CN107721405A - A kind of low temperature calcination prepares M-type strontium ferrite SrFe12O19The method of Preburning material - Google Patents

A kind of low temperature calcination prepares M-type strontium ferrite SrFe12O19The method of Preburning material Download PDF

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Publication number
CN107721405A
CN107721405A CN201711138182.9A CN201711138182A CN107721405A CN 107721405 A CN107721405 A CN 107721405A CN 201711138182 A CN201711138182 A CN 201711138182A CN 107721405 A CN107721405 A CN 107721405A
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strontium ferrite
preburning material
preburning
calcining
type strontium
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CN107721405B (en
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甘金宝
李昕
夏爱林
甘海平
詹涛
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Anhui Xin Magnetic Source Magnetic Industry Co Ltd
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Anhui Xin Magnetic Source Magnetic Industry Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
    • C04B35/2683—Other ferrites containing alkaline earth metals or lead
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/62675—Thermal treatment of powders or mixtures thereof other than sintering characterised by the treatment temperature
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3213—Strontium oxides or oxide-forming salts thereof

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Magnetic Ceramics (AREA)
  • Compounds Of Iron (AREA)

Abstract

The invention discloses a kind of low temperature calcination to prepare M-type strontium ferrite SrFe12O19The method of Preburning material.This method is to analyze pure SrCO3、Fe2O3For raw material, according to atomic ratio Sr/Fe=1:9~1:10 proportionings, are uniformly mixed in ball mill, and then by the raw material of mixing with 5 DEG C/min of calcining heats for being increased to 1180~1250 DEG C, then insulation calcining 2~4 hours, gained powder is M-type strontium ferrite SrFe12O19Preburning material.The Preburning material is characterised by that its (008) peak does not produce misgrowth, to follow-up lifting SrFe12O19The coercivity of product is highly beneficial.Also, because the calcining heat that calcining heat is existing far below Preburning material producer, is advantageous to energy-conserving and environment-protective.

Description

A kind of low temperature calcination prepares M-type strontium ferrite SrFe12O19The method of Preburning material
Technical field
The invention belongs to the preparing technical field of hard ferrite, and in particular to a kind of low temperature calcination prepares M-type strontium iron oxygen Body (SrFe12O19, SrM) Preburning material method.
Background technology
Strontium ferrite (SrFe12O19, SrM) and permanent-magnet material is used as, there is stable six side's magneto-plumbite types (M types) structure, higher Coercivity, magnetic energy product and resistivity, can be used under high frequency occasion, simultaneously as its abundant, cheap raw material and good Chemical stability, be used widely always.At present, due to many reasons, the high-end ferritic production technologies of SrM according to So rest in American-European and Japanese on hand.Big country of the China as SrM ferrite productions, it is badly in need of finding new SrM ferrites life Methods and techniques are produced, to be desirable to catch up with and surpass international high-end product from performance, turn into the power of ferrite production.
One of an important factor for raw material are limitation SrM ferrite performances, the particularly structure and composition of Preburning material, it is right The ferritic performances of SrM have the influence of key.Currently, in order to completely into phase, the contraction of product when reducing follow-up sintering Rate, the calcined temperature of most of Preburning material producer 1300 DEG C even more than.Higher calcined temperature, consume substantial amounts of energy Amount, is unfavorable for energy-conserving and environment-protective.
By carefully studying, it has been found that 1300 DEG C and temperatures above calcining powder sample, it has bright in (008) face Aobvious preferential growth (see accompanying drawing 1), this can cause follow-up sintering ferrite magnetic performance to be particularly coercitive decline.When we will When calcined temperature is reduced to 1200 DEG C, pleasantly surprised discovery, reaction not only greatly reduces calcining heat, and also improves SrM The structure of Preburning material, preferential growth face are (107) and (114) (see accompanying drawing 2), are more beneficial for improving the magnetic of follow-up sintering product Energy.
The content of the invention
Present invention solves the technical problem that it is to provide a kind of improved preparation M-type strontium ferrite SrFe12O19The side of Preburning material Method, this method technique is simple, suitable for industrial production.
Specifically, the invention provides a kind of low temperature calcination to prepare M-type strontium ferrite SrFe12O19The method of Preburning material, its It is characterised by, it is as follows that the method comprising the steps of：
1) to analyze pure SrCO3、Fe2O3For raw material, according to atomic ratio Sr/Fe=1:9~1:10 proportionings, in ball mill In uniformly mix；
2) by the raw material of mixing with 5 DEG C/min of calcining heats for being increased to 1180~1250 DEG C, then insulation calcining 2 ~4 hours, gained powder was M-type strontium ferrite SrFe12O19Preburning material.
Preferably, step 1) SrCO3、Fe2O3According to atomic ratio Sr/Fe=1:9.5 proportionings feed intake.
Preferably, the calcining heat of step 2) is 1200 DEG C.
Preferably, the insulation calcination time of step 2) is 2 hours.
Further, as a preferred embodiment, the invention provides a kind of low temperature calcination to prepare M-type strontium iron oxygen Body SrFe12O19The method of Preburning material, it is characterised in that it is as follows that the method comprising the steps of：
1) to analyze pure SrCO3、Fe2O3For raw material, according to atomic ratio Sr/Fe=1:9.5 proportionings, in ball mill Even mixing；
2) by the raw material of mixing with 5 DEG C/min of calcining heats for being increased to 1200 DEG C, then insulation calcining 2 hours, institute It is M-type strontium ferrite SrFe to obtain powder12O19Preburning material.
The invention provides a kind of M-type strontium ferrite SrFe made from the preparation method of any one as described above12O19Pre-burning Material.
Preferably, M-type strontium ferrite SrFe12O19Preburning material (008) peak does not produce misgrowth.
Further, M-type strontium ferrite SrFe12O19Preburning material has XRD spectrum as shown in Figure 2.
The crucial of this technology invention is being 1 in the Sr/Fe atomic ratios in raw material are increased:9~1:10, preferably 1:9.5 Calcined at a temperature of 1300 DEG C commonly used far below Preburning material producer, calcining gained powder can be caused preferentially along (107) (114) crystal face grows, and effectively improves the ferritic performance of follow-up sintering.Its physical principle is, if in 1300 DEG C of temperature Degree is lower to be calcined, and preferential growth is (008) crystal face, will generate more flat crystal grain, and tiny flat crystal grain will not Beneficial to magnetic property of permanent-magnet material performance itself.
In addition, compared with prior art, the present invention has following technical advantage：
1) calcined temperature is minimum up to 1180~1250 DEG C, preferably 1200 DEG C, is significantly less than existing conventional preburning powdered material About 1300 DEG C used in producer, energy consumption can be greatly lowered, be advantageous to energy-conserving and environment-protective, more suitable for industrialized production.
2) (008) preferential growth crystal face of 1300 DEG C of preburning powders, ferrite prefiring powder obtained by low temperature calcination are different from Using (107) and (114) face as preferential growth face, be advantageous to follow-up ferrite magnetic performance and be particularly coercitive lifting.
Brief description of the drawings
The present invention is further described below in conjunction with the accompanying drawings.
The XRD spectrum for the Strontium ferrite powder that Fig. 1 embodiments 1 (1300 DEG C) obtain
The XRD spectrum for the Strontium ferrite powder that Fig. 2 embodiments 2 (1200 DEG C) obtain
The XRD spectrum for the Strontium ferrite powder that Fig. 3 embodiments 3 (1250 DEG C) obtain
The hysteresis curve figure for the Strontium ferrite powder that Fig. 4 embodiments 1 (1300 DEG C) obtain
The hysteresis curve figure for the Strontium ferrite powder that Fig. 5 embodiments 2 (1200 DEG C) obtain
The hysteresis curve figure for the Strontium ferrite powder that Fig. 6 embodiments 3 (1250 DEG C) obtain
Embodiment
With reference to embodiment, the present invention is further described.
Embodiment 1
First, according to atomic ratio Sr/Fe=1:9.5 proportionings, pure SrCO is analyzed with 3mmol3Analyzed with 14.25mmol pure Fe2O3For raw material, uniformly mixed in ball mill, the raw material of mixing are increased to 1300 DEG C with 5 DEG C/min, are then incubated Calcining 2 hours, gained is SrFe of the present invention12O19Preburning material.
The XRD spectrum of gained Preburning material is as shown in figure 1, hysteresis curve figure is as shown in Figure 4.
Embodiment 2
Compared with Example 1, difference is that calcining heat is 1200 DEG C, and other conditions are identical.The XRD of gained Preburning material Spectrum is as shown in Fig. 2 hysteresis curve figure is as shown in Figure 5.
Embodiment 3
Compared with Example 1, difference is that calcining heat is 1250 DEG C, and other conditions are identical.The XRD of gained Preburning material Spectrum is as shown in figure 3, hysteresis curve figure is as shown in Figure 6.
Comparison diagram 1- Fig. 3, (008) peak intensity of 1300 DEG C of calcining Preburning materials are significantly stronger than other peaks, it appears very sharp； And (008) peak intensity ratio (107) and (114) peak of 1200 DEG C of calcining Preburning materials is much lower, this is consistent with standard spectral line 's；The relative intensity at (008) peak of 1250 DEG C of calcining Preburning materials is still very high, but is compared to Fig. 1, has reduced very It is more.
Comparison diagram 4-6, although the saturation magnetization (68.57emu/g) of 1300 DEG C of Preburning materials is slightly above 1200 DEG C (63.01emu/g), but its coercivity but declines seriously, drops to 1279.8Oe from 2635.5Oe, more than more than 50%, shows So, 1300 DEG C of calcining Preburning materials are unfavorable for the coercitive raising of raw material, and this is obviously close with the misgrowth relation at (008) peak Cut；The saturation magnetization of 1250 DEG C of Preburning materials is 65.3emu/g, is more or less the same with the powder of 1300 DEG C of pre-burnings, and coercivity For 1527.2Oe, the preburning powdered material than 1300 DEG C is greatly increased.
Above content is only that affiliated those skilled in the art are to being retouched to examples of the invention and explanation Various modifications may be made or supplement for the specific embodiment stated, and design without departing from the present invention or surmounts the claims and is defined Scope, protection scope of the present invention all should be belonged to.

Claims (7)

1. a kind of low temperature calcination prepares M-type strontium ferrite SrFe12O19The method of Preburning material, it is characterised in that this method includes step It is rapid as follows：
1) to analyze pure SrCO3、Fe2O3For raw material, according to atomic ratio Sr/Fe=1:9~1:10 proportionings, in ball mill Even mixing；
2) by the raw material of mixing with 5 DEG C/min of calcining heats for being increased to 1180~1250 DEG C, then insulation calcining 2~4 is small When, gained powder is M-type strontium ferrite SrFe12O19Preburning material.
2. preparation method according to claim 1, wherein, step 1) SrCO3、Fe2O3According to atomic ratio Sr/Fe=1:9.5 Proportioning.
3. preparation method according to claim 1, wherein, the calcining heat of step 2) is 1200 DEG C.
4. preparation method according to claim 1, wherein, the insulation calcination time of step 2) is 2 hours.
5. the M-type strontium ferrite SrFe as made from any one of claim 1-4 preparation method12O19Preburning material.
6. M-type strontium ferrite SrFe as claimed in claim 512O19Preburning material, it is characterised in that its (008) peak does not produce Misgrowth.
7. M-type strontium ferrite SrFe as claimed in claim 512O19Preburning material, it is characterised in that it has as shown in Figure 2 XRD spectrum.
CN201711138182.9A 2017-11-16 2017-11-16 Preparation of M-type strontium ferrite SrFe through low-temperature calcination12O19Method for pre-firing materials Active CN107721405B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109776088A (en) * 2019-04-01 2019-05-21 中钢集团南京新材料研究院有限公司 A kind of preparation method of Strontium ferrite powder
CN110240476A (en) * 2019-06-26 2019-09-17 北京信息科技大学 A kind of novel ferrite ceramic material and preparation method thereof
CN116371408A (en) * 2023-04-24 2023-07-04 华中科技大学 Sr-Fe-based oxygen carrier, preparation method thereof and application thereof in reforming hydrogen production/CO

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103304230A (en) * 2013-06-13 2013-09-18 东阳市金砖磁业有限公司 Permanent magnetic ferrite low-temperature pre-sintering powder and preparation method thereof
CN104507889A (en) * 2012-10-11 2015-04-08 Tdk株式会社 Sr ferrite powder, method for manufacturing Sr ferrite sintered magnet, motor, and generator

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104507889A (en) * 2012-10-11 2015-04-08 Tdk株式会社 Sr ferrite powder, method for manufacturing Sr ferrite sintered magnet, motor, and generator
CN103304230A (en) * 2013-06-13 2013-09-18 东阳市金砖磁业有限公司 Permanent magnetic ferrite low-temperature pre-sintering powder and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109776088A (en) * 2019-04-01 2019-05-21 中钢集团南京新材料研究院有限公司 A kind of preparation method of Strontium ferrite powder
CN109776088B (en) * 2019-04-01 2021-11-12 中钢集团南京新材料研究院有限公司 Preparation method of strontium ferrite pre-sintering material
CN110240476A (en) * 2019-06-26 2019-09-17 北京信息科技大学 A kind of novel ferrite ceramic material and preparation method thereof
CN116371408A (en) * 2023-04-24 2023-07-04 华中科技大学 Sr-Fe-based oxygen carrier, preparation method thereof and application thereof in reforming hydrogen production/CO

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Denomination of invention: A method for preparing M-type strontium ferrite SrFe12O19

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