CN104649243B - Nickel phosphate hollow nanospheres and preparation method thereof - Google Patents
Nickel phosphate hollow nanospheres and preparation method thereof Download PDFInfo
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- CN104649243B CN104649243B CN201510072709.7A CN201510072709A CN104649243B CN 104649243 B CN104649243 B CN 104649243B CN 201510072709 A CN201510072709 A CN 201510072709A CN 104649243 B CN104649243 B CN 104649243B
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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, more particularly, to a kind of nickel phosphate hollow nanospheres and its system
Preparation Method.
Background technology
Phosphate has abundant backbone element because of it, therefore has wide application prospect in light, electricity, magnetic and catalytic field, because
This phosphatic synthesis receives much concern.Nickel phosphate, in addition to above-mentioned performance, also acts as pigment and plated material.But with respect to phosphorus
Sour ferrum, the research of nickel phosphate and report are relatively fewer.Hollow nanostructures are because its specific surface area is greatly in electrode material, pigment, suction
The application process such as attached has greater advantage.There is not been reported for the research of the current Hollow nanosphere material with regard to nickel phosphate.
Content of the invention
The present invention provides a kind of step method simply preparing nickel phosphate hollow nanospheres and the phosphoric acid preparing
Nickel hollow nanospheres.
According to the first aspect of the invention, the present invention provide a kind of preparation method of nickel phosphate hollow nanospheres, including
In solution system, so that soluble phosphoric acid dihydric salt is contacted with nickel salt, react under hydrothermal reaction condition, then cool down, wash, do
Dry obtain nickel phosphate hollow nanospheres.
As the preferred version of the present invention, soluble phosphoric acid dihydric salt is 1:0.5 ~ 1:1.5 with the mol ratio of nickel salt.
As the preferred version of the present invention, the temperature of hydro-thermal reaction is 150 ~ 220 DEG C.
As the preferred version of the present invention, the time of hydro-thermal reaction is 4 ~ 20 hours, more preferably 12 hours.
As the preferred version of the present invention, the aqueous solution of soluble phosphoric acid dihydric salt is made to contact with the aqueous solution of nickel salt；More
Preferably make the aqueous solution of soluble phosphoric acid dihydric salt and the aqueous solution of nickel salt.
As the preferred version of the present invention, soluble phosphoric acid dihydric salt is selected from ammonium dihydrogen phosphate, lithium dihydrogen phosphate, di(2-ethylhexyl)phosphate
One of hydrogen sodium and potassium dihydrogen phosphate or at least two combination.
As the preferred version of the present invention, nickel salt is selected from one of nickel acetate, nickel nitrate and nickel sulfate or at least two
Combination.
As the preferred version of the present invention, the concentration of soluble phosphoric acid dihydric salt is 0.02 ~ 0.1mol/l.
As the preferred version of the present invention, the concentration of nickel salt is 0.02 ~ 0.1mol/l.
As the preferred version of the present invention, it is cooled to natural cooling.
As the preferred version of the present invention, washing is to be washed successively using water and ethanol；It is highly preferred that washing is to adopt water
Wash more than 3 times with ethanol successively.
As the preferred version of the present invention, it is dried as drying.
As the preferred version of the present invention, hydro-thermal reaction is carried out in nonmetallic reaction vessel, preferably in polytetrafluoro container
Inside carry out.
According to the second aspect of the invention, the present invention provides the nickel phosphate that a kind of method according to first aspect prepares
Hollow nanospheres.
As the preferred version of the present invention, a diameter of 200 ~ 400 nanometers of nickel phosphate hollow nanospheres.
The present invention adopts soluble phosphoric acid dihydric salt and nickel salt that nickel phosphate hollow nanospheres, the party are obtained under hydrothermal conditions
The nickel phosphate nanosphere of method preparation has the hollow structure of uniqueness, and specific surface area is big.
Brief description
Fig. 1 is the stereoscan photograph of the nickel phosphate hollow nanospheres of the embodiment of the present invention 1 preparation.
Fig. 2 is the x-ray powder diagram of the nickel phosphate hollow nanospheres of the embodiment of the present invention 1 preparation, shows diffraction
Peak intensity (intensity) and the curve linear relationship at 2 θ (2theta) angle, wherein degree degree of a representation (°).
Fig. 3 is the nitrogen adsorption desorption figure of the nickel phosphate hollow nanospheres of the embodiment of the present invention 1 preparation, shows adsorbate
The curve linear relationship of long-pending (volume adsorbed) and relative pressure (relative pressure) and pore-size distribution situation, its
Middle adsorption represents absorption, and desorption represents desorption, and pore diamete represents aperture.
Specific embodiment
Combine accompanying drawing below by specific embodiment the present invention is described in further detail.
One of design of most critical of the present invention is: is obtained under hydrothermal conditions using soluble phosphoric acid dihydric salt and nickel salt
Nickel phosphate hollow nanospheres.
The further design of the present invention is: by controlling the type of predecessor and the hydrothermal condition of ratio and reaction temperature
Under prepare nickel phosphate hollow nanospheres.
One detailed embodiment of the present invention is described as follows:
A kind of preparation method of nickel phosphate hollow nanospheres, including in solution system, make soluble phosphoric acid dihydric salt with
Nickel salt contacts, and reacts, then cool down, wash, being dried to obtain nickel phosphate hollow nanospheres under hydrothermal reaction condition.
Inventor determines through further investigation, and the mol ratio of soluble phosphoric acid dihydric salt and nickel salt is in the model of 1:0.5 ~ 1:1.5
Enclose interior energy and obtain best effect.Although end-product nickel phosphate hollow nanospheres also can be obtained below or above this scope, and
Nickel phosphate nanosphere has the hollow structure of uniqueness, and specific surface area is also relatively large.But, soluble phosphoric acid dihydric salt and nickel salt
The effect that obtains in the range of 1:0.5 ~ 1:1.5 of mol ratio be substantially better than effect beyond above range, show nanometer
Piece area is bigger, hollow nanospheres structure evenly.The mol ratio of soluble phosphoric acid dihydric salt and nickel salt can be 1:0.52,1:
0.55th, 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..
Inventor determines through further investigation, and the temperature of hydro-thermal reaction can obtain best effect in the range of 150 ~ 220 DEG C
Really.Although end-product nickel phosphate hollow nanospheres also can be obtained below or above this scope, and nickel phosphate nanosphere has solely
Special hollow structure, specific surface area is also relatively large.But, the temperature of hydro-thermal reaction obtains in the range of 150 ~ 220 DEG C
Effect is substantially better than the effect beyond above range, show that nanometer sheet area is bigger, hollow nanospheres structure evenly.Hydro-thermal
The temperature of 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 preferable effect in the range of 4 ~ 20 hours, preferably 12 hours.Hydro-thermal is anti-
The time concrete needs answered make the appropriate adjustments according to the temperature of hydro-thermal reaction, if the temperature of hydro-thermal reaction is higher, corresponding hydro-thermal
The time of reaction should be more relatively low, and vice versa.The time of hydro-thermal reaction can be 5 hours, 6 hours, 7 hours, 8 little
When, 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 react 18 hours, 170 DEG C of reactions 16 little
When, 190 DEG C react 14 hours, 200 DEG C react 12 hours, 210 DEG C react 10 hours, 215 DEG C react 8 hours, 220 DEG C reaction 6
Hour etc..
The reaction of one embodiment of the invention is carried out in solution system, wherein soluble phosphoric acid dihydric salt and nickel
Salt contact mode can have multiple, such as in the aqueous solution of soluble phosphoric acid dihydric salt add nickel salt reacted, to nickel
Add soluble phosphoric acid dihydric salt to be reacted in the aqueous solution of salt, add titanium pigment in solvent (as water) simultaneously or successively
Acid dihydride salt and nickel salt are reacted, and add the aqueous solution of nickel salt to be reacted in the aqueous solution of soluble phosphoric acid dihydric salt,
The aqueous solution of soluble phosphoric acid dihydric salt is added to be reacted in the aqueous solution of nickel salt, etc..And can using mixing or
The form of Deca contacted that is to say, that can be directly a kind of reactant is mixed with another kind reactant or
A kind of reactant is added dropwise in another kind of reactant.As the preferred version of the present invention, make the water of soluble phosphoric acid dihydric salt
Solution is contacted with the aqueous solution of nickel salt；More preferably make the aqueous solution of soluble phosphoric acid dihydric salt and the aqueous solution of nickel salt.Send out
A person of good sense determines through further investigation, can be taken by the way of aqueous solution and the aqueous solution of nickel salt of soluble phosphoric acid dihydric salt
Best effect, show that nanometer sheet area is big, hollow nanospheres even structure.
In one embodiment of the invention, soluble phosphoric acid dihydric salt can be selected from ammonium dihydrogen phosphate, lithium dihydrogen phosphate, phosphorus
One of acid dihydride sodium and potassium dihydrogen phosphate or at least two combination.Described combination typical case but the example of indefiniteness ratio
As: the combination of the combination of ammonium dihydrogen phosphate and lithium dihydrogen phosphate, ammonium dihydrogen phosphate and sodium dihydrogen phosphate, ammonium dihydrogen phosphate and phosphoric acid
The combination of the combination of the combination of potassium dihydrogen, lithium dihydrogen phosphate and sodium dihydrogen phosphate, lithium dihydrogen phosphate and potassium dihydrogen phosphate, di(2-ethylhexyl)phosphate
Hydrogen sodium and the combination of potassium dihydrogen phosphate, the combination of ammonium dihydrogen phosphate, lithium dihydrogen phosphate and sodium dihydrogen phosphate, ammonium dihydrogen phosphate, phosphorus
Acid dihydride sodium and the combination of potassium dihydrogen phosphate, the combination of lithium dihydrogen phosphate, sodium dihydrogen phosphate and potassium dihydrogen phosphate, biphosphate
The combination of ammonium, lithium dihydrogen phosphate, sodium dihydrogen phosphate and potassium dihydrogen phosphate, etc..It should be noted that titanium pigment in the present invention
Acid dihydride salt is not limited to above-mentioned four kinds, but from the point of view of the quality from product and cost, preferably above-mentioned four kinds.
In one embodiment of the invention, nickel salt is selected from one of nickel acetate, nickel nitrate and nickel sulfate or at least two
Combination.Described combination typical case but the example of indefiniteness such as: the combination of nickel acetate and nickel nitrate, nickel acetate and nickel sulfate
Combination, the combination of nickel nitrate and nickel sulfate, the combination of nickel acetate, nickel nitrate and nickel sulfate.It should be noted that nickel in the present invention
Salt is not limited to above-mentioned three kinds, but from the point of view of the quality from product and 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, for example
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
Deng.
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 or (such as 25 DEG C) coolings of room temperature etc.；Can be auxiliary temperature-reducing cooling (as in refrigerator cool down) or
Natural cooling.As the preferred version of the present invention, it is cooled to natural cooling.
In one embodiment of the invention, washing is to be washed successively using water and ethanol；More preferably successively washing 3 times with
On, such as 4 times, 5 times or 8 are inferior.
In one embodiment of the invention, drying steps can be adopted and carry out in various manners, for example, can adopt drying side
Formula, or natural air drying mode.As the preferred version of the present invention, it is dried as drying.
The present inventor finds in an experiment, and foreign ion can cause the reduction of nickel phosphate hollow nanospheres product qualities, and
Reaction vessel is one of important channel that foreign ion introduces.Therefore, inventor determines, hydro-thermal reaction is in non-gold through further investigation
Belong in reaction vessel and carry out obtaining preferable effect, preferably carry out in polytetrafluoro container.
Describe the present invention in detail it will be appreciated that embodiment is only exemplary below by specific embodiment, can not manage
Solve as limiting the scope of the invention.
Embodiment 1
Respectively the nickel acetate of the ammonium dihydrogen phosphate aqueous solution of 0.04 mol/l of 20ml and the 0.04mol/l of 20ml is mixed
Together, it is transferred in 50 milliliters of polytetrafluoro container and is fixed in stainless reactor (polytetrafluoro container, it is to avoid use
The metal ion of canister participates in reaction and produces pollution), then with baking oven directly at 180 DEG C, heat 12 hours, question response kettle
Temperature when being naturally reduced to room temperature, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing
It is dried 10 hours in 60 DEG C of baking ovens, that is, obtain nickel phosphate hollow nanospheres.Fig. 1 is the nickel phosphate hollow of the present embodiment 1 preparation
The transmission electron microscope photo of nanosphere.As shown in Figure 1, a diameter of 200-400 nanometer of hollow nanospheres.Fig. 2 is nickel phosphate hollow
The x-ray powder diagram of nanosphere.Fig. 3 is the nitrogen adsorption desorption figure of nickel phosphate hollow nanospheres, and specific surface area is
300m2/g.
Embodiment 2
Respectively the nickel acetate of the ammonium dihydrogen phosphate aqueous solution of 0.04 mol/l of 20ml and the 0.02mol/l of 20ml is mixed
Together, it is transferred in 50 milliliters of polytetrafluoro container and is fixed in stainless reactor (polytetrafluoro container, it is to avoid use
The metal ion of canister participates in reaction and produces pollution), then with baking oven directly at 180 DEG C, heat 12 hours, question response kettle
Temperature when being naturally reduced to room temperature, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing
It is dried 10 hours in 60 DEG C of baking ovens, that is, obtains the nickel phosphate hollow nanospheres of a diameter of 200-400 nanometer, specific surface is 284
m2/g.The transmission electron microscope photo of nickel phosphate hollow nanospheres manufactured in the present embodiment and x-ray powder diagram and embodiment 1 class
Seemingly.
Embodiment 3
Respectively the nickel acetate of the ammonium dihydrogen phosphate aqueous solution of 0.04 mol/l of 20ml and the 0.06mol/l of 20ml is mixed
Together, it is transferred in 50 milliliters of polytetrafluoro container and is fixed in stainless reactor (polytetrafluoro container, it is to avoid use
The metal ion of canister participates in reaction and produces pollution), then with baking oven directly at 180 DEG C, heat 12 hours, question response kettle
Temperature when being naturally reduced to room temperature, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing
It is dried 10 hours in 60 DEG C of baking ovens, that is, obtains the nickel phosphate hollow nanospheres of a diameter of 200-400 nanometer, specific surface is 279
m2/g.The transmission electron microscope photo of nickel phosphate hollow nanospheres manufactured in the present embodiment and x-ray powder diagram and embodiment 1 class
Seemingly.
Embodiment 4
Respectively the nickel acetate of the ammonium dihydrogen phosphate aqueous solution of 0.1 mol/l of 20ml and the 0.1mol/l of 20ml is blended in
Together, it is transferred in 50 milliliters of polytetrafluoro container and is fixed on (polytetrafluoro container, it is to avoid using gold in stainless reactor
The metal ion belonging to container participates in reaction generation pollution), then with baking oven directly at 180 DEG C, heat 12 hours, question response kettle
When temperature is reduced to room temperature naturally, obtained reactant is washed 3 times successively with water and ethanol respectively, the sample after washing is existed
It is dried 10 hours in 60 DEG C of baking ovens, that is, obtains the nickel phosphate hollow nanospheres of a diameter of 200-400 nanometer, specific surface is 267
m2/g.The transmission electron microscope photo of nickel phosphate hollow nanospheres manufactured in the present embodiment and x-ray powder diagram and embodiment 1 class
Seemingly.
Embodiment 5
Respectively the nickel acetate of the lithium dihydrogen phosphate aqueous solution of 0.06 mol/l of 20ml and the 0.06mol/l of 20ml is mixed
Together, it is transferred in 50 milliliters of polytetrafluoro container and is fixed in stainless reactor (polytetrafluoro container, it is to avoid use
The metal ion of canister participates in reaction and produces pollution), then with baking oven directly at 180 DEG C, heat 12 hours, question response kettle
Temperature when being naturally reduced to room temperature, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing
It is dried 10 hours in 60 DEG C of baking ovens, that is, obtains the nickel phosphate hollow nanospheres of a diameter of 200-400 nanometer, specific surface is 252
m2/g.The transmission electron microscope photo of nickel phosphate hollow nanospheres manufactured in the present embodiment and x-ray powder diagram and embodiment 1 class
Seemingly.
Embodiment 6
Respectively the nickel acetate of the biphosphate sodium water solution of 0.06 mol/l of 20ml and the 0.06mol/l of 20ml is mixed
Together, it is transferred in 50 milliliters of polytetrafluoro container and is fixed in stainless reactor (polytetrafluoro container, it is to avoid use
The metal ion of canister participates in reaction and produces pollution), then with baking oven directly at 180 DEG C, heat 12 hours, question response kettle
Temperature when being naturally reduced to room temperature, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing
It is dried 10 hours in 60 DEG C of baking ovens, that is, obtains the nickel phosphate hollow nanospheres of a diameter of 200-400 nanometer, specific surface is 273
m2/g.The transmission electron microscope photo of nickel phosphate hollow nanospheres manufactured in the present embodiment and x-ray powder diagram and embodiment 1 class
Seemingly.
Embodiment 7
Respectively the nickel acetate of the potassium dihydrogen phosphate aqueous solution of 0.06 mol/l of 20ml and the 0.06mol/l of 20ml is mixed
Together, it is transferred in 50 milliliters of polytetrafluoro container and is fixed in stainless reactor (polytetrafluoro container, it is to avoid use
The metal ion of canister participates in reaction and produces pollution), then with baking oven directly at 180 DEG C, heat 12 hours, question response kettle
Temperature when being naturally reduced to room temperature, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing
It is dried 10 hours in 60 DEG C of baking ovens, that is, obtains the nickel phosphate hollow nanospheres of a diameter of 200-400 nanometer, specific surface is 278
m2/g.The transmission electron microscope photo of nickel phosphate hollow nanospheres manufactured in the present embodiment and x-ray powder diagram and embodiment 1 class
Seemingly.
Embodiment 8
Respectively the nickel sulfate of the ammonium dihydrogen phosphate aqueous solution of 0.06 mol/l of 20ml and the 0.06mol/l of 20ml is mixed
Together, it is transferred in 50 milliliters of polytetrafluoro container and is fixed in stainless reactor (polytetrafluoro container, it is to avoid use
The metal ion of canister participates in reaction and produces pollution), then with baking oven directly at 150 DEG C, heat 12 hours, question response kettle
Temperature when being naturally reduced to room temperature, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing
It is dried 10 hours in 60 DEG C of baking ovens, that is, obtains the nickel phosphate hollow nanospheres of a diameter of 200-400 nanometer, specific surface is 270
m2/g.The transmission electron microscope photo of nickel phosphate hollow nanospheres manufactured in the present embodiment and x-ray powder diagram and embodiment 1 class
Seemingly.
Embodiment 9
Respectively the nickel nitrate of the ammonium dihydrogen phosphate aqueous solution of 0.06 mol/l of 20ml and the 0.06mol/l of 20ml is mixed
Together, it is transferred in 50 milliliters of polytetrafluoro container and is fixed in stainless reactor (polytetrafluoro container, it is to avoid use
The metal ion of canister participates in reaction and produces pollution), then with baking oven directly at 150 DEG C, heat 12 hours, question response kettle
Temperature when being naturally reduced to room temperature, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing
It is dried 10 hours in 60 DEG C of baking ovens, that is, obtains the nickel phosphate hollow nanospheres of a diameter of 200-400 nanometer, specific surface is 288
m2/g.The transmission electron microscope photo of nickel phosphate hollow nanospheres manufactured in the present embodiment and x-ray powder diagram and embodiment 1 class
Seemingly.
Embodiment 10
Respectively the nickel nitrate of the ammonium dihydrogen phosphate aqueous solution of 0.06 mol/l of 20ml and the 0.06mol/l of 20ml is mixed
Together, it is transferred in 50 milliliters of polytetrafluoro container and is fixed in stainless reactor (polytetrafluoro container, it is to avoid use
The metal ion of canister participates in reaction and produces pollution), then with baking oven directly at 220 DEG C, heat 12 hours, question response kettle
Temperature when being naturally reduced to room temperature, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing
It is dried 10 hours in 60 DEG C of baking ovens, that is, obtains the nickel phosphate hollow nanospheres of a diameter of 200-400 nanometer, specific surface is 276
m2/g.The transmission electron microscope photo of nickel phosphate hollow nanospheres manufactured in the present embodiment and x-ray powder diagram and embodiment 1 class
Seemingly.
Embodiment 11
Respectively the nickel acetate of the ammonium dihydrogen phosphate aqueous solution of 0.06 mol/l of 20ml and the 0.06mol/l of 20ml is mixed
Together, it is transferred in 50 milliliters of polytetrafluoro container and is fixed in stainless reactor (polytetrafluoro container, it is to avoid use
The metal ion of canister participates in reaction and produces pollution), then with baking oven directly at 150 DEG C, heat 20 hours, question response kettle
Temperature when being naturally reduced to room temperature, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing
It is dried 10 hours in 60 DEG C of baking ovens, that is, obtains the nickel phosphate hollow nanospheres of a diameter of 200-400 nanometer, specific surface is 291
m2/g.The transmission electron microscope photo of nickel phosphate hollow nanospheres manufactured in the present embodiment and x-ray powder diagram and embodiment 1 class
Seemingly.
Embodiment 12
Respectively the nickel nitrate of the ammonium dihydrogen phosphate aqueous solution of 0.02 mol/l of 20ml and the 0.02mol/l of 20ml is mixed
Together, it is transferred in 50 milliliters of polytetrafluoro container and is fixed in stainless reactor (polytetrafluoro container, it is to avoid use
The metal ion of canister participates in reaction and produces pollution), then with baking oven directly at 220 DEG C, heat 4 hours, question response kettle
Temperature when being naturally reduced to room temperature, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing
It is dried 10 hours in 60 DEG C of baking ovens, that is, obtains the nickel phosphate hollow nanospheres of a diameter of 200-400 nanometer, specific surface is 279
m2/g.The transmission electron microscope photo of nickel phosphate hollow nanospheres manufactured in the present embodiment and x-ray powder diagram and embodiment 1 class
Seemingly.
In conjunction with the embodiments as can be seen that the preparation method macroblock quantization step of the nickel phosphate hollow nanospheres of present invention offer is simple
Single, the nickel phosphate hollow nanospheres of preparation have the characteristics that specific surface area is big.
Above content is to further describe it is impossible to assert this with reference to specific embodiment is made for the present invention
Bright it is embodied as being confined to these explanations.For general technical staff of the technical field of the invention, do not taking off
On the premise of present inventive concept, some simple deduction or replace can also be made.
Claims (19)
1., it is characterised in that methods described includes in solution system, making can for a kind of preparation method of nickel phosphate hollow nanospheres
Soluble phosphoric acid dihydric salt is contacted with nickel salt, reacts, then cool down, wash, being dried to obtain described phosphoric acid under hydrothermal reaction condition
Nickel hollow nanospheres.
2. method according to claim 1 it is characterised in that described soluble phosphoric acid dihydric salt and described nickel salt mole
Than for 1:0.5 ~ 1:1.5.
3. method according to claim 1 is it is characterised in that the temperature of described hydro-thermal reaction is 150 ~ 220 DEG C.
4. method according to claim 1 is it is characterised in that the time of described hydro-thermal reaction is 4 ~ 20 hours.
5. method according to claim 1 is it is characterised in that the time of described hydro-thermal reaction is 12 hours.
6. method according to claim 1 it is characterised in that make the aqueous solution of described soluble phosphoric acid dihydric salt with described
The aqueous solution contact of nickel salt.
7. method according to claim 1 it is characterised in that make the aqueous solution of described soluble phosphoric acid dihydric salt with described
The aqueous solution of nickel salt.
8. method according to claim 1 it is characterised in that described soluble phosphoric acid dihydric salt be selected from ammonium dihydrogen phosphate,
One of lithium dihydrogen phosphate, sodium dihydrogen phosphate and potassium dihydrogen phosphate or at least two combination.
9. method according to claim 1 is it is characterised in that described nickel salt is selected from nickel acetate, nickel nitrate and nickel sulfate
A kind of or at least two combination.
10. method according to claim 1 it is characterised in that described soluble phosphoric acid dihydric salt concentration be 0.02 ~
0.1mol/l.
11. methods according to claim 1 are it is characterised in that the concentration of described nickel salt is 0.02 ~ 0.1mol/l.
12. methods according to claim 1 are it is characterised in that described be cooled to natural cooling.
13. methods according to claim 1 are it is characterised in that described washing is to be washed successively using water and ethanol.
14. methods according to claim 1 it is characterised in that described washing be adopt water and ethanol wash successively 3 times with
On.
15. methods according to claim 1 are it is characterised in that described drying is to dry.
16. methods according to claim 1 are it is characterised in that described hydro-thermal reaction is carried out in nonmetallic reaction vessel.
17. methods according to claim 1 are it is characterised in that described hydro-thermal reaction is carried out in polytetrafluoro container.
The nickel phosphate hollow nanospheres that method described in a kind of 18. any one according to claim 1-17 prepares.
19. nickel phosphate hollow nanospheres according to claim 18 it is characterised in that described nickel phosphate hollow nanospheres,
A diameter of 200 ~ 400 nanometers.
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| 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 |
| 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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| 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 |
| CN104332629B (en) * | 2014-10-21 | 2016-09-14 | 浙江大学 | The preparation method of a kind of lithium manganese phosphate hollow nanospheres and product |
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