CN104058448B - A kind of method preparing hydroxyl oxidize indium nano wire and Indium sesquioxide nano particle - Google Patents

A kind of method preparing hydroxyl oxidize indium nano wire and Indium sesquioxide nano particle Download PDF

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CN104058448B
CN104058448B CN201410342197.7A CN201410342197A CN104058448B CN 104058448 B CN104058448 B CN 104058448B CN 201410342197 A CN201410342197 A CN 201410342197A CN 104058448 B CN104058448 B CN 104058448B
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reaction
indium
temperature
rise rate
nano
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CN104058448A (en
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张剑
汤顺熙
吴思
崔啟良
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Jilin University
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Jilin University
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Abstract

A kind of method preparing hydroxyl oxidize indium nano wire and Indium sesquioxide nano particle of the present invention, belongs to technical field prepared by nano material.Preparation is by InCl 34H 2o powder dissolution, in oleyl amine, instills dehydrated alcohol and clarifies to mixing solutions under ultrasound condition; Mixing solutions is at temperature rise rate 4 ~ 8 DEG C/min down to 120 ~ 210 DEG C of reactions 12 ~ 24 hours, and obtained hydroxyl oxidize indium nano wire is or/and Indium sesquioxide nano particle.The present invention, by changing type of heating, greatly reduces the temperature of reaction needed, shortens the reaction times under high temperature rise rate, decreases energy consumption and high temperature to the loss of equipment; By changing temperature rise rate or temperature of reaction, the control to product component, pattern can be realized; And there is comparatively safe, the advantage such as method is simple and reliable, favorable repeatability.

Description

A kind of method preparing hydroxyl oxidize indium nano wire and Indium sesquioxide nano particle
Technical field
The invention belongs to technical field prepared by nano material, particularly a kind of preparation method preparing hydroxyl oxidize indium superfine nanowire and Indium sesquioxide nano cubic block under high temperature rise rate, low temperature.
Background technology
The special effects that nano material produces due to it, as: small-size effect, quantum size effect and macro quanta tunnel effect etc., thus there is the performance not available for conventional material, make it very extensive in the potential application of all respects such as optical material, electricity material, magnetic materials, gas sensor, photochemical catalysis.In recent years, the compound of IIIA race indium, hydroxyl oxidize indium (InOOH), Indium sesquioxide (In 2o 3), indium nitride (InN) as novel semiconductor functional material, there is wider energy gap, higher catalytic activity, be widely applied in photoelectric field, gas sensor, catalyzer.As everyone knows, when the dimension of nano material is reduced to close to exciton Bohr radius time, material has very high specific surface area, and surface atom coordination is incomplete, the key state on surface and the not equal feature of electronic state and inside, the activity site on surface is caused to increase, and along with the reduction of nano material dimension, the smooth degree on surface is deteriorated, and rough atomic steps is progressively formed, greatly can increase the touch opportunity of reaction mass on its surface, the catalytic of material is improved a lot.
Because the size of material and pattern bring very large impact can to its character, therefore current a large amount of research work is all intended to synthesize and has regular morphology, monodispersity is good, size is less nano material.Meanwhile, everybody finds in the method for the nano material of numerous synthesis indium nitride and Indium sesquioxide, is mostly to heat-treat for precursor with its oxyhydroxide to obtain Indium sesquioxide and indium nitride.Current most of Hydrothermal Synthesis InOOH and calcining obtain In 2o 3the temperature of nano material is all higher, and the time is long, and power consumption is large.
The prior art the most close with the present invention is Inorganic Chemistry, Vol.48, No.8,2009,3890-3895.The minimum response temperature 180 DEG C of preparation InOOH nano wire, preparation In 2o 3the temperature of reaction of nano material wants 225 DEG C.And clearly state temperature of reaction at " less than 170 DEG C what all can not get " (see the document the 3891st page of right hurdle 28th ~ 30 row).
First passage of the present invention improves temperature rise rate, and having synthesized hydroxyl oxidize indium superfine nanowire and Indium sesquioxide nano cubic block at a lower temperature, is that no one reported before this.
Summary of the invention
The technical problem to be solved in the present invention is, overcome in the past under traditional heating mode (temperature rise rate is generally lower than 4 DEG C/min) to prepare temperature in hydroxyl oxidize indium and Indium sesquioxide process high, power consumption is large, the shortcoming large to equipment loss, open a kind of at high temperature rise rate, prepare the method for hydroxyl oxidize indium superfine nanowire and Indium sesquioxide nano particle (comprising nano cubic block) under low temperature.
Concrete technical scheme of the present invention is as follows:
Prepare a method for hydroxyl oxidize indium nano wire and Indium sesquioxide nano particle, add InCl by every milliliter of oleyl amine 34H 2the consumption that O powder is 0.015 ~ 0.025 gram is by InCl 34H 2o powder dissolution, in oleyl amine, instills dehydrated alcohol and clarifies to mixing solutions under ultrasound condition; Mixing solutions is poured into heated sealed reaction in reactor, control temperature rise rate at 4 ~ 8 DEG C/min; React 12 ~ 24 hours at temperature of reaction is 120 ~ 210 DEG C; Naturally cool to room temperature after reaction terminates, product is carried out centrifugation, with washes of absolute alcohol, the powder obtaining white after oven dry is hydroxyl oxidize indium nano wire or/and Indium sesquioxide nano particle.
Described InCl 34H 2o 3, purity is preferably 99.99%, described oleyl amine, and purity is preferably 80% ~ 90%, and described dehydrated alcohol is analytical pure.
InCl 34H 2the concentration of O powder dissolution in oleyl amine, to obtained hydroxyl oxidize indium nano wire or/and Indium sesquioxide nano particle does not have too much influence.The dripping quantity of dehydrated alcohol can be 1.5 ~ 1.8 times of oleyl amine by volume.
Temperature rise rate be 4 ~ 8 DEG C/min, temperature of reaction is within the scope of 120 ~ 210 DEG C, along with the raising of temperature rise rate, can temperature of reaction be reduced accordingly, prepare product effects substantially identical.
When controlling temperature rise rate at 8 DEG C/min, temperature of reaction is under 120 ~ 130 DEG C of conditions, insulation reaction 12 ~ 24 hours, or when controlling temperature rise rate at 4 DEG C/min, temperature of reaction is under 160 ~ 170 DEG C of conditions, insulation reaction 12 ~ 24 hours, and obtained is hydroxyl oxidize indium nano wire.
When controlling temperature rise rate at 8 DEG C/min, preferable reaction temperature is under 120 DEG C of conditions, or when controlling temperature rise rate at 4 DEG C/min, preferable reaction temperature is under 160 DEG C of conditions, and obtained is pure hydroxyl oxidize indium nano wire.
When controlling temperature rise rate at 8 DEG C/min, temperature of reaction is under 140 ~ 160 DEG C of conditions, insulation reaction 12 ~ 24 hours, or when controlling temperature rise rate at 4 DEG C/min, temperature of reaction is under 180 ~ 190 DEG C of conditions, insulation reaction 12 ~ 24 hours; The mix products of obtained is hydroxyl oxidize indium nano wire and Indium sesquioxide nano particle.
When controlling temperature rise rate at 8 DEG C/min, temperature of reaction is under 170 ~ 200 DEG C of conditions, insulation reaction 12 ~ 24 hours, or when controlling temperature rise rate at 4 DEG C/min, temperature of reaction is under 200 ~ 210 DEG C of conditions, insulation reaction 12 ~ 24 hours; Obtained is Indium sesquioxide nano cubic block.
When controlling temperature rise rate at 8 DEG C/min, preferable reaction temperature is 180 ~ 190 DEG C, or when controlling temperature rise rate at 4 DEG C/min, preferable reaction temperature is 210 DEG C, and obtained is pure zirconia indium nano cubic block.What obtain under such condition is the Indium sesquioxide nano cubic block that dimension is about 100nm, and the similar Product size prepared than traditional heating mode is little.
In experiment preparation process, with dropper by dehydrated alcohol being added dropwise to containing InCl dropwise 34H 2o 3in the oleyl amine of powder.
Beneficial effect of the present invention is, on the basis of the method for existing one-step synthesis hydroxyl oxidize indium superfine nanowire and Indium sesquioxide nano particle, change type of heating, the temperature of reaction needed is greatly reduced under high temperature rise rate, with the time shortened required for reaction, decrease energy consumption and high temperature to the loss of equipment; By changing temperature rise rate or temperature of reaction, the control to product component, pattern can be realized; And having comparatively safe, method is simple, reliably, the advantages such as favorable repeatability.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the InOOH nano wire of preparation in embodiment 1.
Fig. 2 is the In of preparation in embodiment 1 2o 3the XRD figure of nano cubic block.
Fig. 3 is the TEM picture of the InOOH nano wire of preparation in embodiment 1.
Fig. 4 is the In of preparation in embodiment 1 2o 3the SEM picture of nano cubic block.
Fig. 5 is the In of preparation in embodiment 1 2o 3the TEM picture of nano cubic block.
Fig. 6 is the EDS figure of the InOOH nano wire of preparation in embodiment 1.
Fig. 7 is the In of preparation in embodiment 1 2o 3the EDS figure of nano cubic block.
Fig. 8 is the In of preparation in embodiment 1 2o 3the selected area electron diffraction figure of nano cubic block.
Fig. 9 is the TEM picture of the product of preparation in embodiment 3.
Figure 10 is the TEM picture of the product of preparation in embodiment 4.
Figure 11 is the TEM picture of the product of preparation in embodiment 5.
Figure 12 is the TEM picture of the product of preparation in embodiment 6.
Figure 13 is the TEM picture of the product of preparation in embodiment 7.
Figure 14 is the TEM picture of the product of preparation in embodiment 8.
Figure 15 is the TEM picture of the product of preparation in embodiment 9.
Figure 16 is the TEM picture of the product of preparation in embodiment 10.
Figure 17 is the XRD figure preparing InOOH nano wire in embodiment 14.
Figure 18 is the TEM picture of the InOOH nano wire prepared in embodiment 14.
Figure 19 is the TEM picture of the product of preparation in embodiment 16.
Figure 20 is the XRD figure of the product of preparation in embodiment 17.
Figure 21 be in embodiment 18 preparation irregular In 2o 3nanometer blocks XRD figure.
Figure 22 is the irregular In prepared in embodiment 18 2o 3the TEM picture of nanometer blocks.
Figure 23 is the regular In prepared in embodiment 19 2o 3the TEM picture of nano cubic block.
Embodiment
Embodiment 1, preparation InOOH superfine nanowire and In 2o 3the whole process of nano cubic block.
By the InCl of 0.1g 34H 2o 3powder dissolution, in the oleyl amine of 5ml, instills the dehydrated alcohol of 8ml in ultrasonic process, after solution clarification, mixing solutions is poured into reacting by heating in the reactor of sealing, during heating, temperature rise rate is set as 8 DEG C/min.Temperature of reaction is 120 DEG C, and the reaction times is 12 constantly little, reactor is naturally cooled to room temperature, product is carried out centrifugation, and with washes of absolute alcohol, the powder obtaining white after oven dry is hydroxyl oxidize indium superfine nanowire.
Adopting above-mentioned similar preparation process, is 180 DEG C in temperature of reaction, and the reaction times is that the 24 little powders obtaining white are constantly Indium sesquioxide nano cubic block.
Fig. 1,2 provide respectively be in embodiment 1 preparation InOOH superfine nanowire and In 2o 3the XRD spectra of nano cubic block, proves InOOH and In that product is respectively high-purity 2o 3.
The TEM picture of the InOOH nano wire that Fig. 3 prepares under giving above-mentioned condition.
The In that Fig. 4 prepares under giving above-mentioned condition 2o 3the SEM picture of nano cubic block.
The In that Fig. 5 prepares under giving above-mentioned condition 2o 3the TEM picture of nano cubic block.
Fig. 6,7 sets forth above-mentioned condition under the InOOH nano wire prepared and In 2o 3eDS figure (wherein C, Cu element is from copper mesh) of nano cubic block.
Fig. 8 gives In 2o 3the selected area electron diffraction figure of nano cubic block.
Embodiment 2
According to batching and the preparation process of embodiment 1, temperature of reaction is still 120 DEG C, just will change 24 hours the reaction times into.The InOOH nano wire obtained is substantially identical with embodiment 1.
Embodiment 3
According to batching and the preparation process of embodiment 1, just temperature of reaction is changed into 130 DEG C, the reaction times changes 12 hours into.
The TEM picture of what Fig. 9 provided is product prepared by above-mentioned condition, can find out have a small amount of fluidized agglomerate of nano-size particles to occur in the InOOH nano wire obtained.
Embodiment 4
According to batching and the preparation process of embodiment 1, temperature of reaction is changed into 140 DEG C, the reaction times changes 12 hours into.
The TEM picture of what Figure 10 provided is product prepared by above-mentioned condition, can find out have fluidized agglomerate of nano-size particles to occur in the InOOH nano wire obtained, and larger than the particle diameter in embodiment 3.
Embodiment 5
According to batching and the preparation process of embodiment 1, temperature of reaction is changed into 140 DEG C, the reaction times changes 24 hours into.
The TEM picture of what Figure 11 provided is product prepared by above-mentioned condition, can find out have fluidized agglomerate of nano-size particles to occur in the InOOH nano wire obtained, and larger than the particle diameter in embodiment 4.
Embodiment 6
According to batching and the preparation process of embodiment 1, temperature of reaction is changed into 150 DEG C, the reaction times changes 24 hours into.
The TEM picture of what Figure 12 provided is product prepared by above-mentioned condition, can find out have a large amount of nanometer beads to occur in the InOOH nano wire obtained, and than the regular shape in embodiment 5.
Embodiment 7
According to batching and the preparation process of embodiment 1, temperature of reaction is changed into 160 DEG C, the reaction times changes 24 hours into.
The TEM picture of what Figure 13 provided is product prepared by above-mentioned condition, can find out, have a large amount of nanometer balls to occur, and particle diameter be larger in the InOOH nano wire obtained.
Embodiment 8
According to batching and the preparation process of embodiment 1, temperature of reaction is changed into 170 DEG C, the reaction times changes 24 hours into.
The TEM picture of what Figure 14 provided is product prepared by above-mentioned condition, can find out have the cubic block of a large amount of rules and a small amount of nano wire in product.
Embodiment 9
According to batching and the preparation process of embodiment 1, temperature of reaction is changed into 180 DEG C, the reaction times changes 12 hours into.
The TEM picture of what Figure 15 provided is product prepared by above-mentioned condition, can find out, the In obtained 2o 3a small amount of InOOH nano wire is had in nano cubic block.
Embodiment 10
According to batching and the preparation process of embodiment 1, temperature of reaction is changed into 190 DEG C, the reaction times changes into 24 constantly little, the In obtained 2o 3the nano cubic block size shape that nano cubic block reacts obtained with embodiment 1 is substantially identical.
The TEM picture of what Figure 16 provided is product prepared by above-mentioned condition, can find out, the In obtained 2o 3substantially identical with embodiment 1 of nano cubic block.
Embodiment 11 (as comparative example)
By the InCl of 0.1g 34H 2o 3powder dissolution, in the oleyl amine of 5ml, instills the dehydrated alcohol of 8ml in ultrasonic process, after solution clarification, mixing solutions is poured into reacting by heating in the reactor of sealing, when heating, temperature rise rate is set as 4 DEG C/min.Temperature of reaction is 130 DEG C, and the reaction times is 12-24 hour, after reaction terminates, reactor is naturally cooled to room temperature.
Do not collect precipitation, illustrate when this temperature condition, InOOH nano wire can not be obtained under lower temperature rise rate.
Embodiment 12 (as comparative example)
According to batching and the preparation process of embodiment 11, temperature change is 140 DEG C, and the reaction times is that 12-24 is constantly little, does not collect precipitation, illustrates when this temperature condition, can not obtain InOOH nano wire under lower temperature rise rate.
Embodiment 13 (as comparative example)
According to batching and the preparation process of embodiment 11, temperature change is 150 DEG C, and the reaction times is that 12-24 is constantly little, does not collect precipitation, illustrates when this temperature condition, can not obtain InOOH nano wire under lower temperature rise rate.
Embodiment 14
According to batching and the preparation process of embodiment 11, temperature for a change 160 DEG C, the reaction times is 12 hours, starts to occur throw out.
The XRD figure of what Figure 17 provided is in comparative example 4 product of preparation, proves that product is high-purity InOOH.
The TEM picture of the InOOH nano wire that Figure 18 prepares under giving above-mentioned condition.
Embodiment 15
According to batching and the preparation process of embodiment 11, temperature for a change 160 DEG C, the reaction times is 24 hours, and what obtain is high-purity InOOH nano wire.
Embodiment 16
According to batching and the preparation process of comparing embodiment 11, temperature for a change 180 DEG C, the reaction times is 24 hours.
The TEM picture of what Figure 19 provided is nano wire prepared by above-mentioned condition, can find out, have a large amount of nanometer beads to occur in the InOOH nano wire obtained, pattern is roughly identical with the pattern in embodiment 6.
Embodiment 17
According to batching and the preparation process of embodiment 11, temperature for a change 190 DEG C, the reaction times is 24 hours.
The XRD figure of what Figure 20 provided is product prepared by above-mentioned condition, proves that product is still InOOH and In 2o 3mixture.
Embodiment 18
According to batching and the preparation process of embodiment 11, temperature for a change 200 DEG C, the reaction times is 24 hours.
The XRD figure of what Figure 21 provided is in comparative example 6 product of preparation, proves that product is high-purity In 2o 3.
Figure 22 prepares the In of not too rule under giving above-mentioned condition 2o 3the TEM picture of nano particle.
Embodiment 19
According to batching and the preparation process of embodiment 11, temperature for a change 210 DEG C, the reaction times is 24 hours.
Figure 23 prepares the In of rule under giving above-mentioned condition 2o 3the TEM picture of nano cubic block.

Claims (8)

1. prepare a method for hydroxyl oxidize indium nano wire, add InCl by every milliliter of oleyl amine 34H 2the consumption that O powder is 0.015 ~ 0.025 gram is by InCl 34H 2o powder dissolution, in oleyl amine, instills dehydrated alcohol and clarifies to mixing solutions under ultrasound condition; Mixing solutions is poured into heated sealed reaction in reactor; Naturally cool to room temperature after reaction terminates, product is carried out centrifugation, with washes of absolute alcohol, the powder obtaining white after oven dry is hydroxyl oxidize indium nano wire; It is characterized in that, described reacting by heating, control temperature rise rate at 8 DEG C/min; Temperature of reaction is under 120 ~ 130 DEG C of conditions, insulation reaction 12 ~ 24 hours, or when controlling temperature rise rate at 4 DEG C/min, temperature of reaction is under 160 ~ 170 DEG C of conditions, insulation reaction 12 ~ 24 hours.
2. the method preparing hydroxyl oxidize indium nano wire according to claim 1, is characterized in that, described InCl 34H 2o powder, purity is 99.99%; Described oleyl amine, purity is 80% ~ 90%; Described dehydrated alcohol is analytical pure.
3. the method preparing hydroxyl oxidize indium nano wire according to claim 1 and 2, it is characterized in that, when controlling temperature rise rate at 8 DEG C/min, temperature of reaction is under 120 DEG C of conditions, or when controlling temperature rise rate at 4 DEG C/min, temperature of reaction is under 160 DEG C of conditions, and obtained is pure hydroxyl oxidize indium nano wire.
4. prepare a method for hydroxyl oxidize indium nano wire and Indium sesquioxide nano particle, add InCl by every milliliter of oleyl amine 34H 2the consumption that O powder is 0.015 ~ 0.025 gram is by InCl 34H 2o powder dissolution, in oleyl amine, instills dehydrated alcohol and clarifies to mixing solutions under ultrasound condition; Mixing solutions is poured into heated sealed reaction in reactor; Naturally cool to room temperature after reaction terminates, product is carried out centrifugation, with washes of absolute alcohol, the powder obtaining white after oven dry is the mix products of hydroxyl oxidize indium nano wire and Indium sesquioxide nano particle; It is characterized in that, described reacting by heating, when controlling temperature rise rate at 8 DEG C/min, temperature of reaction is under 140 ~ 160 DEG C of conditions, insulation reaction 12 ~ 24 hours, or when controlling temperature rise rate at 4 DEG C/min, temperature of reaction is under 180 ~ 190 DEG C of conditions, insulation reaction 12 ~ 24 hours.
5. the method preparing hydroxyl oxidize indium nano wire and Indium sesquioxide nano particle according to claim 4, is characterized in that, described InCl 34H 2o powder, purity is 99.99%; Described oleyl amine, purity is 80% ~ 90%; Described dehydrated alcohol is analytical pure.
6. prepare a method for Indium sesquioxide nano cubic block, add InCl by every milliliter of oleyl amine 34H 2the consumption that O powder is 0.015 ~ 0.025 gram is by InCl 34H 2o powder dissolution, in oleyl amine, instills dehydrated alcohol and clarifies to mixing solutions under ultrasound condition; Mixing solutions is poured into heated sealed reaction in reactor; Naturally cool to room temperature after reaction terminates, product is carried out centrifugation, with washes of absolute alcohol, the powder obtaining white after oven dry is Indium sesquioxide nano cubic block; It is characterized in that, described reacting by heating, when controlling temperature rise rate at 8 DEG C/min, temperature of reaction is under 170 ~ 200 DEG C of conditions, insulation reaction 12 ~ 24 hours, or when controlling temperature rise rate at 4 DEG C/min, temperature of reaction is under 200 ~ 210 DEG C of conditions, insulation reaction 12 ~ 24 hours.
7. the method preparing Indium sesquioxide nano cubic block according to claim 6, is characterized in that, described InCl 34H 2o powder, purity is 99.99%; Described oleyl amine, purity is 80% ~ 90%; Described dehydrated alcohol is analytical pure.
8. the method preparing Indium sesquioxide nano cubic block according to claim 6 or 7, is characterized in that, when controlling temperature rise rate at 8 DEG C/min, temperature of reaction is 190 DEG C, or when controlling temperature rise rate at 4 DEG C/min, temperature of reaction is 210 DEG C; Obtained is pure zirconia indium nano cubic block.
CN201410342197.7A 2014-07-18 2014-07-18 A kind of method preparing hydroxyl oxidize indium nano wire and Indium sesquioxide nano particle Expired - Fee Related CN104058448B (en)

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