CN103601235B - A kind of mechanochemical reaction synthesis of nano SrTiO 3powder method - Google Patents

Abstract

The present invention relates to a kind of mechanochemical reaction synthesis of nano SrTiO ₃powder method, at least comprises the steps: 1) get appropriate strontium oxide, titanium dioxide raw material pours beaker into, puts into baking oven, dries 12h; 2) after drying, by two kinds of powders with mol ratio 1:1 Homogeneous phase mixing; 3) cumulative volume of mixed powder+carbonization crow bead is no more than 2/3 of jar cumulative volume; The mass ratio of mixed powder and wolfram varbide bead is 20:1; 4) turn on the power switch, open high energy ball mill lid; 5) according to the flow operations of high-energy ball milling experiment; 6) parameters: rotating speed is 200rpm; A loop cycle is 30 minutes, 7) click beginning button, and machine is started working; 8), after 24 hours, open high energy ball mill lid and the sampling of ball grinder lid, after completing, use alcohol washes ball grinder, for subsequent use after drying; 9) powered-down switch.The present invention has that energy consumption is low, purity is high, particle diameter is little, level of automation is high, the consistence of quality and repeating, the features such as dye thing quantity discharged is few.

Description

A kind of mechanochemical reaction synthesis of nano SrTiO 3powder method

Technical field

The present invention relates to a kind of synthesis of nano SrTiO ₃powder technology, particularly a kind of mechanochemical reaction synthesis of nano SrTiO ₃powder method.

Background technology

SrTiO ₃material is the ternary compound with perovskite structure, and perovskite structure makes it have good chemical stability and thermostability, and ternary compound makes it have good modification and doping space.SrTiO ₃it is little that material has dielectric loss, Heat stability is good, is a kind of excellent electron ceramic material, is widely used in the fields such as high voltage capacitor, grain-boundary layer capacitor, voltage dependent resistor, thermistor, have the advantages such as microminiaturization, high-performance, high reliability.

Traditional SrTiO ₃powder synthesis technique mainly high temperature solid phase synthesis, has energy consumption high (more than 1000 degree), and the shortcoming such as purity is low, particle diameter is large, the fine materials of nanometer scale can not be obtained.The SrTiO that traditional sol-gel method obtains ₃powder body material, the batch of technique is little, and level of automation is low, the consistence of quality and repeat low, and the shortcomings such as organic pollutant discharge.Current domestic production Sr titanate powder, mainly based on traditional high temperature solid-state method, cannot obtain fine powder.

Summary of the invention

The object of this invention is to provide one and have that energy consumption is low, purity is high, particle diameter is little, level of automation is high, the consistence of quality and repeating, a kind of mechanochemical reaction synthesis of nano SrTiO that dye thing quantity discharged is few ₃powder method.

The object of the present invention is achieved like this, a kind of mechanochemical reaction synthesis of nano SrTiO ₃powder method, is characterized in that: at least comprise the steps:

1) get appropriate strontium oxide, titanium dioxide raw material pours beaker into, puts into baking oven, dries 12h;

2) after drying, by two kinds of powders with mol ratio 1:1 Homogeneous phase mixing;

3) cumulative volume of mixed powder+carbonization crow bead is no more than 2/3 of jar cumulative volume; The mass ratio of mixed powder and wolfram varbide bead is 20:1; Wolfram varbide bead forming respectively by diameter Ф 20mm and Ф 10mm, between them, number is than being Ф 20mm/ Ф 10mm=1:2; After discharging material and ball, jar adds sealing-ring, cover lid;

4) turn on the power switch, open high energy ball mill lid;

5) according to the flow operations of high-energy ball milling experiment, fix ball grinder and ball milling lid, finally build enclosing cover lid;

6) parameters: rotating speed is 200rpm; A loop cycle is 30 minutes, wherein, and ball milling 25 minutes/time-out 5 minutes; 24 hours altogether, wherein clean Ball-milling Time 20 hours;

7) click beginning button, machine is started working;

8), after 24 hours, open high energy ball mill lid and the sampling of ball grinder lid, after completing, use alcohol washes ball grinder, for subsequent use after drying;

9) powered-down switch.

Described high energy ball mill adopts German FRITSCH planetary high-energy ball mill.

Described ball grinder is single tank or two tank or four tanks, supporting with ball mill.

Advantage of the present invention is: owing to adopting high-energy ball-milling process synthesis of nano SrTiO ₃powder body material, utilizes mechanical energy strong in high-energy ball-milling process, at ambient temperature Mechano-chemical Synthesizing nanometer SrTiO ₃powder body material, the SrTiO obtained ₃powder body material has that good perovskite structure, homogeneity and consistence are good, powder median size 30 ran.The SrTiO of the nanometer scale that availability is outstanding ₃powder body material, and this kind of technology energy consumption is low, environmental protection (outwards not discharging organic pollutant), mechanization degree is high, is applicable to batch production.

Accompanying drawing explanation

Below in conjunction with embodiment accompanying drawing, the invention will be further described:

Fig. 1 is high-energy ball milling method synthesis of nano SrTiO ₃the schema of powder body material;

The non-ball milling of Fig. 2 (0h(hour)) and clean ball milling 20h(hour) material XRD diffractogram (X-rayDiffractionX ray diffraction) schematic diagram;

Fig. 3 is clean ball milling 20h(hour) material TEM schemes.

Embodiment

As shown in Figure 1, a kind of mechanochemical reaction synthesis of nano SrTiO ₃powder method, at least comprises the steps:

1) get appropriate strontium oxide, titanium dioxide raw material pours beaker into, puts into baking oven, dries 12h;

2) after drying, by strontium oxide and titanium dioxide two kinds of powders with mol ratio 1:1 Homogeneous phase mixing;

3) adding tungsten-carbide ball number in tungsten-carbide ball grinding jar with Ф 20mm/ Ф 10mm=1:2, is that 20:1 adds as in tank by mixed powder by the mass ratio of ball and powder; The cumulative volume of powder and ball is no more than 2/3 of jar cumulative volume; After discharging material and ball, jar adds sealing-ring, cover lid;

4) turn on the power switch, open high energy ball mill lid;

5) according to the flow operations of high-energy ball milling experiment, fix tungsten-carbide ball grinding jar and ball milling lid, finally build enclosing cover lid;

6) parameters: rotating speed is 200rpm; A loop cycle is 30 minutes, wherein, and ball milling 25 minutes/time-out 5 minutes; 24 hours altogether, wherein clean Ball-milling Time 20 hours;

7) click beginning button, machine is started working;

8), after 24 hours, open high energy ball mill lid and the sampling of ball grinder lid, after completing, use alcohol washes ball grinder, for subsequent use after drying;

9) powered-down switch.

Fig. 2 is non-ball milling 0h(hour) and clean ball milling 20h(hour) material XRD crystalline phase figure, show the clean high-energy ball milling through 20 hours through XRD figure spectrum analysis, material is by SrO and TiO ₂the powder machinery chemosynthesis SrTiO of perovskite structure ₃powder body material, through about the mean sizes 30nm of Scherrer formulae discovery crystal grain.

Fig. 3 is that clean ball milling 20h material TEM schemes (transmission electron microscope), is shown: about 30 ran of synthesized material by figure, and the homogeneity of material dispersion sexual valence is good.

Described high energy ball mill adopts German FRITSCH planetary high-energy ball mill.

Ball grinder is single tank or two tank or four tanks, supporting with ball mill.

The ball of tungsten-carbide ball Ф 20mm and Ф 10mm.Wolfram varbide (containing wolfram varbide massfraction 93%, cobalt 6%) material, its relative density is 14.75g/cm ³.

The block construction that the present embodiment does not describe in detail and technique belong to the well-known components of the industry and common structure or conventional means, do not describe one by one here.

Claims (1)

1. a mechanochemical reaction synthesis of nano SrTiO ₃powder method, is characterized in that: at least comprise the steps:

1) get appropriate strontium oxide, titanium dioxide raw material pours beaker into, puts into baking oven, dries 12h;

2) after drying, by two kinds of powders with mol ratio 1:1 Homogeneous phase mixing;

3) cumulative volume of mixed powder+carbonization crow bead is no more than 2/3 of jar cumulative volume; The mass ratio of mixed powder and wolfram varbide bead is 20:1; Wolfram varbide bead forming respectively by diameter Ф 20mm and Ф 10mm, between them, number is than being Ф 20mm/ Ф 10mm=1:2; After discharging material and ball, jar adds sealing-ring, cover lid;

4) turn on the power switch, open high energy ball mill lid;

5) according to the flow operations of high-energy ball milling experiment, fix ball grinder and ball milling lid, finally build enclosing cover lid;

6) parameters: rotating speed is 200rpm; A loop cycle is 30 minutes, wherein, and ball milling 25 minutes/time-out 5 minutes; 24 hours altogether, wherein clean Ball-milling Time 20 hours;

7) click beginning button, machine is started working;

8), after 24 hours, open high energy ball mill lid and the sampling of ball grinder lid, after completing, use alcohol washes ball grinder, for subsequent use after drying;

9) powered-down switch;

Described high energy ball mill adopts German FRITSCH planetary high-energy ball mill;

Described ball grinder is single tank or two tank or four tanks, supporting with ball mill;

Synthesized material particle size is in 30 nanometers, and the homogeneity good dispersity of material.