CN106115648A - A kind of preparation method of one-dimensional linear structure rare earth phosphate nanometer material - Google Patents

A kind of preparation method of one-dimensional linear structure rare earth phosphate nanometer material Download PDF

Info

Publication number
CN106115648A
CN106115648A CN201610461652.4A CN201610461652A CN106115648A CN 106115648 A CN106115648 A CN 106115648A CN 201610461652 A CN201610461652 A CN 201610461652A CN 106115648 A CN106115648 A CN 106115648A
Authority
CN
China
Prior art keywords
rare earth
linear structure
dimensional linear
phosphate
deionized water
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.)
Granted
Application number
CN201610461652.4A
Other languages
Chinese (zh)
Other versions
CN106115648B (en
Inventor
李银艳
徐时清
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.)
China Jiliang University
Original Assignee
China Jiliang University
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 China Jiliang University filed Critical China Jiliang University
Priority to CN201610461652.4A priority Critical patent/CN106115648B/en
Publication of CN106115648A publication Critical patent/CN106115648A/en
Application granted granted Critical
Publication of CN106115648B publication Critical patent/CN106115648B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/37—Phosphates of heavy metals
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Luminescent Compositions (AREA)

Abstract

The preparation method of one-dimensional linear structure rare earth phosphate nanometer material disclosed by the invention, use hydro-thermal reaction method, react with rare earth nitrate simultaneously as reaction reagent and template agent with tetrabutyl ammonium dihydrogen phosphate, synthesizing one-dimensional linear structure rare-earth phosphate LnPO4, wherein Ln=La, Ce, Pr, Nd or Sm.The inventive method is not required to additionally add any organic reagent, so that course of reaction is simple, quick and environmental protection.Present invention process process is simple, it is easy to control, pollution-free, low cost, it is easy to accomplish large-scale production；The one-dimensional linear structure rare earth phosphate nanometer material prepared, purity is high, good dispersion.

Description

A kind of preparation method of one-dimensional linear structure rare earth phosphate nanometer material
Technical field
The present invention relates to the preparation method of a kind of one-dimensional wire rare earth phosphate nanometer material, belong to Inorganic Non-metallic Materials Technical field.
Background technology
RE phosphate has a wide range of applications in fields such as laser material, bioprobe and heat proof materials, utilizes rare earth Phosphate, as substrate, is prepared the Luminescent Materials of Rare-earth Phosphates of lanthanide ion doping, is sent out for understanding and cognition rare earth ion The novel photoelectric material of the principle of light, compounding design has important theory significance.Rare earth phosphate nanometer material, due to nanometer Dimensional effect so that it is show more excellent performance at optics and field of biology, has the biggest researching value and application is latent Power.
The synthesis of traditional rare earth phosphate nanometer material, it usually needs extra addition surfactant and template agent are come real The ordering growth of existing nanostructured.And the interpolation of these reagent makes reaction process complicated, and environment is produced by these organic reagents Raw certain pollution.
Summary of the invention
It is an object of the invention to provide a kind of technique simple, process is easily controllable, the one-dimensional linear structure of environmental protection The preparation method of rare earth phosphate nanometer material.
The preparation method of the one-dimensional linear structure rare earth phosphate nanometer material of the present invention, uses hydro-thermal reaction method, The chemical formula of this RE phosphate is LnPO4, Ln=La, Ce, Pr, Nd or Sm in formula, its preparation process is as follows:
1) being dissolved in deionized water by tetrabutyl ammonium dihydrogen phosphate, compound concentration is the tetrabutyl ammonium dihydrogen phosphate water of 1 mol/L Solution；
2) by rare earth nitrate LnNO3Being dissolved in deionized water, Ln=La, Ce, Pr, Nd or Sm, regulation rare earth ion concentration is 1 mol/L；
3) LnPO is pressed4Stoichiometric proportion, Ln=La, Ce, Pr, Nd or Sm, under stirring, by step 1) prepare four fourths Base ammonium dihydrogen phosphate aqueous solution instill step 2) rare earth nitrate aqueous solution in, LnPO4Precipitation generates, and obtains there is LnPO4Precipitation Mixture；
4) adding mixture in the reactor inner bag of politef, regulating its volume with deionized water is reactor volume 2/3 ~ 4/5, stir at least 5 minutes
5) by step 4) the reactor inner bag that is configured with reaction mass is placed in reactor, airtight, 160oC-200oC is incubated React 8-12 hour, in air, be then naturally cooling to room temperature, take out product, filter, clean with deionized water, dry Dry, obtain one-dimensional linear structure rare earth phosphate nanometer material.
The present invention uses hydro-thermal reaction method, utilizes tetrabutyl ammonium dihydrogen phosphate simultaneously as reaction reagent and template agent at water React with rare earth nitrate under heat condition, synthesizing one-dimensional linear structure RE phosphate, be not required to additionally add any organic reagent, So that course of reaction is simple, quick and environmental protection.Present invention process process is simple, it is easy to control, pollution-free, low cost, it is easy to Realize large-scale production；The one-dimensional linear structure rare earth phosphate nanometer material prepared, purity is high, good dispersion.
Accompanying drawing explanation
Fig. 1 is one-dimensional linear structure PrPO4The XRD figure spectrum of nano material.
Fig. 2 is one-dimensional linear structure PrPO4The scanning electron microscopic picture of nano material.
Fig. 3 is one-dimensional linear structure PrPO4The transmission electron microscope picture of nano material.
Fig. 4 is one-dimensional linear structure SmPO4The scanning electron microscopic picture of nano material.
Detailed description of the invention
Below in conjunction with embodiment, the inventive method is described in further detail.
Embodiment 1
1) being dissolved in deionized water by tetrabutyl ammonium dihydrogen phosphate, compound concentration is the tetrabutyl ammonium dihydrogen phosphate water of 1 mol/L Solution；
2) Lanthanum (III) nitrate is dissolved in deionized water, regulates La3+Ion concentration is 1 mol/L；
3) LaPO is pressed4Stoichiometric proportion, under stirring, by step 1) prepare tetrabutyl ammonium dihydrogen phosphate aqueous solution instill In lanthanum nitrate aqueous solution, LaPO4Precipitation generates, and obtains there is LaPO4The mixture of precipitation；
4) being joined by mixture produced above in the reactor inner bag of politef, regulating its volume with deionized water is The 2/3 of reactor volume, stirs 5 minutes；
5) by step 4) the reactor inner bag that is configured with reaction mass is placed in reactor, airtight, is placed in 160oThe stove of C is protected Temperature, after reacting 8 hours, is naturally cooling to room temperature in air, takes out product, filter, clean with deionized water, dry, Obtain one-dimensional linear structure lanthanum phosphate nano material.
Embodiment 2
1) being dissolved in deionized water by tetrabutyl ammonium dihydrogen phosphate, compound concentration is the tetrabutyl ammonium dihydrogen phosphate water of 1 mol/L Solution；
2) six nitric hydrate praseodymiums are dissolved in deionized water, regulate Pr3+Ion concentration is 1 mol/L；
3) PrPO is pressed4Stoichiometric proportion, under stirring, by step 1) prepare tetrabutyl ammonium dihydrogen phosphate aqueous solution instill nitre In acid praseodymium aqueous solution, PrPO4Precipitation generates, and obtains there is PrPO4The mixture of precipitation；
4) being joined by mixture produced above in the reactor inner bag of politef, regulating its volume with deionized water is The 4/5 of reactor volume, stirs 10 minutes；
5) by step 4) the reactor inner bag that is configured with reaction mass is placed in reactor, airtight, is placed in 180oThe stove of C is protected Temperature, after reacting 10 hours, is naturally cooling to room temperature in air, takes out product, filter, clean with deionized water, dry, Obtain one-dimensional linear structure praseodymium phosphate nano material.Its XRD figure spectrum is shown in Fig. 1, and the nano material obtained as seen from the figure is Pure praseodymium phosphate hexagonal phase, appearance of nano material is shown in Fig. 2, Fig. 3, and the nano material obtained as seen from the figure is single nano wire Structure.Fig. 1, Fig. 2 and Fig. 3 combine and show that the one-dimensional linear structure praseodymium phosphate nano material purity prepared by the method is high, dispersion Property is good.
Embodiment 3
1) being dissolved in deionized water by tetrabutyl ammonium dihydrogen phosphate, compound concentration is the tetrabutyl ammonium dihydrogen phosphate water of 1 mol/L Solution；
2) six nitric hydrate samariums are dissolved in deionized water, regulate Sm3+Ion concentration is 1 mol/L；
3) SmPO is pressed4Stoichiometric proportion, under stirring, by step 1) prepare tetrabutyl ammonium dihydrogen phosphate aqueous solution instill In samaric nitrate aqueous solution, SmPO4Precipitation generates；Obtain there is SmPO4The mixture of precipitation；
4) mixture produced above is joined in the reactor inner bag of politef, regulate its volume with deionized water For the 4/5 of reactor volume, stir 8 minutes；
5) by step 4) the reactor inner bag that is configured with reaction mass is placed in reactor, airtight, is placed in 200oThe stove of C is protected Temperature, after reacting 12 hours, is naturally cooling to room temperature in air, takes out product, filter, clean with deionized water, dry, Obtain one-dimensional linear structure samaric orthophosphate nano material.The appearance of nano material scanning electron microscope (SEM) photograph obtained is shown in Fig. 4, receives for single Nanowire structure, shows that the one-dimensional linear structure samaric orthophosphate nano material purity prepared by the method is high, good dispersion.

Claims (1)

1. a preparation method for one-dimensional linear structure rare earth phosphate nanometer material, the chemical formula of this RE phosphate is LnPO4, Ln=La, Ce, Pr, Nd or Sm in formula, its preparation process is as follows:
1) being dissolved in deionized water by tetrabutyl ammonium dihydrogen phosphate, compound concentration is the tetrabutyl ammonium dihydrogen phosphate water of 1 mol/L Solution；
2) by rare earth nitrate LnNO3Being dissolved in deionized water, Ln=La, Ce, Pr, Nd or Sm, regulation rare earth ion concentration is 1 mol/L；
3) LnPO is pressed4Stoichiometric proportion, Ln=La, Ce, Pr, Nd or Sm, under stirring, by step 1) prepare four fourths Base ammonium dihydrogen phosphate aqueous solution instill step 2) rare earth nitrate aqueous solution in, LnPO4Precipitation generates, and obtains there is LnPO4Precipitation Mixture；
4) adding mixture in the reactor inner bag of politef, regulating its volume with deionized water is reactor volume 2/3 ~ 4/5, stir at least 5 minutes；
5) by step 4) the reactor inner bag that is configured with reaction mass is placed in reactor, airtight, 160oC-200oC is incubated, React 8-12 hour, in air, be then naturally cooling to room temperature, take out product, filter, clean with deionized water, dry Dry, obtain one-dimensional linear structure rare earth phosphate nanometer material.
CN201610461652.4A 2016-06-23 2016-06-23 A kind of preparation method of one-dimensional linear structure rare earth phosphate nanometer material Active CN106115648B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610461652.4A CN106115648B (en) 2016-06-23 2016-06-23 A kind of preparation method of one-dimensional linear structure rare earth phosphate nanometer material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610461652.4A CN106115648B (en) 2016-06-23 2016-06-23 A kind of preparation method of one-dimensional linear structure rare earth phosphate nanometer material

Publications (2)

Publication Number Publication Date
CN106115648A true CN106115648A (en) 2016-11-16
CN106115648B CN106115648B (en) 2018-02-16

Family

ID=57268593

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610461652.4A Active CN106115648B (en) 2016-06-23 2016-06-23 A kind of preparation method of one-dimensional linear structure rare earth phosphate nanometer material

Country Status (1)

Country Link
CN (1) CN106115648B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111747392A (en) * 2020-07-17 2020-10-09 南昌航空大学 Method for preparing semi-hydrated samarium phosphate rodlike nanocrystalline

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101318640A (en) * 2008-05-13 2008-12-10 北京科技大学 Process for synthesizing CePO4 nano-material with monocline structure
CN103569987A (en) * 2013-06-25 2014-02-12 内蒙古大学 Synthesis method for synthesizing monoclinic phase LaPO4: Eu nano-luminescent material by low-temperature hydrothermal method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101318640A (en) * 2008-05-13 2008-12-10 北京科技大学 Process for synthesizing CePO4 nano-material with monocline structure
CN103569987A (en) * 2013-06-25 2014-02-12 内蒙古大学 Synthesis method for synthesizing monoclinic phase LaPO4: Eu nano-luminescent material by low-temperature hydrothermal method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
肖秀珍: ""稀土铌、钽、磷酸盐微纳米发光材料的合成和发光性质"", 《中国博士学位论文全文数据库 工程科技I辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111747392A (en) * 2020-07-17 2020-10-09 南昌航空大学 Method for preparing semi-hydrated samarium phosphate rodlike nanocrystalline
CN111747392B (en) * 2020-07-17 2023-03-14 南昌航空大学 Method for preparing semi-hydrated samarium phosphate rod-shaped nanocrystalline

Also Published As

Publication number Publication date
CN106115648B (en) 2018-02-16

Similar Documents

Publication Publication Date Title
Li et al. Eu3+/Tb3+-doped La2O2CO3/La2O3 nano/microcrystals with multiform morphologies: facile synthesis, growth mechanism, and luminescence properties
CN106854175B (en) Terpyridyl zinc benzoate complex and preparation condition
CN100462307C (en) Method for preparation of niobic acid zinc nano material
Han et al. Synthesis of the superfine high-entropy zirconate nanopowders by polymerized complex method
Sun et al. Preparation and characterization of Eu3+-doped fluorapatite nanoparticles by a hydrothermal method
CN102275942A (en) Preparation method of bismuth silicate nanopowder
CN108793111A (en) A kind of method and products thereof of quick preparation phosphatization cobalt
CN106520121A (en) Preparation method of rare earth-doped gadolinium oxysulfide and oxygen-containing gadolinium sulphate up-conversion phosphor
CN101481103B (en) Method for synthesizing hexagonal phase TbPO4 H2O nano/micron multi-stage structural material
Zhou et al. One-step surfactant-free synthesis of Eu 3+-activated NaTb (MoO 4) 2 microcrystals with controllable shape and their multicolor luminescence properties
CN103131417A (en) Eu doped YPO4 microballoon and preparation method thereof
Mishenina et al. Synthesis and characteristics of CaAl2O4: Eu3+ phosphor prepared by zol-gel method
CN100558946C (en) Be the method that presoma prepares RE borate crystal with the oxide compound under the low temperature
CN102061521A (en) Er-Yb codoping ZnO nano crystal and preparation method thereof
CN105481013A (en) Self-sacrifice template synthetic method for preparing flake-shaped vanadate
CN106115648B (en) A kind of preparation method of one-dimensional linear structure rare earth phosphate nanometer material
CN104326500B (en) A kind of preparation method of fluffy state nano yttrium oxide powder
CN105752957B (en) Using the method for preparing nano-scale rare earth phosphate phosphor from sacrifice template method
Li et al. Synthesis and characterizations of pompon-like Y2O2SO4: Eu3+ phosphors using a UBHP technique based on UAS system
CN105419800A (en) Preparation method of yttrium phosphate vanadate europium-doped or samarium-doped luminescent microspheres
Hernández et al. Structural, morphological, and luminescent properties of tetragonal-phase YPO4: Eu3+
Muresan et al. Thermal behavior of precursors for synthesis of Y 2 SiO 5: Ce phosphor via gel combustion
CN103265060A (en) Preparation method of monodisperse hexagonal-phase sodium yttrium fluoride mesoscopic crystal particles
CN107163939B (en) Preparation method of novel nano composite zinc oxide-based red fluorescent material
CN105603527A (en) Preparation method of zinc oxide nano monocrystals

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant