CN107311635A - A kind of synthetic method of lanthanum zinc doping iron strontium oxide magnetic powder - Google Patents

A kind of synthetic method of lanthanum zinc doping iron strontium oxide magnetic powder Download PDF

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CN107311635A
CN107311635A CN201710511306.7A CN201710511306A CN107311635A CN 107311635 A CN107311635 A CN 107311635A CN 201710511306 A CN201710511306 A CN 201710511306A CN 107311635 A CN107311635 A CN 107311635A
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lanthanum
magnetic powder
ion
oxide magnetic
strontium
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张杭州
尤俊华
王鹏硕
李珺
冯烨
张旭
董玉坤
王齐晖
张城硕
张东勇
安欣
王亮
徐号
勾丹青
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First Hospital of China Medical University
Shenyang University of Technology
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First Hospital of China Medical University
Shenyang University of Technology
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    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/10—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
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    • C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof

Abstract

A kind of synthetic method of lanthanum zinc doping iron strontium oxide magnetic powder, is carried out according to the following steps：(1) Sr, Fe, Zn and La solubility salt compound are dissolved in into water to be well mixed；(2) mixed solution is poured into precipitant solution stirring mixing, stirred under the conditions of 10~80 DEG C to Precipitation；(3) the solid phase precipitation drying after filtering obtains presoma；(4) less than 200 are ground in 700~1200 DEG C of roastings, lanthanum zinc doping iron strontium oxide magnetic powder is obtained.Prepare strontium ferrite using the synthetic method of the present invention directly can be settled out powder from solution at ambient pressure, specific saturation magnetization and more adjustable with lanthanum zinc doping amount than remanent magnetization, be conducive to expanding application of the strontium ferrite in terms of magnetic recording, the effective residual for eliminating sodium ion micro in product and anion, and doped chemical is more uniformly distributed, realize to the controllable of magnetic regulation.

Description

A kind of synthetic method of lanthanum zinc doping iron strontium oxide magnetic powder
Technical field
The invention belongs to field of material technology, more particularly to a kind of synthesis side of lanthanum zinc doping iron strontium oxide magnetic powder Method.
Background technology
Permanent-magnet ferrite has the advantages that raw material are extensive, chemical stability is good, cheap and coercivity is high, therefore its So far it is still most widely used, yield highest permanent-magnet material.But with the development of science and technology, to permanent-magnet ferrite it is also proposed that Higher requirement；In order to obtain high performance ferrite ultra-micro powder, most of researchs are mixed from synthetic method and element Miscellaneous two aspect takes in.
Current preparation method mainly has china-clay method, chemical co-precipitation method, hydro-thermal method, sol-gel process etc.；
(1) hydro-thermal method prepares magnetic powder by HTHP, has reaction speed fast, can prepare normal temperature and be difficult what is prepared The effect of special material；But be not suitable for industrial production, some raw materials be also easy to produce decomposition the problems such as higher to equipment requirement；
(2) china-clay method is the most frequently used method for preparing magnetic powder of industry.This method biggest advantage is that pre-treatment is simple, Production scale is larger；But metal oxide active is relatively low, therefore usually need higher reaction temperature, the defect of particle and should Power is larger；Particle diameter distribution is very wide；Granule-morphology is relatively rough, easily dephasign occurs, and uneven in product；
(3) sol-gel process is also a kind of common method, and product quality is more uniform, and morphology microstructure is relatively easy to control；But This method cost is higher, is not that every kind of system can make with being required in addition to reaction system, production process is used some poison Evil medicine, has very big harm to human body and to the seriously polluted of environment；In addition, easily there is impurity in product, accessory substance is not It is easily separated.
(4) self-propagating high-temperature synthesis, is a kind of solid combustion process, the main heat discharged using lighting after reactant Generation self-propagating combustion formation powder product；Because this method has product purity high, speed is formed soon, it is many without high temperature etc. Advantage, therefore enjoy the concern of researcher；Compared with sol-gel process, this method still has weak point:Synthesis technique compared with It is higher for complicated, preparation condition harshness, equipment requirement, it is unfavorable for extensive preparation；Simultaneously as temperature high in combustion process Gradient and fast cooling velocity, it is easy to obtain metastable thing phase, make obtained material impure, and this is to the large-scale production of industrialization Bring certain difficulty.
(5) cations such as metal are co-precipitated by chemical coprecipitation within a short period of time using precipitating reagent, realize raw material In the mixing of Nano grade, this is conducive to the uniformity for improving product, while equipment is simple, is adapted to large-scale production, Er Qieneng Consumption is relatively low.
It is equal for impurity separation, product although above-mentioned several method can prepare rare earth mixing with nano strontium ferrite It is not so good as coprecipitation in terms of even property.The height crystallization prepared at present using this method, particle is uniform, and coercivity is in certain limit Adjustable product is still less.
The content of the invention
It is an object of the invention to provide a kind of synthetic method of lanthanum zinc doping iron strontium oxide magnetic powder, by normal in low temperature Sr, Fe ion in M-type strontium ferrite are substituted using La, Zn under the conditions of pressure, Sr is directly prepared through calcining1-xFe12-xLaxZnxO19Receive Ground rice body, makes that preparation technology is simple, cost is low, process is easy to operate and controlled.
The method of the present invention is carried out according to the following steps：
1st, Sr, Fe, Zn and La solubility salt are dissolved in deionized water, are uniformly mixed, obtain mixed solution, mixed The concentration for closing iron ion in solution is 1~10mol/L；The mol ratio of wherein strontium ion, iron ion, lanthanum ion and zinc ion is (1-x):(12-x):x:X, wherein x=0.15~0.25；
2nd, mixed solution is poured into stir in precipitant solution and mixed, the addition of precipitating reagent with can precipitate completely strontium from Son, iron ion, lanthanum ion and zinc ion are defined；Then pH value=10 ± 0.2 is adjusted, while being stirred to bubble-free generation； Finally 30~60min of stirring reaction under the conditions of 10~80 DEG C, precipitates and separates out completely；
3rd, the solid phase precipitation for obtaining whole material filterings；Solid phase precipitation is dried under the conditions of 120 ± 5 DEG C and goes water removal Point, obtain presoma；
4, presoma is ground after cross 200 mesh sieves, undersize material 700~1200 DEG C be calcined 2~3h, obtain lanthanum zinc mix Miscellaneous iron strontium oxide magnetic powder, its composition is Sr1-xFe12-xLaxZnxO19。
In above-mentioned Sr, Fe, Zn, La solubility salt, Fe solubility salt selects iron chloride, ferric nitrate, sulfuric acid Iron or ferric acetate；La solubility salt selects lanthanum nitrate, lanthanum acetate or lanthanum chloride；The solubility salt of Sr strontiums selects strontium chloride Or strontium nitrate；Zn solubility salt selects zinc chloride or zinc nitrate.
Above-mentioned precipitant solution selects triethylamine solution, and concentration is 1~2M.
50~300nm of Breadth Maximum of above-mentioned lanthanum zinc doping iron strontium oxide magnetic powder, length-width ratio (5~20):1, it is thick Spend 30~80nm.
52.26~63.11A.m of specific saturation magnetization of above-mentioned lanthanum zinc doping iron strontium oxide magnetic powder2/ Kg, it is interior Report coercivity 138.5~240.1kA/m.
The present invention principle be：Strontium ferrite is doped using lanthanum (rare earth ion), zinc (transition metal ions), adjusted The valence electron quantity and valence electron spin structure of whole strontium ferrite realize the regulation to magnetism of material；Precipitated using triethylamine Agent, can improve product purity relative to using sodium hydroxide, sodium carbonate as precipitating reagent, improve its magnetic；Presoma is ground And in 900 DEG C of roastings so that product crystallization purity is higher.
Prepare strontium ferrite using the synthetic method of the present invention directly can be settled out powder from solution at ambient pressure, than Saturation magnetization and more adjustable with lanthanum zinc doping amount than remanent magnetization, is conducive to expanding strontium ferrite in terms of magnetic recording Using；By improving precipitating reagent, the rare earths such as lanthanum zinc can easily be controlled and transition element doped to strontium by changing lanthanum zinc doping amount In ferrite, cost is reduced relative to collosol and gel, product purity is improved relative to china-clay method；Relative to other co-precipitation Method, effectively eliminates the residual of sodium ion micro in product and anion, and doped chemical is more uniformly distributed, Realize to the controllable of magnetic regulation.
Brief description of the drawings
Fig. 1 is the XRD of the product of the embodiment of the present invention 1；
The product SEM figures that Fig. 2 is x=0.2 in the embodiment of the present invention 1；
Fig. 3 is the hysteresis curve figure of the product of x=0, x=0.2, x=0.25, x=0.3 in the embodiment of the present invention 1；
Fig. 4 is for the specific saturation magnetization (Ms) of each set product of the embodiment of the present invention 1 and than remanent magnetization (Mr) With x change curve；
Fig. 5 is the HCJ of each set product of the embodiment of the present invention 1 with x change curve.
Embodiment
Sr, Fe, Zn, La for being used in the embodiment of the present invention solubility salt is AR purchased in market.
The triethylamine used in the embodiment of the present invention is AR purchased in market.
Roasting uses Muffle furnace in the embodiment of the present invention.
The particle of the lanthanum zinc doping iron strontium oxide magnetic powder obtained in the embodiment of the present invention is hexagon sheet.
PH value is adjusted in the embodiment of the present invention and uses inorganic acid alkali.
Embodiment 1
Sr, Fe, Zn and La solubility salt compound are dissolved in deionized water, while carrying out 6 groups of experiments, and one is carried out The secondary contrast test for being added without Zn and La, is uniformly mixed, and the concentration of iron ion is 1mol/ in 7 groups of mixed solutions of acquisition L；Wherein the mol ratio of strontium ion, iron ion, lanthanum ion and zinc ion is (1-x):(12-x):x:X, x are respectively 0,0.1, 0.15th, 0.2,0.25,0.3 and 0.35；
Fe solubility salt is iron chloride；La solubility salt is lanthanum nitrate；The solubility salt of Sr strontiums is chlorination Strontium；Zn solubility salt is zinc chloride；
Mixed solution is poured into mixing is stirred in precipitant solution, the addition of precipitating reagent with can precipitate completely strontium from Son, iron ion, lanthanum ion and zinc ion are defined；Then pH value=10 ± 0.2 is adjusted, while being stirred to bubble-free generation； Then the stirring reaction 60min under the conditions of 70 DEG C, precipitates and separates out completely；Precipitant solution is triethylamine solution, and concentration is 1M；
The solid phase precipitation that whole material filterings are obtained；Solid phase precipitation is dried under the conditions of 120 ± 5 DEG C and removes moisture removal, Obtain presoma；
200 mesh sieves are crossed after presoma is ground, undersize material is calcined 2h at 900 DEG C, obtains lanthanum zinc doping strontium ferrite magnetic Property powder, its composition be Sr1-xFe12-xLaxZnxO19, 50~300nm of Breadth Maximum, length-width ratio (5~20):1 thickness 30~ The specific saturation magnetization of the lanthanum zinc doping iron strontium oxide magnetic powder of 80nm, wherein x=0.15,0.2 and 0.25 be 52.26~ 63.11A.m2/ Kg, HCJ is 138.5~240.1kA/m；
The XRD of Different Zinc doping powder is as shown in figure 1, x=0.2 and 0.25 product SEM is schemed as shown in Fig. 2 x= 0th, the hysteresis curve of x=0.2, x=0.25 and x=0.3 product is as shown in figure 3, the specific saturation magnetization of each set product (Ms) and than remanent magnetization (Mr) with doping x change curve as shown in figure 4, HCJ with x change curve As shown in Figure 5.
Embodiment 2
Method be the same as Example 1, difference is：
(1) concentration of iron ion is 2mol/L in mixed solution；Fe solubility salt is ferric nitrate；La soluble-salt Class is lanthanum acetate；The solubility salt of Sr strontiums is strontium nitrate；Zn solubility salt is zinc nitrate；
(2) stirring reaction 60min triethylamine solutions concentration is 1.5M under the conditions of 10 DEG C；
(3) 3h is calcined at 700 DEG C, obtains lanthanum zinc doping iron strontium oxide magnetic powder, its composition is Sr1-xFe12- xLaxZnxO19, 100~300nm of Breadth Maximum, length-width ratio (10~20):1,30~60nm of thickness, wherein x=0.15,0.2 and The specific saturation magnetization of 0.25 lanthanum zinc doping iron strontium oxide magnetic powder is 58~61A.m2/ Kg, HCJ is 190 ~230kA/m.
Embodiment 3
Method be the same as Example 1, difference is：
(1) concentration of iron ion is 5mol/L in mixed solution；Fe solubility salt is ferric sulfate；La soluble-salt Class is lanthanum chloride；The solubility salt of Sr strontiums is strontium chloride；Zn solubility salt is zinc chloride；
(2) stirring reaction 30min triethylamine solutions concentration is 2M under the conditions of 80 DEG C；
(3) 2h is calcined at 1200 DEG C, obtains lanthanum zinc doping iron strontium oxide magnetic powder, its composition is Sr1-xFe12- xLaxZnxO19, 80~220nm of Breadth Maximum, length-width ratio (8~15):1,50~80nm of thickness, wherein x=0.15,0.2 and 0.25 Lanthanum zinc doping iron strontium oxide magnetic powder specific saturation magnetization be 55~62A.m2/ Kg, HCJ be 160~ 234kA/m。
Embodiment 4
Method be the same as Example 1, difference is：
(1) concentration of iron ion is 10mol/L in mixed solution；Fe solubility salt is ferric acetate；La solubility Salt is lanthanum nitrate；The solubility salt of Sr strontiums is strontium nitrate；Zn solubility salt is zinc nitrate；
(2) stirring reaction 45min triethylamine solutions concentration is 1.5M under the conditions of 30 DEG C；
(3) 2.5h is calcined at 1000 DEG C, obtains lanthanum zinc doping iron strontium oxide magnetic powder, its composition is Sr1-xFe12- xLaxZnxO19, 150~270nm of Breadth Maximum, length-width ratio (5~9):1,35~75nm of thickness, wherein x=0.15,0.2 and 0.25 Lanthanum zinc doping iron strontium oxide magnetic powder specific saturation magnetization be 53~60A.m2/ Kg, HCJ be 149~ 233kA/m。

Claims (5)

1. a kind of synthetic method of lanthanum zinc doping iron strontium oxide magnetic powder, it is characterised in that carry out according to the following steps：
(1) Sr, Fe, Zn and La solubility salt compound are dissolved in deionized water, are uniformly mixed, obtain mixing molten The concentration of iron ion is 1~10mol/L in liquid, mixed solution；Wherein mole of strontium ion, iron ion, lanthanum ion and zinc ion Than for (1-x):(12-x):x:X, wherein x=0.15~0.25；
(2) mixed solution is poured into stir in precipitant solution and mixed, the addition of precipitating reagent with can precipitate completely strontium ion, Iron ion, lanthanum ion and zinc ion are defined；Then pH value=10 ± 0.2 is adjusted, while being stirred to bubble-free generation；Then 30~60min of stirring reaction under the conditions of 10~80 DEG C, precipitation is separated out completely；
(3) solid phase precipitation for obtaining whole material filterings；Solid phase precipitation is dried under the conditions of 120 ± 5 DEG C and removes moisture removal, is obtained Obtain presoma；
(4) 200 mesh sieves are crossed after presoma is ground, undersize material is calcined 2~3h at 700~1200 DEG C, obtains lanthanum zinc doping strontium Ferrimagnetism powder, its composition is Sr1-xFe12-xLaxZnxO19。
2. a kind of synthetic method of lanthanum zinc doping iron strontium oxide magnetic powder according to claim 1, it is characterised in that institute In Sr, Fe, Zn, La for stating solubility salt, Fe solubility salt selects iron chloride, ferric nitrate, ferric sulfate or ferric acetate； La solubility salt selects lanthanum nitrate, lanthanum acetate or lanthanum chloride；The solubility salt of Sr strontiums selects strontium chloride or strontium nitrate；Zn Solubility salt select zinc chloride or zinc nitrate.
3. a kind of synthetic method of lanthanum zinc doping iron strontium oxide magnetic powder according to claim 1, it is characterised in that institute The precipitant solution stated selects triethylamine solution, and concentration is 1~2M.
4. a kind of synthetic method of lanthanum zinc doping iron strontium oxide magnetic powder according to claim 1, it is characterised in that institute 50~the 300nm of Breadth Maximum for the lanthanum zinc doping iron strontium oxide magnetic powder stated, length-width ratio (5~20):1,30~80nm of thickness.
5. a kind of synthetic method of lanthanum zinc doping iron strontium oxide magnetic powder according to claim 1, it is characterised in that institute 52.26~the 63.11A.m of specific saturation magnetization for the lanthanum zinc doping iron strontium oxide magnetic powder stated2/ Kg, HCJ 138.5~240.1kA/m.
CN201710511306.7A 2017-06-29 2017-06-29 A kind of synthetic method of lanthanum zinc doping iron strontium oxide magnetic powder Pending CN107311635A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108554414A (en) * 2018-05-09 2018-09-21 苏州德捷膜材料科技有限公司 A kind of preparation method of nano-strontium ferrite/Zn ferrite composite material
CN114180638A (en) * 2021-10-25 2022-03-15 成都锦钛精工科技有限公司 Permanent magnetic ferrite magnetic powder prepared from steel mill pickling waste liquid and preparation method thereof

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CN101372417A (en) * 2008-09-25 2009-02-25 中国科学院青海盐湖研究所 High specific saturation magnetization and high coercitive force strontium ferrite magnetic powder and preparation thereof
CN103601483A (en) * 2013-12-03 2014-02-26 沈阳工业大学 Novel synthetic method for lanthanum-manganese doped strontium ferrite magnetic powder

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101372417A (en) * 2008-09-25 2009-02-25 中国科学院青海盐湖研究所 High specific saturation magnetization and high coercitive force strontium ferrite magnetic powder and preparation thereof
CN103601483A (en) * 2013-12-03 2014-02-26 沈阳工业大学 Novel synthetic method for lanthanum-manganese doped strontium ferrite magnetic powder

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108554414A (en) * 2018-05-09 2018-09-21 苏州德捷膜材料科技有限公司 A kind of preparation method of nano-strontium ferrite/Zn ferrite composite material
CN114180638A (en) * 2021-10-25 2022-03-15 成都锦钛精工科技有限公司 Permanent magnetic ferrite magnetic powder prepared from steel mill pickling waste liquid and preparation method thereof
CN114180638B (en) * 2021-10-25 2024-01-05 成都锦钛精工科技有限公司 Permanent magnetic ferrite magnetic powder prepared from pickling waste liquid of steel mill and preparation method thereof

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