CN107265522A - A kind of preparation method of composite nano materials - Google Patents
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Abstract
A kind of preparation method of composite nano materials, belongs to technical field of nanometer material preparation.Comprise the following steps：By Fe（NO3）3·9H2O、Ni（NO3）2·6H2It is uniform rear standby that O and complexing agent are dissolved in ultrasonic mixing after deionized water；Nitrate solution is added into above-mentioned mixed liquor with glass bar drainage, while constantly carrying out magnetic stirring；Ammoniacal liquor or dust technology regulation pH is added dropwise, magnetic stirring, obtains transparent colloidal sol at room temperature；Vitreosol is dehydrated clay into power after be put into tube furnace heat treatment；By NiFe2O4Nanometer powder ultrasonic disperse is added dropwise after tetraethyl orthosilicate, continual ultrasonic and washed, vacuum drying obtains NiFe into ethanol and the mixed solution of deionized water dropwise under ultrasonic state2O4/SiO2Composite nano materials.Preparation method of the present invention is simple to operation, and heat treatment temperature is low, energy-conserving and environment-protective, particle diameter is 35 ~ 39nm, and size is basically identical, substantially spherical in shape, saturation magnetization is 12.65 ~ 15.32emu/g, and coercivity value is zero at room temperature, illustrates to show superparamagnetism at room temperature.
Description
Technical field
The invention belongs to field of nano material preparation, and in particular to a kind of preparation method of composite nano materials.
Background technology
Nano spinel ferrite has good electrically and magnetically property, in magnetic fluid, microwave device, catalyst, magnetic
The field such as high density data storage and sensor is widely applied.NiFe2O4It is soft magnetic materials, the magnetic head of function admirable
Material, rectangular hysteresis material, microwave magnetic property, but also be the mangneto selected by the superior magnetoelectricity conversion composite of processability
Telescopic material, with prospect widely.
However, due to the effect such as nanometer size effect, magnetic dipole gravitation, nano spinel ferrite is easy to reunite, and changes
Learn stability not high, it is oxidizable, and toxicity that may be present in metallic element, thus it is difficult to directly application.And unformed silicon
Material is a kind of with excellent biocompatibility, chemical stability, nontoxic inorganic material, to nano spinel ferrite bag
Cover SiO2Afterwards, it is possible to reduce nano spinel ferrite is interparticle to reunite, and improves chemical stability, and it is possessed biofacies
Capacitive.
But current production technology is more complicated, the temperature of heat treatment is higher, causes cost higher, the life of particle diameter
FeSiO is easily generated in growth process4Or NiSiO4Deng impurity.
The content of the invention
The technical problem of solution：For above-mentioned technical problem, the present invention provides a kind of preparation method of composite nano materials,
Compared with prior art, energy-conserving and environment-protective, simple to operate, the generation without intermediate product can be successfully by NiFe2O4Nano particle
It is scattered in SiO2In matrix, and the product prepared shows superparamagnetism at room temperature.
Technical scheme：A kind of preparation method of composite nano materials, the preparation method comprises the following steps：
（1）By Fe（NO3）3·9H2O、Ni（NO3）2·6H2O and complexing agent are 1 ~ 3 in molar ratio:2~5:3 ~ 5 are dissolved in deionized water
It is standby after ultrasonic mixing is uniform afterwards；
（2）1.5 ~ 2 mol/L nitrate solution is added into step with glass bar drainage（1）Mixed liquor, while constantly carry out
Magnetic stirring, nitrate solution and step（1）Middle Fe（NO3）3·9H2O、Ni（NO3）2·6H2The ratio of the total moles of O and complexing agent
It is worth and is（9~11）L:1 mol；
（3）To step（2）Ammoniacal liquor or dust technology regulation pH to 4 ~ 5 is added dropwise in solution after stirring, at room temperature magnetic stirring 20 ~
24 h, obtain transparent colloidal sol；
（4）By step（3）Described vitreosol dehydrates to form xerogel at 70 ~ 80 DEG C, by the xerogel grinds
It is last to be put into tube furnace 1.5 ~ 2.5 h of processing at 700 ~ 900 DEG C, NiFe is made2O4Nanometer powder；
（5）By above-mentioned NiFe2O4Nanometer powder ultrasonic disperse is into ethanol and the mixed solution of deionized water, under ultrasonic state
It is added dropwise after tetraethyl orthosilicate, the h of continual ultrasonic 2 ~ 3 and washs dropwise, vacuum drying obtains NiFe at a temperature of 50 ~ 60 DEG C2O4 /
SiO2Composite nano materials, NiFe2O4Nanometer powder, ethanol, the ratio of deionized water and tetraethyl orthosilicate are 3 ~ 5 g：100~
150 mL：30 ~50 mL：1 ~3 mL.
Preferably, the step（1）Complexing agent is citric acid, sodium citrate, tartaric acid, sodium potassium tartrate tetrahydrate and winestone
At least one of sour acid amides.
Preferably, the step（1）Middle Fe（NO3）3·9H2O、Ni（NO3）2·6H2The mol ratio of O and complexing agent is 2:
4:5。
Preferably, the step（2）The concentration of middle silver nitrate solution is 1.5 mol/L, nitrate solution and step（1）
Middle Fe（NO3）3·9H2O、Ni（NO3）2·6H2The ratio of the total moles of O and complexing agent is 10 L:1 mol.
Preferably, the step（3）To step（2）Ammoniacal liquor is added dropwise in solution after stirring or dust technology adjusts pH to 5,
The h of magnetic stirring 20, obtains transparent colloidal sol at room temperature.
Preferably, the step（4）Vitreosol is dehydrated to form xerogel at 75 DEG C, by the xerogel
It is put into after claying into power in tube furnace and 2 h is handled at 800 DEG C.
Preferably, the step（5）Washed after the h of continual ultrasonic 2.5, be dried in vacuo and be made at a temperature of 55 DEG C
NiFe2O4 / SiO2Composite nano materials.
Preferably, the step（5）Middle NiFe2O4Nanometer powder, ethanol, the ratio of deionized water and tetraethyl orthosilicate
For 4 g：125 mL：40 mL：2 mL.
Beneficial effect：（1）Preparation method of the present invention is simple to operate, energy-conserving and environment-protective；（2）Technique system of the present invention
Standby NiFe2O4 / SiO2Composite nano materials carry out performance test, and xerogel sample is amorphous state, not corresponding to nitrate
The diffraction maximum of crystallite occurs, in whole NiFe2O4 / SiO2There is no other interphases such as during composite nano materials formation
FeSiO4Or NiSiO4Formation, and particle diameter is 35 ~ 39 nm, and size is basically identical, and substantially spherical in shape, saturated magnetization is strong
Spend for 12.65 ~ 15.32 emu/g, coercivity value is zero at room temperature, illustrates to show superparamagnetism at room temperature.
Embodiment
Embodiment 1
A kind of preparation method of composite nano materials, the preparation method comprises the following steps：
（1）By Fe（NO3）3·9H2O、Ni（NO3）2·6H2O and complexing agent are 1 in molar ratio:2:3 are dissolved in ultrasound after deionized water
It is standby after well mixed；
（2）1.5 mol/L nitrate solution is slowly added into step with glass bar drainage（1）Mixed liquor, while constantly entering
Row magnetic stirring, nitrate solution and step（1）Middle Fe（NO3）3·9H2O、Ni（NO3）2·6H2The total moles of O and complexing agent
Ratio is 9 L:1 mol；
（3）To step（2）Ammoniacal liquor or dust technology regulation pH to 4 is added dropwise in solution after stirring, at room temperature the h of magnetic stirring 20,
Obtain transparent colloidal sol；
（4）By step（3）Described vitreosol dehydrates to form xerogel at 70 DEG C, after the xerogel is clayed into power
It is put into tube furnace and 1.5 h is handled at 700 DEG C, NiFe is made2O4Nanometer powder；
（5）By above-mentioned NiFe2O4Nanometer powder ultrasonic disperse is into ethanol and the mixed solution of deionized water, under ultrasonic state
It is added dropwise after tetraethyl orthosilicate, the h of continual ultrasonic 2 and washs dropwise, vacuum drying obtains NiFe at a temperature of 50 DEG C2O4 / SiO2It is multiple
Close nano material, NiFe2O4Nanometer powder, ethanol, the ratio of deionized water and tetraethyl orthosilicate are 3 g：100 mL：30 mL：1
mL。
NiFe prepared by described technique2O4 / SiO2Composite nano materials carry out performance test, and xerogel sample is non-
Crystalline state, not corresponding to the diffraction maximum appearance of nitrate crystallite, in whole NiFe2O4 / SiO2The mistake of composite nano materials formation
There is no other interphases such as FeSiO in journey4Or NiSiO4Formation, and particle diameter is 39 nm, and size is basically identical, substantially
Spherical in shape, saturation magnetization is 12.65 emu/g, and coercivity value is zero at room temperature, illustrates to show superparamagnetism at room temperature.
Embodiment 2
A kind of preparation method of composite nano materials, the preparation method comprises the following steps：
（1）By Fe（NO3）3·9H2O、Ni（NO3）2·6H2O and complexing agent are 3 in molar ratio:5:5 are dissolved in ultrasound after deionized water
It is standby after well mixed；
（2）2 mol/L nitrate solution is slowly added into step with glass bar drainage（1）Mixed liquor, while constantly carry out
Magnetic stirring, nitrate solution and step（1）Middle Fe（NO3）3·9H2O、Ni（NO3）2·6H2The ratio of the total moles of O and complexing agent
It is worth for 11 L:1 mol；
（3）To step（2）Ammoniacal liquor or dust technology regulation pH to 5 is added dropwise in solution after stirring, at room temperature the h of magnetic stirring 24,
Obtain transparent colloidal sol；
（4）By step（3）Described vitreosol is dehydrated to form xerogel at 80 DEG C, and the xerogel is clayed into power
After be put into tube furnace 2.5 h handled at 900 DEG C, NiFe is made2O4Nanometer powder；
（5）By above-mentioned NiFe2O4Nanometer powder ultrasonic disperse is into ethanol and the mixed solution of deionized water, under ultrasonic state
It is added dropwise after tetraethyl orthosilicate, the h of continual ultrasonic 3 and washs dropwise, vacuum drying obtains NiFe at a temperature of 60 DEG C2O4 / SiO2It is multiple
Close nano material, NiFe2O4Nanometer powder, ethanol, the ratio of deionized water and tetraethyl orthosilicate are 5 g：150 mL：50 mL：
3 mL。
NiFe prepared by described technique2O4 / SiO2Composite nano materials carry out performance test, and xerogel sample is non-
Crystalline state, not corresponding to the diffraction maximum appearance of nitrate crystallite, in whole NiFe2O4 / SiO2The mistake of composite nano materials formation
There is no other interphases such as FeSiO in journey4Or NiSiO4Formation, and particle diameter is 38 nm, and size is basically identical, substantially
Spherical in shape, saturation magnetization is 13.59 emu/g, and coercivity value is zero at room temperature, illustrates to show superparamagnetism at room temperature.
Embodiment 3
A kind of preparation method of composite nano materials, the preparation method comprises the following steps：
（1）By Fe（NO3）3·9H2O、Ni（NO3）2·6H2O and complexing agent are 2 in molar ratio:4:5 are dissolved in ultrasound after deionized water
It is standby after well mixed；
（2）1.5 mol/L nitrate solution is slowly added into step with glass bar drainage（1）Mixed liquor, while constantly entering
Row magnetic stirring, nitrate solution and step（1）Middle Fe（NO3）3·9H2O、Ni（NO3）2·6H2The total moles of O and complexing agent
Ratio is 10 L:1 mol；
（3）To step（2）Ammoniacal liquor or dust technology regulation pH to 5 is added dropwise in solution after stirring, at room temperature the h of magnetic stirring 20,
Obtain transparent colloidal sol；
（4）By step（3）Described vitreosol is dehydrated to form xerogel at 75 DEG C, and the xerogel is clayed into power
After be put into tube furnace 2 h handled at 800 DEG C, NiFe is made2O4Nanometer powder；
（5）By above-mentioned NiFe2O4Nanometer powder ultrasonic disperse is into ethanol and the mixed solution of deionized water, under ultrasonic state
It is added dropwise after tetraethyl orthosilicate, the h of continual ultrasonic 2.5 and washs dropwise, vacuum drying obtains NiFe at a temperature of 55 DEG C2O4 / SiO2
Composite nano materials, NiFe2O4Nanometer powder, ethanol, the ratio of deionized water and tetraethyl orthosilicate are 4 g：125 mL：40
mL：2 mL.
NiFe prepared by described technique2O4 / SiO2Composite nano materials carry out performance test, and xerogel sample is non-
Crystalline state, not corresponding to the diffraction maximum appearance of nitrate crystallite, in whole NiFe2O4 / SiO2The mistake of composite nano materials formation
There is no other interphases such as FeSiO in journey4Or NiSiO4Formation, and particle diameter is 35 nm, and size is basically identical, substantially
Spherical in shape, saturation magnetization is 15.32 emu/g, and coercivity value is zero at room temperature, illustrates to show superparamagnetism at room temperature.
Claims (8)
1. a kind of preparation method of composite nano materials, it is characterised in that the preparation method comprises the following steps：
（1）By Fe（NO3）3·9H2O、Ni（NO3）2·6H2O and complexing agent are 1 ~ 3 in molar ratio:2~5:3 ~ 5 are dissolved in deionized water
It is standby after ultrasonic mixing is uniform afterwards；
（2）1.5 ~ 2 mol/L nitrate solution is added into step with glass bar drainage（1）Mixed liquor, while constantly carry out
Magnetic stirring, nitrate solution and step（1）Middle Fe（NO3）3·9H2O、Ni（NO3）2·6H2The ratio of the total moles of O and complexing agent
It is worth and is（9~11）L:1 mol；
（3）To step（2）Ammoniacal liquor or dust technology regulation pH to 4 ~ 5 is added dropwise in solution after stirring, at room temperature magnetic stirring 20 ~
24 h, obtain transparent colloidal sol；
（4）By step（3）Described vitreosol dehydrates to form xerogel at 70 ~ 80 DEG C, by the xerogel grinds
It is last to be put into tube furnace 1.5 ~ 2.5 h of processing at 700 ~ 900 DEG C, NiFe is made2O4Nanometer powder；
（5）By above-mentioned NiFe2O4Nanometer powder ultrasonic disperse is into ethanol and the mixed solution of deionized water, under ultrasonic state
It is added dropwise after tetraethyl orthosilicate, the h of continual ultrasonic 2 ~ 3 and washs dropwise, vacuum drying obtains NiFe at a temperature of 50 ~ 60 DEG C2O4 /
SiO2Composite nano materials, NiFe2O4Nanometer powder, ethanol, the ratio of deionized water and tetraethyl orthosilicate are 3 ~ 5 g：100~
150 mL：30 ~50 mL：1 ~3 mL.
2. a kind of preparation method of composite nano materials according to claim 1, it is characterised in that the step（1）In
Complexing agent is at least one of citric acid, sodium citrate, tartaric acid, sodium potassium tartrate tetrahydrate and tartaric acid acid amides.
3. a kind of preparation method of composite nano materials according to claim 1, it is characterised in that the step（1）In
Fe（NO3）3·9H2O、Ni（NO3）2·6H2The mol ratio of O and complexing agent is 2:4:5.
4. a kind of preparation method of composite nano materials according to claim 1, it is characterised in that the step（2）In
The concentration of silver nitrate solution is 1.5 mol/L, nitrate solution and step（1）Middle Fe（NO3）3·9H2O、Ni（NO3）2·6H2O
Ratio with the total moles of complexing agent is 10 L:1 mol.
5. a kind of preparation method of composite nano materials according to claim 1, it is characterised in that the step（3）To
Step（2）Ammoniacal liquor or dust technology regulation pH to 5 is added dropwise in solution after stirring, and the h of magnetic stirring 20, obtains transparent at room temperature
Colloidal sol.
6. a kind of preparation method of composite nano materials according to claim 1, it is characterised in that the step（4）Will
Vitreosol dehydrates to form xerogel at 75 DEG C, is put into after the xerogel is clayed into power in tube furnace at 800 DEG C
Handle 2 h.
7. a kind of preparation method of composite nano materials according to claim 1, it is characterised in that the step（5）Hold
Continue and washed after ultrasonic 2.5 h, be dried in vacuo at a temperature of 55 DEG C and NiFe is made2O4 / SiO2Composite nano materials.
8. a kind of preparation method of composite nano materials according to claim 1, it is characterised in that the step（5）In
NiFe2O4Nanometer powder, ethanol, the ratio of deionized water and tetraethyl orthosilicate are 4 g：125 mL：40 mL：2 mL.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108298978A (en) * | 2018-03-29 | 2018-07-20 | 太原理工大学 | A kind of method that sol-gel method prepares CaCu 3 Ti 4 O/nickel ferrite based magnetic loaded compound magnetoelectric ceramic material |
| CN108754324A (en) * | 2018-06-13 | 2018-11-06 | 苏州诺弘添恒材料科技有限公司 | A kind of preparation method of the iron-based soft magnetic body with nano coating |
| CN112892487A (en) * | 2021-01-19 | 2021-06-04 | 广州华晟科创科技发展有限公司 | Composite antibacterial air purifying agent and preparation method thereof |
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| CN102430410A (en) * | 2011-12-31 | 2012-05-02 | 上海大学 | Preparation method of TiO2/SiO2/NiFe2O4 magnetic composite photocatalyst |
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2017
- 2017-06-01 CN CN201710403304.6A patent/CN107265522A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102430410A (en) * | 2011-12-31 | 2012-05-02 | 上海大学 | Preparation method of TiO2/SiO2/NiFe2O4 magnetic composite photocatalyst |
Non-Patent Citations (4)
| Title |
|---|
| A. CHAUDHURI, M.,ET AL.: "Preparation and study of NiFe2O4/SiO2 core–shell nanocomposites", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| MANISH SRIVASTAVA, S., ET AL.: "Investigation on size dependent structural and magnetic behavior of nickel ferrite nanoparticles prepared by sol–gel and hydrothermal methods", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
| NELCY D.S. MOHALLEM, ET AL.: "Magnetic nanocomposite thin films of NiFe2O4/SiO2 prepared by sol–gel process", 《APPLIED SURFACE SCIENCE》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108298978A (en) * | 2018-03-29 | 2018-07-20 | 太原理工大学 | A kind of method that sol-gel method prepares CaCu 3 Ti 4 O/nickel ferrite based magnetic loaded compound magnetoelectric ceramic material |
| CN108754324A (en) * | 2018-06-13 | 2018-11-06 | 苏州诺弘添恒材料科技有限公司 | A kind of preparation method of the iron-based soft magnetic body with nano coating |
| CN112892487A (en) * | 2021-01-19 | 2021-06-04 | 广州华晟科创科技发展有限公司 | Composite antibacterial air purifying agent and preparation method thereof |
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Application publication date: 20171020 |