CN102897821A - Preparation method for cubic-phase Sm2O3 nanorod semiconductor material - Google Patents

Preparation method for cubic-phase Sm2O3 nanorod semiconductor material Download PDF

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CN102897821A
CN102897821A CN2012104018823A CN201210401882A CN102897821A CN 102897821 A CN102897821 A CN 102897821A CN 2012104018823 A CN2012104018823 A CN 2012104018823A CN 201210401882 A CN201210401882 A CN 201210401882A CN 102897821 A CN102897821 A CN 102897821A
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cubic
semiconductor material
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preparation
deionized water
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殷立雄
黄剑锋
郝巍
李嘉胤
吴建鹏
曹丽云
费杰
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a preparation method for cubic-phase Sm2O3 nanorod semiconductor material, which comprises the following steps of: adding analytically-pure Sm(NO3)3.6H2O into deionized water; stirring to obtain solution A; regulating the pH (potential of hydrogen) value of the solution A to 6-12 by NaOH solution to form precursor solution; pouring the precursor solution into a hydrothermal kettle; sealing the hydrothermal kettle; putting the hydrothermal kettle into an electrothermal blowing dry box; after heating and pressurizing reaction is finished, naturally cooling to the room temperature; taking out a product; washing by deionized water, and carrying out centrifugal separation; washing by absolute ethyl alcohol; carrying out centrifugal separation; and after repeatedly washing by the deionized water and the absolute ethyl alcohol successively, drying to obtain the cubic-phase Sm2O3 nanorod semiconductor material.

Description

A kind of Emission in Cubic Sm 2O 3The preparation method of nanometer rod semiconductor material
Technical field
The present invention relates to a kind of preparation method of semiconductor material, be specifically related to a kind of Emission in Cubic Sm 2O 3The preparation method of nanometer rod semiconductor material.
Background technology
Sm 2O 3Be a kind of pale yellow powder, easily deliquescence is water insoluble, is soluble in the material of mineral acid.Sm 2O 3Conversion of energy material, semiconductor material and the high performance catalyst material of a new generation.Nanometer Sm 2O 3Can also be used for ceramic condenser.Aspect magneticsubstance, nanometer Sm 2O 3Mainly for the preparation of rare earth permanent-magnetic material; In addition Sm 2O 3Film also can be used in the spectral filter of electronics body, magneticsubstance and special glass, has wide development prospect should be arranged.
Sm 2O 3Crystal has three kinds of crystal formations, belongs to the oxide compound of polycrystalline inversion of phases, is the monocline crystalline phase under the room temperature, is faint yellow semi-conductor at normal temperatures and pressures, and its fusing point is 2269 ℃, and boiling point is 3507 ℃.When temperature was higher than 850 ℃, the monocline crystalline phase changed a cube crystalline phase into, became the hexagonal crystal phase at 2000 ℃ of left/right rotations.Transformation Sm along with crystal formation 3+Ground state certain variation has occured, thereby cause the performance of Samarium trioxide that variation has occured.These special structures can produce some novel characteristics aspect magnetics, electricity and the optics, thereby have also caused greatly research enthusiasm of people.
The preparation Sm that reports at present 2O 3Method be mainly the low temperature self-propagating combustion method [Bao Lili, Yang Wu, Ni Gang, He Xiaoyan, Lv Weilian. the standby nanometer Sm of low temperature self-propagating combustion legal system 2O 3, Northwest Normal University's journal 2005,41 (5): 40-42]; Sol-gel method [Deng Gengfeng. Zhong Shumei. Chen Huihuang. Zhou Xiaohua. sol-gel method prepares the technical study of ultra-fine Samarium trioxide, rare earth 2007,28 (2): 40-42] and microemulsion method [Geng Shou flower red legend celebrating Chang Pengmei Chen Ya Chinese herbaceous peony. nanometer Sm in the reverse microemulsion liquid medium 2O 3Preparation, 2008,24 (9): 1609-1614]; Also have solid sintering technology [Yanglong Hou, Zhichuan Xu, Sheng Peng, Chuanbing Rong, J.Ping Liu, Shouheng Sun, A Facile Synthesis of SmCo 5Magnets from Core/Shell Co/Sm 2O 3Nanoparticles, 2007,19:3349 – 3352].Low temperature self-propagating combustion method and sol-gel method are the synthetic Sm of high temperature under oxygen atmosphere 2O 3, powder easily reunite and the process cycle of sol-gel long, to Sm 2O 3The utilization ratio of raw material is very little; And solid sintering technology is sintering under the reducing atmosphere condition, also can cause nanocrystalline reunion, the particle abnormal growth.The prepared precursor of microemulsion method also needs could obtain Sm through high-temperature heat treatment simultaneously 2O 3Nanocrystalline, so easy introducing impurity, and powder is easily reunited.In order to reach practical purpose, must the low and convenient feasible Sm of Development and Production cost 2O 3Nanocrystalline preparation technology.Other has report to prepare Sm with microwave-hydrothermal method 2O 3Nanocrystalline [Yin Lixiong, Huang Jianfeng, Cao Liyun etc. a kind of microwave-hydrothermal method prepares Sm 2O 3The method of nano-powder [P]. Chinese patent: 200910021192.], also have [Huang Jianfeng, Xia Changkui, Cao Liyun etc. a kind of method of making ZnO nanometer rod [P]. Chinese patent: 200710019174.2].
Summary of the invention
The object of the present invention is to provide a kind of equipment simple, easily control, and more simple to operate than microwave-hydrothermal method and solvent-thermal method, security is good, cheaply synthesis of cubic phase Sm 2O 3The hydrothermal method of nanometer rod prepares Sm 2O 3The method of nano bar-shape structure.
For achieving the above object, the preparation method that the present invention adopts is as follows:
1) with analytical pure Sm (NO 3) 36H 2O adds deionized water for stirring and makes Sm 3+Concentration is the solution A of 0.1 ~ 1.5mol/L;
2) solution A being adopted the pH value of NaOH solution regulator solution A 35 ~ 50 ℃ of heated and stirred is 6 ~ 12, continues to stir the formation precursor aqueous solution;
3) precursor aqueous solution is poured in the water heating kettle, compactedness is controlled at 50～60%, then seals water heating kettle, put it in the electric drying oven with forced convection, the control hydrothermal temperature is 160～240 ℃, and pressure is 2～20MPa, reacted 6～72 hours, reaction naturally cools to room temperature after finishing;
4) open water heating kettle, take out product with deionized water wash and centrifugation, with absolute ethanol washing and centrifugation, the electric vacunm drying case inner drying that adopts successively deionized water and dehydrated alcohol repeated washing to be placed on 45～65 ℃ for 4～6 times namely obtains Emission in Cubic Sm again 2O 3The nanometer rod semiconductor material.
Magnetic stirrer is adopted in the stirring of described step 1).
The concentration of described NaOH solution is 1～5mol/L.
Described electric drying oven with forced convection adopts DHG-9075A type electric drying oven with forced convection.
Described electric vacunm drying case adopts ZKF030 type electric vacunm drying case.
Because the present invention prepares Sm 2O 3The nanometer rod reaction is once finished in liquid phase, does not need the crystallization and thermal treatment in later stage, thereby has avoided Sm 2O 3The defectives such as impurity are introduced in the reunion that nanometer rod may cause in heat treatment process, grain coarsening and atmosphere reaction, and processing unit is simple.The reunion degree is lighter, the suitable stoichiometric ratio that is easy to get, the Sm of the single cubic phase of grain morphology 2O 3Nanometer rod; Can use more cheap raw material; Save high-temperature calcination and ball milling, avoided impurity to introduce and textural defect.Prepared Sm 2O 3Nanometer rod purity is high, good dispersity, and crystal formation is single, and grain growing is controlled.
The more important thing is that equipment and instrument that hydrothermal method requires are more simple, adopt water as solvent, green, cleaning, harmless and be more conducive to nanometer Sm 2O 3Preferred orientation growth, so more economic, practical.The crystal grain of preparing is grown complete, and pattern is single, and particle diameter is very little and be evenly distributed the nanometer rod that purity is higher.Prepared nanocrystallinely show certain oriented growth trend, and nanocrystalline ultraviolet ray is had the strong absorption effect and visible light is had strong anti-reflection effect.And utilize hydrothermal method simpler than solvent-thermal method, safe and reliable, feasibility is strong and can more be conducive to nanocrystalline oriented growth.
Description of drawings
Fig. 1 is the prepared Emission in Cubic Sm of the present invention 2O 3The XRD figure of nanometer rod;
Fig. 2 is the prepared Emission in Cubic Sm of the present invention 2O 3The SEM figure of nanometer rod.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail.
Embodiment 1:
1) with analytical pure Sm (NO 3) 36H 2Adopt magnetic stirrer to make Sm in the O adding deionized water 3+Concentration is the solution A of 0.5mol/L;
2) the pH value that is the NaOH solution regulator solution A of 1mol/L with solution A 40 ℃ of heated and stirred employing concentration is 6, continues to stir 1 hour formation precursor aqueous solution;
3) precursor aqueous solution is poured in the water heating kettle, compactedness is controlled at 50%, then seals water heating kettle, put it in the DHG-9075A type electric drying oven with forced convection, the control hydrothermal temperature is 180 ℃, and pressure is 8MPa, reacted 48 hours, reaction naturally cools to room temperature after finishing;
4) open water heating kettle, take out product with deionized water wash and centrifugation, with absolute ethanol washing and centrifugation, the ZKF030 type electric vacunm drying case inner drying that adopts successively deionized water and dehydrated alcohol repeated washing to be placed on 50 ℃ for 6 times namely obtains Emission in Cubic Sm again 2O 3The nanometer rod semiconductor material.
Embodiment 2:
1) with analytical pure Sm (NO 3) 36H 2Adopt magnetic stirrer to make Sm in the O adding deionized water 3+Concentration is the solution A of 0.2mol/L;
2) the pH value that is the NaOH solution regulator solution A of 2mol/L with solution A 35 ℃ of heated and stirred employing concentration is 9, continues to stir 1.5 hours formation precursor aqueous solutions;
3) precursor aqueous solution is poured in the water heating kettle, compactedness is controlled at 55%, then seals water heating kettle, put it in the DHG-9075A type electric drying oven with forced convection, the control hydrothermal temperature is 200 ℃, and pressure is 15MPa, reacted 60 hours, reaction naturally cools to room temperature after finishing;
4) open water heating kettle, take out product with deionized water wash and centrifugation, with absolute ethanol washing and centrifugation, the ZKF030 type electric vacunm drying case inner drying that adopts successively deionized water and dehydrated alcohol repeated washing to be placed on 55 ℃ for 4 times namely obtains Emission in Cubic Sm again 2O 3The nanometer rod semiconductor material.
Embodiment 3:
1) with analytical pure Sm (NO 3) 36H 2Adopt magnetic stirrer to make Sm in the O adding deionized water 3+Concentration is the solution A of 0.1mol/L;
2) the pH value that is the NaOH solution regulator solution A of 3.5mol/L with solution A 45 ℃ of heated and stirred employing concentration is 10, continues to stir 2 hours formation precursor aqueous solutions;
3) precursor aqueous solution is poured in the water heating kettle, compactedness is controlled at 50%, then seals water heating kettle, put it in the DHG-9075A type electric drying oven with forced convection, the control hydrothermal temperature is 160 ℃, and pressure is 20MPa, reacted 72 hours, reaction naturally cools to room temperature after finishing;
4) open water heating kettle, take out product with deionized water wash and centrifugation, with absolute ethanol washing and centrifugation, the ZKF030 type electric vacunm drying case inner drying that adopts successively deionized water and dehydrated alcohol repeated washing to be placed on 45 ℃ for 5 times namely obtains Emission in Cubic Sm again 2O 3The nanometer rod semiconductor material.
Embodiment 4:
1) with analytical pure Sm (NO 3) 36H 2Adopt magnetic stirrer to make Sm in the O adding deionized water 3+Concentration is the solution A of 1mol/L;
2) the pH value that is the NaOH solution regulator solution A of 4mol/L with solution A 50 ℃ of heated and stirred employing concentration is 11, continues to stir 2.5 hours formation precursor aqueous solutions;
3) precursor aqueous solution is poured in the water heating kettle, compactedness is controlled at 50%, then seals water heating kettle, put it in the DHG-9075A type electric drying oven with forced convection, the control hydrothermal temperature is 220 ℃, and pressure is 18MPa, reacted 36 hours, reaction naturally cools to room temperature after finishing;
4) open water heating kettle, take out product with deionized water wash and centrifugation, with absolute ethanol washing and centrifugation, the ZKF030 type electric vacunm drying case inner drying that adopts successively deionized water and dehydrated alcohol repeated washing to be placed on 50 ℃ for 6 times namely obtains Emission in Cubic Sm again 2O 3The nanometer rod semiconductor material.
Embodiment 5:
1) with analytical pure Sm (NO 3) 36H 2Adopt magnetic stirrer to make Sm in the O adding deionized water 3+Concentration is the solution A of 0.8mol/L;
2) the pH value that is the NaOH solution regulator solution A of 4.5mol/L with solution A 45 ℃ of heated and stirred employing concentration is 12, continues to stir 3 hours formation precursor aqueous solutions;
3) precursor aqueous solution is poured in the water heating kettle, compactedness is controlled at 60%, then seals water heating kettle, put it in the DHG-9075A type electric drying oven with forced convection, the control hydrothermal temperature is 230 ℃, and pressure is 10MPa, reacted 24 hours, reaction naturally cools to room temperature after finishing;
4) open water heating kettle, take out product with deionized water wash and centrifugation, with absolute ethanol washing and centrifugation, the ZKF030 type electric vacunm drying case inner drying that adopts successively deionized water and dehydrated alcohol repeated washing to be placed on 60 ℃ for 6 times namely obtains Emission in Cubic Sm again 2O 3The nanometer rod semiconductor material.
Embodiment 6:
1) with analytical pure Sm (NO 3) 36H 2Adopt magnetic stirrer to make Sm in the O adding deionized water 3+Concentration is the solution A of 1.5mol/L;
2) the pH value that is the NaOH solution regulator solution A of 5mol/L with solution A 40 ℃ of heated and stirred employing concentration is 7, continues to stir 1.5 hours formation precursor aqueous solutions;
3) precursor aqueous solution is poured in the water heating kettle, compactedness is controlled at 55%, then seals water heating kettle, put it in the DHG-9075A type electric drying oven with forced convection, the control hydrothermal temperature is 240 ℃, and pressure is 2MPa, reacted 6 hours, reaction naturally cools to room temperature after finishing;
4) open water heating kettle, take out product with deionized water wash and centrifugation, with absolute ethanol washing and centrifugation, the ZKF030 type electric vacunm drying case inner drying that adopts successively deionized water and dehydrated alcohol repeated washing to be placed on 65 ℃ for 6 times namely obtains Emission in Cubic Sm again 2O 3The nanometer rod semiconductor material.
The prepared Sm of the present invention as seen from Figure 1 2O 3Nanometer rod purity is high, and diffraction peak is more sharp-pointed, and is single Emission in Cubic Sm 2O 3, with the JCPDS 74-1807Sm of standard 2O 3Card matches.
The prepared Emission in Cubic Sm of the present invention as seen from Figure 2 2O 3Nanometer rod, particle is little and be evenly distributed, and it is lighter to reunite, and presents tiny corynebacterium pattern.

Claims (5)

1. Emission in Cubic Sm 2O 3The preparation method of nanometer rod semiconductor material: it is characterized in that may further comprise the steps:
1) with analytical pure Sm (NO 3) 36H 2O adds deionized water for stirring and makes Sm 3+Concentration is the solution A of 0.1 ~ 1.5mol/L;
2) solution A being adopted the pH value of NaOH solution regulator solution A 35 ~ 50 ℃ of heated and stirred is 6 ~ 12, continues to stir the formation precursor aqueous solution;
3) precursor aqueous solution is poured in the water heating kettle, compactedness is controlled at 50～60%, then seals water heating kettle, put it in the electric drying oven with forced convection, the control hydrothermal temperature is 160～240 ℃, and pressure is 2～20MPa, reacted 6～72 hours, reaction naturally cools to room temperature after finishing;
4) open water heating kettle, take out product with deionized water wash and centrifugation, with absolute ethanol washing and centrifugation, the electric vacunm drying case inner drying that adopts successively deionized water and dehydrated alcohol repeated washing to be placed on 45～65 ℃ for 4～6 times namely obtains Emission in Cubic Sm again 2O 3The nanometer rod semiconductor material.
2. Emission in Cubic Sm according to claim 1 2O 3The preparation method of nanometer rod semiconductor material: it is characterized in that: magnetic stirrer is adopted in the stirring of described step 1).
3. Emission in Cubic Sm according to claim 1 2O 3The preparation method of nanometer rod semiconductor material: it is characterized in that: the concentration of described NaOH solution is 1～5mol/L.
4. Emission in Cubic Sm according to claim 1 2O 3The preparation method of nanometer rod semiconductor material: it is characterized in that: described electric drying oven with forced convection adopts DHG-9075A type electric drying oven with forced convection.
5. Emission in Cubic Sm according to claim 1 2O 3The preparation method of nanometer rod semiconductor material: it is characterized in that: described electric vacunm drying case adopts ZKF030 type electric vacunm drying case.
CN2012104018823A 2012-10-19 2012-10-19 Preparation method for cubic-phase Sm2O3 nanorod semiconductor material Pending CN102897821A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2020204490A (en) * 2019-06-14 2020-12-24 富士電機株式会社 Carbon dioxide gas sensor

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Publication number Priority date Publication date Assignee Title
CN102330081A (en) * 2011-10-13 2012-01-25 陕西科技大学 Method for preparing Sm2O3 film by solvent heat method
CN102432056A (en) * 2011-10-13 2012-05-02 陕西科技大学 Method for preparing Sm2O3 nano crystals by solvent thermal method
CN102502793A (en) * 2011-11-23 2012-06-20 陕西科技大学 Preparation method of rod-shaped SnS nanocrystals

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102330081A (en) * 2011-10-13 2012-01-25 陕西科技大学 Method for preparing Sm2O3 film by solvent heat method
CN102432056A (en) * 2011-10-13 2012-05-02 陕西科技大学 Method for preparing Sm2O3 nano crystals by solvent thermal method
CN102502793A (en) * 2011-11-23 2012-06-20 陕西科技大学 Preparation method of rod-shaped SnS nanocrystals

Non-Patent Citations (1)

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Title
殷立雄: "Sm2O3微晶的水热与溶剂热法制备工艺、结构与性能关系研究", 《陕西科技大学博士学位论文》, 3 September 2012 (2012-09-03), pages 23 - 28 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2020204490A (en) * 2019-06-14 2020-12-24 富士電機株式会社 Carbon dioxide gas sensor
JP7389960B2 (en) 2019-06-14 2023-12-01 富士電機株式会社 carbon dioxide gas sensor

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Application publication date: 20130130