CN102897818A - Method for preparing Sm2O3 semiconductor nanocrystals with hexagonal sheet structures - Google Patents

Method for preparing Sm2O3 semiconductor nanocrystals with hexagonal sheet structures Download PDF

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CN102897818A
CN102897818A CN201210401417XA CN201210401417A CN102897818A CN 102897818 A CN102897818 A CN 102897818A CN 201210401417X A CN201210401417X A CN 201210401417XA CN 201210401417 A CN201210401417 A CN 201210401417A CN 102897818 A CN102897818 A CN 102897818A
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solution
aqueous solution
sm2o3
precursor aqueous
flake structure
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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 method for preparing Sm2O3 semiconductor nanocrystals with hexagonal sheet structures. The method comprises the following steps of: adding analytically pure SmCl3.6H2O into isopropanol to obtain a solution A; adjusting the pH value of the solution A to be 7 to 12 by using a NaOH solution to obtain a precursor solution, and adding cetyl trimethyl ammonium bromide (CTAB) into the precursor solution; pouring the precursor solution into a hydrothermal kettle, sealing the hydrothermal kettle, controlling hydrothermal temperature to be 120 to 200 DEG C and pressure to be 2 to 20MPa, reacting for 6 to 60 hours, and after reaction, naturally cooling to room temperature; and taking a product out, washing the product by using absolute ethanol, performing centrifugal separation, repeating for multiple times, and drying to obtain the Sm2O3 semiconductor nanocrystals with the hexagonal sheet structures. According to the method, the reaction for preparing the Sm2O3 nanocrystals with the hexagonal sheet structures is finished in a liquid phase at one time, and the later-stage crystallization thermal treatment is not required, so that the defects that agglomeration and grain coarsening which are caused in the thermal treatment process of the Sm2O3 nanocrystals, and impurities are introduced by atmosphere reaction can be avoided.

Description

A kind of hexagonal flake structure Sm 2O 3The preparation method of semiconductor nano
Technical field
The present invention relates to a kind of Sm 2O 3Nanocrystalline preparation method, particularly a kind of solvent-thermal method prepares hexagonal flake structure Sm 2O 3The method of semiconductor nano.
Background technology
Sm 2O 3Be a kind of pale yellow powder, easily deliquescence is water insoluble, is soluble in 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 Shouhua, the 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, Advanced Materials 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.
Summary of the invention
The object of the present invention is to provide a kind of equipment simple, easily control, and lower than microwave-hydrothermal method and common hydrothermal method temperature, required pressure more easily obtains, and can control to generate specific pattern, cheaply hexagonal flake structure Sm 2O 3The preparation method of semiconductor nano.The Sm that makes by preparation method of the present invention 2O 3Nanocrystalline purity is high, good dispersity, and crystal formation is single, and grain growing is controlled.
For achieving the above object, the technical solution used in the present invention is:
1) with analytically pure SmCl 36H 2Stir in the O adding Virahol and make Sm 3+Concentration is the solution A of 0.2 ~ 1.5mol/L;
2) solution A being adopted the pH value of NaOH solution regulator solution A 45 ~ 55 ℃ of heated and stirred is 7 ~ 12, continues to stir to form precursor aqueous solution, adds CTAB subsequently in precursor aqueous solution, and its add-on is n=0.5 ~ 2.5 with the ratio of the amount of substance of product theoretical yield; The pH value of again determining precursor aqueous solution is 7 ~ 12;
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 120～200 ℃, and pressure is 2～20MPa, reacted 6～60 hours, reaction naturally cools to room temperature after finishing;
4) open water heating kettle, take out product with absolute ethanol washing and centrifugation, repeat the electric vacunm drying case inner drying that absolute ethanol washing and centrifugation be placed on 45～65 ℃ for 4～6 times and obtain hexagonal flake structure Sm 2O 3Semiconductor nano.
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 hexagonal flake structure Sm 2O 3Nanocrystalline 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 nanocrystalline reunion that 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 hexagonal flake structure Sm that grain morphology is single 2O 3Nanocrystalline; Can use more cheap raw material; Save high-temperature calcination and ball milling, avoided impurity to introduce and textural defect.The more important thing is that equipment and instrument that solvent-thermal method requires are comparatively simple, the employing organic solvent is conducive to obtain required pressure and template is soluble in organic solvent, is more conducive to specific morphology Sm 2O 3Nanocrystalline growth reduces nanocrystalline agglomeration.The crystal grain of preparing is grown complete, and pattern is single, and particle diameter is very little and be evenly distributed the Sm of the hexagonal flake that purity is higher 2O 3Prepared nanocrystallinely have the strong absorption effect and visible light had strong anti-reflection effect ultraviolet ray.And utilize solvent-thermal method can add the various template agent, simply and easily control and generate the nanocrystalline of different-shape, thereby realize the nanocrystalline application of different structure.
Description of drawings
Fig. 1 is the prepared hexagonal flake structure of the present invention Sm 2O 3Nanocrystalline XRD figure;
Fig. 2 is the prepared hexagonal flake structure of the present invention Sm 2O 3Nanocrystalline SEM figure.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail.
Embodiment 1:
1) with analytically pure SmCl 36H 2Adopt magnetic stirrer to make Sm in the O adding Virahol 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 45 ℃ of heated and stirred employing concentration is 9, continue to stir to continue to stir after 1 hour and form precursor aqueous solution, in precursor aqueous solution, add cetyl trimethylammonium bromide (CTAB) subsequently, its add-on is n=0.5 with the ratio of the amount of substance of product theoretical yield, determines that again the pH value of precursor aqueous solution is 9;
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 electric drying oven with forced convection that adopts the DHG-9075A type, the control hydrothermal temperature is 120 ℃, and pressure is 8MPa, reacted 48 hours, reaction naturally cools to room temperature after finishing;
4) open water heating kettle, take out product with absolute ethanol washing and centrifugation, repeat absolute ethanol washing and centrifugation be placed on 50 for 6 times, ℃ ZKF030 type electric vacunm drying case inner drying obtain hexagonal flake structure Sm 2O 3Semiconductor nano.
Embodiment 2:
1) with analytically pure SmCl 36H 2Adopt magnetic stirrer to make Sm in the O adding Virahol 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 50 ℃ of heated and stirred employing concentration is 10, continue to stir to continue to stir after 1.5 hours and form precursor aqueous solution, add cetyl trimethylammonium bromide (CTAB) subsequently in precursor aqueous solution, its add-on is n=1 with the ratio of the amount of substance of product theoretical yield; The pH value of again determining precursor aqueous solution is 10;
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 electric drying oven with forced convection that adopts the DHG-9075A type, the control hydrothermal temperature is 150 ℃, and pressure is 15MPa, reacted 60 hours, reaction naturally cools to room temperature after finishing;
4) open water heating kettle, take out product with absolute ethanol washing and centrifugation, repeat the ZKF030 type electric vacunm drying case inner drying that absolute ethanol washing and centrifugation be placed on 55 ℃ for 4 times and obtain hexagonal flake structure Sm 2O 3Semiconductor nano.
Embodiment 3:
1) with analytically pure SmCl 36H 2Adopt magnetic stirrer to make Sm in the O adding Virahol 3+Concentration is the solution A of 0.1mol/L;
2) the pH value that is the NaOH solution regulator solution A of 2mol/L with solution A 48 ℃ of heated and stirred employing concentration is 11, continue to stir to continue to stir after 2 hours and form precursor aqueous solution, add cetyl trimethylammonium bromide (CTAB) subsequently in precursor aqueous solution, its add-on is n=2 with the ratio of the amount of substance of product theoretical yield; The pH value of again determining precursor aqueous solution is 11;
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 electric drying oven with forced convection that adopts the DHG-9075A type, the control hydrothermal temperature is 180 ℃, and pressure is 20MPa, reacted 72 hours, reaction naturally cools to room temperature after finishing;
4) open water heating kettle, take out product with absolute ethanol washing and centrifugation, repeat the ZKF030 type electric vacunm drying case inner drying that absolute ethanol washing and centrifugation be placed on 45 ℃ for 5 times and obtain hexagonal flake structure Sm 2O 3Semiconductor nano.
Embodiment 4:
1) with analytically pure SmCl 36H 2Adopt magnetic stirrer to make Sm in the O adding Virahol 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 52 ℃ of heated and stirred employing concentration is 12, continue to stir to continue to stir after 2.5 hours and form precursor aqueous solution, add cetyl trimethylammonium bromide (CTAB) subsequently in precursor aqueous solution, its add-on is n=1.5 with the ratio of the amount of substance of product theoretical yield; The pH value of again determining precursor aqueous solution is 12;
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 electric drying oven with forced convection that adopts the DHG-9075A type, the control hydrothermal temperature is 140 ℃, and pressure is 18MPa, reacted 36 hours, reaction naturally cools to room temperature after finishing;
4) open water heating kettle, take out product with absolute ethanol washing and centrifugation, repeat the ZKF030 type electric vacunm drying case inner drying that absolute ethanol washing and centrifugation be placed on 50 ℃ for 6 times and obtain hexagonal flake structure Sm 2O 3Semiconductor nano.
Embodiment 5:
1) with analytically pure SmCl 36H 2Adopt magnetic stirrer to make Sm in the O adding Virahol 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 55 ℃ of heated and stirred employing concentration is 7, continue to stir to continue to stir after 3 hours and form precursor aqueous solution, add cetyl trimethylammonium bromide (CTAB) subsequently in precursor aqueous solution, its add-on is n=2.5 with the ratio of the amount of substance of product theoretical yield; The pH value of again determining precursor aqueous solution is 7;
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 electric drying oven with forced convection that adopts the DHG-9075A type, the control hydrothermal temperature is 200 ℃, and pressure is 10MPa, reacted 24 hours, reaction naturally cools to room temperature after finishing;
4) open water heating kettle, take out product with absolute ethanol washing and centrifugation, repeat the ZKF030 type electric vacunm drying case inner drying that absolute ethanol washing and centrifugation be placed on 60 ℃ for 6 times and obtain hexagonal flake structure Sm 2O 3Semiconductor nano.
Embodiment 6:
1) with analytically pure SmCl 36H 2Adopt magnetic stirrer to make Sm in the O adding Virahol 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 53 ℃ of heated and stirred employing concentration is 8, continue to stir to continue to stir after 1.5 hours and form precursor aqueous solution, add cetyl trimethylammonium bromide (CTAB) subsequently in precursor aqueous solution, its add-on is n=2 with the ratio of the amount of substance of product theoretical yield; The pH value of again determining precursor aqueous solution is 8;
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 electric drying oven with forced convection that adopts the DHG-9075A type, the control hydrothermal temperature is 160 ℃, and pressure is 2MPa, reacted 6 hours, reaction naturally cools to room temperature after finishing;
4) open water heating kettle, take out product with absolute ethanol washing and centrifugation, repeat the ZKF030 type electric vacunm drying case inner drying that absolute ethanol washing and centrifugation be placed on 65 ℃ for 6 times and obtain hexagonal flake structure Sm 2O 3Semiconductor nano.
The prepared Sm of the present invention as seen from Figure 1 2O 3Nanocrystalline purity is high, and diffraction peak is more sharp-pointed, and is single monoclinic phase Sm 2O 3, with the JCPDS 42-1464Sm of standard 2O 3Card matches.
The prepared monoclinic phase Sm of the present invention as seen from Figure 2 2O 3Nanocrystalline, particle is little and be evenly distributed, and it is lighter to reunite, and presents the hexagonal flake structure.

Claims (5)

1. hexagonal flake structure Sm 2O 3The preparation method of semiconductor nano is characterized in that may further comprise the steps:
1) with analytically pure SmCl 36H 2Stir in the O adding Virahol and make Sm 3+Concentration is the solution A of 0.2 ~ 1.5mol/L;
2) solution A being adopted the pH value of NaOH solution regulator solution A 45 ~ 55 ℃ of heated and stirred is 7 ~ 12, continues to stir to form precursor aqueous solution, adds CTAB subsequently in precursor aqueous solution, and its add-on is n=0.5 ~ 2.5 with the ratio of the amount of substance of product theoretical yield; The pH value of again determining precursor aqueous solution is 7 ~ 12;
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 120～200 ℃, and pressure is 2～20MPa, reacted 6～60 hours, reaction naturally cools to room temperature after finishing;
4) open water heating kettle, take out product with absolute ethanol washing and centrifugation, repeat the electric vacunm drying case inner drying that absolute ethanol washing and centrifugation be placed on 45～65 ℃ for 4～6 times and obtain hexagonal flake structure Sm 2O 3Semiconductor nano.
2. hexagonal flake structure Sm according to claim 1 2O 3The preparation method of semiconductor nano is characterized in that: magnetic stirrer is adopted in the stirring of described step 1).
3. hexagonal flake structure Sm according to claim 1 2O 3The preparation method of semiconductor nano is characterized in that: the concentration of described NaOH solution is 1～5mol/L.
4. hexagonal flake structure Sm according to claim 1 2O 3The preparation method of semiconductor nano is characterized in that: described electric drying oven with forced convection adopts DHG-9075A type electric drying oven with forced convection.
5. hexagonal flake structure Sm according to claim 1 2O 3The preparation method of semiconductor nano is characterized in that: described electric vacunm drying case adopts ZKF030 type electric vacunm drying case.
CN201210401417XA 2012-10-19 2012-10-19 Method for preparing Sm2O3 semiconductor nanocrystals with hexagonal sheet structures Pending CN102897818A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104556210A (en) * 2015-01-19 2015-04-29 陕西科技大学 Method for preparing Sm2Sn2O7/SnO2 nano composite by microwave-assisted solvothermal two-step process
CN104556213A (en) * 2015-01-19 2015-04-29 陕西科技大学 Method for preparing Sm2Sn2O7-SnO2 nano composite by microwave hydrothermal-water bath process
CN109022767A (en) * 2018-09-28 2018-12-18 中国恩菲工程技术有限公司 Rare-earth precipitation device and rare-earth precipitation method

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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

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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

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104556210A (en) * 2015-01-19 2015-04-29 陕西科技大学 Method for preparing Sm2Sn2O7/SnO2 nano composite by microwave-assisted solvothermal two-step process
CN104556213A (en) * 2015-01-19 2015-04-29 陕西科技大学 Method for preparing Sm2Sn2O7-SnO2 nano composite by microwave hydrothermal-water bath process
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CN109022767A (en) * 2018-09-28 2018-12-18 中国恩菲工程技术有限公司 Rare-earth precipitation device and rare-earth precipitation method

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Application publication date: 20130130