature fall, to room temperature, can obtain the FeWO of high purity, dendritic, highly crystallized on substrate
4/ FeS nanometer nuclear shell nano-structure.
2. according to preparation method according to claim 1, it is characterized in that: WO in described step (1)
3the heating evaporation method of powder and S powder is evaporation respectively or mixing evaporation, WO when wherein evaporating respectively
3powder is placed on Lu Zhong heat district and S powder is placed on Lu Zhong low-temperature heat district, and the two is at a distance of 5-15mm; And during mixing evaporation, then need WO
3the mass ratio of powder and S powder controls between 10: 1 to 150: 1; Substrate in described step (1) is silicon chip, gallium arsenide film, single-crystal silicon carbide sheet; The Fe film that deposition on substrate in described step (1) one deck 5-50nm is thick; In described step (2), carrier gas flux is that in 100-300 sccm, tube furnace, vacuum tightness is-0.01 to-0.1MPa.
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| CN101353816A (en) * | 2008-07-08 | 2009-01-28 | 中山大学 | Growth method of tungsten oxide pencil-shaped nanostructured array |
| CN101603200A (en) * | 2009-07-10 | 2009-12-16 | 中南大学 | The preparation method of the tungsten crystal whisker array of a kind of diameter and length controlled |
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| CN101353816A (en) * | 2008-07-08 | 2009-01-28 | 中山大学 | Growth method of tungsten oxide pencil-shaped nanostructured array |
| CN101603200A (en) * | 2009-07-10 | 2009-12-16 | 中南大学 | The preparation method of the tungsten crystal whisker array of a kind of diameter and length controlled |
Non-Patent Citations (1)
| Title |
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| Controlled Growth and Characterization of Tungsten Oxide Nanowires Using Thermal Evaporation of WO3 Powder;Yunho Baek et al;《J. Phys. Chem. C》;20070103;第111卷(第3期);1213-1218 * |
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