CN107827148B - 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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- CN107827148B CN107827148B CN201711162647.4A CN201711162647A CN107827148B CN 107827148 B CN107827148 B CN 107827148B CN 201711162647 A CN201711162647 A CN 201711162647A CN 107827148 B CN107827148 B CN 107827148B
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Abstract
The invention discloses a kind of chiasma type indium oxide nanometer material preparation methods, and preparing raw material is inidum chloride (InCl3·4H2O), Qula leads to (Triton x-100), dehydrated alcohol (CH3CH2) and urea (CO (NH OH2)2), preparation methods steps are as follows: a. obtains urea liquid；B. indiumchloride solution is obtained；C. above-mentioned urea liquid and indiumchloride solution are mixed and under agitation leads to 2mL Qula and be add to the above mixed solution and be sufficiently stirred；D. the above-mentioned solution of acquisition is transferred in reaction kettle, then reaction kettle is moved into baking oven, taken out after sustained response 12h at 120 DEG C.After reaction kettle natural cooling, centrifugal treating is successively washed repeatedly with deionized water and dehydrated alcohol.The present invention leads to this structure directing agent by the way that Qula is added, 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 technique
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 the metal oxide semiconductor material of different morphologies and structure, in the material of many patterns and structure
In material, there is the metal oxide semiconductor material of the labyrinths such as 3 D stereo shape to attract the attention of people and study emerging
Interest, this, which is primarily due to this three-dimensional structure, can significantly improve the contact area of material Yu other substances, 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, and it is aobvious to be widely used in solar battery, gas sensor, plate
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 chemical precipitation method, aqueous solvent thermal method, organic solution synthetic method, hot injection method, sol-gel method, microemulsion method, thermal evaporation oxygen
Change method, electric arc put method etc..
Traditional chemical method the problem is that: severe reaction conditions, cost are excessively high, it is difficult to large-scale production；It obtains
Indium oxide product is easy to reunite；Reaction temperature requires high, control difficulty, inconvenient for operation；And obtained indium oxide is to gas
Air-sensitive performance it is relatively low, reduce the using effect of indium oxide nanometer material.
Summary of the invention
The present invention provides a kind of chiasma type indium oxide for the deficiency in existing indium oxide nanometer material technology of preparing
Preparation method of nano material.
The present invention is to solve above-mentioned technical deficiency, uses a kind of novel technical solution, is successfully prepared out a kind of friendship
Forked type indium oxide nanometer material, preparing raw material is 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 dehydrated alcohol under stirring, it is complete is stirred well to urea
Dissolution；
B. a certain amount of InCl is weighed3·4H2O is placed in small beaker, and 10mL deionized water is then added, continues stirring until
InCl3·4H2O is completely dissolved, and obtains colorless and transparent InCl3·4H2O solution；
C. InCl is added under stirring in urea liquid3·4H2In O solution and be sufficiently stirred 30min obtain mixing it is molten
Then 2mL Qula is led to and is add to the above mixed solution by liquid, continue for stirring 20min；
D. finally the solution of acquisition will be transferred in 100mL polytetrafluoroethyllining lining stainless steel cauldron, by reaction kettle
It moves into baking oven, is taken out after sustained response 12h at 120 DEG C；
E. after reaction kettle natural cooling, by the product centrifugation in reaction kettle and then successively with deionized water and anhydrous second
Alcohol washs repeatedly to remove possible foreign ion；
F. white powder is then obtained for 24 hours place the product in dry at 60 DEG C in baking oven, be labeled as In (OH)3(t)；
G. the white powder of acquisition is placed in Muffle furnace, is heat-treated 1h under slow ascending temperature to 500 DEG C of air conditions
The indium oxide nanometer material with good dispersion is synthesized, product labelling obtained is In after heat treatment2O3(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 invention, a certain amount of urea is added in the step a, and using anhydrous
For ethyl alcohol as solvent, the Qula that 2mL is added in selected c is logical, then is successfully synthesized by hydrothermal synthesis and heat-treating methods
The indium oxide gas sensitive of chiasma type.
As a kind of preferred embodiment of the 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 invention, the temperature of the oven drying in the step f is 60 DEG C or so, is done
The dry time is for 24 hours.
The temperature of Muffle furnace in the step g is 500 DEG C, and the time of heat treatment is 1h.
The beneficial effects obtained by the present invention are as follows being: the present invention is that raw material slowly supplies OH by selecting urea-, Qula is added
Lead to this structure directing agent, then successfully synthesizes the indium oxide gas of chiasma type with simple hydrothermal synthesis and heat-treating methods
Quick material finds that urea and Qula work with the formation to chiasma type indium oxide in all, by the chiasma type of acquisition in an experiment
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.
Detailed description of the invention
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 map；
Fig. 4 is In of the present invention2O3(t) hum patterns such as scale topography.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description.
A kind of chiasma type indium oxide nanometer material preparation method, preparing raw material is inidum chloride (InCl3·4H2) and urea O
(CO(NH2)2), steps are as follows for preparation method:
A. a certain amount of urea is added in 120mL dehydrated alcohol under stirring, it is complete is stirred well to urea
Dissolution；
B. a certain amount of InCl is weighed3·4H2O is placed in small beaker, and 10mL deionized water is then added, continues stirring until
InCl3·4H2O is completely dissolved, and obtains colorless and transparent InCl3·4H2O solution；
C. InCl is added under stirring in urea liquid3·4H2In O solution and be sufficiently stirred 30min obtain mixing it is molten
Then 2mL Qula is led to and is add to the above mixed solution by liquid, continue for stirring 20min；
D. finally the solution of acquisition will be transferred in 100mL polytetrafluoroethyllining lining stainless steel cauldron, by reaction kettle
It moves into baking oven, is taken out after sustained response 12h at 120 DEG C；
E. after reaction kettle natural cooling, the product centrifugation in reaction kettle, washing, ethyl alcohol are washed repeatedly possible to remove
Foreign ion；
F. it is then labeled as In (OH) place the product in white powder is obtained in baking oven3(t)；
G. the white powder of acquisition is placed in Muffle furnace, is heat-treated 1h under slow ascending temperature to 500 DEG C of air conditions
The indium oxide nanometer material with good dispersion is synthesized, product labelling obtained is In after heat treatment2O3(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 dehydrated alcohol, and the song of 2mL is added in the step c
It draws and leads to, then successfully synthesize the indium oxide gas sensitive of chiasma type by hydrothermal synthesis 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 for 24 hours.
The temperature of Muffle furnace in the step g is 500 DEG C, and the time of heat treatment is 1h.
For information such as the structure compositions that obtains final product, product X-ray diffraction is subjected to first and Raman is surveyed
Examination: final product according to Fig. 12O3(t) X ray diffracting spectrum, 2 θ range of X-ray diffraction scanning angle 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 °
It Dui Yingyu not In2O3(211), (222), (400), (411), (332), (431), (440), (611), (541), (622),
(631) and (444) crystal face.Wherein (222) diffraction maximum is relatively stronger and sharp, this illustrates crystal edge [111] direction preferential growth,
All diffraction maximums with cubic phase In2O3The standard diagram of (JCPDS No.06-0416) is completely the same, can from figure
Out: the peak shape of diffraction maximum is more sharp, does not find the presence of extra miscellaneous peak, shows that prepared product crystallinity is higher, purity
Preferably；It is In (OH) according to Fig.2,3(t) X-ray diffracting spectrum, 2 θ of X-ray diffraction scanning angle are 20 to 80 ° of figures
In be located 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 cubic phase In (OH)3The standard diagram of (JCPDS No.76-1463) is consistent；According to
It is In shown in Fig. 32O3(t) Raman map, You Tuzhong are clear that In2O3(t) five characteristic peak (132cm-1,
305cm-1, 365cm-1, 494cm-1And 630cm-1), these peaks and c-In2O3Middle InO6In-O vibration peak it is corresponding, the above knot
Fruit shows the In of the cubic phase 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 is In2O3(t) the field emission scanning electron microscope figure under different amplification；It can be with from Fig. 4-a
Find out, experiment obtains the In of a large amount of chiasma types2O3A region in figure is amplified according to different multiples and is obtained by material
Obtain Fig. 4-b and 4-c；It can be seen that product obtained from Fig. 4-b and 4-c to support each other dispersion, pattern is different, overall dimensions
At 5 μm or so, these interference type arrangements are by rodlike In2O3Composition, these rodlike In2O3Material diameter between 200-500nm,
Length is between 1-10 μm；Fig. 4-d is partial enlarged view, can see the mutual support stack of crystal together from Fig. 4-d, this
Gap not of uniform size abundant is formed between a little crystal, this gap is conducive to the diffusion and exchange of gas molecule, so that bottom
Layer crystal body also more quickly can adequately touch under test gas；Fig. 4-e and 4-f is In2O3The transmission electron microscope map of crystal；
The pattern due to this chiasma type can be more intuitive to see from Fig. 4-e, mutually propped up between crystal by the point contacted with each other
It supports and is unable to dense accumulation (lower half portion black portions are Electronic Speculum copper mesh edges in figure) together；Fig. 4-f is single typical
Chiasma type In2O3Structure, while which plays itself, itself all face can effectively reach gas；
In addition, the structure of this chiasma type can also prevent material from putting due to higher surface energy in storage because of the supporting role of itself
Occur agglomeration during setting, preferably maintains the dispersibility of itself.
Chiasma type indium oxide nanometer material preparation method in the present embodiment leads to this structure directing by the way that Qula is added
Agent, then the indium oxide gas sensitive of chiasma type is successfully synthesized with simple hydrothermal synthesis and heat-treating methods, it is testing
Middle discovery urea and Qula work 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 foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (1)
1. a kind of chiasma type indium oxide nanometer material preparation method, which is characterized in that preparing raw material is inidum chloride (InCl3·
4H2) and urea (CO (NH O2)2), and Qula has been selected to lead to (Triton x-100) as structure directing agent, preparation method step
It is as follows:
A. a certain amount of urea is added in 120mL dehydrated alcohol 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, and 10mL deionized water is then added, continues stirring until
InCl3·4H2O is completely dissolved, and obtains colorless and transparent InCl3·4H2O solution；
C. InCl is added under stirring in urea liquid3·4H2In O solution and be sufficiently stirred 30min obtain mixed solution,
Then 2mL Qula is led to and is add to the above mixed solution, continue for stirring 20min；
D. finally the solution of acquisition will be transferred in 100mL polytetrafluoroethyllining lining stainless steel cauldron, reaction kettle is moved into
In baking oven, taken out after sustained response 12h at 120 DEG C；
E. after reaction kettle natural cooling, the product centrifugation in reaction kettle, washing, ethyl alcohol are washed repeatedly to remove possible impurity
Ion；
F. white powder is then obtained for 24 hours place the product in dry at 60 DEG C in baking oven, be 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 conditions
Indium oxide nanometer material with good dispersion, product labelling obtained is In after heat treatment2O3(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。
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| CN112279296B (en) * | 2020-09-30 | 2023-11-07 | 盐城工学院 | Nanometer bicrystal phase indium oxide gas-sensitive material, preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508462A (en) * | 2009-03-11 | 2009-08-19 | 长沙理工大学 | Process for producing flower shaped indium hydroxide powder having high specific surface area |
| CN101857263A (en) * | 2010-06-23 | 2010-10-13 | 东华大学 | Method for preparing nano indium oxide with controllable appearance by hydrothermal method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508462A (en) * | 2009-03-11 | 2009-08-19 | 长沙理工大学 | Process for producing flower shaped indium hydroxide powder having high specific surface area |
| CN101857263A (en) * | 2010-06-23 | 2010-10-13 | 东华大学 | Method for preparing nano indium oxide with controllable appearance by hydrothermal method |
Non-Patent Citations (2)
| Title |
|---|
| Effect of sintering temperature on structural and optical properties of indium(Ⅲ) oxide nanoparticles prepared with Triton X-100 by hydrothermal method;D.Selvakumar et al.;《Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy》;20140605;全文 * |
| Lotus-Root-Like In2O3 Nanostructures: Fabrication, Characterization, and Photoluminescence Properties;Cuiqing Wang et al.;《J. Phys. Chem. C》;20071231;全文 * |
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Denomination of invention: A preparation method of cross indium oxide nano material Effective date of registration: 20211210 Granted publication date: 20191115 Pledgee: Industrial and Commercial Bank of China Limited Lanling sub branch Pledgor: Shandong Shengyang Rubber Plastic Co.,Ltd. Registration number: Y2021980014615 |