CN103466701B - A kind of method that solid state reaction prepares bismuth oxide nano wire - Google Patents

A kind of method that solid state reaction prepares bismuth oxide nano wire Download PDF

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Publication number
CN103466701B
CN103466701B CN201310444056.1A CN201310444056A CN103466701B CN 103466701 B CN103466701 B CN 103466701B CN 201310444056 A CN201310444056 A CN 201310444056A CN 103466701 B CN103466701 B CN 103466701B
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bismuth oxide
oxide nano
nano wire
solid state
state reaction
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CN103466701A (en
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曹亚丽
汪洋
贾殿赠
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Xinjiang University
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Xinjiang University
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Abstract

It is an object of the invention to provide a kind of preparation method of bismuth oxide nano wire, the method, using shirtsleeve operation method, bismuth oxide nano wire can be synthesized through solid state reaction by using cheap raw material.Present invention bismuth nitrate and oxalic acid or oxalates at room temperature by grinding synthesis presoma, and then thermally decompose prepared bismuth oxide nano wire as reactant.The present invention, using raw material cheap and easy to get, by simple grinding, then by appropriate heat treatment, can be obtained bismuth oxide nano material based on solid state reaction.Preparation method is simple, and product yield is high, environment-friendly, it is easy to accomplish the present invention is had extremely wide application prospect.

Description

A kind of method that solid state reaction prepares bismuth oxide nano wire
Technical field
The present invention relates to a kind of method that bismuth oxide nano wire is prepared by solid state reaction.
Background technology
Bismuth oxide is yellow solid.It is a kind of important functional material, is mainly deposited with tetra- kinds of crystal formations of α, β, γ and δ .They have different crystal structures, when temperature is less than 710 DEG C, the α-Bi of monocline2O3Crystal is more stable, and is higher than this temperature δ-the Bi of cubic structure when spending2O3Stabilization, and it is always maintained at 824 DEG C of fusing point.Both phases are the stable forms of bismuth oxide. δ-Bi2O3Structure is similar with fluorite, and oxygen vacancy therein is in be randomly distributed.Because oxonium ion therein has mobility very high, This phase shows ionic conductivity very high.There is the β-Bi of Tetragonal at 650 DEG C2O3.It is believed that it has With δ-Bi2O3Identical oxygen vacancies align.At 639 DEG C, the γ-Bi with body-centered cubic symmetrical structure can be obtained2O3
Bismuth oxide has refractive index and dielectric constant higher, there is significant spy in terms of optical conductor and luminescence generated by light Property.Crystal formation is different, using difference.The application of bismuth oxide widely, it be not only good organic catalyst compound, ceramics Toner, fire-retardant for plastic, drug astringents, glass additive, dioptric glass high and nuclear engineering glass manufacture and nuclear reactor Fuel, and be that a kind of important adulterated powder material can be with significant improvement material property in electron trade.Can be additionally used in system Bismuth compound.Nano bismuth oxide in addition to the property and purposes of the bismuth oxide powder with general granularity, because granularity is thinner, can For the occasion for having particular/special requirement to granularity, such as inorganic pigment, optical material, electronic material, superconductor, specific function ceramics Material, cathode-ray tube inner-wall paint etc..
At present, the synthetic method of industrial bismuth oxide mainly has thermal decomposition method, and neutralization precipitation method successfully synthesizes at present The method of nanoscale bismuth oxide mainly has micro emulsion method, hydrothermal synthesis method, sol-gel process, electrochemical oxidation process etc., these Method building-up process is complicated, and high cost, material heat endurance is poor.Therefore, a kind of preparation method simple and easy to apply is selected, three are prepared Two bismuth nano materials tool is aoxidized to be of great significance.Solid-state chemical reaction method method does not use solvent, with high selectivity, high yield Rate, simple technological process and other advantages, have become a kind of important method of nano materials.
The content of the invention
It is an object of the invention to provide a kind of preparation method of bismuth oxide nano wire, the method is by using cheap Raw material, using shirtsleeve operation method, bismuth oxide nano wire can be synthesized through solid state reaction.
Present invention bismuth nitrate and oxalic acid or oxalates, at room temperature by grinding synthesis presoma, enter as reactant And thermally decompose and bismuth oxide nano wire is obtained.
Ammonium salt of the present invention is ammonium oxalate, one or more of sodium oxalate.
Compared with prior art, the present invention has advantages below:Based on solid state reaction, using cheap and easy to get Raw material, by simple grinding, then by appropriate heat treatment, can be obtained bismuth oxide nano wire.Preparation method is simple, produces Product yield is high, environment-friendly, it is easy to accomplish the present invention is had extremely wide application prospect.
Brief description of the drawings
Fig. 1 is the powder diagram of prepared sample.
Fig. 2 is the projection electron microscope of prepared bismuth oxide.
Specific embodiment
With reference to specific embodiment, the present invention is further elaborated.These embodiments are interpreted as being merely to illustrate The present invention rather than limit the scope of the invention.After the content for having read record of the present invention, based on of the invention The various changes or modification that principle is made to the present invention equally fall into claims of the present invention limited range.
Embodiment one:
In different mortars, finely ground respectively and mixing is for the mol bismuth nitrates of precise 0.01 and 0.02 mol oxalic acid It is even, quickly ground after mixing, with the carrying out of grinding, mixture is changed into white paste, and continuing 30 min of grinding ensures reaction Fully carry out.Presoma is placed in Muffle furnace, 300 DEG C are risen to the heating rate of 10 DEG C/min, in this temperature calcination 30min, gained sample is washed through deionized water, and bismuth oxide nano wire is can obtain after drying at room temperature.
Embodiment two:
In different mortars, finely ground respectively and mixing is for the mol bismuth nitrates of precise 0.01 and 0.03 mol sodium oxalates It is even, quickly ground after mixing, with the carrying out of grinding, mixture is changed into white paste, and continuing 30 min of grinding ensures reaction Fully carry out.Presoma is placed in Muffle furnace, 300 DEG C are risen to the heating rate of 8 DEG C/min, in this temperature calcination 30min, gained sample is washed through deionized water, and bismuth oxide nano wire is can obtain after drying at room temperature.
Embodiment three:
In different mortars, finely ground respectively and mixing is for the mol bismuth nitrates of precise 0.01 and 0.02 mol ammonium oxalate It is even, quickly ground after mixing, with the carrying out of grinding, mixture is changed into white paste, and continuing 30 min of grinding ensures reaction Fully carry out.Presoma is placed in Muffle furnace, 300 DEG C are risen to the heating rate of 10 DEG C/min, in this temperature calcination 30min, gained sample is washed through deionized water, and bismuth oxide nano wire is can obtain after drying at room temperature.

Claims (2)

1. a kind of method that solid state reaction prepares bismuth oxide nano wire, it is comprised the following steps:By bismuth nitrate and grass Acid or oxalates are in molar ratio 1:2 ~ 3 are mixed, and griding reaction obtains presoma for 20 ~ 60 minutes, and presoma is in air gas With heating rate it is 5 ~ 10 DEG C of min in atmosphere-1300 DEG C are risen to, heat treatment 30 minutes is carried out, it is scrubbed dry after heat treatment To final bismuth oxide nano wire.
2. the method for preparing bismuth oxide nano wire according to a kind of solid state reaction described in claim 1, its feature It is:The oxalates is sodium oxalate, one or more of ammonium oxalate.
CN201310444056.1A 2013-09-26 2013-09-26 A kind of method that solid state reaction prepares bismuth oxide nano wire Expired - Fee Related CN103466701B (en)

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Publication number Priority date Publication date Assignee Title
CN107552038A (en) * 2017-09-05 2018-01-09 云南大学 The preparation method and purposes of a kind of nanometer of wire bismuth oxide
CN108212186B (en) * 2018-01-18 2019-08-06 蚌埠学院 A kind of room temperature solid-state reaction prepares bismuth oxide-bismuthyl carbonate nano-complex method
CN108046319B (en) * 2018-01-18 2020-02-21 蚌埠学院 Method for preparing bismuth titanate nano composite oxide through room-temperature solid-phase reaction
CN108262035B (en) * 2018-01-18 2020-05-19 蚌埠学院 Method for synthesizing bismuth trioxide-cerium dioxide nano composite by mechanical ball milling heat treatment two-step method
CN107973343B (en) * 2018-01-18 2019-08-06 蚌埠学院 A kind of method that room temperature solid-state reaction prepares nanometer bismuth oxide
CN108187684B (en) * 2018-01-18 2020-02-21 蚌埠学院 Method for synthesizing bismuth trioxide-cuprous oxide nano compound by mechanical ball milling heat treatment two-step method
CN108383159B (en) * 2018-04-11 2020-04-07 湘潭大学 Bi2O3Preparation method and application of nanosheet material
CN111634944A (en) * 2020-05-08 2020-09-08 深圳氢时代新能源科技有限公司 Preparation method of doped bismuth oxide particles, doped bismuth oxide composite material and preparation method thereof
CN112144028B (en) * 2020-08-17 2021-07-06 广东省测试分析研究所(中国广州分析测试中心) Method for preparing bismuth oxide nanowire film by inverted heating

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CN1073535C (en) * 1998-04-08 2001-10-24 新疆大学 Method for preparing nanometre material by solid phase chemical reaction

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