CN104478410A - Preparation method of nano H-In2O3 ceramic - Google Patents

Preparation method of nano H-In2O3 ceramic Download PDF

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CN104478410A
CN104478410A CN201410757595.5A CN201410757595A CN104478410A CN 104478410 A CN104478410 A CN 104478410A CN 201410757595 A CN201410757595 A CN 201410757595A CN 104478410 A CN104478410 A CN 104478410A
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reaktionsofen
precursor
temperature
pottery
nanometer
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CN104478410B (en
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张金花
余大斌
王燕
王峰
冯玥玥
王自荣
袁忠才
赵大鹏
甘桂华
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ELECTRONIC ENGINEERING COLLEGE PLA
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Abstract

The invention discloses a preparation method of nano H-In2O3 ceramic. The preparation method comprises the following steps: mixing InC13.4H2O, deionized water and ethanediamine evenly, putting the mixture into an drying oven, preserving heat at a drying oven heat preservation temperature of 160-200 DEG C for 20-30 hours, taking out and cooling to a room temperature, washing by use of distilled water and absolute ethyl alcohol, and drying to obtain a precursor; putting the precursor into a reaction container, putting the reaction container with the precursor into a reaction furnace, and preserving heat for 0.8-1.2 hours to obtain H-In2O3 nano crystals, wherein the temperature of the reaction furnace ranges from 300 to 500 DEG C; and putting the H-In2O3 nano crystals into the reaction furnace and preserving heat and pressure for 1-3 hours to obtain the nano H-In2O3 ceramic, wherein the temperature of the reaction furnace ranges from 700 to 1000 DEG C, and the pressure in the reaction furnace ranges from 40 to 70MPa. The preparation method of the nano H-In2O3 ceramic is low in reaction requirements, energy-saving and environment-friendly, and further is simple, and convenient to operate.

Description

A kind of nanometer H-In 20 3the preparation method of pottery
Technical field
The present invention relates to high pressure phase Indium sesquioxide ceramic technology field, particularly relate to a kind of nanometer H-In 2o 3the preparation method of pottery.
Background technology
Indium sesquioxide (In 2o 3) be a kind of new N-shaped transparent semiconductor functional materials, there is wider energy gap, less resistivity and higher catalytic activity, be widely applied in photoelectric field, gas sensor, catalyzer.And In 2o 3when particle size reaches Nano grade except there is above function, also possess the surface effects of nano material, quantum size effect, small-size effect and macro quanta tunnel effect etc.
In a semiconductor material, In 2o 3be have extensively studied decades as the critical function material with high conductivity and visible light transmissivity, be now widely used in various photoelectric device, as solar cell, liquid-crystal display and gas sensor etc.
In the past few decades, people develop multiple In 2o 3technology of preparing, as: sol-gel method, chemical gas phase sink collection method, direct solenoid sputtering method etc.But, the In of various preparation method's gained 2o 3product, comprising its powder body material, nano material and thin-film material is all mainly Emission in Cubic (low pressure phase), and Jie of its corundum structure surely only has little special methods to prepare mutually.Be situated between the In of steady phase corundum structure 2o 3also known as high pressure phase In 2o 3(referred to as H-In 2o 3), it is prepared by the method for phase transformation under the extreme condition of High Temperature High Pressure.Its Emission in Cubic In is under elevated pressure conditions found from Shannon et al 2o 3the H-In of corundum structure can be transformed into 2o 3after, Prewitt et al is at 65kbars and 1100 DEG C of obtained H-In 2o 3, Atou et al shocks by electricity and induces preparation H-In under 15-25GPa condition 2o 3.Except there is excellent photoelectric characteristic and except, H-In 2o 3there is higher thermostability mutually than its low pressure, show that it has potential using value in larger temperature range.
The synthesis H-In of current widespread reports 2o 3method realized by liquid-solid formation mechanism under catalyst action, but this method needs under extreme conditions (higher than 1400 DEG C) to carry out.
Summary of the invention
The technical problem that basic background technology exists, the present invention proposes a kind of nanometer H-In 2o 3the preparation method of pottery, reaction requires low, energy-conserving and environment-protective, and method is simple, easy to operate.
A kind of nanometer H-In that the present invention proposes 2o 3the preparation method of pottery, comprises the steps:
S1, by InCl 34H 2o and deionized water add in reactor, treat InCl 34H 2after O dissolves completely, add quadrol again, then stir, after described reactor sealing, be placed in baking oven and be incubated 20-30h, baking oven holding temperature is 160-200 DEG C, then described reactor is taken out and be cooled to room temperature, obtain mixture with reactor inwall described in distilled water wash, after filtering, use absolute ethanol washing filter cake, then the filtration cakes torrefaction after washing is obtained precursor;
S2, precursor obtained for S1 is placed in reaction vessel, the reaction vessel that precursor is housed is placed in Reaktionsofen and is incubated 0.8-1.2h and obtains H-In 2o 3nanocrystal, Reaktionsofen temperature is 300-500 DEG C;
S3, the H-In that S2 is obtained 2o 3nanocrystal is placed in Reaktionsofen heat-insulation pressure keeping 1-3h and obtains nanometer H-In 2o 3pottery, in Reaktionsofen, temperature is 700-1000 DEG C, and in Reaktionsofen, pressure is 40-70MPa.
Preferably, in S1, InCl 34H 2the mass volume ratio (g/ml) of O and deionized water is 1:1-4, and the volume ratio of deionized water and quadrol is 1-4:30-50.
Preferably, in S1, by volume number is by InCl 34H 2o and 2-3 part deionized water adds in reactor, treats InCl 34H 2after O dissolves completely, add 35-45 part quadrol again, then stir, after described reactor sealing, be placed in baking oven and be incubated 22-28h, baking oven holding temperature is 170-190 DEG C, then described reactor is taken out and be cooled to room temperature, obtain mixture with reactor inwall described in distilled water wash, after filtering, use absolute ethanol washing filter cake, then the filtration cakes torrefaction after washing is obtained precursor, wherein InCl 34H 2the mass volume ratio (g/ml) of O and deionized water is 1:2-3.
Preferably, in S2, precursor obtained for S1 is placed in reaction vessel, the reaction vessel that precursor is housed is placed in Reaktionsofen and is incubated 1h and obtains H-In 2o 3nanocrystal, Reaktionsofen temperature is 300-500 DEG C.
Preferably, in S2, precursor obtained for S1 is placed in reaction vessel, the reaction vessel that precursor is housed is placed in Reaktionsofen and is incubated 1h and obtains H-In 2o 3nanocrystal, Reaktionsofen temperature is 350-450 DEG C.
Preferably, in S3, the H-In obtained by S2 2o 3nanocrystal is placed in Reaktionsofen heat-insulation pressure keeping 1.5-2.5h and obtains nanometer H-In 2o 3pottery, in Reaktionsofen, temperature is 750-950 DEG C, and in Reaktionsofen, pressure is 45-65MPa.
The present invention adopts solvent-thermal method and calcines the method that combines, relative to prior art, can prepare nanometer H-In under comparatively low reaction condition 2o 3pottery.The present invention, in S1, utilizes In 3+easily there is the In (OH) that hydrolysis reaction generates less stable in the basic conditions 3, In (OH) 3precursor InOOH is generated through partial dehydration under lower than the condition of 200 DEG C; In S2, precursor InOOH under lower than the condition of 500 DEG C completely dehydration generate H-In 2o 3crystal, this H-In 2o 3crystal is powder body material, and its granularity may be controlled to nano-scale, for the further research of thermoelectric material is laid a good foundation; In S3, be 40-70MPa by control the temperature of Reaktionsofen be the pressure of 700-900 DEG C and Reaktionsofen, hot pressed sintering 1-3h, makes H-In 2o 3powder body material is easy to shaping and obtains nanometer H-In 2o 3pottery, to this nanometer H-In 2o 3pottery carries out performance test discovery, this nanometer H-In 2o 3pottery still keeps good electroconductibility, and the indium oxide nanocrystalline namely obtained, as the doping phase of thermoelectric material, still has good electroconductibility, for the modification (raising specific conductivity) of thermoelectric material provides technique direction and approach.
Accompanying drawing explanation
Fig. 1 is a kind of nanometer H-In that the present invention proposes 2o 3preparation method's schematic flow sheet of pottery.
Fig. 2 is the X-ray diffractogram of precursor InOOH.
Fig. 3 is precursor InOOH obtains intermediate under temperature is 330 DEG C of conditions X-ray diffractogram through different annealing time, (a) 0h, (b) 0.5h, (c) 1.0h, (d) 1.5h, (e) 2.0h.
Fig. 4 is that after precursor InOOH nano wire dewaters under 300-500 DEG C of normal pressure, gained is product H-In 2o 3x-ray diffractogram.
Embodiment
As shown in Figure 1, Fig. 1 is a kind of nanometer H-In that the present invention proposes 2o 3preparation method's schematic flow sheet of pottery.
With reference to Fig. 1, a kind of nanometer H-In that the present invention proposes 2o 3the preparation method of pottery, comprises the steps:
S1, by InCl 34H 2o and deionized water add in reactor, treat InCl 34H 2after O dissolves completely, add quadrol again, then stir, after described reactor sealing, be placed in baking oven and be incubated 20-30h, baking oven holding temperature is 160-200 DEG C, then described reactor is taken out and be cooled to room temperature, obtain mixture with reactor inwall described in distilled water wash, after filtering, use absolute ethanol washing filter cake, then the filtration cakes torrefaction after washing is obtained precursor;
S2, precursor obtained for S1 is placed in reaction vessel, the reaction vessel that precursor is housed is placed in Reaktionsofen and is incubated 0.8-1.2h and obtains H-In 2o 3nanocrystal, Reaktionsofen temperature is 300-500 DEG C;
S3, the H-In that S2 is obtained 2o 3nanocrystal is placed in Reaktionsofen heat-insulation pressure keeping 1-3h and obtains nanometer H-In 2o 3pottery, in Reaktionsofen, temperature is 700-1000 DEG C, and in Reaktionsofen, pressure is 40-70MPa.
Below, by specific embodiment, technical scheme of the present invention is described in detail.
Embodiment 1
A kind of nanometer H-In that the present invention proposes 2o 3the preparation method of pottery, comprises the steps:
S1, by InCl 34H 2o and deionized water add in reactor, treat InCl 34H 2after O dissolves completely, add quadrol again, then stir, after described reactor sealing, be placed in baking oven and be incubated 20h, baking oven holding temperature is 200 DEG C, then described reactor is taken out and be cooled to room temperature, obtain mixture with reactor inwall described in distilled water wash, after filtering, use absolute ethanol washing filter cake, then the filtration cakes torrefaction after washing is obtained precursor;
S2, precursor obtained for S1 is placed in reaction vessel, the reaction vessel that precursor is housed is placed in Reaktionsofen and is incubated 0.8h and obtains H-In 2o 3nanocrystal, Reaktionsofen temperature is 500 DEG C;
S3, the H-In that S2 is obtained 2o 3nanocrystal is placed in Reaktionsofen heat-insulation pressure keeping 1h and obtains nanometer H-In 2o 3pottery, in Reaktionsofen, temperature is 1000 DEG C, and in Reaktionsofen, pressure is 40MPa.
Embodiment 2
A kind of nanometer H-In that the present invention proposes 2o 3the preparation method of pottery, comprises the steps:
S1, by InCl 34H 2o and deionized water add in reactor, treat InCl 34H 2after O dissolves completely, add quadrol again, then stir, after described reactor sealing, be placed in baking oven and be incubated 30h, baking oven holding temperature is 160 DEG C, then described reactor is taken out and be cooled to room temperature, obtain mixture with reactor inwall described in distilled water wash, after filtering, use absolute ethanol washing filter cake, then the filtration cakes torrefaction after washing is obtained precursor;
S2, precursor obtained for S1 is placed in reaction vessel, the reaction vessel that precursor is housed is placed in Reaktionsofen and is incubated 1.2h and obtains H-In 2o 3nanocrystal, Reaktionsofen temperature is 300 DEG C;
S3, the H-In that S2 is obtained 2o 3nanocrystal is placed in Reaktionsofen heat-insulation pressure keeping 3h and obtains nanometer H-In 2o 3pottery, in Reaktionsofen, temperature is 700 DEG C, and in Reaktionsofen, pressure is 70MPa.
Embodiment 3
A kind of nanometer H-In that the present invention proposes 2o 3the preparation method of pottery, comprises the steps:
S1, by volume number are by InCl 34H 2an O and 2 part deionized water adds in reactor, treats InCl 34H 2after O dissolves completely, add 45 parts of quadrols again, then stir, after described reactor sealing, be placed in baking oven and be incubated 24h, baking oven holding temperature is 185 DEG C, then described reactor is taken out and be cooled to room temperature, obtain mixture with reactor inwall described in distilled water wash, after filtering, use absolute ethanol washing filter cake, then the filtration cakes torrefaction after washing is obtained precursor, wherein InCl 34H 2the mass volume ratio (g/ml) of O and deionized water is 1:2;
S2, precursor obtained for S1 is placed in reaction vessel, the reaction vessel that precursor is housed is placed in Reaktionsofen and is incubated 1h and obtains H-In 2o 3nanocrystal, Reaktionsofen temperature is 450 DEG C;
S3, the H-In that S2 is obtained 2o 3nanocrystal is placed in Reaktionsofen heat-insulation pressure keeping 1.5h and obtains nanometer H-In 2o 3pottery, in Reaktionsofen, temperature is 900 DEG C, and in Reaktionsofen, pressure is 50MPa.
Embodiment 4
A kind of nanometer H-In that the present invention proposes 2o 3the preparation method of pottery, comprises the steps:
S1, by volume number are by InCl 34H 2an O and 3 part deionized water adds in reactor, treats InCl 34H 2after O dissolves completely, add 35 parts of quadrols again, then stir, after described reactor sealing, be placed in baking oven and be incubated 26h, baking oven holding temperature is 175 DEG C, then described reactor is taken out and be cooled to room temperature, obtain mixture with reactor inwall described in distilled water wash, after filtering, use absolute ethanol washing filter cake, then the filtration cakes torrefaction after washing is obtained precursor, wherein InCl 34H 2the mass volume ratio (g/ml) of O and deionized water is 1:3;
S2, precursor obtained for S1 is placed in reaction vessel, the reaction vessel that precursor is housed is placed in Reaktionsofen and is incubated 1h and obtains H-In 2o 3nanocrystal, Reaktionsofen temperature is 350 DEG C;
S3, the H-In that S2 is obtained 2o 3nanocrystal is placed in Reaktionsofen heat-insulation pressure keeping 2.5h and obtains nanometer H-In 2o 3pottery, in Reaktionsofen, temperature is 800 DEG C, and in Reaktionsofen, pressure is 60MPa.
Embodiment 5
A kind of nanometer H-In that the present invention proposes 2o 3the preparation method of pottery, comprises the steps:
S1, by volume number are by InCl 34H 2an O and 1 part deionized water adds in reactor, treats InCl 34H 2after O dissolves completely, add 50 parts of quadrols again, then stir, after described reactor sealing, be placed in baking oven and be incubated 22h, baking oven holding temperature is 190 DEG C, then described reactor is taken out and be cooled to room temperature, obtain mixture with reactor inwall described in distilled water wash, after filtering, use absolute ethanol washing filter cake, then the filtration cakes torrefaction after washing is obtained precursor, wherein InCl 34H 2the mass volume ratio (g/ml) of O and deionized water is 1:1;
S2, precursor obtained for S1 is placed in reaction vessel, the reaction vessel that precursor is housed is placed in Reaktionsofen and is incubated 1h and obtains H-In 2o 3nanocrystal, Reaktionsofen temperature is 500 DEG C;
S3, the H-In that S2 is obtained 2o 3nanocrystal is placed in Reaktionsofen heat-insulation pressure keeping 1.5h and obtains nanometer H-In 2o 3pottery, in Reaktionsofen, temperature is 950 DEG C, and in Reaktionsofen, pressure is 45MPa.
Embodiment 6
A kind of nanometer H-In that the present invention proposes 2o 3the preparation method of pottery, comprises the steps:
S1, by volume number are by InCl 34H 2an O and 4 part deionized water adds in reactor, treats InCl 34H 2after O dissolves completely, add 30 parts of quadrols again, then stir, after described reactor sealing, be placed in baking oven and be incubated 28h, baking oven holding temperature is 170 DEG C, then described reactor is taken out and be cooled to room temperature, obtain mixture with reactor inwall described in distilled water wash, after filtering, use absolute ethanol washing filter cake, then the filtration cakes torrefaction after washing is obtained precursor, wherein InCl 34H 2the mass volume ratio (g/ml) of O and deionized water is 1:4;
S2, precursor obtained for S1 is placed in reaction vessel, the reaction vessel that precursor is housed is placed in Reaktionsofen and is incubated 1h and obtains H-In 2o 3nanocrystal, Reaktionsofen temperature is 300 DEG C;
S3, the H-In that S2 is obtained 2o 3nanocrystal is placed in Reaktionsofen heat-insulation pressure keeping 1.5h and obtains nanometer H-In 2o 3pottery, in Reaktionsofen, temperature is 750 DEG C, and in Reaktionsofen, pressure is 65MPa.
For providing the ratio between reaction mass in above-described embodiment 1 and embodiment 2, be because each reaction mass can all can react by arbitrary proportion, the material unreacted that just often responds is complete, affects the ratio of input and output.
Intermediate product obtained by the present invention and end product are detected, obtain following result:
With reference to the X-ray diffractogram that Fig. 2, Fig. 2 are precursor InOOH.In figure, all diffraction peaks index can turn to the InOOH of orthorhombic phase, and do not have the diffraction peak of other thing phase in the figure, and namely this precursor is the InOOH of pure thing phase.
Reference Fig. 3, Fig. 3 are precursor InOOH obtains intermediate under temperature is 330 DEG C of conditions X-ray diffractogram through different annealing time.In figure, the change of diffraction peak illustrates H-In 2o 3thing is formed gradually along with the decomposition of precursor.Can be found out by these diffractograms, in the whole process that precursor decomposes, sample all remains crystal state, does not occur random intermediate, H-In is described 2o 3nanocrystalline is develop gradually under the crystalline structure of precursor controls.
Reference Fig. 4, Fig. 4 are that after precursor InOOH nano wire dewaters under 300-500 DEG C of normal pressure, gained is product H-In 2o 3x-ray diffractogram.In figure, all diffraction peaks all index can turn to H-In 2o 3.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.

Claims (6)

1. a nanometer H-In 2o 3the preparation method of pottery, is characterized in that, comprise the steps:
S1, by InCl 34H 2o and deionized water add in reactor, treat InCl 34H 2after O dissolves completely, add quadrol again, then stir, after described reactor sealing, be placed in baking oven and be incubated 20-30h, baking oven holding temperature is 160-200 DEG C, then described reactor is taken out and be cooled to room temperature, obtain mixture with reactor inwall described in distilled water wash, after filtering, use absolute ethanol washing filter cake, then the filtration cakes torrefaction after washing is obtained precursor;
S2, precursor obtained for S1 is placed in reaction vessel, the reaction vessel that precursor is housed is placed in Reaktionsofen and is incubated 0.8-1.2h and obtains H-In 2o 3nanocrystal, Reaktionsofen temperature is 300-500 DEG C;
S3, the H-In that S2 is obtained 2o 3nanocrystal is placed in Reaktionsofen heat-insulation pressure keeping 1-3h and obtains nanometer H-In 2o 3pottery, in Reaktionsofen, temperature is 700-1000 DEG C, and in Reaktionsofen, pressure is 40-70MPa.
2. nanometer H-according to claim 1 2o 3the preparation method of pottery, is characterized in that, in S1, and InCl 34H 2the mass volume ratio (g/ml) of O and deionized water is 1:1-4, and the volume ratio of deionized water and quadrol is 1-4:30-50.
3. nanometer H-according to claim 1 or 2 2o 3the preparation method of pottery, it is characterized in that, in S1, by volume number is by InCl 34H 2o and 2-3 part deionized water adds in reactor, treats InCl 34H 2after O dissolves completely, add 35-45 part quadrol again, then stir, after described reactor sealing, be placed in baking oven and be incubated 24-26h, baking oven holding temperature is 175-185 DEG C, then described reactor is taken out and be cooled to room temperature, obtain mixture with reactor inwall described in distilled water wash, after filtering, use absolute ethanol washing filter cake, then the filtration cakes torrefaction after washing is obtained precursor, wherein InCl 34H 2the mass volume ratio (g/ml) of O and deionized water is 1:2-3.
4. nanometer H-according to any one of claim 1-3 2o 3the preparation method of pottery, is characterized in that, in S2, precursor obtained for S1 is placed in reaction vessel, the reaction vessel that precursor is housed is placed in Reaktionsofen and is incubated 1h and obtains H-In 2o 3nanocrystal, Reaktionsofen temperature is 300-500 DEG C.
5. nanometer H-according to any one of claim 1-4 2o 3the preparation method of pottery, is characterized in that, in S2, precursor obtained for S1 is placed in reaction vessel, the reaction vessel that precursor is housed is placed in Reaktionsofen and is incubated 1h and obtains H-In 2o 3nanocrystal, Reaktionsofen temperature is 350-450 DEG C.
6. nanometer H-according to any one of claim 1-5 2o 3the preparation method of pottery, is characterized in that, in S3, and the H-In obtained by S2 2o 3nanocrystal is placed in Reaktionsofen heat-insulation pressure keeping 1.5-2.5h and obtains nanometer H-In 2o 3pottery, in Reaktionsofen, temperature is 750-950 DEG C, and in Reaktionsofen, pressure is 45-65MPa.
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CN102826593A (en) * 2012-09-11 2012-12-19 电子科技大学 Preparation method for indium oxide nanometer material
CN102863014A (en) * 2012-10-18 2013-01-09 荣成百合生物技术有限公司 Preparation method of shape-controllable nano indium oxides

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