CN103588475A

CN103588475A - Preparation method of submicron beta-Li2TiO3

Info

Publication number: CN103588475A
Application number: CN201310521287.8A
Authority: CN
Inventors: 蒲永平; 胡耀; 张磊磊; 万千星; 王培奎
Original assignee: Shaanxi University of Science and Technology
Current assignee: Shaanxi University of Science and Technology
Priority date: 2013-10-28
Filing date: 2013-10-28
Publication date: 2014-02-19

Abstract

The invention discloses a preparation method of submicron beta-Li2TiO3 and belongs to the technical field of nano-powder preparation. The technical scheme comprises the following step: 1) taking a Li2CO3 powder and a TiO2 powder according to the stoichiometric ratio of Li2TiO3, uniformly mixing to obtain a mixed powder, adding NaCl which weighs 0.5-1.5 times the mass of the mixed powder, and fully and uniformly mixing to obtain a mixed material; and 2) calcining the mixed material at 850-1100 DEG C in the air atmosphere, and washing and drying the calcined powder so as to obtain the submicron beta-Li2TiO3. By the method, the problem that beta-Li2TiO3 particle morphology is irregular can be solved. The beta-Li2TiO3 powdery submicron crystal whisker prepared by the method has advantages of narrow distribution range, high purity and good degree of crystallization. The preparation method has advantages of easily-obtained raw material, simple operation and low cost, is environmentally friendly, and is suitable for large-scale industrial production.

Description

A kind of submicron order β-Li 2tiO 3preparation method

Technical field

The invention belongs to nano-powder preparing technical field, be specifically related to a kind of submicron order β-Li ₂tiO ₃preparation method.

Background technology

Be rich in Li ²⁺lithium-based ceramic Li ₂tiO ₃, have considerable lithium atom density, low reactivity, excellent chemical stability, with the good consistency of structured material and good tritium low temperature release performance, be acknowledged as one of SOLID TRITIUM MATERIALS FOR of high comprehensive performance, tool future.The shape of solid tritium multiplication agent can adopt column, ring-type or spherical etc., spherical multiplication agent has the features such as easy to loading and unloading and the easy recovery of residue lithium, and has larger specific surface area, has more passage between bead, permeability is good, is conducive to diffusion and the release of tritium.Therefore,, in fusion reactor design at present, almost all select spherical multiplication agent.Obtain as far as possible many tritiums when multiplication agent is applied on hybrid reactor, bead is contained in capsule, and the tap density of bead is a crucial influence factor.Meanwhile, its lithium content is also a very important parameter of fusion reactor, and the increase of bead lithium content can reduce in order to realize the self-holding to guarantee the enriching quantity of the Li that nuclear reaction is carried out continuously of tritium.Therefore, small size, even, the highdensity tritium multiplication agent of size distribution pelletizing are more suitable for fusion reactor.

Reported that at present solid phase method synthesizes β-Li ₂tiO ₃, as the obtained Li of Chinese patent bulletin CN201310019077.9 ₂tiO ₃often control, size-grade distribution is wide and coarse size by uneven components, stoichiometry difficulty for powder, and be subject to raw material TiO ₂the restriction of structure, its structure is difficult to regulation and control.In addition, also there is relevant chemosynthesis β-Li ₂tiO ₃report, it is advantageous that, the raw material in building-up reactions is the even mixing of atom or molecular level level, easily under cold condition, obtains pure phase β-Li ₂tiO ₃powder, and gained β-Li ₂tiO ₃powder size is evenly distributed, granularity is little, but its synthesis technique is complicated, and operation is difficult for.

Summary of the invention

The object of the present invention is to provide a kind of submicron order β-Li ₂tiO ₃preparation method, the method can solve β-Li ₂tiO ₃the irregular problem of granule-morphology, the β-Li making through the method ₂tiO ₃powder sub-micro whisker cun narrow distribution range, phase purity is higher, and better crystallinity degree.

The present invention is achieved through the following technical solutions:

A kind of submicron order β-Li ₂tiO ₃preparation method, comprise the following steps:

1) press Li ₂tiO ₃stoichiometric ratio, get Li ₂cO ₃powder and TiO ₂powder, mixes to obtain mixed powder, then adds the NaCl of 0.5～1.5 times of mixed powder quality, after fully mixing, obtains batch mixing;

2) by batch mixing at 850 ℃～1100 ℃, in air atmosphere, calcine, the powder after calcining, through washing, dry, obtains submicron order β-Li ₂tiO ₃.

Fully mixing described in step 1) is by mixed powder and NaCl ball milling 3～5h.

Step 2) described washing is that the powder after calcining is washed to and in the solution washing out, no longer contains chlorion; By the powder after calcining be washed to the solution that washes out no longer with AgNO ₃solution produces precipitation; Described water is distilled water.

Step 2) described calcining is batch mixing to be placed in to crucible or retort furnace is calcined.

Step 2) described calcination time is 10～12h.

Compared with prior art, the present invention has following useful technique effect:

The present invention prepares submicron order β-Li ₂tiO ₃method, with Li ₂cO ₃powder and TiO ₂powder is raw material, and raw material is easy to get, synthetic cost is low; β-Li prepared by the present invention ₂tiO ₃, the submicron particles size distribution making through the present invention is narrower, and between 0.5 μ m to 1.5 μ m, X-ray diffraction result shows, and the submicron powder phase purity of preparation is higher, and degree of crystallinity is better, can solve β-Li ₂tiO ₃the irregular problem of granule-morphology.The inventive method technique is simple, and processing ease is low for equipment requirements, and environmental friendliness is applicable to large-scale industrialization and produces.

Further, the present invention washes the powder after calcining with water to the solution washing out and no longer contains chlorion, be in final product, not contain chlorion in order effectively to guarantee, because the existence of chlorion can affect the purity of product, thereby by elutant Ag ⁺check, no longer contains Cl to determine in filtrate ^-thereby, effectively guaranteed the purity of product.

Accompanying drawing explanation

Fig. 1 is the X ray diffracting spectrum of the sample that makes of the present invention;

Fig. 2 is that the sample that the present invention makes amplifies the scanning electron microscope (SEM) photograph of 10,000 times.

Embodiment

Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.

Embodiment 1

1) press Li ₂tiO ₃stoichiometric ratio, get Li ₂cO ₃powder and TiO ₂powder, mixes to obtain mixed powder, then adds the NaCl of 0.5 times of mixed powder quality, after ball milling 3h, obtains batch mixing;

2) batch mixing is placed in to crucible, at 1100 ℃, calcines 10h in air atmosphere, the powder after calcining, through washing, dry, obtains submicron order β-Li ₂tiO ₃; Wherein, described washing is that the powder after calcining is washed to and in the solution washing out, no longer contains chlorion, be about to powder after calcining be washed to the solution that washes out no longer with AgNO ₃solution produces precipitation.

Embodiment 2

1) press Li ₂tiO ₃stoichiometric ratio, get Li ₂cO ₃powder and TiO ₂powder, mixes to obtain mixed powder, then adds the NaCl of 1 times of mixed powder quality, after ball milling 4h, obtains batch mixing;

2) batch mixing is placed in to retort furnace, at 950 ℃, calcines 11h in air atmosphere, the powder after calcining, through washing, dry, obtains submicron order β-Li ₂tiO ₃; Wherein, described washing is that the powder after calcining is washed to distilled water and in the solution washing out, no longer contains chlorion, be about to powder after calcining be washed to the solution that washes out no longer with AgNO ₃solution produces precipitation.

Embodiment 3

1) press Li ₂tiO ₃stoichiometric ratio, get Li ₂cO ₃powder and TiO ₂powder, mixes to obtain mixed powder, then adds the NaCl of 1.5 times of mixed powder quality, after ball milling 5h, obtains batch mixing;

2) batch mixing is placed in to crucible, at 800 ℃, calcines 12h in air atmosphere, the powder after calcining, through distilled water washing, dry, obtains submicron order β-Li ₂tiO ₃; Wherein, described washing is that the powder after calcining is washed to and in the solution washing out, no longer contains chlorion, be about to powder after calcining be washed to the solution that washes out no longer with AgNO ₃solution produces precipitation.

Claims

1. a submicron order β-Li ₂tiO ₃preparation method, it is characterized in that, comprise the following steps:

2. a kind of submicron order β-Li according to claim 1 ₂tiO ₃preparation method, it is characterized in that, fully mixing described in step 1) is by mixed powder and NaCl ball milling 3～5h.

3. a kind of submicron order β-Li according to claim 1 ₂tiO ₃preparation method, it is characterized in that step 2) described washing is that the powder after calcining is washed to and in the solution washing out, no longer contains chlorion.

4. a kind of submicron order β-Li according to claim 3 ₂tiO ₃preparation method, it is characterized in that, by the powder after calcining be washed to the solution that washes out no longer with AgNO ₃solution produces precipitation.

5. according to a kind of submicron order β-Li described in claim 3 or 4 ₂tiO ₃preparation method, it is characterized in that, described water is distilled water.

6. a kind of submicron order β-Li according to claim 1 ₂tiO ₃preparation method, it is characterized in that step 2) described calcining is batch mixing to be placed in to crucible or retort furnace is calcined.

7. a kind of submicron order β-Li according to claim 1 ₂tiO ₃preparation method, it is characterized in that step 2) described calcination time is 10～12h.