CN107369517A - The preparation method of iron-base magnetic composite with nano effect - Google Patents
The preparation method of iron-base magnetic composite with nano effect Download PDFInfo
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- CN107369517A CN107369517A CN201710689362.XA CN201710689362A CN107369517A CN 107369517 A CN107369517 A CN 107369517A CN 201710689362 A CN201710689362 A CN 201710689362A CN 107369517 A CN107369517 A CN 107369517A
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- H—ELECTRICITY
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
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Abstract
The invention belongs to field of nanometer material technology, is related to a kind of preparation method of the iron-base magnetic composite with nano effect.Preparation method proposed by the present invention is that pyrroles, ironic citrate, lanthanum nitrate and cellulose is compound, obtain iron base composite material, iron base composite material is prepared into polyvinyl alcohol iron-based gel again, then with the method progressively to heat up, iron-based plural gel is changed into iron-base magnetic composite.The preparation method of the present invention has superior technique effect compared with existing literature, and the saturation magnetization of prepared iron-base magnetic composite reaches 8907Gs, is conventional ferritic 2.2 times, shows magnetic Nano effect.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of iron-base magnetic composite with nano effect
Preparation method.
Background technology
The characteristic of magnetic Nano material is different from conventional magnetic material, and its reason is associated with the characteristic body with magnetic dependence
Length is managed just at nanometer scale, such as：Magnetic single domain size, superparamagnetism critical dimension, exchange interaction length, and electronics
Mean free path etc. is generally in 1-100nm magnitudes, will when the size of magnetic is suitable with these feature physical lengths
Unusual magnetic property is presented.
The application of magnetic Nano material is to be related to every field.In machinery, electronics, optics, magnetics, chemistry and biology
Field has a wide range of applications.The birth of nanoscale science and technology will produce far-reaching influence to human society.And have can
Can fundamentally solve many problems of facing mankind.The significant problems such as the particularly energy, human health and environmental protection.Magnetic
Nano material is biomedical in new material, the energy, information by as one, the nanometer material science field star to yield unusually brilliant results
Very important effect is played etc. every field.
Su Bitao etc. is with Fe (NO3)3.9H2O and Ni (NO3)2.6H20 is raw material, is being not added with any alkaline precipitating agent and height
Under conditions of warm Crystallizing treatment, by the optimization to experiment condition (including solvent, solvent heat temperature and time), solvent heat is utilized
The step of method one is prepared for the NiFe204 magnetic Nano materials with good crystallinity and superparamagnetism.As a result show：Use H2O and
EtOH-H2O makees solvent and is unfavorable for NiFe2O4Generation；Solvent is made with EtOH, in order to obtain the higher NiFe of purity2O4Magnetic
Nano material, it is ensured that appropriate solvent heat temperature and time；Magnetic component NiFe in the magnetic property and material of resulting materials2O4
Content it is relevant with its crystallization degree.The advantages of preparation method is most prominent is simple, quick, cost is low, is eliminated from source
Pollution, and the magnetism of material of gained can be excellent.(Chinese Journal of Inorganic Chemistry, 2016,32：69-73.), Liu Li etc. describes a kind of temperature
With the method for lossless immobilization laccase, and its degradation behavior to synthetic dyestuffs have studied.Co deposited synthesis second is used first
The magnetic nano-particle of ethylenediamine tetraacetic acid (EDTA) (EDTA) functionalization, and with Cu2+For abutment, by chelation by laccase it is immobilized in
The magnetic nano-particle surface of EDTA functionalization.Magnetic immobilized laccase is received by transmission electron microscope, ultraviolet-visible spectrometer etc.
Rice material is characterized.Immobilization laccase magnetic Nano material size has good magnetic response ability in 15nm or so.
(environmental project, 2017,35：38-42)；The it is proposeds such as Gong Aiqin modify Fe304 magnetic Nano materials with carboxymethyl-hydroxypropyl beta-CD
Material, to pb in water body2+、Cu2+Absorption studied, and with atomic absorption spectrophotometry in adsorption liquid and eluent
Metal ion content is detected, find synthesis sorbing material to Pb2+ adsorption rate more than 95%, to Cu2+Adsorption rate
More than 85%.(chemical research and application, 2016,28：16801687).
Nano effect just refers to that nano material has unusual or unusual physics, chemistry not available for traditional material special
Property, non-conductive if originally conductive copper is to a certain nanoscale boundary, the silica that insulated originally, crystal etc. are received a certain
Start conduction during meter level boundary.This is due to that nano material has that particle size is small, specific surface area is big, surface energy is high, surface is former
The features such as sub- proportion is big, and its distinctive three big effect：Skin effect, small-size effect and macroscopic quantum tunneling effect
Should.Compared with existing literature, the technical problem to be solved in the present invention is not only to prepare the nano material of higher magnetic, but with group
Point and preparation technology regulate and control, prepare magnetic composite, using the cooperative effect between each component in composite, realize magnetic
Composite material nanometer effect it is controllable, precisely show.
The content of the invention
The invention belongs to field of nanometer material technology, is related to a kind of preparation side of the iron-base magnetic composite with nano effect
Method.Preparation method proposed by the present invention is that pyrroles, ironic citrate, lanthanum nitrate and cellulose is compound, obtains iron base composite material,
Iron base composite material is prepared into polyvinyl alcohol iron-based gel again, then with the method progressively to heat up, iron-based plural gel turned
It is melted into iron-base magnetic composite.
The preparation method of the present invention has following features：(1) it is different from the technical problem that general literature solves, the present invention
Focus on by component and preparation technology to regulate and control the size of iron-base magnetic composite and magnetic Nano effect；(2) it is of the invention
The magnetic Nano effect of acquisition is not apparent, once component or preparation technology change, then magnetic Nano effect disappears, i.e.,
On how obtaining magnetic Nano effect, existing literature can not enlighten from theory or experimentally to the present invention；(3) with existing text
Offering and compare, the present invention has superior technique effect, and the saturation magnetization of prepared iron-base magnetic composite reaches 8907Gs,
It is conventional ferritic 2.2 times, shows magnetic Nano effect.
A kind of preparation method of iron-base magnetic composite with nano effect proposed by the present invention, it is characterised in that system
Standby technique is as follows：
(1) prepared by iron base composite material：The sulfuric acid that pyrroles and molar concentration are 1M is mixed at room temperature, pyrroles and sulfuric acid
Mol ratio is 1: 10, is stirred 10 minutes；Add cellulose, the mass ratio of pyrroles and cellulose is 1: 1, is stirred 20 minutes；So
After be cooled to 0 DEG C, be added dropwise the citric acid solution that molar concentration is 1M, the mol ratio of pyrroles and ironic citrate is 1: 1, continues to stir
Mix 2 hours；The lanthanum nitrate hexahydrate that molar concentration is 0.1M is added dropwise again, the mol ratio of pyrroles and lanthanum nitrate is 10: 1, continues stirring 2
Hour；Then 24 hours are stood at 0 DEG C, filtered, solid is washed, filtered 4 times, to filtrate with distilling water washing, filtering again repeatedly
For neutrality, solid is placed in baking oven, is heated 3 hours in 120 DEG C, is obtained iron base composite material.
(2) prepared by iron-based plural gel：Iron base composite material is ground into the particle of 100-120 mesh, adds distilled water, iron
The mass ratio of based composites and distilled water is 1: 20, is stirred 20 minutes；90 DEG C are again heated to, adds boric acid, boric acid and distillation
The mass ratio of water is 1: 100, is stirred 10 minutes；Adding polyvinyl alcohol, the mass ratio of polyvinyl alcohol and distilled water is 1: 20, after
Continuous stirring 2 hours, is subsequently cooled to 25 DEG C, obtains iron-based plural gel.
(3) prepared by iron-base magnetic composite：Iron-based plural gel is positioned in Muffle furnace, is heated to 100 DEG C, is maintained
3 hours；300 DEG C are again heated to, is maintained 1 hour；450 DEG C are again heated to, is maintained 1 hour；600 DEG C are again heated to, maintenance 1 is small
When；800 DEG C are then heated to, is maintained 1 hour, cooling, obtains iron-base magnetic composite, magnetic coupling material is observed with transmission electron microscope
The average grain diameter of material is 52nm, and the saturation magnetization that iron-base magnetic composite is measured with vibrating specimen magnetometer (VSM) is
8907Gs。
If not using the method progressively to heat up, the present invention also provides following technical scheme as a comparison：
(1) prepared by iron base composite material：The sulfuric acid that pyrroles and molar concentration are 1M is mixed at room temperature, pyrroles and sulfuric acid
Mol ratio is 1: 10, is stirred 10 minutes；Add cellulose, the mass ratio of pyrroles and cellulose is 1: 1, is stirred 20 minutes；So
After be cooled to 0 DEG C, be added dropwise the citric acid solution that molar concentration is 1M, the mol ratio of pyrroles and ironic citrate is 1: 1, continues to stir
Mix 2 hours；The lanthanum nitrate hexahydrate that molar concentration is 0.1M is added dropwise again, the mol ratio of pyrroles and lanthanum nitrate is 10: 1, continues stirring 2
Hour；Then 24 hours are stood at 0 DEG C, filtered, solid is washed, filtered 4 times, to filtrate with distilling water washing, filtering again repeatedly
For neutrality, solid is placed in baking oven, is heated 3 hours in 120 DEG C, is obtained iron base composite material.
(2) prepared by iron-based plural gel：Iron base composite material is ground into the particle of 100-120 mesh, adds distilled water, iron
The mass ratio of based composites and distilled water is 1: 20, is stirred 20 minutes；90 DEG C are again heated to, adds boric acid, boric acid and distillation
The mass ratio of water is 1: 100, is stirred 10 minutes；Adding polyvinyl alcohol, the mass ratio of polyvinyl alcohol and distilled water is 1: 20, after
Continuous stirring 2 hours, is subsequently cooled to 25 DEG C, obtains iron-based plural gel.
(3) prepared by iron-base magnetic composite：Iron-based plural gel is positioned in Muffle furnace, is heated to 800 DEG C, is maintained
7 hours, cooling, iron-base magnetic composite is obtained, the average grain diameter that magnetic composite is observed with transmission electron microscope is 98nm, with shaking
The saturation magnetization that dynamic sample magnetometer (VSM) measures iron-base magnetic composite is 2311Gs.
If not being prepared into iron-based plural gel, the present invention also provides following technical scheme as a comparison：
(1) prepared by iron base composite material：The sulfuric acid that pyrroles and molar concentration are 1M is mixed at room temperature, pyrroles and sulfuric acid
Mol ratio is 1: 10, is stirred 10 minutes；Add cellulose, the mass ratio of pyrroles and cellulose is 1: 1, is stirred 20 minutes；So
After be cooled to 0 DEG C, be added dropwise the citric acid solution that molar concentration is 1M, the mol ratio of pyrroles and ironic citrate is 1: 1, continues to stir
Mix 2 hours；The lanthanum nitrate hexahydrate that molar concentration is 0.1M is added dropwise again, the mol ratio of pyrroles and lanthanum nitrate is 10: 1, continues stirring 2
Hour；Then 24 hours are stood at 0 DEG C, filtered, solid is washed, filtered 4 times, to filtrate with distilling water washing, filtering again repeatedly
For neutrality, solid is placed in baking oven, is heated 3 hours in 120 DEG C, is obtained iron base composite material.
(2) prepared by iron-base magnetic composite：Iron base composite material is positioned in Muffle furnace, is heated to 100 DEG C, is maintained
3 hours；300 DEG C are again heated to, is maintained 1 hour；450 DEG C are again heated to, is maintained 1 hour；600 DEG C are again heated to, maintenance 1 is small
When；800 DEG C are then heated to, is maintained 1 hour, cooling, obtains iron-base magnetic composite, magnetic coupling material is observed with transmission electron microscope
The average grain diameter of material is 91nm, and the saturation magnetization that iron-base magnetic composite is measured with vibrating specimen magnetometer (VSM) is
1139Gs。
If it is raw material to be added without lanthanum nitrate, the present invention also provides following technical scheme as a comparison：
(1) prepared by iron base composite material：The sulfuric acid that pyrroles and molar concentration are 1M is mixed at room temperature, pyrroles and sulfuric acid
Mol ratio is 1: 10, is stirred 10 minutes；Add cellulose, the mass ratio of pyrroles and cellulose is 1: 1, is stirred 20 minutes；So
After be cooled to 0 DEG C, be added dropwise the citric acid solution that molar concentration is 1M, the mol ratio of pyrroles and ironic citrate is 1: 1, continues to stir
Mix 2 hours；Then 0 DEG C stand 24 hours, filter, solid with distillation water washing, filter again, repeatedly washing, suction filtration 4 times, extremely
Filtrate is neutrality, and solid is placed in baking oven, is heated 3 hours in 120 DEG C, is obtained iron base composite material.
(2) prepared by iron-based plural gel：Iron base composite material is ground into the particle of 100-120 mesh, adds distilled water, iron
The mass ratio of based composites and distilled water is 1: 20, is stirred 20 minutes；90 DEG C are again heated to, adds boric acid, boric acid and distillation
The mass ratio of water is 1: 100, is stirred 10 minutes；Adding polyvinyl alcohol, the mass ratio of polyvinyl alcohol and distilled water is 1: 20, after
Continuous stirring 2 hours, is subsequently cooled to 25 DEG C, obtains iron-based plural gel.
(3) prepared by iron-base magnetic composite：Iron-based plural gel is positioned in Muffle furnace, is heated to 100 DEG C, is maintained
3 hours；300 DEG C are again heated to, is maintained 1 hour；450 DEG C are again heated to, is maintained 1 hour；600 DEG C are again heated to, maintenance 1 is small
When；800 DEG C are then heated to, is maintained 1 hour, cooling, obtains iron-base magnetic composite, magnetic coupling material is observed with transmission electron microscope
The average grain diameter of material is 63nm, and the saturation magnetization that iron-base magnetic composite is measured with vibrating specimen magnetometer (VSM) is
3461Gs。
If replacing ironic citrate, lanthanum trichloride to replace lanthanum nitrate as raw material using ferric trichloride, the present invention also provides as follows
Technical scheme is as a comparison：
(1) prepared by iron base composite material：The sulfuric acid that pyrroles and molar concentration are 1M is mixed at room temperature, pyrroles and sulfuric acid
Mol ratio is 1: 10, is stirred 10 minutes；Add cellulose, the mass ratio of pyrroles and cellulose is 1: 1, is stirred 20 minutes；So
After be cooled to 0 DEG C, be added dropwise the liquor ferri trichloridi that molar concentration is 1M, the mol ratio of pyrroles and ferric trichloride is 1: 1, continues to stir
Mix 2 hours；The lanthanum trichloride solution that molar concentration is 0.1M is added dropwise again, the mol ratio of pyrroles and lanthanum trichloride is 10: 1, is continued
Stirring 2 hours；Then 24 hours being stood at 0 DEG C, filtered, solid is washed, filtered 4 times with distilling water washing, filtering again repeatedly,
It is neutrality to filtrate, solid is placed in baking oven, is heated 3 hours in 120 DEG C, is obtained iron base composite material.
(2) prepared by iron-based plural gel：Iron base composite material is ground into the particle of 100120 mesh, adds distilled water, iron
The mass ratio of based composites and distilled water is 1: 20, is stirred 20 minutes；90 DEG C are again heated to, adds boric acid, boric acid and distillation
The mass ratio of water is 1: 100, is stirred 10 minutes；Adding polyvinyl alcohol, the mass ratio of polyvinyl alcohol and distilled water is 1: 20, after
Continuous stirring 2 hours, is subsequently cooled to 25 DEG C, obtains iron-based plural gel.
(3) prepared by iron-base magnetic composite：Iron-based plural gel is positioned in Muffle furnace, is heated to 100 DEG C, is maintained
3 hours；300 DEG C are again heated to, is maintained 1 hour；450 DEG C are again heated to, is maintained 1 hour；600 DEG C are again heated to, maintenance 1 is small
When；800 DEG C are then heated to, is maintained 1 hour, cooling, obtains iron-base magnetic composite, magnetic coupling material is observed with transmission electron microscope
The average grain diameter of material is 41nm, and the saturation magnetization that iron-base magnetic composite is measured with vibrating specimen magnetometer (VSM) is
2891Gs。
If replacing lanthanum nitrate using europium nitrate, the present invention also provides following technical scheme as a comparison as raw material：
(1) prepared by iron base composite material：The sulfuric acid that pyrroles and molar concentration are 1M is mixed at room temperature, pyrroles and sulfuric acid
Mol ratio is 1: 10, is stirred 10 minutes；Add cellulose, the mass ratio of pyrroles and cellulose is 1: 1, is stirred 20 minutes；So
After be cooled to 0 DEG C, be added dropwise the citric acid solution that molar concentration is 1M, the mol ratio of pyrroles and ironic citrate is 1: 1, continues to stir
Mix 2 hours；The europium nitrate solution that molar concentration is 0.1M is added dropwise again, the mol ratio of pyrroles and europium nitrate is 10: 1, continues stirring 2
Hour；Then 24 hours are stood at 0 DEG C, filtered, solid is washed, filtered 4 times, to filtrate with distilling water washing, filtering again repeatedly
For neutrality, solid is placed in baking oven, is heated 3 hours in 120 DEG C, is obtained iron base composite material.
(2) prepared by iron-based plural gel：Iron base composite material is ground into the particle of 100-120 mesh, adds distilled water, iron
The mass ratio of based composites and distilled water is 1: 20, is stirred 20 minutes；90 DEG C are again heated to, adds boric acid, boric acid and distillation
The mass ratio of water is 1: 100, is stirred 10 minutes；Adding polyvinyl alcohol, the mass ratio of polyvinyl alcohol and distilled water is 1: 20, after
Continuous stirring 2 hours, is subsequently cooled to 25 DEG C, obtains iron-based plural gel.
(3) prepared by iron-base magnetic composite：Iron-based plural gel is positioned in Muffle furnace, is heated to 100 DEG C, is maintained
3 hours；300 DEG C are again heated to, is maintained 1 hour；450 DEG C are again heated to, is maintained 1 hour；600 DEG C are again heated to, maintenance 1 is small
When；800 DEG C are then heated to, is maintained 1 hour, cooling, obtains iron-base magnetic composite, magnetic coupling material is observed with transmission electron microscope
The average grain diameter of material is 55nm, and the saturation magnetization that iron-base magnetic composite is measured with vibrating specimen magnetometer (VSM) is
3011Gs。
If it is raw material to be added without cellulose, the present invention also provides following technical scheme as a comparison：
(1) prepared by iron base composite material：The sulfuric acid that pyrroles and molar concentration are 1M is mixed at room temperature, pyrroles and sulfuric acid
Mol ratio is 1: 10, is stirred 10 minutes；0 DEG C is subsequently cooled to, the citric acid solution that molar concentration is 1M, pyrroles and lemon is added dropwise
The mol ratio of lemon acid iron is 1: 1, continues stirring 2 hours；The lanthanum nitrate hexahydrate that molar concentration is 0.1M, pyrroles and nitric acid are added dropwise again
The mol ratio of lanthanum is 10: 1, continues stirring 2 hours；Then 0 DEG C stand 24 hours, filter, solid with distill water washing, take out again
Filter, wash, filter 4 times repeatedly, be neutrality to filtrate, solid is placed in baking oven, is heated 3 hours in 120 DEG C, is obtained iron-based composite wood
Material.
(2) prepared by iron-based plural gel：Iron base composite material is ground into the particle of 100-120 mesh, adds distilled water, iron
The mass ratio of based composites and distilled water is 1: 20, is stirred 20 minutes；90 DEG C are again heated to, adds boric acid, boric acid and distillation
The mass ratio of water is 1: 100, is stirred 10 minutes；Adding polyvinyl alcohol, the mass ratio of polyvinyl alcohol and distilled water is 1: 20, after
Continuous stirring 2 hours, is subsequently cooled to 25 DEG C, obtains iron-based plural gel.
(3) prepared by iron-base magnetic composite：Iron-based plural gel is positioned in Muffle furnace, is heated to 100 DEG C, is maintained
3 hours；300 DEG C are again heated to, is maintained 1 hour；450 DEG C are again heated to, is maintained 1 hour；600 DEG C are again heated to, maintenance 1 is small
When；800 DEG C are then heated to, is maintained 1 hour, cooling, obtains iron-base magnetic composite, magnetic coupling material is observed with transmission electron microscope
The average grain diameter of material is 78nm, and the saturation magnetization that iron-base magnetic composite is measured with vibrating specimen magnetometer (VSM) is
2122Gs。
Conventional ferritic saturation magnetization is 4000Gs or so, and the technique effect of correlation technique scheme is not over normal
It is horizontal to advise ferritic saturation magnetization, illustrates when technical scheme changes, or raw material are simply replaced, then magnetic Nano
Effect disappears, and the technique effect (nano effect) in the present invention is that magnetic composite each component acts synergistically under special process
Result, when component or technique change, the synergistic mechanism in composite between each component changes in theory, i.e., not
It is different with the inherent Solicitation mechanism of the technique effect (such as nano effect) of composite, therefore, what the present patent application was claimed
Technical scheme is unique and creative.
Embodiment
The invention is further illustrated by the following examples
Embodiment 1
0.1mol pyrroles is mixed with the sulfuric acid that 1000ml molar concentrations are 1M at room temperature, stirred 10 minutes；Add
6.7g celluloses, stir 20 minutes；0 DEG C is subsequently cooled to, the citric acid solution that 100ml molar concentrations are 1M is added dropwise, continues
Stirring 2 hours；The lanthanum nitrate hexahydrate that 10ml molar concentrations are 0.1M is added dropwise again, continues stirring 2 hours；Then 24 are stood at 0 DEG C
Hour, suction filtration, solid is washed, filtered 4 times with distilling water washing, filtering again repeatedly, to filtrate to be neutral, solid placement baking oven
In, heated 3 hours in 120 DEG C, obtain iron base composite material.
10g iron base composite materials are ground into the particle of 100-120 mesh, add 200g distilled water, are stirred 20 minutes；Again plus
Heat adds 2g boric acid to 90 DEG C, stirs 10 minutes；10g polyvinyl alcohol is added, continues stirring 2 hours, is subsequently cooled to 25
DEG C, obtain iron-based plural gel.
10g iron-based plural gels are positioned in Muffle furnace, are heated to 100 DEG C, are maintained 3 hours；300 DEG C are again heated to,
Maintain 1 hour；450 DEG C are again heated to, is maintained 1 hour；600 DEG C are again heated to, is maintained 1 hour；800 DEG C are then heated to, dimension
Hold 1 hour, cool down, obtain iron-base magnetic composite, the average grain diameter that magnetic composite is observed with transmission electron microscope is 52nm, is used
The saturation magnetization that vibrating specimen magnetometer (VSM) measures iron-base magnetic composite is 8907Gs.
Embodiment 2
0.1mol pyrroles is mixed with the sulfuric acid that 1000ml molar concentrations are 1M at room temperature, stirred 10 minutes；Add
6.7g celluloses, stir 20 minutes；0 DEG C is subsequently cooled to, the citric acid solution that 100ml molar concentrations are 1M is added dropwise, continues
Stirring 2 hours；The lanthanum nitrate hexahydrate that 10ml molar concentrations are 0.1M is added dropwise again, continues stirring 2 hours；Then 24 are stood at 0 DEG C
Hour, suction filtration, solid is washed, filtered 4 times with distilling water washing, filtering again repeatedly, to filtrate to be neutral, solid placement baking oven
In, heated 3 hours in 120 DEG C, obtain iron base composite material.
10g iron base composite materials are ground into the particle of 100-120 mesh, add 200g distilled water, are stirred 20 minutes；Again plus
Heat adds 2g boric acid to 90 DEG C, stirs 10 minutes；10g polyvinyl alcohol is added, continues stirring 2 hours, is subsequently cooled to 25
DEG C, obtain iron-based plural gel.
10g iron-based plural gels are positioned in Muffle furnace, are heated to 800 DEG C, are maintained 7 hours, cooling, obtain iron-base magnetic
Composite, the average grain diameter that magnetic composite is observed with transmission electron microscope is 98nm, is measured with vibrating specimen magnetometer (VSM)
The saturation magnetization of iron-base magnetic composite is 2311Gs.
Embodiment 3
0.1mol pyrroles is mixed with the sulfuric acid that 1000ml molar concentrations are 1M at room temperature, stirred 10 minutes；Add
6.7g celluloses, stir 20 minutes；0 DEG C is subsequently cooled to, the citric acid solution that 100ml molar concentrations are 1M is added dropwise, continues
Stirring 2 hours；The lanthanum nitrate hexahydrate that 10ml molar concentrations are 0.1M is added dropwise again, continues stirring 2 hours；Then 24 are stood at 0 DEG C
Hour, suction filtration, solid is washed, filtered 4 times with distilling water washing, filtering again repeatedly, to filtrate to be neutral, solid placement baking oven
In, heated 3 hours in 120 DEG C, obtain iron base composite material.
10g iron base composite materials are positioned in Muffle furnace, are heated to 100 DEG C, are maintained 3 hours；300 DEG C are again heated to,
Maintain 1 hour；450 DEG C are again heated to, is maintained 1 hour；600 DEG C are again heated to, is maintained 1 hour；800 DEG C are then heated to, dimension
Hold 1 hour, cool down, obtain iron-base magnetic composite, the average grain diameter that magnetic composite is observed with transmission electron microscope is 91nm, is used
The saturation magnetization that vibrating specimen magnetometer (VSM) measures iron-base magnetic composite is 1139Gs.
Embodiment 4
0.1mol pyrroles is mixed with the sulfuric acid that 1000ml molar concentrations are 1M at room temperature, stirred 10 minutes；Add
6.7g celluloses, stir 20 minutes；0 DEG C is subsequently cooled to, the citric acid solution that 100ml molar concentrations are 1M is added dropwise, continues
Stirring 2 hours；Then 24 hours being stood at 0 DEG C, filtered, solid is washed, filtered 4 times with distilling water washing, filtering again repeatedly,
It is neutrality to filtrate, solid is placed in baking oven, is heated 3 hours in 120 DEG C, is obtained iron base composite material.
10g iron base composite materials are ground into the particle of 100-120 mesh, add 200g distilled water, are stirred 20 minutes；Again plus
Heat adds 2g boric acid to 90 DEG C, stirs 10 minutes；10g polyvinyl alcohol is added, continues stirring 2 hours, is subsequently cooled to 25
DEG C, obtain iron-based plural gel.
10g iron-based plural gels are positioned in Muffle furnace, are heated to 100 DEG C, are maintained 3 hours；300 DEG C are again heated to,
Maintain 1 hour；450 DEG C are again heated to, is maintained 1 hour；600 DEG C are again heated to, is maintained 1 hour；800 DEG C are then heated to, dimension
Hold 1 hour, cool down, obtain iron-base magnetic composite, the average grain diameter that magnetic composite is observed with transmission electron microscope is 63nm, is used
The saturation magnetization that vibrating specimen magnetometer (VSM) measures iron-base magnetic composite is 3461Gs.
Embodiment 5
0.1mol pyrroles is mixed with the sulfuric acid that 1000ml molar concentrations are 1M at room temperature, stirred 10 minutes；Add
6.7g celluloses, stir 20 minutes；0 DEG C is subsequently cooled to, the liquor ferri trichloridi that 100ml molar concentrations are 1M is added dropwise, continues
Stirring 2 hours；The lanthanum trichloride solution that 10ml molar concentrations are 0.1M is added dropwise again, continues stirring 2 hours；Then in 0 DEG C of standing
24 hours, filter, solid is washed, filtered 4 times with distilling water washing, filtering again repeatedly, is neutrality to filtrate, and solid placement is dried
In case, heated 3 hours in 120 DEG C, obtain iron base composite material.
10g iron base composite materials are ground into the particle of 100-120 mesh, add 200g distilled water, are stirred 20 minutes；Again plus
Heat adds 2g boric acid to 90 DEG C, stirs 10 minutes；10g polyvinyl alcohol is added, continues stirring 2 hours, is subsequently cooled to 25
DEG C, obtain iron-based plural gel.
10g iron-based plural gels are positioned in Muffle furnace, are heated to 100 DEG C, are maintained 3 hours；300 DEG C are again heated to,
Maintain 1 hour；450 DEG C are again heated to, is maintained 1 hour；600 DEG C are again heated to, is maintained 1 hour；800 DEG C are then heated to, dimension
Hold 1 hour, cool down, obtain iron-base magnetic composite, the average grain diameter that magnetic composite is observed with transmission electron microscope is 41nm, is used
The saturation magnetization that vibrating specimen magnetometer (VSM) measures iron-base magnetic composite is 2891Gs.
Embodiment 6
0.1mol pyrroles is mixed with the sulfuric acid that 1000ml molar concentrations are 1M at room temperature, stirred 10 minutes；Add
6.7g celluloses, stir 20 minutes；0 DEG C is subsequently cooled to, the citric acid solution that 100ml molar concentrations are 1M is added dropwise, continues
Stirring 2 hours；The europium nitrate solution that 10ml molar concentrations are 0.1M is added dropwise again, continues stirring 2 hours；Then 24 are stood at 0 DEG C
Hour, suction filtration, solid is washed, filtered 4 times with distilling water washing, filtering again repeatedly, to filtrate to be neutral, solid placement baking oven
In, heated 3 hours in 120 DEG C, obtain iron base composite material.
10g iron base composite materials are ground into the particle of 100-120 mesh, add 200g distilled water, are stirred 20 minutes；Again plus
Heat adds 2g boric acid to 90 DEG C, stirs 10 minutes；10g polyvinyl alcohol is added, continues stirring 2 hours, is subsequently cooled to 25
DEG C, obtain iron-based plural gel.
10g iron-based plural gels are positioned in Muffle furnace, are heated to 100 DEG C, are maintained 3 hours；300 DEG C are again heated to,
Maintain 1 hour；450 DEG C are again heated to, is maintained 1 hour；600 DEG C are again heated to, is maintained 1 hour；800 DEG C are then heated to, dimension
Hold 1 hour, cool down, obtain iron-base magnetic composite, the average grain diameter that magnetic composite is observed with transmission electron microscope is 55nm, is used
The saturation magnetization that vibrating specimen magnetometer (VSM) measures iron-base magnetic composite is 3011Gs.
Embodiment 7
0.1mol pyrroles is mixed with the sulfuric acid that 1000ml molar concentrations are 1M at room temperature, stirred 10 minutes；Then cool down
To 0 DEG C, the citric acid solution that 100ml molar concentrations are 1M is added dropwise, continues stirring 2 hours；10ml molar concentrations are added dropwise again is
0.1M lanthanum nitrate hexahydrate, continue stirring 2 hours；Then 0 DEG C stand 24 hours, filter, solid with distill water washing, take out again
Filter, wash, filter 4 times repeatedly, be neutrality to filtrate, solid is placed in baking oven, is heated 3 hours in 120 DEG C, is obtained iron-based composite wood
Material.
10g iron base composite materials are ground into the particle of 100-120 mesh, add 200g distilled water, are stirred 20 minutes；Again plus
Heat adds 2g boric acid to 90 DEG C, stirs 10 minutes；10g polyvinyl alcohol is added, continues stirring 2 hours, is subsequently cooled to 25
DEG C, obtain iron-based plural gel.
10g iron-based plural gels are positioned in Muffle furnace, are heated to 100 DEG C, are maintained 3 hours；300 DEG C are again heated to,
Maintain 1 hour；450 DEG C are again heated to, is maintained 1 hour；600 DEG C are again heated to, is maintained 1 hour；800 DEG C are then heated to, dimension
Hold 1 hour, cool down, obtain iron-base magnetic composite, the average grain diameter that magnetic composite is observed with transmission electron microscope is 78nm, is used
The saturation magnetization that vibrating specimen magnetometer (VSM) measures iron-base magnetic composite is 2122Gs.
Claims (1)
1. a kind of preparation method of the iron-base magnetic composite with nano effect, it is characterised in that comprise the following steps that：
(1) prepared by iron base composite material：Pyrroles is mixed with the sulfuric acid that molar concentration is 1M at room temperature, mole of pyrroles and sulfuric acid
Than for 1: 10, stirring 10 minutes；Add cellulose, the mass ratio of pyrroles and cellulose is 1: 1, is stirred 20 minutes；Then it is cold
But to 0 DEG C, the citric acid solution that molar concentration is 1M is added dropwise, the mol ratio of pyrroles and ironic citrate is 1: 1, continues stirring 2
Hour；The lanthanum nitrate hexahydrate that molar concentration is 0.1M is added dropwise again, the mol ratio of pyrroles and lanthanum nitrate is 10: 1, and it is small to continue stirring 2
When；Then 24 hours are stood at 0 DEG C, filtered, solid is washed, filtered 4 times, be to filtrate with distilling water washing, filtering again repeatedly
Neutrality, solid are placed in baking oven, are heated 3 hours in 120 DEG C, are obtained iron base composite material；
(2) prepared by iron-based plural gel：Iron base composite material is ground into the particle of 100-120 mesh, adds distilled water, iron-based is multiple
The mass ratio of condensation material and distilled water is 1: 20, is stirred 20 minutes；It is again heated to 90 DEG C, adds boric acid, boric acid and distilled water
Mass ratio is 1: 100, is stirred 10 minutes；Add polyvinyl alcohol, the mass ratio of polyvinyl alcohol and distilled water is 1：20, continue to stir
Mix 2 hours, be subsequently cooled to 25 DEG C, obtain iron-based plural gel；
(3) prepared by iron-base magnetic composite：Iron-based plural gel is positioned in Muffle furnace, is heated to 100 DEG C, maintenance 3 is small
When；300 DEG C are again heated to, is maintained 1 hour；450 DEG C are again heated to, is maintained 1 hour；600 DEG C are again heated to, is maintained 1 hour；So
After be heated to 800 DEG C, maintain 1 hour, cooling, obtain iron-base magnetic composite, magnetic composite is observed with transmission electron microscope
Average grain diameter, the saturation magnetization of iron-base magnetic composite is measured with vibrating specimen magnetometer (VSM).
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