CN106830910A - A kind of preparation method of strontium ferrite magnetic powder - Google Patents

A kind of preparation method of strontium ferrite magnetic powder Download PDF

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CN106830910A
CN106830910A CN201611191278.7A CN201611191278A CN106830910A CN 106830910 A CN106830910 A CN 106830910A CN 201611191278 A CN201611191278 A CN 201611191278A CN 106830910 A CN106830910 A CN 106830910A
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mixture
preparation
standby
sodium
magnetic powder
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周国胜
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MAANSHAN QIJIN MAGNET CO Ltd
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MAANSHAN QIJIN MAGNET CO Ltd
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Abstract

The invention discloses a kind of preparation method of strontium ferrite magnetic powder, belong to magnetic material processing technique field, specifically include following steps：（1）Raw material preparation,（2）Calcination process.Obtained strontium ferrite magnetic powder of the invention has good magnetic property, its HCJ and saturation magnetization are effectively lifted, HCJ reaches more than 4000Oe, residual magnetization reaches more than 3500Gs, effectively improve the use characteristic of product, and the sintering temperature needed for this method is not more than 1000 DEG C, production cost is effectively reduced, promotional value is higher.

Description

A kind of preparation method of strontium ferrite magnetic powder
Technical field
The invention belongs to magnetic material processing technique field, and in particular to a kind of preparation method of strontium ferrite magnetic powder.
Background technology
Magnetic material, usually said magnetic material refers to ferromagnetic substance, is ancient and the quite varied function of purposes Material, and the magnetic of material was just recognized and was applied by people in the past early in 3000, such as ancient Chinese native magnet As compass.Modem magnetic materials have been widely used among our life, for example, permanent-magnet material is used as into motor, should For the core material in transformer, the magneto-optic disk used as memory, computer magnetic recording floppy disk etc..Ferrite permanent-magnet Material is one kind of permanent-magnet material, and it is with BaFe12O19Phase, SrFe12O19The permanent magnetism material based on solid solution is mutually obtained with them Material.A large amount of strategic materials such as nickel, cobalt have not only been saved in its appearance, and are hard magnetic material in high band, such as portion of television set During part, microwave and the application of other national defence devices etc. opens new approach.Ferrite Material serves not only as telecommunication The magnet of phonographic recorder, microphone, sound pick-up, telephone set and various instrument in device, and in pollution treatment, medical biotechnology Also it is widely applied with the aspect such as typographical display, strontium ferrite is the one kind in ferrite.Sol-gel process is existing preparation One of conventional method of strontium ferrite magnetic powder, current the method there is a problem that product magnetic property it is relatively low, using poor quality.
The content of the invention
The present invention is intended to provide a kind of preparation method of strontium ferrite magnetic powder.
The present invention is achieved through the following technical solutions：
A kind of preparation method of strontium ferrite magnetic powder, comprises the following steps：
（1）Raw material preparation：
A. after mixing strontium carbonate and ferric crystals, then nitric acid and deionized water dissolving are added, is subsequently adding diethylenetriamine The sodium of five methylenephosphonic acid salt five, sodium gluconate and polyvinyl alcohol, obtain mixed liquor A standby after being stirred continuously uniformly；
B. to specialist additive is added in the mixed liquor A obtained by operation a, it is 6.0 ~ 6.5 then to adjust solution ph, obtains mixed liquor B is standby；The specialist additive is made up of the material of following weight portion：45 ~ 48 part of three oxidation second secretary, 11 ~ 14 parts of calcium chloride, 5 ~ 8 parts of vanadic anhydrides, 2 ~ 4 parts of magnesia, 3 ~ 6 parts of sodium metasilicate, 4 ~ 7 parts of barium carbonates；
C. the mixed liquid B obtained by b will be operated to be placed in reactor, heating keeping temperature is 60 ~ 65 DEG C, continuous heating treatment 30 ~ Mixture C is obtained after 40min standby；
（2）Calcination process：
By step（1）The mixture C of gained is placed in roasting device, is first heated to 500 ~ 550 DEG C, after persistently processing 22 ~ 24 min, 720 ~ 750 DEG C are warming up to again, after persistently processing 20 ~ 22 min, 930 ~ 960 DEG C is continuously heating to, and persistently process 40 ~ 42min, so After rise again to 840 ~ 860 DEG C, persistently process 10 ~ 15 min after, 950 ~ 980 DEG C are finally warming up to again, persistently process 50 ~ 55min .
Further, step（1）Strontium carbonate and ferric crystals described in operation a are by strontium and iron mol ratio when mixing 1：13 are mixed.
Further, step（1）Operation a described in the sodium of diethylene triamine pentamethylene phosphonic salt five, sodium gluconate and The addition of polyvinyl alcohol is the 40 ~ 50% of strontium carbonate and ferric crystals gross mass, wherein diethylene triamine pentamethylene phosphonic salt The mass ratio of five sodium, sodium gluconate and polyvinyl alcohol is 5：2：3.
Further, step（1）The preparation method of the specialist additive described in operation b, comprises the following steps：
（1）First aoxidize second secretary, calcium chloride, vanadic anhydride, magnesia, sodium metasilicate and barium carbonate by three to mix jointly, stirring is equal Mixture D is obtained after even standby；
（2）The 83 ~ 86% of mixture D gross mass are first taken, is placed under nitrogen environment, continuous ball mill grinding to granular size is Mixture E is obtained after 15 ~ 25 μm standby, then the mixture D of residual mass is placed under nitrogen environment, continuous ball mill grinding to particle Size is standby to obtain mixture F after 250 ~ 350nm；
（3）By step（2）The mixture E of gained mixes with mixture F, after being stirred with 2400 ~ 2500 revs/min of rotating speed .
The present invention has the advantages that：
The present invention is main complexing agent with the sodium of diethylene triamine pentamethylene phosphonic salt five, coordinates sodium gluconate and polyvinyl alcohol to help network The addition of mixture, effectively improves the anisotropic increase of strontium ferrite, the growth of the crystal grain of promotion, and to burner hearth harm compared with Small, the additive that uniqueness is prepared can effectively lift compactness when strontium ferrite magnetic powder is sintered, and improve overall magnetic conductivity, and it is pressed After granular size carries out grade separation ratio, the porosity in crystal boundary and crystal grain can be effectively reduced, promote the carrying out of solid phase reaction, reduced Temperature value needed for sintering, further improves overall processing characteristics and final product quality, and what is carried out in roasting process returns Temperature operation can effectively lift the uniformity of strontium ferrite granular grows, improve its sphericity, reduce lasting roasting and life occur The unordered probability of length, and then improve the characteristic of product.Finally under the common mating reaction of each step, the obtained strontium of the present invention Ferromagnetic oxide powder has good magnetic property, and its HCJ and saturation magnetization are effectively lifted, HCJ Up to more than 4000Oe, residual magnetization reaches more than 3500Gs, effectively improves the use characteristic of product, and the sintering needed for this method Temperature is not more than 1000 DEG C, effectively reduces production cost, and promotional value is higher.
Specific embodiment
Embodiment 1
A kind of preparation method of strontium ferrite magnetic powder, comprises the following steps：
（1）Raw material preparation：
A. after mixing strontium carbonate and ferric crystals, then nitric acid and deionized water dissolving are added, is subsequently adding diethylenetriamine The sodium of five methylenephosphonic acid salt five, sodium gluconate and polyvinyl alcohol, obtain mixed liquor A standby after being stirred continuously uniformly；
B. to specialist additive is added in the mixed liquor A obtained by operation a, it is 6.0 ~ 6.5 then to adjust solution ph, obtains mixed liquor B is standby；The specialist additive is made up of the material of following weight portion：45 part of three oxidation second secretary, 11 parts of calcium chloride, 5 part of five oxygen Change two vanadium, 2 parts of magnesia, 3 parts of sodium metasilicate, 4 parts of barium carbonates；
C. the mixed liquid B obtained by b will be operated to be placed in reactor, heating keeping temperature is 60 DEG C, after continuous heating treatment 30min Obtain mixture C standby；
（2）Calcination process：
By step（1）The mixture C of gained is placed in roasting device, is first heated to 500 DEG C, after persistently processing 22 min, then is heated up To 720 DEG C, after persistently processing 20min, 930 DEG C are continuously heating to, persistently process 40min, then risen again to 840 DEG C, lasting place After reason 10min, 950 DEG C are finally warming up to again, persistently process 50min.
Further, step（1）Strontium carbonate and ferric crystals described in operation a are by strontium and iron mol ratio when mixing 1：13 are mixed.
Further, step（1）Operation a described in the sodium of diethylene triamine pentamethylene phosphonic salt five, sodium gluconate and The addition of polyvinyl alcohol is the 40% of strontium carbonate and ferric crystals gross mass, wherein diethylene triamine pentamethylene phosphonic salt five The mass ratio of sodium, sodium gluconate and polyvinyl alcohol is 5：2：3.
Further, step（1）The preparation method of the specialist additive described in operation b, comprises the following steps：
（1）First aoxidize second secretary, calcium chloride, vanadic anhydride, magnesia, sodium metasilicate and barium carbonate by three to mix jointly, stirring is equal Mixture D is obtained after even standby；
（2）First take the 83% of mixture D gross mass, be placed under nitrogen environment, continuous ball mill grinding to granular size be 15 ~ Mixture E is obtained after 25 μm standby, then the mixture D of residual mass is placed under nitrogen environment, continuous ball mill grinding is big to particle It is small be after 250 ~ 350nm mixture F is standby；
（3）By step（2）The mixture E of gained mixes with mixture F, after being stirred with 2400 revs/min of rotating speed.
Embodiment 2
A kind of preparation method of strontium ferrite magnetic powder, comprises the following steps：
（1）Raw material preparation：
A. after mixing strontium carbonate and ferric crystals, then nitric acid and deionized water dissolving are added, is subsequently adding diethylenetriamine The sodium of five methylenephosphonic acid salt five, sodium gluconate and polyvinyl alcohol, obtain mixed liquor A standby after being stirred continuously uniformly；
B. to specialist additive is added in the mixed liquor A obtained by operation a, it is 6.0 ~ 6.5 then to adjust solution ph, obtains mixed liquor B is standby；The specialist additive is made up of the material of following weight portion：48 part of three oxidation second secretary, 14 parts of calcium chloride, 8 part of five oxygen Change two vanadium, 4 parts of magnesia, 6 parts of sodium metasilicate, 7 parts of barium carbonates；
C. the mixed liquid B obtained by b will be operated to be placed in reactor, heating keeping temperature is 65 DEG C, after continuous heating treatment 40min Obtain mixture C standby；
（2）Calcination process：
By step（1）The mixture C of gained is placed in roasting device, is first heated to 550 DEG C, after persistently processing 24 min, then is heated up To 750 DEG C, after persistently processing 22 min, 960 DEG C are continuously heating to, persistently process 42min, then risen again to 860 DEG C, lasting place After managing 15 min, 980 DEG C are finally warming up to again, persistently process 55min.
Further, step（1）Strontium carbonate and ferric crystals described in operation a are by strontium and iron mol ratio when mixing 1：13 are mixed.
Further, step（1）Operation a described in the sodium of diethylene triamine pentamethylene phosphonic salt five, sodium gluconate and The addition of polyvinyl alcohol is the 50% of strontium carbonate and ferric crystals gross mass, wherein diethylene triamine pentamethylene phosphonic salt five The mass ratio of sodium, sodium gluconate and polyvinyl alcohol is 5：2：3.
Further, step（1）The preparation method of the specialist additive described in operation b, comprises the following steps：
（1）First aoxidize second secretary, calcium chloride, vanadic anhydride, magnesia, sodium metasilicate and barium carbonate by three to mix jointly, stirring is equal Mixture D is obtained after even standby；
（2）First take the 86% of mixture D gross mass, be placed under nitrogen environment, continuous ball mill grinding to granular size be 15 ~ Mixture E is obtained after 25 μm standby, then the mixture D of residual mass is placed under nitrogen environment, continuous ball mill grinding is big to particle It is small be after 250 ~ 350nm mixture F is standby；
（3）By step（2）The mixture E of gained mixes with mixture F, after being stirred with 2500 revs/min of rotating speed.
Comparative example 1
This comparative example 1 compared with Example 1, with etc. mass parts common commercially available additive step of replacing（1）Raw material preparation In specialist additive, method and step all same in addition.
Comparative example 2
This comparative example 2 compared with Example 2, saves step（2）Warming up treatment operation described in calcination process, in addition Method and step all same.
Control group
The process for preparing sol-gel of existing strontium ferrite magnetic powder.
In order to contrast effect of the present invention, attribute test is carried out to magnetic product obtained in above-mentioned five kinds of methods, specific contrast Data are as shown in table 1 below：
Table 1
Remanent magnetism Br（Gs） HCJ Hcj（Oe） Curie temperature（℃）
Embodiment 1 3680 788
Embodiment 2 3750 795
Comparative example 1 3500 720
Comparative example 2 3440 700
Control group 3100 631
As upper table 1 as can be seen that magnetic overall characteristic is preferable obtained in the inventive method, use value is higher.

Claims (4)

1. a kind of preparation method of strontium ferrite magnetic powder, it is characterised in that comprise the following steps：
（1）Raw material preparation：
A. after mixing strontium carbonate and ferric crystals, then nitric acid and deionized water dissolving are added, is subsequently adding diethylenetriamine The sodium of five methylenephosphonic acid salt five, sodium gluconate and polyvinyl alcohol, obtain mixed liquor A standby after being stirred continuously uniformly；
B. to specialist additive is added in the mixed liquor A obtained by operation a, it is 6.0 ~ 6.5 then to adjust solution ph, obtains mixed liquor B is standby；The specialist additive is made up of the material of following weight portion：45 ~ 48 part of three oxidation second secretary, 11 ~ 14 parts of calcium chloride, 5 ~ 8 parts of vanadic anhydrides, 2 ~ 4 parts of magnesia, 3 ~ 6 parts of sodium metasilicate, 4 ~ 7 parts of barium carbonates；
C. the mixed liquid B obtained by b will be operated to be placed in reactor, heating keeping temperature is 60 ~ 65 DEG C, continuous heating treatment 30 ~ Mixture C is obtained after 40min standby；
（2）Calcination process：
By step（1）The mixture C of gained is placed in roasting device, is first heated to 500 ~ 550 DEG C, after persistently processing 22 ~ 24 min, 720 ~ 750 DEG C are warming up to again, after persistently processing 20 ~ 22 min, 930 ~ 960 DEG C is continuously heating to, and persistently process 40 ~ 42min, so After rise again to 840 ~ 860 DEG C, persistently process 10 ~ 15 min after, 950 ~ 980 DEG C are finally warming up to again, persistently process 50 ~ 55min .
2. a kind of preparation method of strontium ferrite magnetic powder according to claim 1, it is characterised in that step（1）In operation a Described strontium carbonate and ferric crystals are by strontium and iron mol ratio 1 when mixing：13 are mixed.
3. a kind of preparation method of strontium ferrite magnetic powder according to claim 1, it is characterised in that step（1）In operation a The addition of the described sodium of diethylene triamine pentamethylene phosphonic salt five, sodium gluconate and polyvinyl alcohol is strontium carbonate and ferric nitrate The 40 ~ 50% of crystal gross mass, the wherein quality of the sodium of diethylene triamine pentamethylene phosphonic salt five, sodium gluconate and polyvinyl alcohol Than being 5：2：3.
4. a kind of preparation method of strontium ferrite magnetic powder according to claim 1, it is characterised in that step（1）In operation b The preparation method of described specialist additive, comprises the following steps：
（1）First aoxidize second secretary, calcium chloride, vanadic anhydride, magnesia, sodium metasilicate and barium carbonate by three to mix jointly, stirring is equal Mixture D is obtained after even standby；
（2）The 83 ~ 86% of mixture D gross mass are first taken, is placed under nitrogen environment, continuous ball mill grinding to granular size is Mixture E is obtained after 15 ~ 25 μm standby, then the mixture D of residual mass is placed under nitrogen environment, continuous ball mill grinding to particle Size is standby to obtain mixture F after 250 ~ 350nm；
（3）By step（2）The mixture E of gained mixes with mixture F, after being stirred with 2400 ~ 2500 revs/min of rotating speed .
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Application publication date: 20170613