CN104649243A - Nickel phosphate hollow nanospheres and preparation method thereof - Google Patents
Nickel phosphate hollow nanospheres and preparation method thereof Download PDFInfo
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- CN104649243A CN104649243A CN201510072709.7A CN201510072709A CN104649243A CN 104649243 A CN104649243 A CN 104649243A CN 201510072709 A CN201510072709 A CN 201510072709A CN 104649243 A CN104649243 A CN 104649243A
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Abstract
The invention discloses nickel phosphate hollow nanospheres and a preparation method thereof. The preparation method comprises the following steps: contacting soluble dihydric phosphate with a nickel salt in a solution system, reacting under a hydro-thermal reaction condition, and then cooling, washing and drying to obtain the nickel phosphate hollow nanospheres. The nickel phosphate hollow nanospheres prepared by the method disclosed by the invention has the characteristics of large specific area which can reach 250-300m<2>/g.
Description
Technical field
The present invention relates to inorganic functional nano material technical field, particularly relate to a kind of nickelous phosphate hollow nanospheres and preparation method thereof.
Background technology
Phosphoric acid salt enriches backbone element because it has, therefore has wide application prospect at optical, electrical, magnetic and catalytic field, and therefore phosphatic synthesis receives much concern.Nickelous phosphate, except above-mentioned performance, also can be used as pigment and plated material.But relative to tertiary iron phosphate, the research of nickelous phosphate is relative less with report.Hollow nanostructures has greater advantage at application methodes such as electrode materials, pigment, absorption greatly because of its specific surface area.There is not been reported in the research of the current Hollow nanosphere material about nickelous phosphate.
Summary of the invention
The invention provides a kind of method that step prepares nickelous phosphate hollow nanospheres simply and the nickelous phosphate hollow nanospheres prepared.
According to a first aspect of the invention, the invention provides a kind of preparation method of nickelous phosphate hollow nanospheres, be included in solution system, soluble phosphoric acid dihydric salt is contacted with nickel salt, react under hydrothermal reaction condition, then cool, wash, drying obtains nickelous phosphate hollow nanospheres.
As preferred version of the present invention, the mol ratio of soluble phosphoric acid dihydric salt and nickel salt is 1:0.5 ~ 1:1.5.
As preferred version of the present invention, the temperature of hydro-thermal reaction is 150 ~ 220 DEG C.
As preferred version of the present invention, the time of hydro-thermal reaction is 4 ~ 20 hours, is more preferably 12 hours.
As preferred version of the present invention, the aqueous solution of soluble phosphoric acid dihydric salt is contacted with the aqueous solution of nickel salt; More preferably the aqueous solution of soluble phosphoric acid dihydric salt and the aqueous solution of nickel salt is made.
As preferred version of the present invention, soluble phosphoric acid dihydric salt is selected from the combination of a kind of in primary ammonium phosphate, monometallic, SODIUM PHOSPHATE, MONOBASIC and potassium primary phosphate or at least two kinds.
As preferred version of the present invention, nickel salt is selected from the combination of a kind of in nickelous acetate, nickelous nitrate and single nickel salt or at least two kinds.
As preferred version of the present invention, the concentration of soluble phosphoric acid dihydric salt is 0.02 ~ 0.1mol/L.
As preferred version of the present invention, the concentration of nickel salt is 0.02 ~ 0.1mol/L.
As preferred version of the present invention, be cooled to naturally cooling.
As preferred version of the present invention, wash as adopting water and ethanol to wash successively; More preferably, wash as adopting water and ethanol to wash more than 3 times successively.
As preferred version of the present invention, dry for drying.
As preferred version of the present invention, hydro-thermal reaction is carried out in nonmetal reaction vessel, preferably carries out in polytetrafluoro container.
According to a second aspect of the invention, the invention provides a kind of nickelous phosphate hollow nanospheres prepared according to the method for first aspect.
As preferred version of the present invention, nickelous phosphate hollow nanospheres diameter is 200 ~ 400 nanometers.
The present invention adopts soluble phosphoric acid dihydric salt and nickel salt obtained nickelous phosphate hollow nanospheres under hydrothermal conditions, and nickelous phosphate nanometer ball prepared by the method has unique hollow structure, and specific surface area is large.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of nickelous phosphate hollow nanospheres prepared by the embodiment of the present invention 1.
Fig. 2 is the X-ray powder diffraction figure of nickelous phosphate hollow nanospheres prepared by the embodiment of the present invention 1, shows the curved line relation at diffraction peak intensity (Intensity) and 2 θ (2theta) angle, wherein degree expressing degree (°).
Fig. 3 is the nitrogen adsorption desorption figure of nickelous phosphate hollow nanospheres prepared by the embodiment of the present invention 1, show curved line relation and the pore size distribution situation of adsorption volume (Volume adsorbed) and relative pressure (Relative pressure), wherein adsorption represents absorption, desorption represents desorption, and Pore Diamete represents aperture.
Embodiment
By reference to the accompanying drawings the present invention is described in further detail below by embodiment.
One of design of most critical of the present invention is: adopt soluble phosphoric acid dihydric salt and nickel salt obtained nickelous phosphate hollow nanospheres under hydrothermal conditions.
The present invention further conceives and is: under controlling the type of precursor and the hydrothermal condition of ratio and temperature of reaction, prepare nickelous phosphate hollow nanospheres.
The present invention's detailed embodiment is described as follows:
A preparation method for nickelous phosphate hollow nanospheres, is included in solution system, soluble phosphoric acid dihydric salt is contacted with nickel salt, reacts, then cool, wash under hydrothermal reaction condition, drying obtains nickelous phosphate hollow nanospheres.
Contriver determines through further investigation, and the mol ratio of soluble phosphoric acid dihydric salt and nickel salt can obtain best effect in the scope of 1:0.5 ~ 1:1.5.Although also can obtain end product nickelous phosphate hollow nanospheres below or above this scope, and nickelous phosphate nanometer ball has unique hollow structure, and specific surface area is also relatively large.But the successful that the mol ratio of soluble phosphoric acid dihydric salt and nickel salt obtains in the scope of 1:0.5 ~ 1:1.5 is better than the effect beyond above-mentioned scope, show that nanometer sheet area is larger, hollow nanospheres structure evenly.The mol ratio of soluble phosphoric acid dihydric salt and nickel salt can be 1:0.52,1:0.55,1:0.6,1:0.8,1:0.9,1:1,1:1.1,1:1.2,1:1.25,1:1.35,1:1.42,1:1.45,1:1.48 etc.
Contriver determines through further investigation, and the temperature of hydro-thermal reaction can obtain best effect in the scope of 150 ~ 220 DEG C.Although also can obtain end product nickelous phosphate hollow nanospheres below or above this scope, and nickelous phosphate nanometer ball has unique hollow structure, and specific surface area is also relatively large.But the successful that the temperature of hydro-thermal reaction obtains in the scope of 150 ~ 220 DEG C is better than the effect beyond above-mentioned scope, show that nanometer sheet area is larger, hollow nanospheres structure evenly.The temperature of hydro-thermal reaction can be 152 DEG C, 158 DEG C, 160 DEG C, 165 DEG C, 168 DEG C, 175 DEG C, 180 DEG C, 188 DEG C, 192 DEG C, 194 DEG C, 197 DEG C, 203 DEG C, 207 DEG C, 209 DEG C, 212 DEG C, 215 DEG C, 217 DEG C, 219 DEG C etc.
The time of hydro-thermal reaction can obtain good effect in the scope of 4 ~ 20 hours, is preferably 12 hours.The time of hydro-thermal reaction specifically needs to make the appropriate adjustments according to the temperature of hydro-thermal reaction, if the temperature of hydro-thermal reaction is higher, the time of corresponding hydro-thermal reaction should be more relatively low, and vice versa.Time of hydro-thermal reaction can be 5 hours, 6 hours, 7 hours, 8 hours, 9 hours, 12 hours, 14 hours, 15 hours, 17 hours, 18.5 hours, 19.5 hours etc.
Typical case but the hydrothermal temperature of indefiniteness and time is such as: 160 DEG C of reactions, 18 hours, 170 DEG C reactions, 16 hours, 190 DEG C reactions, 14 hours, 200 DEG C reactions, 12 hours, 210 DEG C reactions, 10 hours, 215 DEG C reactions, 8 hours, 220 DEG C reactions 6 hours etc.
The reaction of one embodiment of the invention is carried out in solution system, the mode that wherein soluble phosphoric acid dihydric salt contacts with nickel salt can have multiple, such as in the aqueous solution of soluble phosphoric acid dihydric salt, add nickel salt to react, in the aqueous solution of nickel salt, add soluble phosphoric acid dihydric salt react, to solvent (as water) is simultaneously middle or priority adds soluble phosphoric acid dihydric salt and nickel salt reacts, the aqueous solution adding nickel salt in the aqueous solution of soluble phosphoric acid dihydric salt reacts, the aqueous solution adding soluble phosphoric acid dihydric salt in the aqueous solution of nickel salt reacts, etc..And the form of mixing or dropping can be adopted to contact, and that is, can be directly mixed with another kind of reactant by a kind of reactant, also can be added dropwise in another kind of reactant by a kind of reactant.As preferred version of the present invention, the aqueous solution of soluble phosphoric acid dihydric salt is contacted with the aqueous solution of nickel salt; More preferably the aqueous solution of soluble phosphoric acid dihydric salt and the aqueous solution of nickel salt is made.Contriver determines through further investigation, adopts the mode of the aqueous solution of soluble phosphoric acid dihydric salt and the aqueous solution of nickel salt can obtain best effect, shows that nanometer sheet area is large, hollow nanospheres even structure.
In one embodiment of the invention, soluble phosphoric acid dihydric salt can be selected from the combination of a kind of in primary ammonium phosphate, monometallic, SODIUM PHOSPHATE, MONOBASIC and potassium primary phosphate or at least two kinds.Described combination typical case but the example of indefiniteness be such as: the combination of primary ammonium phosphate and monometallic, the combination of primary ammonium phosphate and SODIUM PHOSPHATE, MONOBASIC, the combination of primary ammonium phosphate and potassium primary phosphate, the combination of monometallic and SODIUM PHOSPHATE, MONOBASIC, the combination of monometallic and potassium primary phosphate, the combination of SODIUM PHOSPHATE, MONOBASIC and potassium primary phosphate, primary ammonium phosphate, the combination of monometallic and SODIUM PHOSPHATE, MONOBASIC, primary ammonium phosphate, the combination of SODIUM PHOSPHATE, MONOBASIC and potassium primary phosphate, monometallic, the combination of SODIUM PHOSPHATE, MONOBASIC and potassium primary phosphate, primary ammonium phosphate, monometallic, the combination of SODIUM PHOSPHATE, MONOBASIC and potassium primary phosphate, etc..It should be noted that, in the present invention, soluble phosphoric acid dihydric salt is not limited to above-mentioned four kinds, but considers from the quality of product and the angle of cost, preferably above-mentioned four kinds.
In one embodiment of the invention, nickel salt is selected from the combination of a kind of in nickelous acetate, nickelous nitrate and single nickel salt or at least two kinds.Described combination typical case but the example of indefiniteness be such as: the combination of nickelous acetate and nickelous nitrate, the combination of nickelous acetate and single nickel salt, the combination of nickelous nitrate and single nickel salt, the combination of nickelous acetate, nickelous nitrate and single nickel salt.It should be noted that, in the present invention, nickel salt is not limited to above-mentioned three kinds, but considers from the quality of product and the angle of cost, preferably above-mentioned three kinds.
In one embodiment of the invention, the concentration of soluble phosphoric acid dihydric salt is 0.02 ~ 0.1mol/L, such as 0.03mol/L, 0.04mol/L, 0.06mol/L, 0.075mol/L, 0.08mol/L, 0.085mol/L, 0.09mol/L, 0.095mol/L, 0.098mol/L etc.
In one embodiment of the invention, the concentration of nickel salt is 0.02 ~ 0.1mol/L, such as 0.03mol/L, 0.04mol/L, 0.06mol/L, 0.075mol/L, 0.08mol/L, 0.085mol/L, 0.09mol/L, 0.095mol/L, 0.098mol/L etc.
In one embodiment of the invention, cooling step can be adopted and carry out in various manners, can be low temperature (such as 4 DEG C) cooling, also can be normal temperature (such as 25 DEG C) cooling etc.; Can be auxiliary temperature-reducing cooling (as cooled in refrigerator), also can be naturally cooling.As preferred version of the present invention, be cooled to naturally cooling.
In one embodiment of the invention, wash as adopting water and ethanol to wash successively; More preferably wash more than 3 times successively, as 4 times, 5 times or 8 inferior.
In one embodiment of the invention, drying step can be adopted and carry out in various manners, such as, can adopt drying mode, or natural air drying mode.As preferred version of the present invention, dry for drying.
The present inventor finds in an experiment, and foreign ion can cause the reduction of nickelous phosphate hollow nanospheres product qualities, and reaction vessel is one of important channel of foreign ion introducing.Therefore, contriver determines through further investigation, and hydro-thermal reaction carries out obtaining good effect in nonmetal reaction vessel, preferably carries out in polytetrafluoro container.
Describe the present invention in detail below by specific embodiment, should be appreciated that embodiment is only exemplary, can not limiting the scope of the invention be interpreted as.
Embodiment 1
Respectively the ammonium dihydrogen phosphate aqueous solution of 0.04 mol/L of 20ml and the nickelous acetate of the 0.04mol/L of 20ml are mixed, to be transferred in the polytetrafluoro container of 50 milliliters and to be fixed on (polytetrafluoro container in stainless reactor, avoid the metal ion using metal vessel to participate in reaction and produce pollution), then with baking oven directly at 180 DEG C, heat 12 hours, when the temperature of question response still is reduced to room temperature naturally, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing in 60 DEG C of baking ovens dry 10 hours, namely nickelous phosphate hollow nanospheres is obtained.Fig. 1 is the transmission electron microscope photo of nickelous phosphate hollow nanospheres prepared by the present embodiment 1.As shown in Figure 1, the diameter of hollow nanospheres is 200-400 nanometer.Fig. 2 is the X-ray powder diffraction figure of nickelous phosphate hollow nanospheres.Fig. 3 is the nitrogen adsorption desorption figure of nickelous phosphate hollow nanospheres, and specific surface area is 300m
2/ g.
Embodiment 2
Respectively the ammonium dihydrogen phosphate aqueous solution of 0.04 mol/L of 20ml and the nickelous acetate of the 0.02mol/L of 20ml are mixed, to be transferred in the polytetrafluoro container of 50 milliliters and to be fixed on (polytetrafluoro container in stainless reactor, avoid the metal ion using metal vessel to participate in reaction and produce pollution), then with baking oven directly at 180 DEG C, heat 12 hours, when the temperature of question response still is reduced to room temperature naturally, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing in 60 DEG C of baking ovens dry 10 hours, namely the nickelous phosphate hollow nanospheres that diameter is 200-400 nanometer is obtained, specific surface is 284 m
2/ g.The transmission electron microscope photo of nickelous phosphate hollow nanospheres prepared by the present embodiment and X-ray powder diffraction figure similar to Example 1.
Embodiment 3
Respectively the ammonium dihydrogen phosphate aqueous solution of 0.04 mol/L of 20ml and the nickelous acetate of the 0.06mol/L of 20ml are mixed, to be transferred in the polytetrafluoro container of 50 milliliters and to be fixed on (polytetrafluoro container in stainless reactor, avoid the metal ion using metal vessel to participate in reaction and produce pollution), then with baking oven directly at 180 DEG C, heat 12 hours, when the temperature of question response still is reduced to room temperature naturally, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing in 60 DEG C of baking ovens dry 10 hours, namely the nickelous phosphate hollow nanospheres that diameter is 200-400 nanometer is obtained, specific surface is 279 m
2/ g.The transmission electron microscope photo of nickelous phosphate hollow nanospheres prepared by the present embodiment and X-ray powder diffraction figure similar to Example 1.
Embodiment 4
Respectively the ammonium dihydrogen phosphate aqueous solution of 0.1 mol/L of 20ml and the nickelous acetate of the 0.1mol/L of 20ml are mixed, to be transferred in the polytetrafluoro container of 50 milliliters and to be fixed on (polytetrafluoro container in stainless reactor, avoid the metal ion using metal vessel to participate in reaction and produce pollution), then with baking oven directly at 180 DEG C, heat 12 hours, when the temperature of question response still is reduced to room temperature naturally, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing in 60 DEG C of baking ovens dry 10 hours, namely the nickelous phosphate hollow nanospheres that diameter is 200-400 nanometer is obtained, specific surface is 267 m
2/ g.The transmission electron microscope photo of nickelous phosphate hollow nanospheres prepared by the present embodiment and X-ray powder diffraction figure similar to Example 1.
Embodiment 5
Respectively the nickelous acetate of the monometallic aqueous solution of 0.06 mol/L of 20ml and the 0.06mol/L of 20ml is mixed, to be transferred in the polytetrafluoro container of 50 milliliters and to be fixed on (polytetrafluoro container in stainless reactor, avoid the metal ion using metal vessel to participate in reaction and produce pollution), then with baking oven directly at 180 DEG C, heat 12 hours, when the temperature of question response still is reduced to room temperature naturally, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing in 60 DEG C of baking ovens dry 10 hours, namely the nickelous phosphate hollow nanospheres that diameter is 200-400 nanometer is obtained, specific surface is 252 m
2/ g.The transmission electron microscope photo of nickelous phosphate hollow nanospheres prepared by the present embodiment and X-ray powder diffraction figure similar to Example 1.
Embodiment 6
Respectively the nickelous acetate of the biphosphate sodium water solution of 0.06 mol/L of 20ml and the 0.06mol/L of 20ml is mixed, to be transferred in the polytetrafluoro container of 50 milliliters and to be fixed on (polytetrafluoro container in stainless reactor, avoid the metal ion using metal vessel to participate in reaction and produce pollution), then with baking oven directly at 180 DEG C, heat 12 hours, when the temperature of question response still is reduced to room temperature naturally, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing in 60 DEG C of baking ovens dry 10 hours, namely the nickelous phosphate hollow nanospheres that diameter is 200-400 nanometer is obtained, specific surface is 273 m
2/ g.The transmission electron microscope photo of nickelous phosphate hollow nanospheres prepared by the present embodiment and X-ray powder diffraction figure similar to Example 1.
Embodiment 7
Respectively the potassium dihydrogen phosphate aqueous solution of 0.06 mol/L of 20ml and the nickelous acetate of the 0.06mol/L of 20ml are mixed, to be transferred in the polytetrafluoro container of 50 milliliters and to be fixed on (polytetrafluoro container in stainless reactor, avoid the metal ion using metal vessel to participate in reaction and produce pollution), then with baking oven directly at 180 DEG C, heat 12 hours, when the temperature of question response still is reduced to room temperature naturally, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing in 60 DEG C of baking ovens dry 10 hours, namely the nickelous phosphate hollow nanospheres that diameter is 200-400 nanometer is obtained, specific surface is 278 m
2/ g.The transmission electron microscope photo of nickelous phosphate hollow nanospheres prepared by the present embodiment and X-ray powder diffraction figure similar to Example 1.
Embodiment 8
Respectively the ammonium dihydrogen phosphate aqueous solution of 0.06 mol/L of 20ml and the single nickel salt of the 0.06mol/L of 20ml are mixed, to be transferred in the polytetrafluoro container of 50 milliliters and to be fixed on (polytetrafluoro container in stainless reactor, avoid the metal ion using metal vessel to participate in reaction and produce pollution), then with baking oven directly at 150 DEG C, heat 12 hours, when the temperature of question response still is reduced to room temperature naturally, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing in 60 DEG C of baking ovens dry 10 hours, namely the nickelous phosphate hollow nanospheres that diameter is 200-400 nanometer is obtained, specific surface is 270 m
2/ g.The transmission electron microscope photo of nickelous phosphate hollow nanospheres prepared by the present embodiment and X-ray powder diffraction figure similar to Example 1.
Embodiment 9
Respectively the ammonium dihydrogen phosphate aqueous solution of 0.06 mol/L of 20ml and the nickelous nitrate of the 0.06mol/L of 20ml are mixed, to be transferred in the polytetrafluoro container of 50 milliliters and to be fixed on (polytetrafluoro container in stainless reactor, avoid the metal ion using metal vessel to participate in reaction and produce pollution), then with baking oven directly at 150 DEG C, heat 12 hours, when the temperature of question response still is reduced to room temperature naturally, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing in 60 DEG C of baking ovens dry 10 hours, namely the nickelous phosphate hollow nanospheres that diameter is 200-400 nanometer is obtained, specific surface is 288 m
2/ g.The transmission electron microscope photo of nickelous phosphate hollow nanospheres prepared by the present embodiment and X-ray powder diffraction figure similar to Example 1.
Embodiment 10
Respectively the ammonium dihydrogen phosphate aqueous solution of 0.06 mol/L of 20ml and the nickelous nitrate of the 0.06mol/L of 20ml are mixed, to be transferred in the polytetrafluoro container of 50 milliliters and to be fixed on (polytetrafluoro container in stainless reactor, avoid the metal ion using metal vessel to participate in reaction and produce pollution), then with baking oven directly at 220 DEG C, heat 12 hours, when the temperature of question response still is reduced to room temperature naturally, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing in 60 DEG C of baking ovens dry 10 hours, namely the nickelous phosphate hollow nanospheres that diameter is 200-400 nanometer is obtained, specific surface is 276 m
2/ g.The transmission electron microscope photo of nickelous phosphate hollow nanospheres prepared by the present embodiment and X-ray powder diffraction figure similar to Example 1.
Embodiment 11
Respectively the ammonium dihydrogen phosphate aqueous solution of 0.06 mol/L of 20ml and the nickelous acetate of the 0.06mol/L of 20ml are mixed, to be transferred in the polytetrafluoro container of 50 milliliters and to be fixed on (polytetrafluoro container in stainless reactor, avoid the metal ion using metal vessel to participate in reaction and produce pollution), then with baking oven directly at 150 DEG C, heat 20 hours, when the temperature of question response still is reduced to room temperature naturally, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing in 60 DEG C of baking ovens dry 10 hours, namely the nickelous phosphate hollow nanospheres that diameter is 200-400 nanometer is obtained, specific surface is 291 m
2/ g.The transmission electron microscope photo of nickelous phosphate hollow nanospheres prepared by the present embodiment and X-ray powder diffraction figure similar to Example 1.
Embodiment 12
Respectively the ammonium dihydrogen phosphate aqueous solution of 0.02 mol/L of 20ml and the nickelous nitrate of the 0.02mol/L of 20ml are mixed, to be transferred in the polytetrafluoro container of 50 milliliters and to be fixed on (polytetrafluoro container in stainless reactor, avoid the metal ion using metal vessel to participate in reaction and produce pollution), then with baking oven directly at 220 DEG C, heat 4 hours, when the temperature of question response still is reduced to room temperature naturally, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing in 60 DEG C of baking ovens dry 10 hours, namely the nickelous phosphate hollow nanospheres that diameter is 200-400 nanometer is obtained, specific surface is 279 m
2/ g.The transmission electron microscope photo of nickelous phosphate hollow nanospheres prepared by the present embodiment and X-ray powder diffraction figure similar to Example 1.
Can find out, preparation method's macroblock quantization step of nickelous phosphate hollow nanospheres provided by the invention is simple, and the nickelous phosphate hollow nanospheres of preparation has the large feature of specific surface area in conjunction with the embodiments.
Above content is in conjunction with concrete embodiment further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made.
Claims (10)
1. the preparation method of a nickelous phosphate hollow nanospheres, it is characterized in that, described method is included in solution system, and soluble phosphoric acid dihydric salt is contacted with nickel salt, react under hydrothermal reaction condition, then cool, wash, drying obtains described nickelous phosphate hollow nanospheres.
2. method according to claim 1, is characterized in that, the mol ratio of described soluble phosphoric acid dihydric salt and described nickel salt is 1:0.5 ~ 1:1.5.
3. method according to claim 1, is characterized in that, the temperature of described hydro-thermal reaction is 150 ~ 220 DEG C;
Preferably, the time of described hydro-thermal reaction is 4 ~ 20 hours, is preferably 12 hours.
4. method according to claim 1, is characterized in that, the aqueous solution of described soluble phosphoric acid dihydric salt is contacted with the aqueous solution of described nickel salt; Preferably make the aqueous solution of described soluble phosphoric acid dihydric salt and the aqueous solution of described nickel salt.
5. method according to claim 1, is characterized in that, described soluble phosphoric acid dihydric salt is selected from the combination of a kind of in primary ammonium phosphate, monometallic, SODIUM PHOSPHATE, MONOBASIC and potassium primary phosphate or at least two kinds;
Preferably, described nickel salt is selected from the combination of a kind of in nickelous acetate, nickelous nitrate and single nickel salt or at least two kinds.
6. method according to claim 1, is characterized in that, the concentration of described soluble phosphoric acid dihydric salt is 0.02 ~ 0.1mol/L;
Preferably, the concentration of described nickel salt is 0.02 ~ 0.1mol/L.
7. method according to claim 1, is characterized in that, described in be cooled to naturally cooling;
Preferably, described washing is washed successively for adopting water and ethanol; More preferably, described washing is washed more than 3 times successively for adopting water and ethanol;
Preferably, described drying is for drying.
8. method according to claim 1, is characterized in that, described hydro-thermal reaction is carried out in nonmetal reaction vessel, preferably carries out in polytetrafluoro container.
9. the nickelous phosphate hollow nanospheres for preparing of the method according to any one of claim 1-8.
10. nickelous phosphate hollow nanospheres according to claim 9, is characterized in that, described nickelous phosphate hollow nanospheres, and diameter is 200 ~ 400 nanometers.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106698381A (en) * | 2016-11-26 | 2017-05-24 | 华东理工大学 | Method for preparing cubical nickel phosphate nano-cages |
| CN108083250A (en) * | 2018-02-07 | 2018-05-29 | 济南大学 | A kind of porous amorphous phosphoric acid nickel nano particle of soft pompon shape and preparation method thereof |
| CN113264515A (en) * | 2021-05-19 | 2021-08-17 | 西北工业大学 | Nickel phosphate nanotube multi-stage assembly structure material and preparation method and application thereof |
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| WO2009137592A2 (en) * | 2008-05-08 | 2009-11-12 | 3M Innovative Properties Company | Surface-modified nanoparticles |
| CN103337633A (en) * | 2013-07-04 | 2013-10-02 | 哈尔滨工程大学 | In-situ carbon coating preparation method for secondary lithium ion battery cathode material lithium nickel phosphate |
| CN104332629A (en) * | 2014-10-21 | 2015-02-04 | 浙江大学 | Preparation method of hollow lithium manganese phosphate nano balls and product |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009137592A2 (en) * | 2008-05-08 | 2009-11-12 | 3M Innovative Properties Company | Surface-modified nanoparticles |
| CN103337633A (en) * | 2013-07-04 | 2013-10-02 | 哈尔滨工程大学 | In-situ carbon coating preparation method for secondary lithium ion battery cathode material lithium nickel phosphate |
| CN104332629A (en) * | 2014-10-21 | 2015-02-04 | 浙江大学 | Preparation method of hollow lithium manganese phosphate nano balls and product |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106698381A (en) * | 2016-11-26 | 2017-05-24 | 华东理工大学 | Method for preparing cubical nickel phosphate nano-cages |
| CN108083250A (en) * | 2018-02-07 | 2018-05-29 | 济南大学 | A kind of porous amorphous phosphoric acid nickel nano particle of soft pompon shape and preparation method thereof |
| CN113264515A (en) * | 2021-05-19 | 2021-08-17 | 西北工业大学 | Nickel phosphate nanotube multi-stage assembly structure material and preparation method and application thereof |
| CN113264515B (en) * | 2021-05-19 | 2023-11-17 | 西北工业大学 | Nickel phosphate nanotube multistage assembly structure material and preparation method and application thereof |
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