CN107827148A - A kind of chiasma type indium oxide nanometer material preparation method - Google Patents
A kind of chiasma type indium oxide nanometer material preparation method Download PDFInfo
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- CN107827148A CN107827148A CN201711162647.4A CN201711162647A CN107827148A CN 107827148 A CN107827148 A CN 107827148A CN 201711162647 A CN201711162647 A CN 201711162647A CN 107827148 A CN107827148 A CN 107827148A
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- chiasma type
- nanometer material
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- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910003437 indium oxide Inorganic materials 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000004202 carbamide Substances 0.000 claims abstract description 38
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000004044 response Effects 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 230000002459 sustained effect Effects 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- 229910021617 Indium monochloride Inorganic materials 0.000 claims description 9
- APHGZSBLRQFRCA-UHFFFAOYSA-M indium(1+);chloride Chemical compound [In]Cl APHGZSBLRQFRCA-UHFFFAOYSA-M 0.000 claims description 9
- 229910001868 water Inorganic materials 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- ZMFWDTJZHRDHNW-UHFFFAOYSA-N indium;trihydrate Chemical compound O.O.O.[In] ZMFWDTJZHRDHNW-UHFFFAOYSA-N 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- 238000003786 synthesis reaction Methods 0.000 claims description 5
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 claims description 3
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 3
- 230000001174 ascending effect Effects 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 238000002372 labelling Methods 0.000 claims description 3
- 238000000643 oven drying Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 239000003643 water by type Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims 1
- 239000007789 gas Substances 0.000 abstract description 19
- 238000012360 testing method Methods 0.000 abstract description 7
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 239000008367 deionised water Substances 0.000 abstract description 2
- 229910021641 deionized water Inorganic materials 0.000 abstract description 2
- HNLXNOZHXNSSPN-UHFFFAOYSA-N 2-[2-[2-[2-[2-[2-[2-[4-(2,4,4-trimethylpentan-2-yl)phenoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethanol Chemical compound CC(C)(C)CC(C)(C)C1=CC=C(OCCOCCOCCOCCOCCOCCOCCO)C=C1 HNLXNOZHXNSSPN-UHFFFAOYSA-N 0.000 abstract 1
- 238000013019 agitation Methods 0.000 abstract 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 abstract 1
- 239000000047 product Substances 0.000 description 11
- 239000013078 crystal Substances 0.000 description 9
- 238000001228 spectrum Methods 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 210000003027 ear inner Anatomy 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
Classifications
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- 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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- 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
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of chiasma type indium oxide nanometer material preparation method, preparing raw material is inidum chloride (InCl3·4H2O), Qula leads to (Triton x 100), absolute ethyl alcohol (CH3CH2) and urea (CO (NH OH2)2), its preparation methods steps are as follows：A. urea liquid is obtained；B. indiumchloride solution is obtained；C. above-mentioned urea liquid and indiumchloride solution are mixed and under agitation leads to 2mL Qulas and be added in above-mentioned mixed solution and be sufficiently stirred；D. the above-mentioned solution of acquisition is transferred in reactor, then reactor is moved into baking oven, taken out at 120 DEG C after sustained response 12h.After question response kettle natural cooling, centrifugal treating, successively washed repeatedly with deionized water and absolute ethyl alcohol.The present invention leads to this structure directing agent by adding Qula, the chiasma type indium oxide of acquisition is prepared into gas sensor and has carried out air-sensitive test to multiple gases, relative to common oxidation phosphide material, the indium oxide of this chiasma type can significantly improve its air-sensitive performance to multiple gases.
Description
Technical field
The present invention relates to a kind of its technical field of nanometer material preparation, especially a kind of chiasma type for gas sensor
Indium oxide nanometer material preparation method.
Background technology
Metal oxide semiconductor material has important and is widely applied in industrial production and daily life, but its
Performance understands the difference because of pattern, size, Spatial Dimension and structure etc. and difference is huge, in order to improve the original of material as far as possible
Performance, people have synthesized different morphologies and the metal oxide semiconductor material of structure, in many patterns and the material of structure
In material, the metal oxide semiconductor material for having the labyrinths such as 3 D stereo shape attracts the attention of people and studied emerging
Interest, this, which is primarily due to this 3-D solid structure, can significantly improve the contact area of material and other materials, and then improve reaction
Efficiency, it is significant in fields such as fuel cell, catalysis, gas-monitoring and electrochemistry.
Nano indium oxide is a kind of important inorganic powder, is widely used in solar cell, gas sensor, flat board and shows
Show the numerous areas such as device, opto-electronic device and Organic Light Emitting Diode.It is main currently used for synthesis different-shape indium oxide method
There are the hot method of chemical precipitation method, aqueous solvent, organic solution synthetic method, hot injection, sol-gel process, microemulsion method, thermal evaporation oxygen
Change method, electric arc put method etc..
The problem of traditional chemical method is present be:Severe reaction conditions, cost are too high, it is difficult to large-scale production；Obtain
Indium oxide product is easily reunited；Reaction temperature requires high, and control is difficult, inconvenient for operation；And obtained indium oxide is to gas
Air-sensitive performance than relatively low, reduce the using effect of indium oxide nanometer material.
The content of the invention
The present invention is for the deficiency in existing indium oxide nanometer material technology of preparing, there is provided a kind of chiasma type indium oxide
Preparation method of nano material.
The present invention employs a kind of novel technical scheme, is successfully prepared out a kind of friendship to solve above-mentioned technical deficiency
Forked type indium oxide nanometer material, preparing raw material are inidum chloride (InCl3·4H2) and urea (CO (NH O2)2), preparation method step
It is as follows：
A. a certain amount of urea is added in 120mL absolute ethyl alcohols under stirring, it is complete is stirred well to urea
Dissolving；
B. a certain amount of InCl is weighed3·4H2O is placed in small beaker, is then added 10mL deionized waters, is continued stirring until
InCl3·4H2O is completely dissolved, and obtains the InCl of water white transparency3·4H2O solution；
C. urea liquid is added into InCl under stirring3·4H2In O solution and be sufficiently stirred 30min obtain mixing it is molten
Liquid, then 2mL Qulas are led to and are added in above-mentioned mixed solution, continue for stirring 20min；
D. finally the solution of acquisition will be transferred in 100mL polytetrafluoroethyllining lining stainless steel cauldrons, by reactor
Move into baking oven, taken out at 120 DEG C after sustained response 12h；
E. after question response kettle natural cooling, by the product centrifugation in reactor and then priority deionized water and anhydrous second
Alcohol is washed repeatedly to remove possible foreign ion；
F. and then product is placed in baking oven and 24h acquisition white powders is dried at 60 DEG C, labeled as In (OH)3(t)；
G. the white powder of acquisition is placed in Muffle furnace, 1h is heat-treated under slow ascending temperature to 500 DEG C of air conditionses
Indium oxide nanometer material of the synthesis with good dispersion, the product labelling obtained after heat treatment is In2O3(t)；
H. in water-heat process, the reaction principle of urea：
CO(NH2)2+H2O→2NH3+CO2
NH3+H2O→NH4++OH-
In3++3OH-→In(OH)3
In3++n(urea)→[In(urea)n]3+
[In(urea)n]3++3OH-→In(OH)3(urea)m+(n-m)urea
As a kind of preferred embodiment of the present invention, a certain amount of urea is added in the step a, and using anhydrous
Ethanol as solvent, lead to, then is successfully synthesized by Hydrothermal Synthesiss and heat-treating methods by the Qula that 2mL is added in selected c
The indium oxide gas sensitive of chiasma type.
As a kind of preferred embodiment of the present invention, the temperature of the baking oven in the step d is 120 DEG C, the duration
For 12h.
As a kind of preferred embodiment of the present invention, the temperature of the oven drying in the step f is 60 DEG C or so, is done
The dry time is 24h.
The temperature of Muffle furnace in the step g is 500 DEG C, and the time of heat treatment is 1h.
The beneficial effect that is reached of the present invention is：The present invention is by being that raw material slowly supplies OH from urea-, add Qula
Lead to this structure directing agent, then the indium oxide gas of chiasma type is successfully synthesized with simple Hydrothermal Synthesiss and heat-treating methods
Quick material, find that urea and Qula work with the formation to chiasma type indium oxide in all in an experiment, by the chiasma type of acquisition
Indium oxide is prepared into gas sensor and has carried out air-sensitive test to multiple gases, and test result shows：Relative to common oxidation
Phosphide material, the indium oxide of this chiasma type can significantly improve its air-sensitive performance to multiple gases.
Brief description of the drawings
Fig. 1 is In of the present invention2O3(t) X-ray diffracting spectrum；
Fig. 2 is In of the present invention (OH)3(t) X-ray diffracting spectrum；
Fig. 3 is In of the present invention2O3(t) Raman collection of illustrative plates；
Fig. 4 is In of the present invention2O3(t) hum patterns such as scale topography.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes.
A kind of chiasma type indium oxide nanometer material preparation method, preparing raw material are inidum chloride (InCl3·4H2) and urea O
(CO(NH2)2), preparation method step is as follows：
A. a certain amount of urea is added in 120mL absolute ethyl alcohols under stirring, it is complete is stirred well to urea
Dissolving；
B. a certain amount of InCl is weighed3·4H2O is placed in small beaker, is then added 10mL deionized waters, is continued stirring until
InCl3·4H2O is completely dissolved, and obtains the InCl of water white transparency3·4H2O solution；
C. urea liquid is added into InCl under stirring3·4H2In O solution and be sufficiently stirred 30min obtain mixing it is molten
Liquid, then 2mL Qulas are led to and are added in above-mentioned mixed solution, continue for stirring 20min；
D. finally the solution of acquisition will be transferred in 100mL polytetrafluoroethyllining lining stainless steel cauldrons, by reactor
Move into baking oven, taken out at 120 DEG C after sustained response 12h；
E. after question response kettle natural cooling, the product centrifugation in reactor, washing, ethanol are washed repeatedly possible to remove
Foreign ion；
F. and then product is placed in baking oven and obtains white powder, labeled as In (OH)3(t)；
G. the white powder of acquisition is placed in Muffle furnace, 1h is heat-treated under slow ascending temperature to 500 DEG C of air conditionses
Indium oxide nanometer material of the synthesis with good dispersion, the product labelling obtained after heat treatment is In2O3(t)；
H. in water-heat process, the reaction principle of urea：
CO(NH2)2+H2O→2NH3+CO2
NH3+H2O→NH4 ++OH-
In3++3OH-→In(OH)3
In3++n(urea)→[In(urea)n]3+
[In(urea)n]3++3OH-→In(OH)3(urea)m+(n-m)urea。
One of raw material in the step a is urea, and selected solvent is absolute ethyl alcohol, and 2mL song is added in the step c
Draw and lead to, then the indium oxide gas sensitive of chiasma type is successfully synthesized by Hydrothermal Synthesiss and heat-treating methods.
The temperature of baking oven in the step d is 120 DEG C, duration 12h.
The temperature of oven drying in the step f is 60 DEG C or so, and the dry time is 24h.
The temperature of Muffle furnace in the step g is 500 DEG C, and the time of heat treatment is 1h.
In order to obtain the information such as the structure composition of final product, product X-ray diffraction is subjected to first and Raman is surveyed
Examination：The final product according to Fig. 12O3(t) X ray diffracting spectrum, the θ scopes of X-ray diffraction scanning angle 2 are 5 to 80 °
Diffraction maximum point at 21.8,30.8,35.7,38.1,42.1,45.9,51.3,56.3,59.4,60.8,62.4 and 63.9 °
Dui Yingyu not In2O3(211), (222), (400), (411), (332), (431), (440), (611), (541), (622),
And (444) crystal face (631).Wherein (222) diffraction maximum is relatively stronger and sharp, this explanation crystal edge [111] direction preferential growth,
All diffraction maximums with Emission in Cubic In2O3The standard diagram of (JCPDS No.06-0416) is completely the same, can from figure
Go out：The peak shape of diffraction maximum is more sharp, does not find the presence of unnecessary miscellaneous peak, shows that prepared product crystallinity is higher, purity
Preferably；It is In (OH) according to Fig. 23(t) X-ray diffracting spectrum, the θ of X-ray diffraction scanning angle 2 are 20 to 80 ° of figures
In positioned at 22.4,31.8,35.6,39.1,42.5,45.6,51.3,56.5,66.3,70.9 and 75.4 ° place diffraction maximum distinguish
Corresponding to In (OH)3(200), (220), (013), (222), (321), (400), (420), (422), (440), (442) and
(620) crystal face, all diffraction maximums with Emission in Cubic In (OH)3The standard diagram of (JCPDS No.76-1463) is consistent；According to
It is In shown in Fig. 32O3(t) Raman collection of illustrative plates, by being clear that In in figure2O3(t) five characteristic peak (132cm-1,
305cm-1, 365cm-1, 494cm-1And 630cm-1), these peaks and c-In2O3Middle InO6In-O vibration peaks it is corresponding, above knot
Fruit shows the In of the Emission in Cubic of synthesis2O3Nanocrystal, the pure free from admixture of crystal, crystallinity are good.
In order to further obtain In2O3(t) information such as scale topography, use field emission scanning electron microscope and transmission electron microscope pair
Product is studied, and Fig. 4 a-d are In2O3(t) the field emission scanning electron microscope figure under different amplification；Can be with from Fig. 4-a
Find out, experiment obtains the In of a large amount of chiasma types2O3Material, a region in figure is amplified according to different multiples and obtained
Obtain Fig. 4-b and 4-c；Obtained product is can be seen that from Fig. 4-b and 4-c and supports each other scattered, and pattern is different, overall dimensions
At 5 μm or so, these interference type arrangements are by bar-shaped In2O3Composition, these bar-shaped In2O3Material diameter between 200-500nm,
Length is between 1-10 μm；Fig. 4-d are partial enlarged drawings, and the mutual support stack of crystal is can see together from Fig. 4-d, this
Abundant space not of uniform size is formed between a little crystal, this space is advantageous to the diffusion and exchange of gas molecule so that bottom
Layer crystal body also more quickly can sufficiently touch under test gas；Fig. 4-e and 4-f are In2O3The transmission electron microscope collection of illustrative plates of crystal；
It can more be intuitive to see due to the pattern of this chiasma type from Fig. 4-e, mutually be propped up by the point contacted with each other between crystal
Support and be unable to dense accumulation (the latter half black portions are Electronic Speculum copper mesh edges in figure) together；Fig. 4-f are single typical
Chiasma type In2O3Structure, while the structure multi-point support plays itself, itself all face can effectively reach gas；
In addition, the structure of this chiasma type can also prevent material from being put because of higher surface energy in storage because of the supporting role of itself
Occur agglomeration during putting, preferably maintain the dispersiveness of itself.
Chiasma type indium oxide nanometer material preparation method in the present embodiment, lead to this structure directing by adding Qula
Agent, then the indium oxide gas sensitive of chiasma type is successfully synthesized with simple Hydrothermal Synthesiss and heat-treating methods, testing
Middle discovery urea and Qula are worked with the formation to chiasma type indium oxide in all, and the chiasma type indium oxide of acquisition is prepared into gas
Quick element has simultaneously carried out air-sensitive test to multiple gases, and test result shows：Relative to common oxidation phosphide material, this intersection
The indium oxide of type can significantly improve its air-sensitive performance to multiple gases.
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention,
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still may be used
To be modified to the technical scheme described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic.
Within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., it should be included in the present invention's
Within protection domain.
Claims (5)
1. a kind of chiasma type indium oxide nanometer material preparation method, it is characterised in that preparing raw material is inidum chloride (InCl3·
4H2) and urea (CO (NH O2)2), and selected Qula to lead to (Tritonx-100) and be used as structure directing agent.Preparation method step is such as
Under：
A. a certain amount of urea is added in 120mL absolute ethyl alcohols under stirring, is stirred well to urea and is completely dissolved；
B. a certain amount of InCl is weighed3·4H2O is placed in small beaker, is then added 10mL deionized waters, is continued stirring until
InCl3·4H2O is completely dissolved, and obtains the InCl of water white transparency3·4H2O solution；
C. urea liquid is added into InCl under stirring3·4H2In O solution and be sufficiently stirred 30min obtain mixed solution,
Then 2mL Qulas are led to and be added in above-mentioned mixed solution, continue for stirring 20min；
D. finally the solution of acquisition will be transferred in 100mL polytetrafluoroethyllining lining stainless steel cauldrons, reactor is moved into
In baking oven, taken out at 120 DEG C after sustained response 12h；
E. after question response kettle natural cooling, the product centrifugation in reactor, washing, ethanol are washed repeatedly to remove possible impurity
Ion；
F. and then product is placed in baking oven and 24h acquisition white powders is dried at 60 DEG C, labeled as In (OH)3(t)；
G. the white powder of acquisition is placed in Muffle furnace, 1h synthesis is heat-treated under slow ascending temperature to 500 DEG C of air conditionses
Indium oxide nanometer material with good dispersion, the product labelling obtained after heat treatment are In2O3(t)；
H. in water-heat process, the reaction principle of urea：
CO(NH2)2+H2O→2NH3+CO2
NH3+H2O→NH4 ++OH-
In3++3OH-→In(OH)3
In3++n(urea)→[In(urea)n]3+
[In(urea)n]3++3OH-→In(OH)3(urea)m+(n-m)urea。
2. the preparation method of chiasma type indium oxide nanometer material according to claim 1, it is characterised in that the step a
It is middle to add a certain amount of urea, and use absolute ethyl alcohol as solvent, addition 2mL Qula is led in step c, then passes through hydro-thermal
Synthesis and heat-treating methods successfully synthesize the indium oxide gas sensitive of chiasma type.
3. the preparation method of chiasma type indium oxide nanometer material according to claim 1, it is characterised in that the step d
In baking oven temperature be 120 DEG C at, duration 12h.
4. the preparation method of chiasma type indium oxide nanometer material according to claim 1, it is characterised in that the step f
In oven drying temperature be 60 DEG C or so, the dry time is 24h.
5. the preparation method of chiasma type indium oxide nanometer material according to claim 1, it is characterised in that the step g
In Muffle furnace temperature be 500 DEG C, the time of heat treatment is 1h.
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| CN112279296A (en) * | 2020-09-30 | 2021-01-29 | 盐城工学院 | Nano-twin-crystal-phase indium oxide gas-sensitive material and preparation method and application thereof |
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