CN103482671B - Method for preparing Sm(OH)3 nanometer crystal in homogenous precipitation mode - Google Patents

Method for preparing Sm(OH)3 nanometer crystal in homogenous precipitation mode Download PDF

Info

Publication number
CN103482671B
CN103482671B CN201310422141.8A CN201310422141A CN103482671B CN 103482671 B CN103482671 B CN 103482671B CN 201310422141 A CN201310422141 A CN 201310422141A CN 103482671 B CN103482671 B CN 103482671B
Authority
CN
China
Prior art keywords
ageing
nanocrystalline
solution
distilled water
liquid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201310422141.8A
Other languages
Chinese (zh)
Other versions
CN103482671A (en
Inventor
黄剑锋
王丹
殷立雄
曹丽云
郝巍
吴建鹏
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yancheng julonghu Business Cluster Development Co.,Ltd.
Original Assignee
Shaanxi University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shaanxi University of Science and Technology filed Critical Shaanxi University of Science and Technology
Priority to CN201310422141.8A priority Critical patent/CN103482671B/en
Publication of CN103482671A publication Critical patent/CN103482671A/en
Application granted granted Critical
Publication of CN103482671B publication Critical patent/CN103482671B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Crystals, And After-Treatments Of Crystals (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Disclosed is a method for preparing an Sm(OH)3 nanometer crystal in a homogenous precipitation mode. Sm(NO3)3 6H2O is dissolved in an appropriate amount of distilled water to obtain a solution A with the concentration of Sm3+ being 0.05-0.30 mol/L; pure diethylenetriamine is used for regulating the pH of the solution A to be 8.5-10.5, and the solution continues being stirred for 1-2h to form a reaction liquid precursor; the reaction liquid precursor is placed in a water bath to be aged, and is naturally cooled to room temperature after the reaction is finished; products are washed sequentially by distilled water and absolute ethyl alcohol in a centrifuge mode, the products are collected to be dried for 2-4h in a vacuum mode, and finally the Sm(OH)3 nanometer crystal is obtained. The method is convenient to operate, low in energy consumption and good in safety. The obtained Sm(OH)3 nanometer crystal is high in purity, high in crystallinity, uniform in shape and appearance and good in dispersity.

Description

A kind of sluggish precipitation prepares Sm (OH) 3nanocrystalline method
Technical field
The present invention relates to a kind of preparation method of nano semiconductor material, be specifically related to a kind of sluggish precipitation and prepare Sm (OH) 3nanocrystalline method.
Background technology
Sm (OH) 3a kind of white powder, water insoluble, be soluble in mineral acid.Sm (OH) 3as typical rare earth metal hydroxide material, nano level Sm (OH) 3with the characteristic of rare earth and nano material, in multiple fields of the functional materialss such as high efficiency light-emitting device, magneticsubstance, catalytic material, there is potential using value.
Sm 2o 3the Conversion of energy material of a new generation, semiconductor material and high performance catalyst material, nanometer Sm 2o 3can be used for ceramic condenser, prepare rare earth permanent-magnetic material etc.But because synthesis Sm 2o 3reaction activity higher, therefore Sm (OH) can be utilized 3nano level Sm is prepared in nanocrystalline conduct 2o 3precursor.In addition, monodimension nanometer material can produce the feature of some novelties as these special structures such as nanometer rod, nanotube, nano belt in magnetics, electricity and optics etc., thus causes people's research enthusiasm greatly.
The method of prepared rare-earth hydroxide is hydrothermal method [Y.-P.Fang at present, A.-W.Xu, L.-P.You, Hydrothermal Synthesis of Rare Earth (Tb, Y) Hydroxide and Oxide Nanotubes [J], Advanced Functional Materials, 2003,13 (12): 955-960].But the preparation cycle of hydrothermal method is longer, complex process and energy consumption is high.
Summary of the invention
A kind of sluggish precipitation is the object of the present invention is to provide to prepare Sm (OH) 3nanocrystalline method, the method is easy to operate, energy consumption is low and security is good, the Sm (OH) obtained 3nanocrystalline purity is high, and crystallinity is strong, and pattern evenly and good dispersity.
In order to achieve the above object, the present invention adopts technical scheme to comprise the following steps:
1) by Sm (NO 3) 36H 2o is dissolved in distilled water and is made into Sm 3+concentration is the solution A of 0.05 ~ 0.30mol/L;
2) under agitation adopt pH value to 8.5 ~ 10.5 of diethylenetriamine regulator solution A, then continue stirring 1 ~ 2.5h, forming reactions precursor liquid;
3) by reaction precursor liquid ageing 1 ~ 3h at 65 ~ 90 DEG C, then naturally cool to room temperature, obtain ageing liquid;
4), after being filtered by ageing liquid, solid product is obtained; By solid product centrifuge washing 4 ~ 6 times repeatedly, and use distilled water and absolute ethanol washing respectively at every turn, the solid product after having washed to be placed in vacuum drying oven dry 2 ~ 4h at 60 ~ 80 DEG C, to obtain Sm (OH) 3nanocrystalline.
Described Sm (NO 3) 36H 2o and diethylenetriamine all adopt analytical pure.
Described step 2) in stirring adopt magnetic agitation.
In described step 3), reaction solution is placed in water-bath and carries out ageing.
Compared with prior art, beneficial effect of the present invention is:
The present invention prepares the mutually bar-shaped Sm of six side (OH) with sluggish precipitation 3nanocrystalline, meanwhile, in preparation Sm (OH) 3organic bases diethylenetriamine is utilized to regulate the pH of reaction system in nanocrystalline process; Test proves, adopts Sm (OH) prepared by sluggish precipitation 3nanocrystalline purity is high, and crystallinity is strong, and pattern evenly and good dispersity.The method raw material is easy to get, and processing unit is simple, and energy consumption is low, and reaction completes through the short period in the liquid phase, and this reaction is carried out at ambient pressure, and with water as reaction solvent, security is good, and feasibility is strong, so very economical, practical, has good industrial prospect.In addition, the organic bases diethylenetriamine adopted in adjust ph process not only can provide alkaline environment as alkali source, can also as complexing agent to Sm (OH) 3nanocrystalline microtexture produces regulating and controlling effect.
Accompanying drawing explanation
Fig. 1 is the Sm (OH) prepared by the embodiment of the present invention 1 3nanocrystalline XRD figure;
Fig. 2 is the Sm (OH) prepared by the embodiment of the present invention 1 3sEM figure during nanocrystalline amplification 50,000 times.
Embodiment
Embodiment 1:
1) by analytical pure Sm (NO 3) 36H 2o is dissolved in 50mL distilled water and is made into Sm 3+concentration is the solution A of 0.05mol/L;
2) adopt the pH value to 9.0 of analytical pure diethylenetriamine regulator solution A under magnetic stirring, continue then continuous stirring 1h, forming reactions precursor liquid;
3) reaction precursor liquid is placed in water-bath ageing 1.5h at 80 DEG C, then naturally cools to room temperature, obtain ageing liquid;
4), after being filtered by ageing liquid, solid product is obtained; Solid product is used successively distilled water and dehydrated alcohol centrifuge washing, washing times is 4 ~ 6 times, to be then placed in electric vacunm drying case dry 3h at 60 DEG C, to obtain the Sm (OH) that thing is six side's phases mutually 3nanocrystalline.
As can be seen from Figure 1 obtained Sm (OH) 3purity high, crystallinity is strong, and obviously, thing is six side's phases mutually in orientation growth.
As can be seen from Figure 2 product appearance pattern is thinner club shaped structure and is evenly distributed, better dispersed.
Embodiment 2:
1) by analytical pure Sm (NO 3) 36H 2o is dissolved in 50mL distilled water and is made into Sm 3+concentration is the solution A of 0.10mol/L;
2) adopt the pH value to 9.5 of analytical pure diethylenetriamine regulator solution A under magnetic stirring, continue then continuous stirring 1.5h, forming reactions precursor liquid;
3) reaction precursor liquid is placed in water-bath ageing 3h at 65 DEG C, then naturally cools to room temperature, obtain ageing liquid;
4), after being filtered by ageing liquid, solid is obtained; Solid product is used successively distilled water and dehydrated alcohol centrifuge washing, washing times is 4 ~ 6 times, to be then placed in electric vacunm drying case dry 3h at 60 DEG C, to obtain the Sm (OH) that thing is six side's phases mutually 3nanocrystalline.
Embodiment 3:
1) by analytical pure Sm (NO 3) 36H 2o is dissolved in 50mL distilled water and is made into Sm 3+concentration is the solution A of 0.15mol/L;
2) adopt the pH value to 8.5 of analytical pure diethylenetriamine regulator solution A under magnetic stirring, then continue to stir 1h, forming reactions precursor liquid;
3) reaction precursor liquid is placed in water-bath ageing 2.5h at 70 DEG C, then naturally cools to room temperature and obtain ageing liquid;
4), after being filtered by ageing liquid, solid is obtained; Solid product is used successively distilled water and dehydrated alcohol centrifuge washing, washing times is 4 ~ 6 times, to be then placed in electric vacunm drying case dry 3h at 60 DEG C, to obtain the Sm (OH) that thing is six side's phases mutually 3nanocrystalline.
Embodiment 4:
1) by analytical pure Sm (NO 3) 36H 2o is dissolved in 30mL distilled water and is made into Sm 3+concentration is the solution A of 0.20mol/L;
2) adopt the pH value to 10.0 of analytical pure diethylenetriamine regulator solution A under magnetic stirring, then continue to stir 2h, forming reactions precursor liquid;
3) reaction precursor liquid is placed in water-bath ageing 1.5h at 85 DEG C, then naturally cools to room temperature, obtain ageing liquid;
4), after being filtered by ageing liquid, solid is obtained; Solid product is used successively distilled water and dehydrated alcohol centrifuge washing, washing times is 4 ~ 6 times, to be then placed in electric vacunm drying case dry 3h at 60 DEG C, to obtain the Sm (OH) that thing is six side's phases mutually 3nanocrystalline.
Embodiment 5:
1) by pure for component analysis Sm (NO 3) 36H 2o is dissolved in 50mL distilled water and is made into Sm 3+concentration is the solution A of 0.30mol/L;
2) adopt the pH value to 10.5 of analytical pure diethylenetriamine regulator solution A under magnetic stirring, then continue to stir 2.5h, forming reactions precursor liquid;
3) reaction precursor liquid is placed in water-bath ageing 1h at 90 DEG C, then naturally cools to room temperature, obtain ageing liquid;
4), after being filtered by ageing liquid, solid is obtained; Solid product is used successively distilled water and dehydrated alcohol centrifuge washing, washing times is 4 ~ 6 times, to be then placed in electric vacunm drying case dry 3h at 60 DEG C, to obtain the Sm (OH) that thing is six side's phases mutually 3nanocrystalline.
Embodiment 6:
1) by pure for component analysis Sm (NO 3) 36H 2o is dissolved in 50mL distilled water and is made into Sm 3+concentration is the solution A of 0.30mol/L;
2) adopt the pH value to 10.5 of analytical pure diethylenetriamine regulator solution A under magnetic stirring, then continue to stir 2.5h, forming reactions precursor liquid;
3) reaction precursor liquid is placed in water-bath ageing 1h at 90 DEG C, then naturally cools to room temperature, obtain ageing liquid;
4), after being filtered by ageing liquid, solid is obtained; Solid product is used successively distilled water and dehydrated alcohol centrifuge washing, washing times is 4 ~ 6 times, to be then placed in electric vacunm drying case dry 2h at 80 DEG C, to obtain the Sm (OH) that thing is six side's phases mutually 3nanocrystalline.
Embodiment 7:
1) by analytical pure Sm (NO 3) 36H 2o is dissolved in 50mL distilled water and is made into Sm 3+concentration is the solution A of 0.15mol/L;
2) adopt the pH value to 8.5 of analytical pure diethylenetriamine regulator solution A under magnetic stirring, then continue to stir 1h, forming reactions precursor liquid;
3) reaction precursor liquid is placed in water-bath ageing 2.5h at 70 DEG C, then naturally cools to room temperature and obtain ageing liquid;
4), after being filtered by ageing liquid, solid is obtained; Solid product is used successively distilled water and dehydrated alcohol centrifuge washing, washing times is 4 ~ 6 times, to be then placed in electric vacunm drying case dry 4h at 70 DEG C, to obtain the Sm (OH) that thing is six side's phases mutually 3nanocrystalline.

Claims (4)

1. a sluggish precipitation prepares Sm (OH) 3nanocrystalline method, is characterized in that, comprises the following steps:
1) by Sm (NO 3) 36H 2o is dissolved in distilled water and is made into Sm 3+concentration is the solution A of 0.05 ~ 0.30mol/L;
2) under agitation adopt pH value to 8.5 ~ 10.5 of diethylenetriamine regulator solution A, then continue stirring 1 ~ 2.5h, forming reactions precursor liquid;
3) by reaction precursor liquid ageing 1 ~ 3h at 65 ~ 90 DEG C, then naturally cool to room temperature, obtain ageing liquid;
4), after being filtered by ageing liquid, solid product is obtained; By solid product centrifuge washing 4 ~ 6 times repeatedly, and use distilled water and absolute ethanol washing respectively at every turn, the solid product after having washed to be placed in vacuum drying oven dry 2 ~ 4h at 60 ~ 80 DEG C, to obtain Sm (OH) 3nanocrystalline.
2. sluggish precipitation according to claim 1 prepares Sm (OH) 3nanocrystalline method, is characterized in that: described Sm (NO 3) 36H 2o and diethylenetriamine all adopt analytical pure.
3. sluggish precipitation according to claim 1 prepares Sm (OH) 3nanocrystalline method, is characterized in that: described step 2) in stirring adopt magnetic agitation.
4. sluggish precipitation according to claim 1 prepares Sm (OH) 3nanocrystalline method, is characterized in that: in described step 3), reaction solution is placed in water-bath and carries out ageing.
CN201310422141.8A 2013-09-16 2013-09-16 Method for preparing Sm(OH)3 nanometer crystal in homogenous precipitation mode Active CN103482671B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310422141.8A CN103482671B (en) 2013-09-16 2013-09-16 Method for preparing Sm(OH)3 nanometer crystal in homogenous precipitation mode

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310422141.8A CN103482671B (en) 2013-09-16 2013-09-16 Method for preparing Sm(OH)3 nanometer crystal in homogenous precipitation mode

Publications (2)

Publication Number Publication Date
CN103482671A CN103482671A (en) 2014-01-01
CN103482671B true CN103482671B (en) 2015-04-22

Family

ID=49823343

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310422141.8A Active CN103482671B (en) 2013-09-16 2013-09-16 Method for preparing Sm(OH)3 nanometer crystal in homogenous precipitation mode

Country Status (1)

Country Link
CN (1) CN103482671B (en)

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103922384A (en) * 2014-04-14 2014-07-16 陕西科技大学 Method for preparing cubic phase Sm2O3 nano crystal with combination of uniform precipitation-thermal treatment
CN104556199B (en) * 2015-01-19 2016-03-30 陕西科技大学 A kind of homogeneous phase hydrothermal method that adopts prepares Sm (OH) 3the method of/CuO nano-complex
CN105032392A (en) * 2015-07-27 2015-11-11 陕西科技大学 Method for preparing SmCO3 (OH)/ZnO nanocomposite by homogeneous hydrothermal method
CN105642323B (en) * 2016-01-12 2018-02-23 陕西科技大学 One kind prepares Sm (OH) using in situ deposition method3/AgPO4The method of nano-complex
CN106044831B (en) * 2016-05-27 2017-09-22 商洛学院 A kind of sluggish precipitation prepares sheet SmOHCO3Nanocrystalline method
CN106219595B (en) * 2016-07-05 2017-11-21 陕西科技大学 A kind of precipitation method prepare Sm (OH)3The method of/CdS nano-complexes
CN106166494B (en) * 2016-07-05 2018-12-11 陕西科技大学 A kind of sluggish precipitation preparation Sm (OH)3The method of/CdS nano-complex
CN106219588B (en) * 2016-07-18 2018-06-19 陕西科技大学 A kind of rodlike La (OH) prepared using homogeneous precipitation bath oiling3Nano material and its method
CN109502626A (en) * 2018-12-19 2019-03-22 陕西科技大学 A kind of method that sol-gal process prepares lanthanum hydroxide

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1586715A (en) * 2004-07-08 2005-03-02 清华大学 Preparation and use of samarium oxide catalyst
CN101717108A (en) * 2009-11-12 2010-06-02 济南大学 Industrial preparation method of rare earth hydrate and oxide nano-rod

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1586715A (en) * 2004-07-08 2005-03-02 清华大学 Preparation and use of samarium oxide catalyst
CN101717108A (en) * 2009-11-12 2010-06-02 济南大学 Industrial preparation method of rare earth hydrate and oxide nano-rod

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Lanthanide hydroxide nanorods and their thermal decomposition to lanthanide;Ning Zhang et al.;《Materials Chemistry and Physics》;20091231;第114卷;第160-167页 *
纳米二氧化铈的低温水热一步法合成;陈建君等;《材料导报》;20091130;第23卷;第145-146、150页 *

Also Published As

Publication number Publication date
CN103482671A (en) 2014-01-01

Similar Documents

Publication Publication Date Title
CN103482671B (en) Method for preparing Sm(OH)3 nanometer crystal in homogenous precipitation mode
CN102320658B (en) Method for synthesizing alkaline earth metal vanadate micro/nano materials by adopting hydrothermal/solvothermal method
CN102154695B (en) Nickel oxide nano rod array material, method for preparing same and application thereof
CN109280938B (en) V-doped Ni in flower ball shape3S2NF self-supporting electrode material and preparation method thereof
CN104030335A (en) Method for preparing Sm(OH)3/ZnO nano-composite by using homogeneous hydrothermal method
CN103922384A (en) Method for preparing cubic phase Sm2O3 nano crystal with combination of uniform precipitation-thermal treatment
CN102923784B (en) Preparation method of FeWO4 nanowire
CN102951686A (en) Preparation method for granular manganese tungstate nanocrystals
CN102432056B (en) Method for preparing Sm2O3 nano crystals by solvent thermal method
CN102408132B (en) Method for preparing nanometer lanthanum ferrite powder by using microwave process
CN105731518B (en) Normal-temperature crystallization preparation method of octahedron cuprous oxide crystal
CN104402065A (en) Preparation method of spheroidic CoS2 nanometer powder
CN107935047B (en) A kind of control synthetic method of different-shape and the nano-manganese dioxide of size
CN104556194B (en) A kind of low temperature water-bath legal system is for hollow tubular Sm (OH) 3the method of/ZnO nano mixture
CN106268887A (en) A kind of composite photo-catalyst CdS/LaPO4and its preparation method and application
CN103482672B (en) Preparation method of hexagonal-prism-shaped Sm(OH)3 nanocrystalline
CN102145923A (en) Method for preparing porous flaky Co3O4 microspheres
CN107628641A (en) A kind of titanium dioxide nano thread and preparation method thereof
CN108328650B (en) One one-step hydro-thermal synthesis method of one-dimensional Perovskite Phase lead titanates nanofiber
CN101774603B (en) Preparation method of mesoporous magnesium borate microsphere
CN103466688A (en) Method for preparing ZnS nanosheet
CN103950993B (en) A kind of preparation method of taraxacum shape tricobalt tetroxide
CN103332742A (en) Method for preparing alpha-MoO3 nanobelts by microwave-ultrasonic-ultraviolet process
CN103408064B (en) Method for preparing indium oxide cubes through microwave-assisted hydrothermal method
CN105399147A (en) Octahedral-structure CoS2 powder anode material for thermal batteries and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20201217

Address after: Floor 6, building 6, Xinlong Plaza, Xindu street, Chengnan New District, Yancheng City, Jiangsu Province, 224000 (CND)

Patentee after: Yancheng julonghu Business Cluster Development Co.,Ltd.

Address before: No. 1, Weiyang District university garden, Xi'an, Shaanxi Province, Shaanxi

Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY