CN106219610A - A kind of preparation method of Conjugate ferrite nano magnetic material - Google Patents
A kind of preparation method of Conjugate ferrite nano magnetic material Download PDFInfo
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Abstract
The present invention relates to the preparation method of a kind of Conjugate ferrite nano magnetic material, belong to nano magnetic material technical field.The invention provides the preparation method of a kind of Conjugate ferrite nano magnetic material.The present invention passes through liquid fermentation and culture bacillus acidophilus, it is centrifugally separating to obtain ferment product, concentrated precipitate with ethanol prepares bacterial polysaccharides, add when cobalt nitrate and ferric nitrate collosol and gel form Conjugate ferrite, layer protecting film is formed on Conjugate ferrite surface, make its increase accelerate flocculation and obtain gel of no longer reuniting, decomposing removal bacterial polysaccharides after high-temperature calcination makes the Conjugate ferrite of cladding expose, i.e. can get Conjugate ferrite nano magnetic material, solve and use sol-gal process at present, the nanometer ferrite of the preparation such as coprecipitation, easily produce reunion, the problem making magnetic nanoparticle bad dispersibility, use can be widely popularized.
Description
Technical field
The present invention relates to the preparation method of a kind of Conjugate ferrite nano magnetic material, belong to nano magnetic material technology neck
Territory.
Background technology
Ferrite is a kind of novel nonmetal magnetic material developed rapidly from the forties in 20th century.With metallic magnetic
Property material is compared, and ferrite has that resistivity is big, dielectric properties are high, have the advantages such as higher pcrmeability when high frequency.Ferrum oxygen
Body magnetic material can use chemical molecular formula MFe2O4Represent.Ferrite magnetic material is the mixing by sintering these metallic compounds
Thing and manufacture.The main feature resistivity of ferrite magnetic material is much larger than metallicl magnetic material, it is suppressed that eddy current
Produce, make ferrimagnetism can apply to high frequency field.Conjugate ferrite magnetic micro-powder has the Wuli-Shili-Renli system approach of uniqueness, urges
Change characteristic and magnetic characteristic.As stupid power and resistivity can reach the level of high tens times than magnetic alloy, high frequency pcrmeability is higher, single
Unit's ferrite magnetocrystalline anisotropy constant at room temperature is up to about 2.7 × 105J·m-3, bigger magneto-optic is had in visible region
Deflection angle, stable chemical performance and anti-corrosion, wear-resisting, thus its diameter of particle and dc magnetization parameter can be adjusted to suitably
Scope is used as magnetic recording media, to ensure to improve constantly packing density under the conditions of enough signal to noise ratios.Along with sending out of science and technology
Exhibition, ferrite is not only increasingly extensive in electronics industry application such as communication broadcast, dynamic control, computing technique and instrument and meters,
Have become as indispensable ingredient, and show and the aspect such as pollution process in space travel, satellite communication, information.
Owing to ferrite performance is good, low cost, technique can save simply, again a large amount of noble metal, it has also become high frequency light current has in field very much
A kind of nonmetal magnetic material of development prospect.It can be high as a kind of its operating frequency of magnetic material, and magnetic spectrum characteristic is good, at present
It is widely used to the sides such as mutual inductance device, magnetic core bearing, permutator, information storage, magnetic fluid, microwave absorption and medical diagnosis
Face.In recent years, the preparation of magnetic Nano material is increasingly paid close attention to by people, develops different types of Nanometer Cobalt Ferrite Oxide material
Material becomes the focus of current magnetic material research.At present, traditional nano material uses sol-gel process, hydro-thermal method, co-precipitation
, owing to ferromagnetic material is easily reunited, there is prepared magnetic nanoparticle dispersion in the nano soft magnetism Zn ferrite of the preparation such as method
Property difference defect.
Summary of the invention
The technical problem to be solved: for the nanometer using sol-gel process, coprecipitation etc. to prepare at present
Ferrite, owing to ferromagnetic material is easily reunited, the defect of the magnetic nanoparticle bad dispersibility generally prepared, the invention provides one
Plant the preparation method of Conjugate ferrite nano magnetic material.The present invention passes through liquid fermentation and culture bacillus acidophilus, and centrifugation obtains
To ferment product, concentrated precipitate with ethanol prepares bacterial polysaccharides, adds when forming Conjugate ferrite at cobalt nitrate and ferric nitrate collosol and gel
Enter, form layer protecting film on Conjugate ferrite surface so that it is no longer reuniting with increasing and accelerate flocculation obtains gel, after high-temperature calcination
Decomposing removal bacterial polysaccharides makes the Conjugate ferrite of cladding expose, and i.e. can get Conjugate ferrite nano magnetic material, solves at present
Use the nanometer ferrite of the preparation such as sol-gel process, coprecipitation, easily produce reunion so that magnetic nanoparticle disperses
Property difference problem, use can be widely popularized.
For solving above-mentioned technical problem, the technical solution used in the present invention:
(1) weigh 8～10g Carnis Bovis seu Bubali creams, 8～10g peptone, 3～5g yeast extract, 1～2g dipotassium hydrogen phosphate, 3～5g sodium acetate,
1～2g Triammonium citrate, 18～20g glucose and 15～20g agar join in 1000～1200mL distilled water, stir
Afterwards with concentration be 1mol/L salt acid for adjusting pH to 6.0～6.5, with autoclave sterilizer, at 120～130 DEG C sterilizing 20～
30min obtains fermentation medium；
(2) by inoculum concentration be 10% will activation after bacillus acidophilus access in above-mentioned fermentation medium, at 35～40 DEG C with
200～300r/min rotating speed shake flask fermentations cultivate 28～32h, cultivate and use horizontal centrifuge with 10000 after terminating at 4～6 DEG C
～12000r/min rotating speed frozen centrifugation 15～20min, separate removal filtering residue and obtain high fermentation liquid；
(3) 1/3 that above-mentioned fermentation liquid vacuum concentration pot is concentrated into its original volume obtains Fermented Condensed liquid, adds in concentrated solution
Its volume 5～dehydrated alcohol of 7 times, staticly settle overnight in 4～6 DEG C of ice-water baths, and sucking filtration obtains filtering residue, with dehydrated alcohol repeatedly
It is dried after washing 3～5 times, obtains bacillus acidophilus's fermentation polysaccharides；
(4) weigh 7.0～7.5g cobalt nitrates and 20.0～20.5g ferric nitrates are dissolved in 50～100g deionized waters, 50～60
Stirring 1～2h under DEG C water-bath, adding 100～120mL concentration is 0.5mol/L citric acid solution, is placed on magnetic stirrer
It is stirred with 200～300r/min rotating speeds, during stirring, adds 3～5g above-mentioned bacillus acidophilus's fermentation polysaccharides,
Continue stirring 10～15min and obtain mixed liquor；
(5) dropwise dripping mass concentration in above-mentioned mixed liquor is 25% ammonia until pH of mixed is to reaching 7.0～7.5, raises
Bath temperature is to 70～80 DEG C and to continue stirring until mixed liquor be collosol state, by the colloidal sol blast drier that obtains with 230
～250 DEG C of temperature be dried 2～3h after obtain gel；
(6) gel obtained above is put in tube type resistance furnace, be warming up to 750～850 DEG C of guarantors with 10 DEG C/min rate program
Discharging after temperature calcining 3～4h, with corundum mortar grinder 1～2h 200 mesh standard sieves excessively, obtains Conjugate ferrite nano-magnetic material
Material.
The concrete application process of the present invention: the saturated magnetic strength of Conjugate ferrite nano magnetic material that the present invention prepares > 1.7, occupy
In temperature be 500～520 DEG C, resistivity is 1.17～1.41 μ Ω m, and saturation field intensity is 33000～33500A/m, magnetic conductance
Rate is 120～130mH/m, and loss is 10.8～12.3W, and sensitivity is 0.5%/(A m-1).
The present invention is compared with additive method, and Advantageous Effects is:
(1) the Conjugate ferrite nano magnetic material that prepared by the present invention solves and uses sol-gel process, coprecipitation etc. to make at present
Standby nanometer ferrite, easily produces reunion so that the problem of magnetic nanoparticle bad dispersibility, have good stability and
Dispersibility；
(2) the Conjugate ferrite nano magnetic material that prepared by the present invention has even particle size distribution, and product purity is high, and saturated magnetization is strong
Spend high feature, can be widely applied to nanometer Magnet technical field.
Detailed description of the invention
First 8～10g Carnis Bovis seu Bubali creams, 8～10g peptone, 3～5g yeast extract, 1～2g dipotassium hydrogen phosphate, 3～5g vinegar are weighed
Acid sodium, 1～2g Triammonium citrate, 18～20g glucose and 15～20g agar join in 1000～1200mL distilled water, stir
Mix after uniformly with concentration be 1mol/L salt acid for adjusting pH to 6.0～6.5, with autoclave sterilizer, go out at 120～130 DEG C
Bacterium 20～30min obtains fermentation medium；Secondly it is 10% the bacillus acidophilus after activation to be accessed above-mentioned fermentation culture by inoculum concentration
In base, at 35～40 DEG C with 200～300r/min rotating speed shake flask fermentations cultivate 28～32h, cultivate terminate after at 4～6 DEG C
With horizontal centrifuge with 10000～12000r/min rotating speed frozen centrifugations 15～20min, separate removal filtering residue and obtain high fermentation
Liquid；
1/3 that above-mentioned fermentation liquid vacuum concentration pot is concentrated into its original volume again obtains Fermented Condensed liquid, adds in concentrated solution
Entering its volume 5～dehydrated alcohol of 7 times, staticly settle overnight in 4～6 DEG C of ice-water baths, sucking filtration obtains filtering residue, anti-with dehydrated alcohol
After backwashing is dried after washing 3～5 times, obtains bacillus acidophilus's fermentation polysaccharides；Then weigh 7.0～7.5g cobalt nitrates and 20.0～
20.5g ferric nitrate is dissolved in 50～100g deionized waters, stirs 1～2h, add 100～120mL under 50～60 DEG C of water-baths
Concentration is 0.5mol/L citric acid solution, is placed on magnetic stirrer and is stirred with 200～300r/min rotating speeds, in stirring
During add 3～5g above-mentioned bacillus acidophilus's fermentation polysaccharides, continue stirring 10～15min and obtain mixed liquor；Again up
Stating and dropwise dripping mass concentration in mixed liquor is 25% ammonia until pH of mixed is to reaching 7.0～7.5, raises bath temperature extremely
70～80 DEG C and to continue stirring until mixed liquor be collosol state, by the colloidal sol blast drier that obtains with 230～250 DEG C of temperature
Gel is obtained after being dried 2～3h；Finally gel obtained above is put in tube type resistance furnace, with 10 DEG C/min rate program liter
Temperature is incubated discharging after calcining 3～4h to 750～850 DEG C, with corundum mortar grinder 1～2h 200 mesh standard sieves excessively, obtains ferro-cobalt
Oxysome nano magnetic material.
Example 1
First 8g Carnis Bovis seu Bubali cream, 8g peptone, 3g yeast extract, 1g dipotassium hydrogen phosphate, 3g sodium acetate, 1g Triammonium citrate, 18g are weighed
Glucose and 15g agar join in 1000mL distilled water, after stirring with concentration be 1mol/L salt acid for adjusting pH to 6.0,
With autoclave sterilizer, at 120 DEG C, sterilizing 20min obtains fermentation medium；Secondly by inoculum concentration be 10% will after activation addicted to
Lactobacillus lactis accesses in above-mentioned fermentation medium, cultivates 28h with 200r/min rotating speed shake flask fermentation at 35 DEG C, cultivates after terminating
With horizontal centrifuge with 10000r/min rotating speed frozen centrifugation 15min at 4 DEG C, separate removal filtering residue and obtain high fermentation liquid；
1/3 that above-mentioned fermentation liquid vacuum concentration pot is concentrated into its original volume again obtains Fermented Condensed liquid, adds it in concentrated solution
The dehydrated alcohol that volume is 5 times, staticly settles overnight in 4 DEG C of ice-water baths, and sucking filtration obtains filtering residue, with dehydrated alcohol cyclic washing 3 times
Rear dry, obtain bacillus acidophilus's fermentation polysaccharides；Then weigh 7.0g cobalt nitrate and 20.0g ferric nitrate is dissolved in 50g deionized water
In, under 50 DEG C of water-baths, stir 1h, adding 100mL concentration is 0.5mol/L citric acid solution, is placed on magnetic stirrer
It is stirred with 200r/min rotating speed, during stirring, adds 3g above-mentioned bacillus acidophilus fermentation polysaccharides, continue stirring
10min obtains mixed liquor；Stating again up and dropwise dripping mass concentration in mixed liquor is that 25% ammonia is until pH of mixed is to reaching
7.0, to 70 DEG C and to continue stirring until mixed liquor be collosol state to raise bath temperature, by the colloidal sol blast drier that obtains with
230 DEG C of temperature obtain gel after being dried 3h；Finally gel obtained above is put in tube type resistance furnace, with 10 DEG C/min speed
Discharging after 3h is calcined in temperature programming to 750 DEG C of insulations, with corundum mortar grinder 1h 200 mesh standard sieves excessively, obtains Conjugate ferrite
Nano magnetic material.
The saturated magnetic strength of Conjugate ferrite nano magnetic material 1.8 that the present invention prepares, Curie temperature is 500 DEG C, and resistivity is
1.17 μ Ω m, saturation field intensity is 33000A/m, and pcrmeability is 120mH/m, is lost as 10.8W, and sensitivity is 0.5%/(A
m-1).
Example 2
First 9g Carnis Bovis seu Bubali cream, 9g peptone, 4g yeast extract, 1g dipotassium hydrogen phosphate, 4g sodium acetate, 1g Triammonium citrate, 19g are weighed
Glucose and 17g agar join in 1100mL distilled water, after stirring with concentration be 1mol/L salt acid for adjusting pH to 6.3,
With autoclave sterilizer, at 125 DEG C, sterilizing 25min obtains fermentation medium；Secondly by inoculum concentration be 10% will after activation addicted to
Lactobacillus lactis accesses in above-mentioned fermentation medium, cultivates 30h with 250r/min rotating speed shake flask fermentation at 37 DEG C, cultivates after terminating
With horizontal centrifuge with 11000r/min rotating speed frozen centrifugation 17min at 5 DEG C, separate removal filtering residue and obtain high fermentation liquid；
1/3 that above-mentioned fermentation liquid vacuum concentration pot is concentrated into its original volume again obtains Fermented Condensed liquid, adds it in concentrated solution
The dehydrated alcohol that volume is 6 times, staticly settles overnight in 5 DEG C of ice-water baths, and sucking filtration obtains filtering residue, with dehydrated alcohol cyclic washing 4 times
Rear dry, obtain bacillus acidophilus's fermentation polysaccharides；Then weigh 7.3 cobalt nitrates and 20.3g ferric nitrate is dissolved in 70g deionized water
In, under 55 DEG C of water-baths, stir 2h, adding 110mL concentration is 0.5mol/L citric acid solution, is placed on magnetic stirrer
It is stirred with 250r/min rotating speed, during stirring, adds 4g above-mentioned bacillus acidophilus fermentation polysaccharides, continue stirring
13min obtains mixed liquor；Stating again up and dropwise dripping mass concentration in mixed liquor is that 25% ammonia is until pH of mixed is to reaching
7.3, to 75 DEG C and to continue stirring until mixed liquor be collosol state to raise bath temperature, by the colloidal sol blast drier that obtains with
240 DEG C of temperature obtain gel after being dried 2h；Finally gel obtained above is put in tube type resistance furnace, with 10 DEG C/min speed
Discharging after 3h is calcined in temperature programming to 800 DEG C of insulations, with corundum mortar grinder 1h 200 mesh standard sieves excessively, obtains Conjugate ferrite
Nano magnetic material.
The saturated magnetic strength of Conjugate ferrite nano magnetic material 1.9 that the present invention prepares, Curie temperature is 510 DEG C, and resistivity is
1.35 μ Ω m, saturation field intensity is 33400A/m, and pcrmeability is 110mH/m, is lost as 11.2W, and sensitivity is 0.5%/(A
m-1).
Example 3
First weigh 10g Carnis Bovis seu Bubali cream, 10g peptone, 5g yeast extract, 2g dipotassium hydrogen phosphate, 5g sodium acetate, 2g Triammonium citrate,
20g glucose and 20g agar join in 1200mL distilled water, after stirring with concentration be 1mol/L salt acid for adjusting pH extremely
6.5, with autoclave sterilizer, at 130 DEG C, sterilizing 30min obtains fermentation medium；Secondly after being 10% general's activation by inoculum concentration
Bacillus acidophilus access in above-mentioned fermentation medium, at 40 DEG C with 300r/min rotating speed shake flask fermentation cultivate 32h, cultivate knot
At 6 DEG C, high fermentation is obtained with horizontal centrifuge with 12000r/min rotating speed frozen centrifugation 20min, separation removal filtering residue after bundle
Liquid；1/3 that above-mentioned fermentation liquid vacuum concentration pot is concentrated into its original volume again obtains Fermented Condensed liquid, adds in concentrated solution
The dehydrated alcohol of its volume 7 times, staticly settles overnight in 6 DEG C of ice-water baths, and sucking filtration obtains filtering residue, with dehydrated alcohol cyclic washing 5
It is dried all over rear, obtains bacillus acidophilus's fermentation polysaccharides；Then weigh 7.5g cobalt nitrate and 20.5g ferric nitrate is dissolved in 100g deionization
In water, stirring 2h under 60 DEG C of water-baths, adding 120mL concentration is 0.5mol/L citric acid solution, is placed on magnetic stirrer
On be stirred with 300r/min rotating speed, stirring during add 5g above-mentioned bacillus acidophilus fermentation polysaccharides, continue to stir
Mix 15min and obtain mixed liquor；Stating again up and dropwise dripping mass concentration in mixed liquor is that 25% ammonia is until pH of mixed is to reaching
7.5, to 80 DEG C and to continue stirring until mixed liquor be collosol state to raise bath temperature, by the colloidal sol blast drier that obtains with
250 DEG C of temperature obtain gel after being dried 2.5h；Finally gel obtained above is put in tube type resistance furnace, with 10 DEG C/min speed
Discharging after 4h is calcined in rate temperature programming to 850 DEG C of insulations, with corundum mortar grinder 2h 200 mesh standard sieves excessively, obtains ferro-cobalt oxygen
Body nano magnetic material.
The saturated magnetic strength of Conjugate ferrite nano magnetic material 2.0 that the present invention prepares, Curie temperature is 520 DEG C, and resistivity is
1.41 μ Ω m, saturation field intensity is 33500A/m, and pcrmeability is 130mH/m, is lost as 12.3W, and sensitivity is 0.5%/(A
m-1).
Claims (1)
1. the preparation method of a Conjugate ferrite nano magnetic material, it is characterised in that concrete preparation process is:
(1) weigh 8～10g Carnis Bovis seu Bubali creams, 8～10g peptone, 3～5g yeast extract, 1～2g dipotassium hydrogen phosphate, 3～5g sodium acetate,
1～2g Triammonium citrate, 18～20g glucose and 15～20g agar join in 1000～1200mL distilled water, stir
Afterwards with concentration be 1mol/L salt acid for adjusting pH to 6.0～6.5, with autoclave sterilizer, at 120～130 DEG C sterilizing 20～
30min obtains fermentation medium；
(2) by inoculum concentration be 10% will activation after bacillus acidophilus access in above-mentioned fermentation medium, at 35～40 DEG C with
200～300r/min rotating speed shake flask fermentations cultivate 28～32h, cultivate and use horizontal centrifuge with 10000 after terminating at 4～6 DEG C
～12000r/min rotating speed frozen centrifugation 15～20min, separate removal filtering residue and obtain high fermentation liquid；
(3) 1/3 that above-mentioned fermentation liquid vacuum concentration pot is concentrated into its original volume obtains Fermented Condensed liquid, adds in concentrated solution
Its volume 5～dehydrated alcohol of 7 times, staticly settle overnight in 4～6 DEG C of ice-water baths, and sucking filtration obtains filtering residue, with dehydrated alcohol repeatedly
It is dried after washing 3～5 times, obtains bacillus acidophilus's fermentation polysaccharides；
(4) weigh 7.0～7.5g cobalt nitrates and 20.0～20.5g ferric nitrates are dissolved in 50～100g deionized waters, 50～60
Stirring 1～2h under DEG C water-bath, adding 100～120mL concentration is 0.5mol/L citric acid solution, is placed on magnetic stirrer
It is stirred with 200～300r/min rotating speeds, during stirring, adds 3～5g above-mentioned bacillus acidophilus's fermentation polysaccharides,
Continue stirring 10～15min and obtain mixed liquor；
(5) dropwise dripping mass concentration in above-mentioned mixed liquor is 25% ammonia until pH of mixed is to reaching 7.0～7.5, raises
Bath temperature is to 70～80 DEG C and to continue stirring until mixed liquor be collosol state, by the colloidal sol blast drier that obtains with 230
～250 DEG C of temperature be dried 2～3h after obtain gel；
(6) gel obtained above is put in tube type resistance furnace, be warming up to 750～850 DEG C of guarantors with 10 DEG C/min rate program
Discharging after temperature calcining 3～4h, with corundum mortar grinder 1～2h 200 mesh standard sieves excessively, obtains Conjugate ferrite nano-magnetic material
Material.
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