CN101486482B - Method for preparing Sm2O3 nano powder by microwave-hydrothermal method - Google Patents

Method for preparing Sm2O3 nano powder by microwave-hydrothermal method Download PDF

Info

Publication number
CN101486482B
CN101486482B CN2009100211923A CN200910021192A CN101486482B CN 101486482 B CN101486482 B CN 101486482B CN 2009100211923 A CN2009100211923 A CN 2009100211923A CN 200910021192 A CN200910021192 A CN 200910021192A CN 101486482 B CN101486482 B CN 101486482B
Authority
CN
China
Prior art keywords
solution
hydrothermal
hours
microwave
nano
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.)
Expired - Fee Related
Application number
CN2009100211923A
Other languages
Chinese (zh)
Other versions
CN101486482A (en
Inventor
殷立雄
黄剑锋
曹丽云
李娟莹
黄艳
马小波
朱佳
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.)
Shaanxi University of Science and Technology
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 CN2009100211923A priority Critical patent/CN101486482B/en
Publication of CN101486482A publication Critical patent/CN101486482A/en
Application granted granted Critical
Publication of CN101486482B publication Critical patent/CN101486482B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Powder Metallurgy (AREA)
  • Hard Magnetic Materials (AREA)

Abstract

The invention discloses a method for preparing Sm2O3 nano powder by a microwave hydro-thermal method, wherein, analytically pure SmCl3 question mark 6H2O is added into de-ionized water and stirred in a magnetic stirring apparatus to obtain a transparent solution A; the transparent solution A is heated and the pH value of the solution A is adjusted to be 5.4 to 6.0 by an ammonia solution so as to form a solution B; the solution B is poured into a microwave hydro-thermal kettle which is then sealed and put into an MDS-8 type warm-pressing dual-control microwave hydro-thermal reactor for carrying out hydro-thermal reaction, and then naturally cooled to the room temperature after the completion of the reaction; the hydro-thermal kettle is opened and products are centrifugalized with the speedof 4,000 rev./minute so as to ensure that indirect and loose product particles are obtained; and then the product particles are arranged in a vacuum drying chamber for drying. As the reaction for preparing Sm2O3 nano powder is completed by one-time operation in liquid phase, post annealing heat treatment is not needed. Furthermore, the method has simple processing equipment and low cost, the prepared nano material has uniform particle size which ranges from 10nm to 50nm, and is evenly distributed.

Description

A kind of microwave-hydrothermal method prepares Sm 2O 3The method of nano-powder
Technical field
The present invention relates to a kind of preparation Sm 2O 3The method of nano-powder, particularly a kind of microwave hydrothermal prepares Sm 2O 3The method of nano-powder.
Background technology
Sm 2O 3Be a kind of pale yellow powder, easily deliquescence is water insoluble, is soluble in mineral acid.Sm 2O 3Be the Conversion of energy material and the optoelectronic thin film material of a new generation.Sm 2O 3Film can be used to prepare optical switch, data storage, photo-electric conversion element and electrical switch etc.; Sm 2O 3Film also can be used in the spectral filter of electronics body, magneticsubstance and special glass; Nanometer Sm in addition 2O 3Can also be used for ceramic condenser and catalyzer aspect, have wide development prospect should be arranged
The preparation Sm that is reported at present 2O 3The method of optical thin film is mainly vacuum evaporation [V.A.Rozhkov, A.Yu.Trusova, I.G.Berezhnoy.Silicon MIS structuresusing samarium oxide films.Thin Solid Films 325 (1998) 151-155] and the method [A.A.Dakhel.dielecyric and optical properties ofsamarium oxide thin films, Journal of Alloys and Compounds365 (2004) 233-239] of atmosphere evaporation.The method of vacuum evaporation is to heat Sm under vacuum condition 2O 3, deposition obtains Sm on low temperature base version 2O 3Film.The method of atmosphere evaporation is to heat Sm under oxygen atmosphere 2O 3, deposition obtains Sm on low temperature base version 2O 3Film.These two kinds of methods are all very high to equipment requirements, and equipment and instrument is relatively more expensive, owing to evaporation exists in entire container, to Sm 2O 3Utilization ratio of raw materials is very little.Other has report Hydrothermal Preparation Sm 2O 3Film [Huang Jianfeng, Cao Liyun, Huang Yan etc. a kind of hydrothermal preparation Sm 2O 3The method of film [P]. Chinese patent: 200510096004.5,2006-03-01.] and sol-gel method prepare Sm 2O 3[Deng Gengfeng, Zhong Shumei, Chen Huihuang etc. sol-gel method prepares the technical study [J] of ultra-fine Samarium trioxide. rare earth, 2007,28 (2): 40-42].
Summary of the invention
The object of the present invention is to provide a kind of equipment simple, control easily, preparation time is short, synthesizes the Sm that cost is low and prepare 2O 3The higher microwave-hydrothermal method of nano-powder purity prepares Sm 2O 3The method of nano-powder.
For achieving the above object, the technical solution used in the present invention is:
1) at first, with analytical pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.5～2mol/L;
2) secondly, clear solution A was stirred 3～5 hours at 45～55 ℃, and to adopt mass percent be that to regulate the pH value that makes solution be 5.4～6.0 formation solution B for 5～10% ammonia soln;
3) then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 67～80%, sealing microwave hydrothermal still puts it in the two control of the temperature and pressure microwave hydrothermal reaction, and hydrothermal temperature is controlled at 110～200 ℃, reacted 1～4 hour, reaction naturally cools to room temperature after finishing;
4) last, open water heating kettle, product with 4000 rev/mins of centrifugations, then with dehydrated alcohol or washed with isopropyl alcohol 4 times, is made the product particle indirectly and loose, and places 80～120 ℃ vacuum drying oven inner drying can obtain Sm after 4～8 hours 2O 3Nano-powder.
Because the present invention prepares Sm 2O 3Nano-powder is reflected in the liquid phase and once finishes, and do not need the annealing thermal treatment in later stage, and processing unit is simple, and cost is low, and nano material epigranular, the particle size of preparation are 10-50nm, are uniformly dispersed.And utilize the microwave hydrothermal method can better improve the quality of nano-powder and shorten the reaction times than simple hydrothermal method.
Embodiment
Embodiment 1: at first, and with analytical pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.8mol/L; Secondly, clear solution A was stirred 3 hours at 55 ℃, and to adopt mass percent be that to regulate the pH value that makes solution be 5.4 formation solution B for 8% ammonia soln; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 80%, and sealing microwave hydrothermal still puts it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction, and hydrothermal temperature is controlled at 110 ℃, reacts 4 hours, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, product with 4000 rev/mins of centrifugations, is used absolute ethanol washing 4 times then, make the product particle indirectly with loose, and place 100 ℃ vacuum drying oven inner drying can obtain Sm after 6 hours 2O 3Nano-powder.
Embodiment 2: at first, and with analytical pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 1.7mol/L; Secondly, clear solution A was stirred 4 hours at 48 ℃, and to adopt mass percent be that to regulate the pH value that makes solution be 5.6 formation solution B for 5% ammonia soln; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 75%, and sealing microwave hydrothermal still puts it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction, and hydrothermal temperature is controlled at 180 ℃, reacts 2 hours, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, product with 4000 rev/mins of centrifugations, is used washed with isopropyl alcohol 4 times then, make the product particle indirectly with loose, and place 80 ℃ vacuum drying oven inner drying can obtain Sm after 5 hours 2O 3Nano-powder.
Embodiment 3: at first, and with analytical pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 1.0mol/L; Secondly, clear solution A was stirred 5 hours at 52 ℃, and to adopt mass percent be that to regulate the pH value that makes solution be 5.9 formation solution B for 9% ammonia soln; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 67%, and sealing microwave hydrothermal still puts it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction, and hydrothermal temperature is controlled at 150 ℃, reacts 3 hours, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, product with 4000 rev/mins of centrifugations, is used absolute ethanol washing 4 times then, make the product particle indirectly with loose, and place 120 ℃ vacuum drying oven inner drying can obtain Sm after 4 hours 2O 3Nano-powder.
Embodiment 4: at first, and with analytical pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.5mol/L; Secondly, clear solution A was stirred 5 hours at 45 ℃, and to adopt mass percent be that to regulate the pH value that makes solution be 5.5 formation solution B for 7% ammonia soln; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 70%, and sealing microwave hydrothermal still puts it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction, and hydrothermal temperature is controlled at 130 ℃, reacts 3 hours, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, product with 4000 rev/mins of centrifugations, is used washed with isopropyl alcohol 4 times then, make the product particle indirectly with loose, and place 90 ℃ vacuum drying oven inner drying can obtain Sm after 7 hours 2O 3Nano-powder.
Embodiment 5: at first, and with analytical pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 1.3mol/L; Secondly, clear solution A was stirred 4 hours at 50 ℃, and to adopt mass percent be that to regulate the pH value that makes solution be 6.0 formation solution B for 10% ammonia soln; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 73%, and sealing microwave hydrothermal still puts it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction, and hydrothermal temperature is controlled at 160 ℃, reacts 2 hours, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, product with 4000 rev/mins of centrifugations, is used absolute ethanol washing 4 times then, make the product particle indirectly with loose, and place 110 ℃ vacuum drying oven inner drying can obtain Sm after 5 hours 2O 3Nano-powder.
Embodiment 6: at first, and with analytical pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 2mol/L; Secondly, clear solution A was stirred 3 hours at 53 ℃, and to adopt mass percent be that to regulate the pH value that makes solution be 5.7 formation solution B for 6% ammonia soln; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 78%, and sealing microwave hydrothermal still puts it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction, and hydrothermal temperature is controlled at 200 ℃, reacts 1 hour, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, product with 4000 rev/mins of centrifugations, then with dehydrated alcohol or washed with isopropyl alcohol 4 times, is made the product particle indirectly and loose, and places 95 ℃ vacuum drying oven inner drying can obtain Sm after 5 hours 2O 3Nano-powder.

Claims (7)

1. a microwave-hydrothermal method prepares Sm 2O 3The method of nano-powder is characterized in that:
1) at first, with analytical pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.5～2mol/L;
2) secondly, clear solution A was stirred 3～5 hours at 45～55 ℃, and to adopt mass percent be that to regulate the pH value that makes solution be 5.4～6.0 formation solution B for 5～10% ammonia soln;
3) then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 67～80%, sealing microwave hydrothermal still puts it in the two control of the temperature and pressure microwave hydrothermal reaction, and hydrothermal temperature is controlled at 110～200 ℃, reacted 1～4 hour, reaction naturally cools to room temperature after finishing;
4) last, open water heating kettle, product with 4000 rev/mins of centrifugations, then with dehydrated alcohol or washed with isopropyl alcohol 4 times, is made the product particle indirectly and loose, and places 80～120 ℃ vacuum drying oven inner drying can obtain Sm after 4～8 hours 2O 3Nano-powder.
2. microwave-hydrothermal method according to claim 1 prepares Sm 2O 3The method of nano-powder is characterized in that: at first, and with analytical pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.8mol/L; Secondly, clear solution A was stirred 3 hours at 55 ℃, and to adopt mass percent be that to regulate the pH value that makes solution be 5.4 formation solution B for 8% ammonia soln; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 80%, and sealing microwave hydrothermal still puts it in the two control of the temperature and pressure microwave hydrothermal reaction, and hydrothermal temperature is controlled at 110 ℃, reacts 4 hours, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, product with 4000 rev/mins of centrifugations, is used absolute ethanol washing 4 times then, make the product particle indirectly with loose, and place 100 ℃ vacuum drying oven inner drying can obtain Sm after 6 hours 2O 3Nano-powder.
3. microwave-hydrothermal method according to claim 1 prepares Sm 2O 3The method of nano-powder is characterized in that: at first, and with analytical pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 1.7mol/L; Secondly, clear solution A was stirred 4 hours at 48 ℃, and to adopt mass percent be that to regulate the pH value that makes solution be 5.6 formation solution B for 5% ammonia soln; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 75%, and sealing microwave hydrothermal still puts it in the two control of the temperature and pressure microwave hydrothermal reaction, and hydrothermal temperature is controlled at 180 ℃, reacts 2 hours, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, product with 4000 rev/mins of centrifugations, is used washed with isopropyl alcohol 4 times then, make the product particle indirectly with loose, and place 80 ℃ vacuum drying oven inner drying can obtain Sm after 5 hours 2O 3Nano-powder.
4. microwave-hydrothermal method according to claim 1 prepares Sm 2O 3The method of nano-powder is characterized in that: at first, and with analytical pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 1.0mol/L; Secondly, clear solution A was stirred 5 hours at 52 ℃, and to adopt mass percent be that to regulate the pH value that makes solution be 5.9 formation solution B for 9% ammonia soln; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 67%, and sealing microwave hydrothermal still puts it in the two control of the temperature and pressure microwave hydrothermal reaction, and hydrothermal temperature is controlled at 150 ℃, reacts 3 hours, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, product with 4000 rev/mins of centrifugations, is used absolute ethanol washing 4 times then, make the product particle indirectly with loose, and place 120 ℃ vacuum drying oven inner drying can obtain Sm after 4 hours 2O 3Nano-powder.
5. microwave-hydrothermal method according to claim 1 prepares Sm 2O 3The method of nano-powder is characterized in that: at first, and with analytical pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.5mol/L; Secondly, clear solution A was stirred 5 hours at 45 ℃, and to adopt mass percent be that to regulate the pH value that makes solution be 5.5 formation solution B for 7% ammonia soln; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 70%, and sealing microwave hydrothermal still puts it in the two control of the temperature and pressure microwave hydrothermal reaction, and hydrothermal temperature is controlled at 130 ℃, reacts 3 hours, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, product with 4000 rev/mins of centrifugations, is used washed with isopropyl alcohol 4 times then, make the product particle indirectly with loose, and place 90 ℃ vacuum drying oven inner drying can obtain Sm after 7 hours 2O 3Nano-powder.
6. microwave-hydrothermal method according to claim 1 prepares Sm 2O 3The method of nano-powder is characterized in that: at first, and with analytical pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 1.3mol/L; Secondly, clear solution A was stirred 4 hours at 50 ℃, and to adopt mass percent be that to regulate the pH value that makes solution be 6.0 formation solution B for 10% ammonia soln; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 73%, and sealing microwave hydrothermal still puts it in the two control of the temperature and pressure microwave hydrothermal reaction, and hydrothermal temperature is controlled at 160 ℃, reacts 2 hours, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, product with 4000 rev/mins of centrifugations, is used absolute ethanol washing 4 times then, make the product particle indirectly with loose, and place 110 ℃ vacuum drying oven inner drying can obtain Sm after 5 hours 2O 3Nano-powder.
7. microwave-hydrothermal method according to claim 1 prepares Sm 2O 3The method of nano-powder is characterized in that: at first, and with analytical pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 2mol/L; Secondly, clear solution A was stirred 3 hours at 53 ℃, and to adopt mass percent be that to regulate the pH value that makes solution be 5.7 formation solution B for 6% ammonia soln; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 78%, and sealing microwave hydrothermal still puts it in the two control of the temperature and pressure microwave hydrothermal reaction, and hydrothermal temperature is controlled at 200 ℃, reacts 1 hour, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, product with 4000 rev/mins of centrifugations, then with dehydrated alcohol or washed with isopropyl alcohol 4 times, is made the product particle indirectly and loose, and places 95 ℃ vacuum drying oven inner drying can obtain Sm after 5 hours 2O 3Nano-powder.
CN2009100211923A 2009-02-19 2009-02-19 Method for preparing Sm2O3 nano powder by microwave-hydrothermal method Expired - Fee Related CN101486482B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2009100211923A CN101486482B (en) 2009-02-19 2009-02-19 Method for preparing Sm2O3 nano powder by microwave-hydrothermal method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2009100211923A CN101486482B (en) 2009-02-19 2009-02-19 Method for preparing Sm2O3 nano powder by microwave-hydrothermal method

Publications (2)

Publication Number Publication Date
CN101486482A CN101486482A (en) 2009-07-22
CN101486482B true CN101486482B (en) 2011-03-02

Family

ID=40889572

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2009100211923A Expired - Fee Related CN101486482B (en) 2009-02-19 2009-02-19 Method for preparing Sm2O3 nano powder by microwave-hydrothermal method

Country Status (1)

Country Link
CN (1) CN101486482B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105785484B (en) * 2016-05-06 2017-09-01 浙江工贸职业技术学院 A kind of automatically cleaning optical resin lens and preparation method thereof
CN107963660A (en) * 2016-10-19 2018-04-27 张家港市沙源检测技术有限公司 A kind of Sm2O3Adulterate ZrO2Raw powder's production technology

Also Published As

Publication number Publication date
CN101486482A (en) 2009-07-22

Similar Documents

Publication Publication Date Title
CN109368702B (en) Preparation method of tungsten-bronze-structured cesium tungstate
CN102330081B (en) Method for preparing Sm2O3 film by solvent heat method
CN107308957B (en) Spherical Bi2S3/Bi2WO6Preparation method of heterojunction photocatalytic material
CN102432056B (en) Method for preparing Sm2O3 nano crystals by solvent thermal method
CN104016408A (en) Synthetic method of sodium niobate nanowire
CN106809877A (en) A kind of preparation method of D phase hypovanadic oxides
CN105129861A (en) Preparation method for bismuth ferrite BiFeO3 nanosheet
CN101486482B (en) Method for preparing Sm2O3 nano powder by microwave-hydrothermal method
CN107651707A (en) An a kind of step hydro-thermal using tartaric acid as reducing agent prepares molybdenum doping VO2(M) method of powder
CN101494170B (en) Method for preparing Sm2O3 film by microwave assisted hydrothermal process
CN104192890A (en) Method for preparing carbon-dope zinc oxide nanopillars
CN108654663B (en) Boron-nitrogen co-doped single crystal mesoporous TiO prepared by mixed nitrate molten salt method2Method for catalyzing materials
CN104876279A (en) Method for preparing Co-doped BiFeO3
CN115198362B (en) Negative thermal expansion material CaSnF 6 And a method for preparing the same
CN101838011B (en) Preparation method of CuAlO2 microcrystal
CN103922412A (en) Method for preparing flaky SmWO4(OH) with microwave hydrothermal method
CN102774879B (en) Preparation method of dual-phase coexistence one-dimensional structure tin dioxide
CN105399147A (en) Octahedral-structure CoS2 powder anode material for thermal batteries and preparation method thereof
CN105129841B (en) Preparation method of indium oxide with octahedral morphology
CN111874959B (en) SmMoO 4 (OH)-Ni(OH) 2 Preparation method of nano-sheet
CN105600814B (en) One kind prepares flower-like structure Cu2The method of O photoelectric materials
CN100359044C (en) Hydrothermal Sm2O3 film preparing process
CN102897818A (en) Method for preparing Sm2O3 semiconductor nanocrystals with hexagonal sheet structures
CN102659169B (en) Method for preparing zinc oxide micro-nano tooth-shaped rods and zinc oxide micro-nano pine cones
CN103922409B (en) A kind of ellipsoid shape SmW 2o 6(OH) 3the preparation method of crystallite

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
C17 Cessation of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20110302

Termination date: 20140219