CN101508462A - Process for producing flower shaped indium hydroxide powder having high specific surface area - Google Patents
Process for producing flower shaped indium hydroxide powder having high specific surface area Download PDFInfo
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- CN101508462A CN101508462A CNA2009100428329A CN200910042832A CN101508462A CN 101508462 A CN101508462 A CN 101508462A CN A2009100428329 A CNA2009100428329 A CN A2009100428329A CN 200910042832 A CN200910042832 A CN 200910042832A CN 101508462 A CN101508462 A CN 101508462A
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Abstract
The invention relates to a method for preparing flower indium hydroxide with high specific surface area, which belongs to the technical field of inorganic material preparing process. The method uses In<3+> water soluble salt as an indium source, urea as an alkali source and sodium dodecyl sulfate as a surfactant to prepare indium hydroxide powder by a hydro-thermal method, wherein the compositions react at a constant temperature for 12 to 24 hours under a low-temperature hydrothermal condition of between 90 and 105 DEG C; and precipitate is obtained through filtration after the reactant is cooled to room temperature, and is washed, centrifugally precipitated and dried to obtain the flower high specific surface area indium hydroxide assembled by nanometer flakes. The method has the advantages that the method prepares the flower indium hydroxide by the low-temperature hydro-thermal method, not only can make crystal sufficiently grow under unrestricted condition with advantages of high specific surface area, controllable appearance and size of the crystal, perfect crystal and the like, but also can obtain powder body with specific surface area of between 20 and 40 m<2>g; and XRD diffraction indicates that a main crystal phase is In(OH)<3> and grows with preferred orientation along (100) direction, and impurity phase is InOOH with content totally less than 12 percent. The system has excellent application prospect in microelectronics, photoelectricity, sensing devices, catalysts, alkaline cells and other fields.
Description
Technical field
The invention belongs to the inorganic material preparation process technical field, particularly relate to the preparation method of the flower-shaped indium hydroxide of high-specific surface area.
Background technology
Indium (In) is an IIIA family element, and for having the low melting point metal of tetragonal structure, it is easy to the III-V family alloy semiconductor of synthesis example such as InN, InGaN, InP and InAs, can be used for making photodiode photoelectric devices such as (LED).In recent years, along with development of science and technology, indium and compound thereof have been widely used in synthetic, the infrared detector of manufacturing, semiconductor material of various alloys and the manufacturing and the industries such as tumour radiotherapy in the clinical medicine and radionuclide-imaging of oscillator.Indium hydroxide is as a kind of compound of indium, can be as the Photodegradation catalyst of hardly degraded organic substances such as benzene and the high-efficiency sustained-release agent in the alkaline cell, the indium tin oxide for preparing after the doped tin (ITO) has high visible light transmissivity and good electrical conductivity and is applied to flat-panel monitor industry based on liquid-crystal display in addition, so the compound of indium has widely in industrial production and daily life and uses.
The method for preparing Indium sesquioxide and indium hydroxide thereof at present both at home and abroad is a lot, mainly contains aqua-solution method, thermal decomposition method, homogeneous coprecipitation method, sol-gel method, hydrothermal method etc.Wherein adopt aqua-solution method (Lu Xinchong etc., patent of invention publication number CN1412117) process characteristic mainly is that the additive that utilize to add is controlled growing up of indium tin hydroxide and obtained high-quality ball shaped nano tin indium oxide powder, but has serious reunion and the particle size range shortcoming such as wide that distributes with the sample of aqua-solution method preparation.The employing thermal decomposition method (Si Dipankatu is rare etc., patent of invention publication number CN176120) process characteristic mainly is the compound of burning indium and tin in oxidizing atmosphere flame, be translated into indium tin composite oxides nanometer spherical powder, but the complicated operating process of this method, condition are difficult to control.In addition, ((clock is promoted culture etc. to adopt the homogeneous coprecipitation method, patent of invention publication number CN1305957), (Song Ning etc., patent of invention publication number CN101214994), (Zhang Jianrong etc., patent of invention publication number CN1775693)) process characteristic is the salts solution of indium metal and metallic tin is dissolved emulsification respectively, co-precipitation behind the thorough mixing, washing is filtered, again oven dry, calcination, quenching at last grinds, spherical powder, though technology is simple, cycle is short, easy to operate, less demanding to equipment, but have outstanding agglomeration in concrete preparation process, available particle active surface is greatly limited.Adopt sol-gel method ((Hu Qilin etc., patent of invention publication number CN101041459), (Zhou Huijuan etc., patent of invention publication number CN1225898)) process characteristic is with the metal alkoxide to be starting raw material, utilize the hydrolysis condensation reaction of alkoxide to form gel network structure, but, be not suitable for preparation technology's requirement of large-scale low-cost because the metal alkoxide of indium tin costs an arm and a leg and is difficult for obtaining.In these methods, hydrothermal method can make crystal fully growth under non-limited condition, has crystal morphology, controlled amount, advantages such as complete crystallization, also control easily of reaction conditions simultaneously.The research of having reported at present that utilizes Hydrothermal Preparation indium hydroxide or Indium sesquioxide seldom, as a kind of preparation method's (accounting for Jinhua etc., patent of invention publication number CN101182031) of indium oxide nano thread ordered collective, this is invented with InCl
3Be raw material, nonpolar alkane is solvent, and amino dodecane, oleic acid are as tensio-active agent, place baking oven in 120-280 ℃ of isothermal reaction 5-40h, product washing, alcohol are washed after drying, obtain the nano thread ordered congeries of InOOH, InOOH obtains In 450-440 ℃ of annealing down
2O
3Nano thread ordered congeries.
More than the preparation-obtained spherical powder of preparation method of relevant indium hydroxide, the less and particle that forms of reuniting of available active surface also is spherical morphology.And also do not have at present the report of the flower-shaped indium hydroxide that high-specific surface area, the controlled nanometer lamella of pattern assemble in the pertinent literature.
Summary of the invention
The object of the present invention is to provide a kind of step simple, the easy to operate method for preparing flower shaped indium hydroxide powder having high specific surface area.
And in order to obtain high-specific surface area, the controlled flower-shaped indium hydroxide of pattern, technical scheme of the present invention is: to contain In
3+The water-soluble inorganic salt brine solution be the indium source, urea (CO (NH
2)
2) be alkali source, sodium lauryl sulphate (SDS) is a tensio-active agent, and above reactant after ultrasonic concussion, is reacted 12-24h sealed reactor 90-105 ℃ of low-temperature hydrothermal; Cold filtration obtains throw out through washing, and centrifugation promptly gets flower-shaped indium hydroxide after the oven dry.
By method of the present invention, the contriver prepares successful high-specific surface area first, pattern is flower shaped indium hydroxide powder having (In (OH)
3), described flower-shaped being meant on the indium hydroxide powder having surface is to assemble the height ratio table by the nanometer lamella to amass, pattern is flower-shaped.Product degree of crystallinity height of the present invention, productive rate height, good dispersity, and presoma obtains In behind 400 ℃ of calcining 1h
2O
3Powder, its floriform appearance remains unchanged.
Contain In
3+The concentration of water-soluble inorganic salt brine solution is preferably 0.01-0.2mol/L.
The tensio-active agent sodium lauryl sulphate, its content is preferably In
3+The 0.5-2 of amount of substance doubly.
Described content of urea is preferably In
3+The 5-7 of amount of substance doubly.
Contain In
3+The water-soluble inorganic salt brine solution be preferably indiumchloride solution or indium nitrate solution.
Temperature rise rate in the reactor is 5-10 ℃/min.
The preparation process that the preparation method of flower shaped indium hydroxide powder having of the present invention is concrete is:
The preparation volumetric molar concentration is the In that contains of 0.01-0.2mol/L
3+The aqueous solution of inorganic salt, (its content is In to add the tensio-active agent sodium lauryl sulphate in the deployed water-soluble salt that contains indium
3+The 0.5-2 of amount of substance is doubly), (content of urea is In as alkali source to add urea again in above-mentioned solution
3+The 5-7 of amount of substance is doubly), ultrasonic then concussion after stirring, is in the stainless steel cauldron of tetrafluoroethylene with the mixed solution liner of packing into, the sealing back is in 90-105 ℃ of low-temperature hydrothermal reaction 12-24h.Take out postcooling to room temperature, the throw out that filtration is obtained is that the mixing solutions of 1:1 washs with the volume ratio of second alcohol and water, centrifugation, and 80-90 ℃ of oven dry promptly obtains flower shaped indium hydroxide powder having.
The invention has the advantages that: the present invention adopts the flower-shaped indium hydroxide of Hydrothermal Preparation, can make crystal fully growth under non-limited condition, have the specific surface area height, crystal morphology, controlled amount, advantages such as complete crystallization, and the BET of the powder that obtains is at 20-40m
2/ g, XRD diffraction show that principal crystalline phase is In (OH)
3And along [100] direction preferred orientation growth, dephasign is that InOOH and content are all less than 12%.This system has good prospects for application in fields such as microelectronics, photoelectricity, susceptible device susceptor, catalyzer, alkaline celies.
Description of drawings
Fig. 1 is the typical SEM photo of the flower-shaped powder of embodiment 1 preparation
Fig. 2 is the typical SEM photo of the flower-shaped powder of embodiment 2 preparations
Fig. 3 is the typical SEM photo of the flower-shaped powder of embodiment 3 preparations
Embodiment
Following examples are intended to illustrate the present invention rather than limitation of the invention further.
Embodiment 1:
The preparation volumetric molar concentration is the aqueous solution 80mL of the indium chloride inorganic salt of 0.01mol/L, adds tensio-active agent sodium lauryl sulphate 0.0008mol, and the urea that adds 0.004mol again is as alkali source.Behind the ultrasonic concussion number minute, be in the stainless steel cauldron of tetrafluoroethylene with the mixed solution 100mL liner of packing into, the sealing back is in 90 ℃ of low-temperature hydrothermal reaction 12h.Take out, be cooled to room temperature, the throw out that filtration is obtained is that the mixing solutions of 1:1 washs with the volume ratio of second alcohol and water, centrifugation, and 80 ℃ of oven dry promptly obtain flower shaped indium hydroxide powder having.The powder BET that obtains is 38m
2/ g, XRD diffraction show and be mainly along [100] direction preferred orientation, and the amount that contains InOOH is 8%.As shown in Figure 1.
Embodiment 2:
The preparation volumetric molar concentration is the indium chloride aqueous solution 80mL of 0.1mol/L, adds 0.008mol sodium lauryl sulphate and 0.048mol urea.Temperature of reaction is 95 ℃, and the reaction times is 18h, and can obtain BET is 31m
2/ g contains InOOH amount and is 10% flower shaped indium hydroxide powder having.All the other are with embodiment 1.As shown in Figure 2.
Embodiment 3:
The preparation volumetric molar concentration is the indium nitrate aqueous solution 80mL of 0.2mol/L, adds 0.032mol sodium lauryl sulphate and 0.112mol urea.Temperature of reaction is 105 ℃, and the reaction times is 24h, and can obtain BET is 23m
2/ g contains InOOH amount and is 11% flower shaped indium hydroxide powder having.All the other are with embodiment 1.As shown in Figure 3.
Claims (6)
1, the preparation method of flower shaped indium hydroxide powder having high specific surface area is characterized in that to contain In
3+The water-soluble inorganic salt brine solution be the indium source, urea is alkali source, sodium lauryl sulphate is a tensio-active agent, with above reactant after ultrasonic concussion, at sealed reactor 90-105 ℃ of low-temperature hydrothermal reaction 12-24h; Cold filtration obtains throw out through washing, and centrifugation promptly gets flower-shaped indium hydroxide after the oven dry.
2, the preparation method of flower shaped indium hydroxide powder having high specific surface area according to claim 1 is characterized in that containing In
3+The concentration of water-soluble inorganic salt is 0.01-0.2mol/L.
3, the preparation method of flower shaped indium hydroxide powder having high specific surface area according to claim 2 is characterized in that the tensio-active agent sodium lauryl sulphate, and its content is 0.5-2 times of In3+ amount of substance.
4,, it is characterized in that described content of urea is In according to the preparation method of each described flower shaped indium hydroxide powder having high specific surface area of claim 1-3
3+The 5-7 of amount of substance doubly.
5, the preparation method of flower shaped indium hydroxide powder having high specific surface area according to claim 1 is characterized in that containing In
3+The water-soluble inorganic salt brine solution be indiumchloride solution or indium nitrate solution.
6, the preparation method of flower shaped indium hydroxide powder having high specific surface area according to claim 1 is characterized in that the temperature rise rate in the reactor is 5-10 ℃/min.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857263A (en) * | 2010-06-23 | 2010-10-13 | 东华大学 | Method for preparing nano indium oxide with controllable appearance by hydrothermal method |
| CN102134092A (en) * | 2011-02-17 | 2011-07-27 | 四川大学 | Simple preparation method of hollow-spherical and flower-shaped indium oxide with secondary structure and application |
| CN102826593A (en) * | 2012-09-11 | 2012-12-19 | 电子科技大学 | Preparation method for indium oxide nanometer material |
| CN103241767A (en) * | 2012-10-26 | 2013-08-14 | 河南圣玛斯光电科技有限公司 | Microemulsion-solvothermal technique of orthorhombic InOOH |
| CN105664973A (en) * | 2016-02-26 | 2016-06-15 | 大连理工大学 | Three-dimensional flower-like In2S3/In2O3 composite microsphere photocatalytic material and preparation method thereof |
| CN107827148A (en) * | 2017-11-21 | 2018-03-23 | 临沂大学 | A kind of chiasma type indium oxide nanometer material preparation method |
| CN110436514A (en) * | 2018-05-05 | 2019-11-12 | 北京化工大学 | The preparation method and application of transition metal element doped flower-shaped indium oxide gas sensitive |
| CN113877556A (en) * | 2021-10-18 | 2022-01-04 | 常州大学 | Indium oxyhydroxide/modified attapulgite photocatalytic composite material and preparation method and application thereof |
-
2009
- 2009-03-11 CN CNA2009100428329A patent/CN101508462A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857263A (en) * | 2010-06-23 | 2010-10-13 | 东华大学 | Method for preparing nano indium oxide with controllable appearance by hydrothermal method |
| CN102134092A (en) * | 2011-02-17 | 2011-07-27 | 四川大学 | Simple preparation method of hollow-spherical and flower-shaped indium oxide with secondary structure and application |
| CN102134092B (en) * | 2011-02-17 | 2013-03-27 | 四川大学 | Simple preparation method of hollow-spherical and flower-shaped indium oxide with secondary structure and application |
| CN102826593A (en) * | 2012-09-11 | 2012-12-19 | 电子科技大学 | Preparation method for indium oxide nanometer material |
| CN103241767A (en) * | 2012-10-26 | 2013-08-14 | 河南圣玛斯光电科技有限公司 | Microemulsion-solvothermal technique of orthorhombic InOOH |
| CN103241767B (en) * | 2012-10-26 | 2014-12-24 | 河南圣玛斯光电科技有限公司 | Microemulsion-solvothermal technique of orthorhombic InOOH |
| CN105664973A (en) * | 2016-02-26 | 2016-06-15 | 大连理工大学 | Three-dimensional flower-like In2S3/In2O3 composite microsphere photocatalytic material and preparation method thereof |
| CN107827148A (en) * | 2017-11-21 | 2018-03-23 | 临沂大学 | A kind of chiasma type indium oxide nanometer material preparation method |
| CN107827148B (en) * | 2017-11-21 | 2019-11-15 | 临沂大学 | A kind of chiasma type indium oxide nanometer material preparation method |
| CN110436514A (en) * | 2018-05-05 | 2019-11-12 | 北京化工大学 | The preparation method and application of transition metal element doped flower-shaped indium oxide gas sensitive |
| CN113877556A (en) * | 2021-10-18 | 2022-01-04 | 常州大学 | Indium oxyhydroxide/modified attapulgite photocatalytic composite material and preparation method and application thereof |
| CN113877556B (en) * | 2021-10-18 | 2023-01-17 | 常州大学 | Indium oxyhydroxide/modified attapulgite photocatalytic composite material and preparation method and application thereof |
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