CN105152192A - Preparation method of magnesium oxide/rare-earth oxide core-shell-structure flower-like nano composite material - Google Patents

Preparation method of magnesium oxide/rare-earth oxide core-shell-structure flower-like nano composite material Download PDF

Info

Publication number
CN105152192A
CN105152192A CN201510597046.0A CN201510597046A CN105152192A CN 105152192 A CN105152192 A CN 105152192A CN 201510597046 A CN201510597046 A CN 201510597046A CN 105152192 A CN105152192 A CN 105152192A
Authority
CN
China
Prior art keywords
flower
magnesium
preparation
minutes
rare
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
CN201510597046.0A
Other languages
Chinese (zh)
Other versions
CN105152192B (en
Inventor
陈伟凡
李治洲
刘洋
谭友德
张庆飞
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.)
Nanchang University
Original Assignee
Nanchang 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 Nanchang University filed Critical Nanchang University
Priority to CN201510597046.0A priority Critical patent/CN105152192B/en
Publication of CN105152192A publication Critical patent/CN105152192A/en
Application granted granted Critical
Publication of CN105152192B publication Critical patent/CN105152192B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The invention relates to a preparation method of a magnesium oxide/rare-earth oxide core-shell-structure flower-like nano composite material, which comprises the following steps: weighing a corresponding amount of previously prepared magnesium hydroxide template according to the preparation quantity and rare-earth element/magnesium stoichiometric proportion of the magnesium oxide/rare-earth oxide core-shell-structure flower-like nano composite material, preparing a corresponding volume of 0.01-0.2 mol/L rare-earth salt solution with the pH value of 3-7, adding the template into the rare-earth salt solution, stirring at room temperature for 20-120 minutes, filtering, washing, drying at 60-100 DEG C for 120-240 minutes, and calcining at 400-900 DEG C for 30-240 minutes to obtain the end product. The preparation process is simple, quick and spontaneous, and does not use any additive; the template can be easily subjected to mass preparation; the shape and size of the template can be well inherited to the precursor and end product; and the product has favorable dispersity, and the particle size is 1-2 mu m or so.

Description

The preparation method of a kind of magnesium oxide/rare earth oxide nucleocapsid structure flower-like nanometer matrix material
Technical field
The invention belongs to the preparation field of matrix material, relate to the preparation method of nucleocapsid structure flower-like nanometer matrix material.
Technical background
In recent years, Core-shell structure material is obtained for widespread use in fields such as catalysis, absorption, medical science, luminescences due to the structures and characteristics of its uniqueness.Rare earth element is due to its special 4f electronic orbit layer, it is made to have much special character, at luminescent material, catalytic material, the fields such as biomaterial all obtain extensive and deep application, particularly about the Core-shell structure material of rare earth oxide becomes the focus of research, the current method preparing Core-shell structure material mainly contains sol-gel method, homogeneous precipitation method, hydrothermal method, self-assembly method, flame aerosols method etc., the most process of these methods is complicated, need comparatively high temps, strict to equipment requirements, be difficult to a large amount of preparation, be difficult to control to pattern and particle diameter, the coating layer formed is uneven.Homogeneous precipitation method utilizes precipitation from homogeneous solution (PFHS) agent that rare earth ion is deposited in oxide surface, then obtain the method for nucleocapsid structure product through Overheating Treatment.Hua-JunFeng etc. obtain spherical, monodispersed SiO by the homogeneous hydrolysis controlling urea 2y 2o 3: Eu 3+fluorescent material [Feng, H.-J., etal., MaterialsLetters, 2006.60 (6): 737-740.]; The people such as LizhuTong [15]by homogeneous phase solution at 180 DEG C of heating 8h, prepare Fe 3o 4y 2o 3: Eu 3+fluorescent material [Tong, L., etal., JournalofMaterialsScience, 2011.47 (1): 132-137].Although this method is relatively simple, but there are some shortcomings being difficult to overcome, such as, coating efficiency is low, and part rare-earth precipitation is scattered and can not be adsorbed in the solution; Be that physics is coated between coating layer and kernel, connect with molecular force, structure is not fine and close; Adding of tensio-active agent, for system introduces new foreign ion; Coating layer amount is difficult to control; And, if kernel reaches nano-scale, very easily to reunite in homogeneous phase solution, thus cannot be coated, therefore, find a kind of quick, simple, method prepares Core-shell structure material is efficiently need the problem of solution badly.
This patent proposes from sacrificing template synthesis magnesium oxide/rare earth oxide nucleocapsid structure flower-like nanometer matrix material, to be easy to magnesium hydroxide that is a large amount of, that prepare fast for template, while load hydrogen rare earth oxide, template is also consumed, and reaction process is quick, simple to operate, can prepare in a large number; Do not mix tensio-active agent in reaction process, avoid and introduce unnecessary foreign ion; By the pattern, the size that control the pattern of magnesium hydroxide template, size can control product; The clad structure of preparation is coated by chemical bond force, and clad structure is fine and close, and does not have free sedimentation, does not produce waste; In addition, add proportioning by what simply control reactant, can directly control coating layer amount, be a kind of quick, simple, efficient, easily large-scale promotion prepare clad structure MATERIALS METHODS.
At present from sacrificing template synthesis nano material, being mainly used in and preparing on one-dimentional structure material, hollow structure material, and studying very few in the application of three-dimensional structure material.If the people such as Li are with Cd (OH) 2nano wire, for certainly sacrificing template, by certainly sacrificing method, utilizes anionresin, and has prepared CdS nano-hollow pipe [Li, X., H.Chu, andY.Li, JournalofSolidStateChemistry, 2006.179 (1): 96-102]; The people such as YiLi utilize CdOHCl micron bar aggregation bunch for certainly sacrificing template, and glass dish has successfully been prepared CdX (X=S, Se) micron tube [Li, Y., etal. .JournalofSolidStateChemistry, 2004.177 (12): 4386-4393].The synthesis of the flower-shaped 3-D nano, structure of current nucleocapsid yet there are no bibliographical information.Mg (OH) 2as presoma kernel, thermal treatment obtains the nucleocapsid structure that MgO is kernel, load rare earth oxide, and the character fusing point of MgO is high, and stable in properties under the exciting of high temperature and light wave, is extremely suitable for doing inner nuclear material.
Summary of the invention
The object of the invention is the preparation method proposing a kind of magnesium oxide/rare earth oxide nucleocapsid structure flower-like nanometer matrix material, prepare flower-shaped Core-shell structure material simply, fast, efficiently.The method adopts Mg (OH) 2as certainly sacrificing template, on its surface, precipitation conversion reaction occurs, obtain presoma through cationic exchange, its reaction equation is:
3Mg(OH) 2+RE 3+→RE(OH) 3+3Mg 2+
Wherein, RE is one or more in Y, Sc, La, Ce, Pr, Nd, Po, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu.
Method of the present invention comprises the following steps:
(1) according to the magnesium oxide/preparation amount of rare earth oxide nucleocapsid structure flower-like nanometer matrix material and the stoichiometric ratio of rare earth element and magnesium thereof, the flower-shaped magnesium hydroxide being used as template of respective amount is taken;
(2) according to the magnesium oxide/preparation amount of rare earth oxide nucleocapsid structure flower-like nanometer matrix material and the stoichiometric ratio of rare earth element and magnesium thereof, the concentration of preparation respective volume is 0.01 ~ 0.2mol/L and pH value is the rare earths salt of 3 ~ 7;
(3) flower-shaped magnesium hydroxide prepared by step (1) is added in the earth solution that step (2) prepares, at room temperature, stirs after 20 ~ 120 minutes, filter, washing, at 60 ~ 100 DEG C, dry 120 ~ 240 minutes;
(4) product step (3) obtained, at 400 ~ 900 DEG C, is calcined 30 ~ 240 minutes, is obtained final product.
In the step (1) of preparation method of the present invention, the preparation of flower-shaped magnesium hydroxide is according to following steps: take the solution that appropriate magnesium salts is mixed with 2mol/L, under 20 ~ 60 DEG C of conditions, while stir, while drip 30% strong aqua in magnesium salt solution, when solution ph is 10.5, namely stop dripping ammoniacal liquor and stirring, the suspension liquid obtained at room temperature ageing 30 ~ 120 minutes, filter, wash, drying, obtains flower-shaped magnesium hydroxide, and magnesium salts used is one or more in magnesium sulfate, magnesium nitrate or magnesium chloride.
In the step (2) of preparation method of the present invention, the rare-earth salts prepared is one or more in the nitrate of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, yttrium or scandium, chlorate or vitriol; The nitrate of the corresponding rare earth of rare earths salt deionized water dissolving, muriate or vitriol are formulated, or formulated with the corresponding rare earth oxide of corresponding acid dissolve, oxyhydroxide or carbonated rare earth.
According to Lan Shi Chemical manual the 16 edition, Mg (OH) 2k spbe 5.61 × 10 -6, and RE (OH) 3k spmostly be less than 1 × 10 -22.Due to both huge spreads, Mg (OH) 2will be RE (OH) by spontaneous transformation in aqueous 3.According to calculation of thermodynamics, the variable quantity of this reaction standard Gibbs function is at normal temperatures and pressures about-65kJ/mol (Δ G<0), show at normal temperatures and pressures this thermodynamics of reactions to be spontaneous, research shows kinetically, this reaction can react completely in 30min, and speed is quick.Because magnesium hydroxide only has trace ionization in aqueous, therefore define an OH on its surface -the concentration gradient layer of ion, has maximum concentration on its surface, reduces gradually in solution, and therefore, first rare earth hydrate grows at the surface nucleation of magnesium hydroxide.Just because of rare earth hydrate by chemical reaction, be deposited directly to template surface, therefore coating layer and kernel coated by chemical bond force, molecular force connects finer and close; And magnesium hydroxide template is also consumed while conversion, do not need the process of follow-up removal template, simple to operate; Rare earth hydrate is all deposited on template surface, does not have free sedimentation, and coating efficiency is high, does not produce waste; In this reaction, do not use tensio-active agent, avoid the introducing of unnecessary foreign ion; The pattern of the product heredity well pattern of template, by the pattern of simple Control architecture, just can control product morphology.
The present invention has that preparation process is simple, mild condition, quick, spontaneous, do not use tensio-active agent, template is easy to a large amount of preparation, and the pattern of template, size can be entailed presoma and final product well, prepared product favorable dispersity, particle diameter is about 1 ~ 2 μm.The present invention relates to the fields such as luminescence, absorption, catalysis, to the preparation of nuclear-shell structured nano-composite material, there is important dissemination.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of prepared magnesium hydroxide template, and as seen from the figure, obtained magnesium hydroxide template is the spherical flower-like structure of particle diameter 1-2 μm.
Fig. 2 is the transmission electron microscope photo of prepared magnesium hydroxide template, and as seen from the figure, the flower-like structure of obtained magnesium hydroxide template is assembled by many nanometer sheet, and the thickness of sheet is about 10nm.
Fig. 3 is the XRD figure spectrum of prepared magnesium hydroxide template, and as shown in Figure 3, obtained magnesium hydroxide template and the characteristic diffraction peak of JCPDS44-1482 magnesium hydroxide coincide.
MgO/ (the Y of Fig. 4 prepared by embodiment 1 0.95eu 0.05) 2o 3the XRD figure spectrum of nucleocapsid structure flower-like nanometer matrix material.As seen from the figure, MgO and Y is had 2o 3the characteristic diffraction peak of two kinds of thing phases, due to Eu 3+enter Y 2o 3lattice, not there is Eu 2o 3characteristic diffraction peak.
MgO/ (the Y of Fig. 5 prepared by embodiment 1 0.95eu 0.05) 2o 3the stereoscan photograph of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, the obtained product heredity flower-like structure pattern of template, from the illustration in the upper right corner, petal surface is by one deck nano particle in load.
MgO/ (the Y of Fig. 6 prepared by embodiment 1 0.95eu 0.05) 2o 3the transmission electron microscope photo of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, obtained product is flower-like structure, and the surface of petal is by many nano particles in load.
MgO/ (the Y of Fig. 7 prepared by embodiment 1 0.95eu 0.05) 2o 3the high-resolution-ration transmission electric-lens photo of nucleocapsid structure flower-like nanometer matrix material monolithic petal, as seen from the figure, the obtained every sheet petal of product is a monocrystalline, and the spacing of inner material is 0.211nm, correspond to (200) crystal face of MgO; The spacing of the nanoparticle of load is above 0.306nm, correspond to Y 2o 3: Eu 3+(222) crystal face.
MgO/ (the Y of Fig. 8 prepared by embodiment 1 0.95eu 0.05) 2o 3the electron diffraction photo of nucleocapsid structure flower-like nanometer matrix material monolithic petal, as seen from the figure, the spacing that inner diffraction ring is corresponding is 0.211nm, correspond to Y 2o 3: Eu 3+(222) crystal face; The spacing that outside diffraction spot is corresponding is 0.306nm, correspond to (200) crystal face of MgO.This result is consistent with the result that high-resolution-ration transmission electric-lens is observed.
MgO/ (the Y of Fig. 9 prepared by embodiment 2 0.97tb 0.03) 2o 3the XRD figure spectrum of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, has MgO and Y 2o 3the characteristic diffraction peak of two kinds of thing phases, due to Tb 3+enter Y 2o 3lattice, there is not the characteristic diffraction peak of Tb oxide compound.
MgO/ (the Y of Figure 10 prepared by embodiment 2 0.97tb 0.03) 2o 3the stereoscan photograph of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, the obtained product heredity flower-like structure pattern of template, and petal surface is by one deck (Y in load 0.97tb 0.03) 2o 3nano particle.
The MgO/Pr of Figure 11 prepared by embodiment 3 6o 11the XRD figure spectrum of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, has MgO and Pr in obtained product 6o 11the characteristic diffraction peak of two kinds of thing phases.
The MgO/Pr of Figure 12 prepared by embodiment 3 6o 11the stereoscan photograph of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, the obtained product heredity flower-like structure pattern of template, and petal surface is by one deck Pr in load 6o 11nanoparticle.
The MgO/Nd of Figure 13 prepared by embodiment 4 2o 3the XRD figure spectrum of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, has MgO and Nd in obtained product 2o 3the characteristic diffraction peak of two kinds of thing phases.
The MgO/Nd of Figure 14 prepared by embodiment 4 2o 3the stereoscan photograph of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, the obtained product heredity flower-like structure pattern of template, and petal surface is by one deck Nd in load 2o 3nanoparticle.
The MgO/Gd of Figure 15 prepared by embodiment 5 2o 3the XRD figure spectrum of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, has MgO and Gd in obtained product 2o 3the characteristic diffraction peak of two kinds of thing phases.
The MgO/Gd of Figure 16 prepared by embodiment 5 2o 3the stereoscan photograph of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, the obtained product heredity flower-like structure pattern of template, and petal surface is by one deck Gd in load 2o 3nano particle.
The MgO/Dy of Figure 17 prepared by embodiment 6 2o 3the XRD figure spectrum of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, has MgO and Dy in obtained product 2o 3the characteristic diffraction peak of two kinds of thing phases.
The MgO/Dy of Figure 18 prepared by embodiment 6 2o 3the stereoscan photograph of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, the obtained product heredity flower-like structure pattern of template, and petal surface is by one deck Dy in load 2o 3nanoparticle.
The MgO/Ho of Figure 19 prepared by embodiment 7 2o 3the XRD figure spectrum of nucleocapsid structure flower-like nanometer matrix material.As seen from the figure, MgO and Ho is had in obtained product 2o 3the characteristic diffraction peak of two kinds of thing phases.
The MgO/Ho of Figure 20 prepared by embodiment 7 2o 3the stereoscan photograph of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, the obtained product heredity flower-like structure pattern of template, and petal surface is by one deck Ho in load 2o 3nanoparticle.
The MgO/Er of Figure 21 prepared by embodiment 8 2o 3the XRD figure spectrum of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, has MgO and Er in obtained product 2o 3the characteristic diffraction peak of two kinds of thing phases.
The MgO/Er of Figure 22 prepared by embodiment 8 2o 3the stereoscan photograph of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, the obtained product heredity flower-like structure pattern of template, and petal surface is by one deck Er in load 2o 3nanoparticle.
The MgO/Tm of Figure 23 prepared by embodiment 9 2o 3the XRD figure spectrum of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, has MgO and Tm in obtained product 2o 3the characteristic diffraction peak of two kinds of thing phases.
The MgO/Tm of Figure 24 prepared by embodiment 9 2o 3the stereoscan photograph of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, the obtained product heredity flower-like structure pattern of template, and petal surface is by one deck Tm in load 2o 3nanoparticle.
The MgO/Yb of Figure 25 prepared by embodiment 10 2o 3the XRD figure spectrum of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, has MgO and Yb in obtained product 2o 3the characteristic diffraction peak of two kinds of thing phases.
The MgO/Yb of Figure 26 prepared by embodiment 10 2o 3the stereoscan photograph of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, the obtained product heredity flower-like structure pattern of template, and petal surface is by one deck Yb in load 2o 3nanoparticle.
The MgO/Lu of Figure 27 prepared by embodiment 11 2o 3the XRD figure spectrum of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, has MgO and Lu in obtained product 2o 3the characteristic diffraction peak of two kinds of thing phases.
The MgO/Lu of Figure 28 prepared by embodiment 11 2o 3the stereoscan photograph of nucleocapsid structure flower-like nanometer matrix material, as seen from the figure, the obtained product heredity flower-like structure pattern of template, and petal surface is by one deck Pr in load 6o 11nanoparticle.
Embodiment
The present invention will be described further by following examples.
The Preparation and characterization of flower-shaped magnesium hydroxide template, takes 48.1475gMgSO 4powder, is mixed with the MgSO of 200ml2mol/L 4solution, under 60 DEG C of water bath condition, while stir, in solution, dropwise drip mass concentration is 30% strong aqua, when the pH value of solution arrives 10.5, namely stop dripping ammoniacal liquor and stirring, the suspension liquid obtained is ageing 120min at room temperature, filters, washing, 80 DEG C of dry 240min, obtain flower-shaped magnesium hydroxide.Prepared magnesium hydroxide adopts scanning electronic microscope, transmission electron microscope and X-ray diffractometer to characterize respectively, and result respectively as shown in Figure 1, Figure 2, Figure 3 shows.
Embodiment 1.
According to MgO/ (Y 0.95eu 0.05) 2o 3the preparation amount 1.0000g of nucleocapsid structure flower-like nanometer matrix material and composition formula Mg thereof 0.70y 0.19eu 0.01the stoichiometric ratio of magnesium and rare earth in O, takes the flower-shaped magnesium hydroxide template of 1.1662g, and the concentration of preparation 50ml is 0.08mol/L and pH value is the (Y of 6 0.95eu 0.05) (NO 3) 3solution, adds (Y by flower-shaped magnesium hydroxide 0.95eu 0.05) (NO 3) 3in solution, at room temperature, stir after 60 minutes, filter, wash, at 80 DEG C, dry 240 minutes, finally at 800 DEG C, calcine 60 minutes, obtain final product.
Embodiment 2.
According to MgO/ (Y 0.97tb 0.03) 2o 3the preparation amount 1.0000g of nucleocapsid structure flower-like nanometer matrix material and composition formula Mg thereof 0.700y 0194tb 0.006the stoichiometric ratio of magnesium and rare earth in O, takes the flower-shaped magnesium hydroxide template of 1.1662g, and the concentration of preparation 50ml is 0.08mol/L and pH value is the (Y of 6 0.97tb 0.03) (NO 3) 3solution, adds (Y by flower-shaped magnesium hydroxide 0.97tb 0.03) (NO 3) 3in solution, at room temperature, stir after 60 minutes, filter, wash, at 80 DEG C, dry 240 minutes, finally at 800 DEG C, calcine 60 minutes, obtain final product.
Embodiment 3.
According to MgO/Pr 6o 11the preparation amount 1.0000g of nucleocapsid structure flower-like nanometer matrix material and chemical formula Mg thereof 0.70pr 0.20the stoichiometric ratio of magnesium and praseodymium in O, takes the flower-shaped magnesium hydroxide template of 1.1662g, preparation 50ml concentration be 0.08mol/L and pH value be 6 Pr (NO 3) 3solution, adds Pr (NO by flower-shaped magnesium hydroxide 3) 3in solution, at room temperature, stir after 60 minutes, filter, wash, at 80 DEG C, dry 240 minutes, finally at 800 DEG C, calcine 60 minutes, obtain final product.
Embodiment 4.
According to MgO/Nd 2o 3the preparation amount 1.0000g of nucleocapsid structure flower-like nanometer matrix material and composition formula Mg thereof 0.70nd 0.20the stoichiometric ratio of magnesium and neodymium in O, takes the flower-shaped magnesium hydroxide template of 1.1662g, preparation 50ml concentration be 0.08mol/L and pH value be 6 Nd (NO 3) 3solution, adds Nd (NO by flower-shaped magnesium hydroxide 3) 3in solution, at room temperature, stir after 60 minutes, filter, wash, at 80 DEG C, dry 240 minutes, finally at 800 DEG C, calcine 60 minutes, obtain final product.
Embodiment 5.
According to MgO/Gd 2o 3the preparation amount 1.0000g of nucleocapsid structure flower-like nanometer matrix material and composition formula Mg thereof 0.70gd 0.20the stoichiometric ratio of magnesium and gadolinium in O, takes the flower-shaped magnesium hydroxide template of 1.1662g, preparation 50ml concentration be 0.08mol/L and pH value be 6 Gd (NO 3) 3solution, adds Gd (NO by flower-shaped magnesium hydroxide 3) 3in solution, at room temperature, stir after 60 minutes, filter, wash, at 80 DEG C, dry 240 minutes, finally at 800 DEG C, calcine 60 minutes, obtain final product.
Embodiment 6.
According to MgO/Dy 2o 3the preparation amount 1.0000g of nucleocapsid structure flower-like nanometer matrix material and composition formula Mg thereof 0.70gd 0.20the stoichiometric ratio of magnesium and dysprosium in O, takes the flower-shaped magnesium hydroxide template of 1.1662g, preparation 50ml concentration be 0.08mol/L and pH value be 6 Dy (NO 3) 3solution, adds Dy (NO by flower-shaped magnesium hydroxide 3) 3in solution, at room temperature, stir after 60 minutes, filter, wash, at 80 DEG C, dry 240 minutes, finally at 800 DEG C, calcine 60 minutes, obtain final product.
Embodiment 7.
According to MgO/Ho 2o 3the preparation amount 1.0000g of nucleocapsid structure flower-like nanometer matrix material and composition formula Mg thereof 0.70ho 0.20the stoichiometric ratio of magnesium and holmium in O, takes the flower-shaped magnesium hydroxide template of 1.1662g, preparation 50ml concentration be 0.08mol/L and pH value be 6 Ho (NO 3) 3solution, adds Ho (NO by flower-shaped magnesium hydroxide 3) 3in solution, at room temperature, stir after 60 minutes, filter, wash, at 80 DEG C, dry 240 minutes, finally at 800 DEG C, calcine 60 minutes, obtain final product.
Embodiment 8.
According to MgO/Er 2o 3the preparation amount 1.0000g of nucleocapsid structure flower-like nanometer matrix material and composition formula Mg thereof 0.70er 0.20the stoichiometric ratio of magnesium and erbium in O, takes the flower-shaped magnesium hydroxide template of 1.1662g, preparation 50ml concentration be 0.08mol/L and pH value be 6 Er (NO 3) 3solution, adds Er (NO by flower-shaped magnesium hydroxide 3) 3in solution, at room temperature, stir after 60 minutes, filter, wash, at 80 DEG C, dry 240 minutes, finally at 800 DEG C, calcine 60 minutes, obtain final product.
Embodiment 9.
According to MgO/Tm 2o 3the preparation amount 1.0000g of nucleocapsid structure flower-like nanometer matrix material and composition formula Mg thereof 0.70tm 0.20the stoichiometric ratio of magnesium and thulium in O, takes the flower-shaped magnesium hydroxide template of 1.1662g, preparation 50ml concentration be 0.08mol/L and pH value be 6 Tm (NO 3) 3solution, adds Tm (NO by flower-shaped magnesium hydroxide 3) 3in solution, at room temperature, stir after 60 minutes, filter, wash, at 80 DEG C, dry 240 minutes, finally at 800 DEG C, calcine 60 minutes, obtain final product.
Embodiment 10.
According to MgO/Yb 2o 3the preparation amount 1.0000g of nucleocapsid structure flower-like nanometer matrix material and composition formula Mg thereof 0.70yb 0.20the stoichiometric ratio of magnesium and ytterbium in O, takes the flower-shaped magnesium hydroxide template of 1.1662g, preparation 50ml concentration be 0.08mol/L and pH value be 6 Yb (NO 3) 3solution, adds Yb (NO by flower-shaped magnesium hydroxide 3) 3in solution, at room temperature, stir after 60 minutes, filter, wash, at 80 DEG C, dry 240 minutes, finally at 800 DEG C, calcine 60 minutes, obtain final product.
Embodiment 11.
According to MgO/Lu 2o 3the preparation amount 1.0000g of nucleocapsid structure flower-like nanometer matrix material and composition formula Mg thereof 0.70lu 0.20the stoichiometric ratio of magnesium and lutetium in O, takes the flower-shaped magnesium hydroxide template of 1.1662g, preparation 50ml concentration be 0.08mol/L and pH value be 6 Lu (NO 3) 3solution, adds Lu (NO by flower-shaped magnesium hydroxide 3) 3in solution, at room temperature, stir after 60 minutes, filter, wash, at 80 DEG C, dry 240 minutes, finally at 800 DEG C, calcine 60 minutes, obtain final product.

Claims (1)

1. a preparation method for magnesium oxide/rare earth oxide nucleocapsid structure flower-like nanometer matrix material, is characterized in that comprising the following steps:
(1) according to the magnesium oxide/preparation amount of rare earth oxide nucleocapsid structure flower-like nanometer matrix material and the stoichiometric ratio of rare earth element and magnesium thereof, the flower-shaped magnesium hydroxide being used as template of respective amount is taken;
(2) according to the magnesium oxide/preparation amount of rare earth oxide nucleocapsid structure flower-like nanometer matrix material and the stoichiometric ratio of rare earth element and magnesium thereof, the concentration of preparation respective volume is 0.01 ~ 0.2mol/L and pH value is the rare earths salt of 3 ~ 7;
(3) flower-shaped magnesium hydroxide prepared by step (1) is added in the earth solution that step (2) prepares, at room temperature, stirs after 20 ~ 120 minutes, filter, washing, at 60 ~ 100 DEG C, dry 120 ~ 240 minutes;
(4) product step (3) obtained, at 400 ~ 900 DEG C, is calcined 30 ~ 240 minutes, is obtained final product;
In step (1), the preparation of flower-shaped magnesium hydroxide is according to following steps: take the solution that appropriate magnesium salts is mixed with 2mol/L, under 20 ~ 60 DEG C of conditions, while stir, while drip 30% strong aqua in magnesium salt solution, when solution ph is 10.5, namely stop dripping ammoniacal liquor and stirring, the suspension liquid obtained at room temperature ageing 30 ~ 120 minutes, filter, wash, drying, obtains flower-shaped magnesium hydroxide, and magnesium salts used is one or more in magnesium sulfate, magnesium nitrate or magnesium chloride;
In step (2), the rare-earth salts prepared is one or more in the nitrate of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, yttrium or scandium, chlorate or vitriol; The nitrate of the corresponding rare earth of rare earths salt deionized water dissolving, muriate or vitriol are formulated, or formulated with the corresponding rare earth oxide of corresponding acid dissolve, oxyhydroxide or carbonated rare earth.
CN201510597046.0A 2015-09-17 2015-09-17 A kind of preparation method of magnesia/rare earth oxide core shell structure flower-like nanometer composite Active CN105152192B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510597046.0A CN105152192B (en) 2015-09-17 2015-09-17 A kind of preparation method of magnesia/rare earth oxide core shell structure flower-like nanometer composite

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510597046.0A CN105152192B (en) 2015-09-17 2015-09-17 A kind of preparation method of magnesia/rare earth oxide core shell structure flower-like nanometer composite

Publications (2)

Publication Number Publication Date
CN105152192A true CN105152192A (en) 2015-12-16
CN105152192B CN105152192B (en) 2016-08-24

Family

ID=54793320

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510597046.0A Active CN105152192B (en) 2015-09-17 2015-09-17 A kind of preparation method of magnesia/rare earth oxide core shell structure flower-like nanometer composite

Country Status (1)

Country Link
CN (1) CN105152192B (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110560026A (en) * 2019-09-19 2019-12-13 江苏晶晶新材料有限公司 preparation method and application of magnesium oxide solid base anthraquinone degradation product regeneration catalyst
CN111392780A (en) * 2020-03-26 2020-07-10 陈宛莎 Composite oxide nano-particles capable of emitting THz frequency and preparation method thereof
CN113816480A (en) * 2021-10-09 2021-12-21 中国铝业股份有限公司 Medicament and method for removing fluorine from mixed solution containing sulfate and fluoride ions
US20220225610A1 (en) * 2019-07-15 2022-07-21 Aqua Resources Corporation Hydroxides monolayer nanoplatelet and methods of preparing same

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5914287A (en) * 1996-12-06 1999-06-22 Shin-Etsu Chemical Co., Ltd. Hydroxide-coated rare earth oxide particles
CN104070141A (en) * 2014-05-24 2014-10-01 芜湖浙鑫新能源有限公司 Rare earth coated and magnesium oxide based ceramic core
CN104313664A (en) * 2014-09-30 2015-01-28 扬州大学 Surface treatment method for rare earth magnesium alloy product

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5914287A (en) * 1996-12-06 1999-06-22 Shin-Etsu Chemical Co., Ltd. Hydroxide-coated rare earth oxide particles
CN104070141A (en) * 2014-05-24 2014-10-01 芜湖浙鑫新能源有限公司 Rare earth coated and magnesium oxide based ceramic core
CN104313664A (en) * 2014-09-30 2015-01-28 扬州大学 Surface treatment method for rare earth magnesium alloy product

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20220225610A1 (en) * 2019-07-15 2022-07-21 Aqua Resources Corporation Hydroxides monolayer nanoplatelet and methods of preparing same
CN110560026A (en) * 2019-09-19 2019-12-13 江苏晶晶新材料有限公司 preparation method and application of magnesium oxide solid base anthraquinone degradation product regeneration catalyst
CN111392780A (en) * 2020-03-26 2020-07-10 陈宛莎 Composite oxide nano-particles capable of emitting THz frequency and preparation method thereof
CN111392780B (en) * 2020-03-26 2023-04-25 陈宛莎 Composite oxide nano particle capable of emitting THz frequency and preparation method thereof
CN113816480A (en) * 2021-10-09 2021-12-21 中国铝业股份有限公司 Medicament and method for removing fluorine from mixed solution containing sulfate and fluoride ions
CN113816480B (en) * 2021-10-09 2023-10-24 中国铝业股份有限公司 Medicament and method for removing fluorine from mixed solution containing sulfate radical and fluorine ions

Also Published As

Publication number Publication date
CN105152192B (en) 2016-08-24

Similar Documents

Publication Publication Date Title
Li et al. Uniform colloidal spheres for (Y1− x Gd x) 2O3 (x= 0–1): Formation mechanism, compositional impacts, and physicochemical properties of the oxides
CN103317141B (en) Method for preparing metal nanoparticles
CN100462307C (en) Method for preparation of niobic acid zinc nano material
CN103407969B (en) A kind of three-dimensional ordered macroporous-gas-phase permeation-precipitation method of mesopore metal oxide or composite oxides and products obtained therefrom
CN103418316A (en) Preparation method of modified micro-granules
CN105152192A (en) Preparation method of magnesium oxide/rare-earth oxide core-shell-structure flower-like nano composite material
CN109678193B (en) Preparation method of nano cerium oxide particles
CN112239223B (en) Preparation method of rare earth oxide powder with large specific surface area
Zhao et al. Inorganic-salt-induced morphological transformation and luminescent performance of GdF 3 nanostructures
CN108083316A (en) A kind of preparation method of nano rareearth oxidate powder body
CN100411996C (en) Method for preparting Nano powder of zirconia
CN102134089B (en) Fusiform large-scale cerium based composite oxide powder and preparation method thereof
CN101381092A (en) Method for preparing large granularity and large specific surface area spherical yttrium oxide
CN101665503B (en) Rare earth coordination compound, rare earth oxide and preparing method thereof
CN101260299A (en) Method for preparing yttrium gadolinium oxide and europium nano luminescent powder by micro-emulsion method
CN102659154A (en) Method for preparing nano alpha-Al2O3 powder
KR101734300B1 (en) Method for producing metal/ceramic nanostructure, metal/ceramic nanostructure produced by the same, and catalyst containing the same
CN103025847B (en) Metal nano particles doped with silicate luminescent materials and preparation methods thereof
CN109879305B (en) Preparation of micron-sized monodisperse LaAlO3:xMm+Method for producing spherical particles
CN102992377A (en) Method for preparing nano rare earth oxide through microwave sol-gel technology
CN102583495B (en) Preparation method of rare earth metal ion doping cerium oxide nanometer material
CN102115213B (en) Method for preparing cobaltosic oxide nanorod by using microemulsion
CN103508492B (en) Method for rapidly preparing NdWO4(OH) nanopowder
CN103771482B (en) A kind of preparation method of high-purity nanometer yttrium aluminium garnet powder
CN100503775C (en) Preparation of nanometer spherical red CaSiO3:Eu3+ phosphor

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