CN104310460B - A kind of preparation method of indium compound nano material - Google Patents
A kind of preparation method of indium compound nano material Download PDFInfo
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- CN104310460B CN104310460B CN201410522021.XA CN201410522021A CN104310460B CN 104310460 B CN104310460 B CN 104310460B CN 201410522021 A CN201410522021 A CN 201410522021A CN 104310460 B CN104310460 B CN 104310460B
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- 150000002472 indium compounds Chemical class 0.000 title claims abstract description 128
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000011240 wet gel Substances 0.000 claims abstract description 78
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000000034 method Methods 0.000 claims abstract description 39
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims abstract description 38
- 230000008569 process Effects 0.000 claims abstract description 27
- 239000001294 propane Substances 0.000 claims abstract description 26
- 239000000499 gel Substances 0.000 claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 23
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- 238000000352 supercritical drying Methods 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 9
- 238000005516 engineering process Methods 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 3
- 230000006855 networking Effects 0.000 abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 24
- 239000000243 solution Substances 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 17
- 229910052738 indium Inorganic materials 0.000 description 16
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 16
- 239000002904 solvent Substances 0.000 description 16
- 239000000463 material Substances 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 11
- 229910021641 deionized water Inorganic materials 0.000 description 11
- 239000002245 particle Substances 0.000 description 8
- 230000008901 benefit Effects 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 5
- 239000000376 reactant Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000005660 chlorination reaction Methods 0.000 description 4
- 229960004756 ethanol Drugs 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000006068 polycondensation reaction Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 150000004703 alkoxides Chemical class 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000009432 framing Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 231100000614 poison Toxicity 0.000 description 3
- 230000007096 poisonous effect Effects 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910001449 indium ion Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 1
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- -1 and during changing Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910000337 indium(III) sulfate Inorganic materials 0.000 description 1
- XGCKLPDYTQRDTR-UHFFFAOYSA-H indium(iii) sulfate Chemical compound [In+3].[In+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XGCKLPDYTQRDTR-UHFFFAOYSA-H 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000011896 sensitive detection Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
The invention discloses the preparation method of a kind of indium compound nano material, the method includes: by adding gel catalyst expoxy propane in inorganic indium compound solution, obtain the wet gel of indium compound；The wet gel of described indium compound is carried out pretreatment, obtains pretreated indium chloride wet gel；The wet gel of described pretreated indium compound is dried process, obtains indium compound nano material.By the way, the present invention prepares the indium compound nano material of gained and has complete internal networking structure.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, particularly relate to a kind of indium compound nanometer
The preparation method of material.
Background technology
Indium compound is semiconducting compound, has the characteristic of quasiconductor, and it is in a semiconductor material
There is very important effect, be widely applied to solaode, gas sensor, catalyst
Etc. various fields.
The method preparing indium compound nano material is various, including magnetron sputtering method, hydrothermal synthesis method,
Electro-deposition method etc..Wherein, sol-gel method is easy with its process, with low cost, be prone to
The features such as large-scale production are particularly subject to pay attention to.Sol-gal process is exactly by precursor material under liquid phase
Uniformly mixing, and be hydrolyzed, be condensed chemical reaction, form the wet solidifying of three-dimensional space network structure
Glue, gel prepares the material with nanostructured adjustability through dry, sintering curing.And lead to
Cross nanometer indium compound material prepared by collosol and gel and have that good dispersion, granulation uniformity be high, ratio
The advantages such as surface area is big, answer in fields such as air-sensitive detection, optics absorption degradation, photocatalysis it
With serving the biggest facilitation effect, therefore the nanometer indium compound that research is prepared at sol-gel method
Material is significant.
But, there is surface tension in the solvent within gel skeleton, at common drying condition
Lower meeting causes the collapse of skeleton so that the indium compound nano material internal particle preparing gained is mutual
Cluster and overall structure crush.
Summary of the invention
The technical problem that present invention mainly solves is to provide the preparation of a kind of indium compound nano material
Method, it is possible to avoid preparing the indium compound mutual cluster of nano material internal particle of gained and whole
Body structure crushes so that the indium compound nano material preparing gained has complete internal network knot
Structure.
For solving above-mentioned technical problem, the technical scheme that the present invention uses is: provide a kind of indium
The preparation method of compound nano-material, including: urge inorganic indium compound solution adds gel
Agent expoxy propane, obtains the wet gel of indium compound；The wet gel of described indium compound is carried out
Pretreatment, obtains pretreated indium chloride wet gel；By described pretreated indium compound
Wet gel is dried process, obtains indium compound nano material.
Wherein, described inorganic indium compound is indium chloride.
Wherein, described indium chloride is 1:13.7～1:27.4 with the mol ratio of described expoxy propane.
Wherein, the concentration of described indiumchloride solution is 1mol/L～2mol/L.
Wherein, described indiumchloride solution includes: dehydrated alcohol, the addition phase of described dehydrated alcohol
Concentration to described indium chloride is 0.125mol/L～0.5mol/L.
Wherein, described pretreatment includes: burin-in process, heat treatment and Solvent exchange drying.
Wherein, the wet gel of described indium compound is carried out the step of burin-in process, including:
Under one predetermined condition, the surface of the wet gel of described indium compound is covered dehydrated alcohol, to carry out
Burin-in process；
Wherein, the wet gel of described indium compound is carried out the step of heat treatment, including:
Wherein, the wet gel of the indium compound after described burin-in process is entered under the second predetermined condition
Row heat treatment；The wet gel of described indium compound is carried out Solvent exchange drying, including: by described
The wet gel of the indium compound after heat treatment is cooled to room temperature, then under the 3rd predetermined condition, and will
The wet gel of described indium compound is put in organic solvent and is soaked, to displace described indium compound
The moisture content of residual in the hole of wet gel.
Wherein, the temperature of described first predetermined condition is 24 DEG C～26 DEG C；Described second predetermined condition
Be temperature be 50～80 DEG C, heat treatment time is 24～48 hours；Described 3rd predetermined condition
Temperature is identical with the temperature of the first predetermined condition.
Wherein, described first predetermined condition also includes that ageing treatment time is 1 week～2 weeks；Described
3rd predetermined condition also includes that soak time is 24～48 hours.
Wherein, described dried, is to utilize Supercritical Drying Technology, after described pretreatment
The wet gel of indium compound be dried, obtain indium compound nano material, including: by described
The wet gel of pretreated indium compound, being placed in temperature is 0 DEG C～5 DEG C, is placed on liquid CO2
High pressure equipment in, at least 1 day standing time；Liquid CO will be placed on2High pressure equipment in
The wet gel of described pretreated indium compound, the temperature in described high pressure equipment be 30～
45 DEG C, the pressure in described high pressure equipment is 5～10MPa, the state of described high pressure equipment is kept
6～8 hours；After pressure in described high pressure equipment is down to normal pressure, by the temperature of described high pressure equipment
Degree is down to room temperature, obtains the indium compound nano material that described drying is formed.
The invention has the beneficial effects as follows: be different from the situation of prior art, the present invention is by inorganic indium
Polymer solution adds gel catalyst expoxy propane, obtains the wet gel of indium compound；By described
The wet gel of indium compound carries out pretreatment；The wet gel of described pretreated indium compound is entered
Row dried, obtains indium compound nano material.Dried refers to by utilizing supercritical drying
Dry technology so that wet gel is dehydrated in the supercritical state, forms indium compound nano material；And
Wet gel is dehydrated in the supercritical state, maintains the internal networking structure of indium compound nano material
Complete, it is to avoid use conventional heating techniques or centrifugation technique to cause indium compound to be received when being dehydrated
The mutual cluster of internal particle of rice material and the shortcoming of Integral-crushing；It addition, by using epoxy
Propane is as gel catalyst, and the indium compound block materials of preparation has porosity height, specific surface
Long-pending big, structural integrity, microscopic particles is little, reaches the advantages such as nanometer scale；Further, inorganic
Indium compound, as presoma, is compared other organic alkoxide of use and is had cost as presoma
Low, green non-poisonous advantage.
Accompanying drawing explanation
Fig. 1 is the flow chart of preparation method first embodiment of indium compound nano material of the present invention；
Fig. 2 is the flow chart of preparation method second embodiment of indium compound nano material of the present invention；
Fig. 3 is the flow chart of preparation method the 3rd embodiment of indium compound nano material of the present invention；
Fig. 4 is the indium chemical combination that the preparation method according to indium compound nano material of the present invention prepares
The scanning electron microscope schematic diagram of thing nano material；
Fig. 5 is the indium compound prepared according to the preparation method of indium compound nano material of the present invention
The transmission electron microscope schematic diagram of nano material；
Fig. 6 is the indium compound prepared according to the preparation method of indium compound nano material of the present invention
The nitrogen adsorption desorption curve synoptic diagram of nano material.
Detailed description of the invention
The present invention is described in detail with embodiment below in conjunction with the accompanying drawings.
Refer to preparation method one embodiment party that Fig. 1, Fig. 1 are indium compound nano materials of the present invention
The flow chart of formula, as it can be seen, the preparation method of indium compound nano material includes:
Step S101: by adding gel catalyst expoxy propane in inorganic indium compound solution, obtain
The wet gel of indium compound.
Inorganic indium compound includes but not limited to: indium chloride, indium phosphide, indium nitrate, indium sulfate etc..
Inorganic indium compound solution can be aqueous solution, it is also possible to adds other in aqueous miscible with water
Organic solvent, such as ethanol, methanol etc..Gel catalyst refers in gel reaction, promotes
The mutual polycondensation of hydrated ion in solution and form the solvent of wet gel.Expoxy propane mixes with water section
Molten, miscible with ethanol, ether, therefore, expoxy propane, as proton capture agent, promotes in solution
The mutual polycondensation of hydrated ion and form the wet gel of indium compound, by this method, the indium of preparation
Compound nano-material has that porosity is high, specific surface area big, structural integrity, and microscopic particles is little,
Reach the advantages such as nanometer scale；And, inorganic indium compound, as presoma, is compared and is used other
Organic alkoxide has low cost, green non-poisonous advantage as presoma.
Step S102: the wet gel of indium compound is carried out pretreatment, obtains pretreated chlorination
Indium wet gel；
The purpose that the wet gel of indium compound carries out pretreatment is to be dried more easily.Due to
Containing a lot of moisture in the hole of the wet gel of indium compound, for the ease of being dried, can pass through
Burin-in process, or heat treatment, or Solvent exchange drying, or carry out successively burin-in process,
Heat treatment and Solvent exchange drying.Can certainly be other the pretreatment being conducive to being dried,
Do not limit at this.
Step S103: the wet gel of pretreated indium compound is dried process, obtains indium
Compound nano-material.
For so-called supercritical drying is the critical point for material a certain in system, generally refer to
Mixed with the component that bigger content and critical point are relatively low in mixture system, by heating up, pressurizeing
During to a certain temperature, pressure, if system status is in critical (temperature, the pressure exceeding this component
State by force), this component presents solid-liquid phase interface extinction tests, then can accelerate solution-air, gas-solid
Mass transfer, heat transfer, weaken general drying process interfacial tension to solid particulate matter structural damage.
There is surface tension in the solvent within gel skeleton, can cause bone under common drying condition
The collapse of frame；Supercritical drying is intended to the control by pressure and temperature, makes solvent in dry run
In reach itself critical point, complete liquid phase to the hypercritical transition of gas phase；During solvent without
Substantially surface tension, completes the wet gel transformation to aeroge on the premise of maintaining framing structure.
Embodiment of the present invention will add gel catalyst expoxy propane in inorganic indium compound solution,
Obtain the wet gel of indium compound；The wet gel of described indium compound is carried out pretreatment；By described
The wet gel of pretreated indium compound is dried process, obtains indium compound nano material.
Dried refers to by utilizing Supercritical Drying Technology so that wet gel takes off in the supercritical state
Water, forms indium compound nano material；And wet gel is dehydrated in the supercritical state, maintain indium
The internal networking structure of compound nano-material complete, it is to avoid use conventional heating techniques or centrifugal
The mutual cluster of internal particle and the entirety of indium compound nano material is caused when technology is dehydrated
Broken shortcoming；It addition, by using expoxy propane as gel catalyst, the indium chemical combination of preparation
Thing block materials has that porosity is high, specific surface area big, structural integrity, and microscopic particles is little, reaches
The advantages such as nanometer scale；Further, inorganic indium compound, as presoma, is compared and is used other
Organic alkoxide has low cost, green non-poisonous advantage as presoma.
Wherein, inorganic indium compound is indium chloride.Now, indium chloride and expoxy propane addition
Mol ratio is 1:13.7～1:27.4, and such as, indium chloride with the mol ratio of expoxy propane addition is
1:13.7,1:20.5 or 1:27.4.
Further, the concentration of indiumchloride solution is 1mol/L～2mol/L, such as: indium chloride is molten
The concentration of liquid is 1mol/L, 1.5mol/L or 2mol/L.Wherein, indiumchloride solution includes nothing
Water-ethanol, the addition of dehydrated alcohol is 0.125mol/L～0.5 relative to the concentration of indium chloride
Mol/L, such as: the addition of dehydrated alcohol relative to the concentration of indium chloride be 0.125mol/L,
0.32mol/L or 0.5mol/L.Certainly, indiumchloride solution can also include methanol.
Such as: step S101, in an actual application, specifically may is that
Under room temperature, adding indium chloride in deionized water, stirring, until being completely dissolved, must be clarified
Bright concentration is the indiumchloride solution of 1mol/L-2mol/L；Then, add dehydrated alcohol, anhydrous
Ethanol addition is relative indium chloride concentration: 0.125mol/L-0.5mol/L, stirring while adding,
Dissolve and form clear transparent solutions；Finally, gel catalyst expoxy propane, indium chloride and ring are added
The molar ratio range of Ethylene Oxide addition is 1:13.7 1:27.4, continues agitating solution, along with
Being gradually increased of propylene oxide concentrations, solution gradually and forms milky indium chloride colloidal sol；By chlorine
Change to pour in mould after indium colloidal sol stirs and stand, form indium chloride wet gel.
Wherein, refering to Fig. 2, the pretreatment in step S102 includes but not limited to: burin-in process,
Heat treatment and Solvent exchange drying, particular content is as follows:
Wet gel to indium compound carries out the step of heat treatment, including:
Step S102a: under the first predetermined condition, covers the surface of the wet gel of indium compound
Dehydrated alcohol, to carry out burin-in process.
The wet gel of indium compound is carried out the step of heat treatment, including:
Step S102b: by the wet gel of the indium compound after burin-in process under the second predetermined condition
Carry out heat treatment.
Heat treatment can be carried out in heating furnace, and further, heat treatment can enter in Muffle furnace
OK.
The wet gel of indium compound is carried out the step of Solvent exchange drying, including:
Step S102c: the wet gel of the indium compound after heat treatment is cooled to room temperature, then exists
Under 3rd predetermined condition, the wet gel of indium compound is put in organic solvent and soak, to displace
The moisture content of residual in the hole of the wet gel of indium compound.
Wherein, organic solvent can be ethanol, methanol etc..
First predetermined condition is the condition of burin-in process, and the second predetermined condition is the condition of heat treatment,
3rd predetermined condition is the condition of Solvent exchange drying.First predetermined condition, the second predetermined condition with
And the 3rd predetermined condition need in actual applications to determine according to concrete experiment.
Wherein, the temperature of the first predetermined condition is 24 DEG C～26 DEG C；The temperature of the second predetermined condition is
50～80 DEG C, heat treatment time is 24～48 hours；The temperature of the 3rd predetermined condition is pre-with first
The temperature of fixed condition is identical.
Further, the first predetermined condition also includes that ageing treatment time is 1 week～2 weeks；3rd
Predetermined condition also includes that soak time is 24～48 hours.
It should be noted that in actual applications, the wet gel of indium compound is carried out pretreatment,
Can specifically determine to carry out which pretreatment, do not limit at this according to practical situation.
Wherein, refering to Fig. 3, in step s 103, dried is to utilize Supercritical Drying Technology,
The wet gel of pretreated indium compound is dried, obtains indium compound nano material, tool
Body step includes:
Step S103a: by the wet gel of pretreated indium compound, be placed in temperature be 0 DEG C～
5 DEG C, be placed on full liquid CO2High pressure equipment in, at least 1 day standing time.
Step S103b: liquid CO will be placed on2High pressure equipment in pretreated indium chemical combination
The wet gel of thing, the temperature in high pressure equipment is 30～45 DEG C, the pressure in high pressure equipment be 5～
10MPa, persistently keeps 6～8 hours by the state of high pressure equipment.
Step S103c: after the pressure in high pressure equipment is down to normal pressure, by the temperature of high pressure equipment
It is down to room temperature, obtains being dried the indium compound nano material of formation.
High pressure equipment is preferably autoclave.The indium compound nano material prepared by upper described method
In block, and internal structure has three-dimensional network loose structure.Supercritical drying process is intended to lead to
Excess pressure and the control of temperature, make solvent reach the critical point of itself in dry run, complete
Liquid phase is to the hypercritical transition of gas phase, and during changing, solvent is without obvious surface tension, makes
The wet gel transformation to dry nano material must be completed on the premise of maintaining framing structure.
The principle of preparation method of the present invention is: utilize inorganic indium compound to form hydrogen-oxygen water after being dissolved in water
Close indium ion, then by add proton capture agent expoxy propane with reach to promote solution is hydrated from
Son mutually polycondensation and form wet gel, then utilize supercritical drying process by the liquid in wet gel
Replace with gas, finally prepare block indium compound nano material.
Reader is best understood from the present invention for convenience, below in conjunction with specific embodiment to the present invention's
Preparation method is described further.
Embodiment 1:
Indium chloride is dissolved in deionized water, then adds dehydrated alcohol and expoxy propane, chlorination
Indium, deionized water, dehydrated alcohol and expoxy propane ratio are 0.9g:3ml:24ml:4.2ml,
Add above-mentioned each reactant in the case of being sufficiently stirred for successively, after about 20 minutes, obtain indium
The wet gel of compound.The wet gel of indium compound, after overaging 2 weeks and washing with alcohol 3 times, enters
Row supercritical drying process, can obtain block indium compound nano material, and its density is about
200mg/cm3, specific surface area is 400m2·g-1, this indium compound nano material is scanned through electricity
Sub-microscope (Scanning Electron Microscope, referred to as SEM), it is thus achieved that image
As shown in Figure 4.
Embodiment 2:
Indium chloride is dissolved in deionized water, then adds dehydrated alcohol and expoxy propane, chlorination
Indium, deionized water, dehydrated alcohol and expoxy propane ratio are 1.385g:3ml:24ml:4.2ml,
In the case of being sufficiently stirred for, add above-mentioned each reactant successively, after about 20 minutes, obtain indium
The wet gel of compound.The wet gel of indium compound after overaging 2 weeks and washing with alcohol 3 times,
Carrying out supercritical drying process, can obtain block indium compound nano material, its density is about
300mg/cm3, this indium compound nano material is through transmission electron microscope (Transmission
Electron Microscope, referred to as TEM), it is thus achieved that image is as shown in Figure 5.
Embodiment 3:
Indium chloride is dissolved in deionized water, then interpolation methanol and expoxy propane, indium chloride,
Deionized water, methanol and expoxy propane ratio are 1.385g:3ml:24ml:4.2ml, are fully stirring
Add above-mentioned each reactant in the case of mixing successively, after about 20 minutes, obtain indium compound
Wet gel.The wet gel of indium compound, after overaging 1 week and methanol wash 3 times, carries out super facing
Boundary's drying process, can obtain block indium compound nano material, and its density is about 350mg/cm3。
Embodiment 4:
Indium chloride is dissolved in deionized water, then adds dehydrated alcohol and expoxy propane, chlorination
Indium, deionized water, dehydrated alcohol and expoxy propane ratio are 0.9g:6ml:24ml:4.2ml,
Add above-mentioned each reactant in the case of being sufficiently stirred for successively, after about 20 minutes, obtain indium
The wet gel of compound.The wet gel of indium compound, after overaging 1 week and washing with alcohol 3 times, enters
Row supercritical drying process, can obtain block indium compound material, and its specific surface area is about 230
m2·g-1, even particle distribution, about 30nm.
Embodiment 5:
Indium chloride is dissolved in deionized water, then interpolation methanol and expoxy propane, indium chloride,
The ratio of deionized water, methanol and expoxy propane is 1.8g:6ml:24ml:4.2ml, is fully stirring
Add above-mentioned each reactant in the case of mixing successively, after about 20 minutes, obtain indium compound
Wet gel.The wet gel of indium compound through overaging 2 weeks and washing with alcohol repeatedly after, carry out super facing
Boundary's drying process, can obtain block indium compound nano material, its nitrogen adsorption desorption curve such as figure
Shown in 6.
In the present invention, inorganic indium compound is utilized to form hydrogen-oxygen hydration indium ion after being dissolved in water, so
Afterwards by adding proton capture agent expoxy propane to reach to promote the mutual polycondensation of hydrated ion in solution
And form wet gel, then utilize supercritical drying process that the liquid in wet gel is replaced with gas
Body, finally prepares block indium compound nano material.And supercritical drying process is intended to pass through pressure
With the control of temperature, make solvent reach the critical point of itself in dry run, complete liquid phase extremely
The hypercritical transition of gas phase, and solvent is without obvious surface tension during changing so that in dimension
Complete the wet gel transformation to dry nano material on the premise of holding framing structure, obtain block indium chemical combination
Thing nano material, and this block indium compound nano material has three-dimensional network loose structure.
The foregoing is only embodiments of the present invention, not thereby limit the patent model of the present invention
Enclosing, every equivalent structure utilizing description of the invention and accompanying drawing content to be made or equivalence flow process become
Change, or be directly or indirectly used in other relevant technical fields, be the most in like manner included in the present invention's
In scope of patent protection.
Claims (7)
1. the preparation method of an indium compound nano material, it is characterised in that including:
By inorganic indium compound solution adds gel catalyst expoxy propane, obtain the wet gel of indium compound；
Under the first predetermined condition, the surface of the wet gel of described indium compound is covered dehydrated alcohol, to carry out burin-in process, the wet gel of the indium compound after described burin-in process is carried out heat treatment under the second predetermined condition, the wet gel of the indium compound after described heat treatment is cooled to room temperature, then under the 3rd predetermined condition, the wet gel of described indium compound is put in organic solvent and soak, with the moisture remained in displacing the hole of the wet gel of described indium compound, obtain pretreated indium chloride wet gel；
Utilize Supercritical Drying Technology, the wet gel of described pretreated indium compound is dried process and obtains indium compound nano material；
Described inorganic indium compound is indium chloride.
The preparation method of indium compound nano material the most according to claim 1, it is characterised in that described indium chloride is 1:13.7～1:27.4 with the mol ratio of described expoxy propane.
The preparation method of indium compound nano material the most according to claim 1, it is characterised in that the concentration of described indiumchloride solution is 1mol/L～2mol/L.
4., according to the preparation method of indium compound nano material described in claim 1 or 3, it is characterised in that described indiumchloride solution includes: dehydrated alcohol, the concentration of the most described indium chloride of addition of described dehydrated alcohol is 0.125mol/L～0.5mol/L.
The preparation method of indium compound nano material the most according to claim 1, it is characterised in that the temperature of described first predetermined condition is 24 DEG C～26 DEG C；The temperature of described second predetermined condition is 50～80 DEG C, heat treatment time 24～48 hours；The temperature of described 3rd predetermined condition is identical with the temperature of the first predetermined condition.
The preparation method of indium compound nano material the most according to claim 5, it is characterised in that described first predetermined condition also includes that ageing treatment time is 1 week～2 weeks；Described 3rd predetermined condition also includes that soak time is 24～48 hours.
Method the most according to claim 1, it is characterised in that the described wet gel by described pretreated indium compound is dried, and obtains indium compound nano material, including:
By the wet gel of described pretreated indium chloride, being placed in temperature is 0 DEG C～5 DEG C, is placed on liquid CO2High pressure equipment in, at least 1 day standing time；
Liquid CO will be placed on2High pressure equipment in the wet gel of described pretreated indium chloride, the temperature in described high pressure equipment is 30～45 DEG C, and the pressure in described high pressure equipment is 5～10MPa, and the state of described high pressure equipment is persistently kept 6～8 hours；
After pressure in described high pressure equipment is down to normal pressure, the temperature of described high pressure equipment is down to room temperature, obtains the indium compound nano material that described drying is formed.
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| CN102001698A (en) * | 2010-10-26 | 2011-04-06 | 江苏大学 | Preparation method of indium oxide mesoporous nanospheres |
| CN103157410A (en) * | 2013-03-13 | 2013-06-19 | 中国科学院化学研究所 | Aerogel preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102001698A (en) * | 2010-10-26 | 2011-04-06 | 江苏大学 | Preparation method of indium oxide mesoporous nanospheres |
| CN103157410A (en) * | 2013-03-13 | 2013-06-19 | 中国科学院化学研究所 | Aerogel preparation method |
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| Title |
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| "环氧化物法制备锑掺杂氧化锡气凝胶";虞秋捷等;《物理化学学报》;20140331(第3期);第500-507页 * |
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