CN101767819B - Preparation method of BaTi2O5 nano wire - Google Patents

Preparation method of BaTi2O5 nano wire Download PDF

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Publication number
CN101767819B
CN101767819B CN2010100289070A CN201010028907A CN101767819B CN 101767819 B CN101767819 B CN 101767819B CN 2010100289070 A CN2010100289070 A CN 2010100289070A CN 201010028907 A CN201010028907 A CN 201010028907A CN 101767819 B CN101767819 B CN 101767819B
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bati
nano wire
raw material
product
obtains
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CN101767819A (en
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戴英
邓兆
陈文�
裴新美
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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Abstract

The invention relates to a method for preparing a BaTi2O5 nano wire. In the method, the nano wire is prepared through molten salt, the selection of a precursor and the control of a technological condition. The method comprises the following steps of: (1) mixing a barium source raw material, a titanium source raw material and a molten salt raw material according to a molar ratio of 1:2:20:20 of BaC2O4.0.5H2O to TiO2 to NaCl to KCl to obtain a mixture; (2) ball milling the obtained mixture in an alcohol or water medium to obtain powder; (3) drying the obtained powder in an oven and then placing the dried powder in a muffle furnace for sintering at high temperature to obtain a product after sintering; and (4) furnace cooling the product after sintering, then washing and drying. The invention has simple process and good repeatability, and the used raw materials are industrial raw materials which have low price and are easy to obtain; during preparing, poisonous metal organic compounds are not used, thus the method meets the requirement on environment; the nano wire can be prepared in a large scale and is suitable for industrial production; and the application range is wide.

Description

BaTi＜sub〉2＜/sub〉O＜sub〉5＜/sub〉preparation method of nano wire
Technical field
The invention belongs to nano material and field of nanometer technology, be specifically related to a kind of BaTi 2O 5The preparation method of nano wire.
Background technology
BaTi 2O 5BaO-TiO 2High temperature in the binary system steady phase that is situated between, in recent years, Japanese scholars has been found the ferroelectric properties that it is new, arouses great concern BaTi 2O 5Become a kind of novel lead-free ferroelectric material.
At present about BaTi 2O 5Report also few, in the existing report, the person that has the foreign study is melted (floating zone) method and has been prepared monocrystalline BaT with floating 2O 5Block materials, b direction of principal axis dielectric constant reaches 20500 during 748K.The person has prepared needle-like BaT with method for quick cooling also to have the foreign study 2O 5Monocrystalline is also studied its ferroelectric and dielectric properties, finds that Curie temperature is 430 ℃, and the dielectric constant on the b direction of principal axis is up to 30000, and spontaneous polarization strength is up to 7 μ c/cm under the room temperature 2, show good ferroelectric and dielectric properties.Also has the foreign study person to adopt the SPS method to prepare to mix the fine and close BaTi of KF 2O 5Pottery.People calculate by First Principle at present, have explained BaTi 2O 5Has ferroelectric reason.This shows BaTi 2O 5As a kind of novel lead-free ferroelectric material, its unique performance makes it have the potentiality of extensive use.But the BaTiO with respect to perovskite structure 3, the ferroelectric materials such as PZT are to BaTi 2O 5Research just at the early-stage.The at present domestic preparation BaTi that there is not yet 2O 5The report of nano wire, existing preparation method is based on Liquid preparation methods in the world, has compared obviously different from the present invention.So searching technology is simple, with low cost, the BaTi of high yield 2O 5The preparation method of monodimension nanometer material is necessary.
Summary of the invention
Technical problem to be solved by this invention is: in order to solve problems of the prior art, provide a kind of technology simple, low-cost, can mass-produced BaTi 2O 5The preparation method of nano wire.
The present invention solves its technical problem and adopts following technical scheme:
Preparation BaTi provided by the invention 2O 5The method of nano wire, specifically: by the selection of fused salt, precursor and the control of process conditions, adopt suitability for industrialized production to prepare BaTi 2O 5Nano wire.This method specifically is to adopt the method that may further comprise the steps:
(1) will mix with the fused salt raw material through stoichiometric barium source raw material, titanium source raw material, obtain mixture.
Described barium source raw material, titanium source raw material and fused salt raw material are pressed BaC 2O 40.5H 2O: TiO 2: the mol ratio of NaCl: KCl is 1: 2: 20: 20 ratio is mixed.
Used barium source raw material is a barium oxalate.Used titanium source raw material is a titanium dioxide, and titanium dioxide is the anatase octahedrite phase.Used fused salt raw material is sodium-chlor and Repone K mixing salt, and its mole proportioning is 1: 1.
(2) mixture that obtains is carried out ball milling in ethanol or water medium, obtain powder.
(3) powder that obtains is dried in baking oven after, place the retort furnace high-temperature calcination, Heating temperature be higher than sodium-chlor and Repone K mixing salt melt temperature, the product after obtaining calcining.
(4) product after will calcining with the stove cooling after, washing is dry.
With hot wash repeatedly, and use AgNO 3Solution detects to not finding Cl -Till the ion.Adopt oven drying, be 6～12 hours time of drying,
Through above-mentioned steps, obtain described BaTi 2O 5Nano wire.Resulting BaTi 2O 5Nanowire product is white, and its length is 15 microns～50 microns, and its cross sectional shape is square.
The present invention compared with prior art has following main advantage:
One. technology is simple, favorable reproducibility, and raw materials used for the general industry raw material, cheap and easy to get, low cost.
They are two years old. and do not use deleterious organometallic compound in the preparation, meet environmental requirement.
They are three years old. can prepare in a large number.
They are four years old. applied range.As a kind of novel lead-free short of electricity material, BaTi 2O 5Nano wire can be widely used in the applications such as nano-device, film, pottery, composite.
Description of drawings
Fig. 1 is BaTi 2O 5The XRD figure of nano wire.
Fig. 2 is BaTi 2O 5The low power SEM figure of nano wire.
Fig. 3 is BaTi 2O 5The high power SEM figure of nano wire.
Fig. 4 is BaTi 2O 5The nano wire end view drawing of nano wire.
Fig. 5 is BaTi 2O 5The TEM figure of nano wire.
Fig. 6 is BaTi 2O 5The high-resolution TEM figure of nano wire.
Fig. 7 is BaTi 2O 5The SEAD figure of nano wire.
Fig. 8 is BaTi 2O 5The power spectrum of nano wire.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1:
1. raw material: technical pure barium oxalate, anatase phase titanium dioxide, NaCl, KCl.
2. prepare in accordance with the following steps BaTi 2O 5Nano wire
1). with following four kinds of raw materials: 1. barium oxalate, 2. titanium dioxide (Anatase), 3. sodium chloride, 4. potassium chloride is pressed BaC 2O 40.5H 2O: TiO 2: the mol ratio of NaCl: KCl is 1: 2: 20: 20 ratio is mixed, and be specially: barium oxalate is 1.4073g, and titanium dioxide is 0.9585g, and sodium chloride is 7.0130g, and potassium chloride is 8.9460g;
2). with mixture ball milling 30min in ethanol (or water) medium of step 1);
3). with step 2) powder that obtains dries in 60 ℃ of baking ovens;
4). the dry powder that step 3) is obtained places corundum crucible, 870 ℃ of insulation 9h in retort furnace;
5). with step 4) product is after cooling off with stove, usefulness hot water (80 ℃) washs repeatedly, and uses 0.1mol/LAgNO 3Solution detects to not finding Cl -Ion, drying is 6～12 hours in 80 ℃ of baking ovens, obtains white BaTi 2O 5Nanowire product.
BaTi 2O 5The XRD figure of nanowire product sees Fig. 1, BaTi 2O 5The SEM figure of nanowire product sees Fig. 2-4, BaTi 2O 5The TEM figure of nanowire product, electron diffraction diagram, power spectrum is seen Fig. 5-8.
The position of each diffraction maximum and relative intensity all match with JCPDS card (85-0476) among Fig. 1, show that product is monoclinic phase BaTi 2O 5, there is not other diffraction peak of mixing in the XRD collection of illustrative plates, illustrate that molten-salt growth method that the present invention proposes can prepare the BaTi of single phase 2O 5
From Fig. 2-5 as can be seen the synthetic product pattern be wire, have square cross section (length 80-200nm, wide 70-150nm), length be several microns to tens of micron.
Fig. 6-7 has further shown prepared BaTi 2O 5Nano wire is monocrystal nanowire, and crystal structure and JCPDS card (85-0476) match.
BaTi as can be seen from Figure 8 2O 5Nano wire only has Ba, Ti and three kinds of elements of O.
Analytical test shows that the product that obtains is pure phase BaTi 2O 5Nano wire, nano wire have square cross section (length 80-200nm, wide 70-150nm), and length reaches 15 microns～50 microns, the productive rate height.
Present embodiment has illustrated BaTi 2O 5The preparation method of nano wire utilizes technical scheme of the present invention can prepare in enormous quantities BaTi 2O 5Nano wire, so embodiments of the invention are not limited thereto.
Embodiment 2:
1. raw material: technical pure barium oxalate, anatase phase titanium dioxide, NaCl, KCl.
2. prepare in accordance with the following steps BaTi 2O 5Nano wire
1). with following four kinds of raw materials: 1. barium oxalate, 2. titanium dioxide (Anatase), 3. sodium chloride, 4. potassium chloride is pressed BaC 2O 40.5H 2O: TiO 2: the mol ratio of NaCl: KCl is 1: 2: 20: 20 ratio is mixed, and be specially: barium oxalate is 2.8146g, and titanium dioxide is 1.9171g, and sodium chloride is 14.0262g, and potassium chloride is 17.8922g.
2). with mixture ball milling 30min in ethanol (or water) medium of step 1);
3). with step 2) powder that obtains dries in 60 ℃ of baking ovens;
4). the dry powder that step 3) is obtained places corundum crucible, 870 ℃ of insulation 9h in retort furnace;
5). with step 4) product is after cooling off with stove, usefulness hot water (80 ℃) washs repeatedly, and uses 0.1mol/LAgNO 3Solution detects to not finding Cl -Ion, drying is 6～12 hours in 80 ℃ of baking ovens, obtains white BaTi 2O 5Nanowire product.
Acquired results is consistent with example 1.
Embodiment 3:
1. raw material: technical pure barium oxalate, anatase phase titanium dioxide, NaCl, KCl.
2. prepare in accordance with the following steps BaTi 2O 5Nano wire
1). with following four kinds of raw materials: 1. barium oxalate, 2. titanium dioxide (Anatase), 3. sodium chloride, 4. potassium chloride is pressed BaC 2O 40.5H 2O: TiO 2: the mol ratio of NaCl: KCl is 1: 2: 20: 20 ratio is mixed, and be specially: barium oxalate is 1.4073g, and titanium dioxide is 0.9585g, and sodium chloride is 7.0130g, and potassium chloride is 8.9460g.
2). with mixture ball milling 30min in ethanol (or water) medium of step 1);
3). with step 2) powder that obtains dries in 60 ℃ of baking ovens;
4). the dry powder that step 3) is obtained places corundum crucible, 890 ℃ of insulation 9h in retort furnace;
5). with step 4) product is after cooling off with stove, usefulness hot water (80 ℃) washs repeatedly, and uses 0.1mol/LAgNO 3Solution detects to not finding Cl -Ion, drying is 6～12 hours in 80 ℃ of baking ovens, obtains white BaTi 2O 5Nanowire product.
Acquired results is consistent with example 1.

Claims (5)

1. one kind prepares BaTi 2O 5The method of nano wire is characterized in that preparing BaTi by the selection of fused salt, precursor and the control of process conditions 2O 5Nano wire specifically is to adopt the method that may further comprise the steps:
(1) barium source raw material, the titanium source raw material with metering mixes with the fused salt raw material, obtains mixture; Described barium source raw material, titanium source raw material and fused salt raw material are pressed BaC 2O 40.5H 2O: TiO 2: the mol ratio of NaCl: KCl is 1: 2: 20: 20 mixed;
(2) mixture that obtains is carried out ball milling in ethanol or water medium, obtain powder;
(3) powder that obtains is dried in baking oven after, place the retort furnace high-temperature calcination, calcining temperature should be higher than sodium-chlor and Repone K mixing salt melt temperature, the product after obtaining calcining;
(4) product after will calcining with the stove cooling after, washing is dry;
Through above-mentioned steps, obtain described BaTi 2O 5Nano wire.
2. BaTi according to claim 1 2O 5The preparation method of nano wire is characterized in that: used titanium source raw material is titanium dioxide, and titanium dioxide is Anatase.
3. BaTi according to claim 1 2O 5The preparation method of nano wire is characterized in that: the mixture that obtains is carried out the ball milling mixing in ethanol or aqueous medium.
4. BaTi according to claim 1 2O 5The preparation method of nano wire is characterized in that: the product after will calcining with hot wash repeatedly, and is used AgNO after cooling off with stove 3Solution detects to not finding Cl -Ion, drying is 6～12 hours in the baking oven, obtains white BaTi 2O 5Nanowire product.
5. BaTi according to claim 1 2O 5The preparation method of nano wire is characterized in that: the BaTi that obtains 2O 5Nano wire, its length are 15 microns～50 microns, and its cross sectional shape is square.
CN2010100289070A 2010-01-04 2010-01-04 Preparation method of BaTi2O5 nano wire Expired - Fee Related CN101767819B (en)

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CN102584335B (en) * 2012-01-13 2013-08-14 武汉理工大学 Preparation method of BaTi2O5 thin films growing in a preferred orientation
CN104925856B (en) * 2015-07-07 2016-11-02 北京工业大学 Two step molten-salt growth methods prepare BaTiO3the method of nano wire
CN108794940B (en) * 2018-06-21 2020-04-28 北京工业大学 Texture BaTi2O5Preparation method of PVDF flexible piezoelectric composite material

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