CN1447356A - Material powder of manganese-zinc power soft magnet ferrite and its preparation method - Google Patents

Material powder of manganese-zinc power soft magnet ferrite and its preparation method Download PDF

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CN1447356A
CN1447356A CN 03115906 CN03115906A CN1447356A CN 1447356 A CN1447356 A CN 1447356A CN 03115906 CN03115906 CN 03115906 CN 03115906 A CN03115906 A CN 03115906A CN 1447356 A CN1447356 A CN 1447356A
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powder
material powder
manganese
power soft
ferrite material
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CN1252743C (en
Inventor
陈卫锋
孔毅
陆麒发
仇学同
刘国平
徐辉宇
顾燮峰
黄子谦
冯炜
唐俊睿
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Shanghai Bao Steel Magnetics Co.,Ltd.
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SHANGHAI BAO STEEL TIANTONG MAGNETIC MATERIALS CO Ltd
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Abstract

Manganese-zinc soft magnetic ferrite material powder is made through five working procedures: admixture, preburning, coarse cracking, sand mill and spraying-granulation by using Fe2O3, Mn3O4, and ZnO as main materials. The produced material powder has advantages of lower power consumption, high saturation induction density Bs, low cost and superior performances.

Description

Manganese-zinc power soft ferrite material powder and preparation method thereof
Technical field
The invention belongs to the soft magnetic material technical field, be specifically related to a kind of manganese-zinc power soft ferrite material powder and preparation method thereof.
Background technology
In the world, Japanese, European manufacturer develops first generation LPL (power soft ferrite) the beginning of the seventies, and the typical trade mark has the H45 of H3S, FDK and the 3C8 of Philip, generally only is used for the domestic switch power supply about 20kHz; At the beginning of the eighties at the end of the seventies, state is extrapolated through improved second generation LPL; The middle and later periods eighties, competitively develop the third generation material that the high frequency power consumption significantly reduces, practical frequency generally can reach 100-500kHz abroad again, 3F3 as the N47 of the H63B of H7C4 (PC40), the FDK of TDK and H45C, Siemens and N67, Philip, except that making traditional EE, EI, EC magnetic core, also have ETD, PQ, RM magnetic core, these novel magnetic cores only are applicable to that frequency is the high frequency switch power of hundreds of kHz.
There are 898 factories, 4390 factories, Changshu Radio Appliances Factory, Taixing magnetic material factory, Co., Ltd of Tian Tong Electronics etc. in the domestic soft magnetic ferrite manufacturer that begins to take shape.Wherein 898 factories, 9, R2KB1, R2KDB, the R2KB3 of 899 factories exploitations reach or near third generation LPL Ferrite Material standard, the LPL Ferrite Material that these factories produce, and its power loss is big, and it is low to adapt to frequency.
Summary of the invention
The object of the present invention is to provide that a kind of production cost is low, power loss is low, adapt to the high manganese-iron power soft ferrite material powder of frequency.
A kind of manganese-iron power soft ferrite material powder that the present invention proposes is by Fe 2O 3, Mn 3O 4, ZnO forms, each composition and consumption thereof are as follows:
Fe 2O 3???58-79wt％
Mn 3O 4???15-30wt％
ZnO????????5-15wt％
Auxiliary material 0-7wt%,
Satisfy total amount 100%.
In the above-mentioned prescription, auxiliary material comprises dispersant, defoamer, additive etc., and wherein, dispersant can adopt the di(2-ethylhexyl)phosphate octanol.It is the compound of polyether-type fatty acid ester that defoamer can adopt Main Ingredients and Appearance.Additive is SiO 2, CaCO 3, V 2O 5, Nb 2O 5Deng a kind of or appoint several mixtures.According to crystallography induced crystallization method principle, induce spinelle to shift to an earlier date rapid crystallization mutually, can reduce the required activation energy of solid phase reaction, thereby solve big, the poor activity of iron oxide red raw material average grain diameter, with the little problem of slow response of other raw material contacts area.The power consumption of the soft magnetic ferrite powder of in addition, can bigger reduction producing.
A kind of manganese-iron power soft ferrite material powder, preparation method thereof that the present invention proposes is as follows:
1, mixes: accurately take by weighing above-mentioned various raw material by the raw material proportioning, adopt ball mill or vibrator to mix, incorporation time is 10～40 minutes, and mixed powder particle size is controlled at about 1.0-1.5 μ m, purpose is that raw material is mixed, and solid phase reaction is complete when being beneficial to pre-burning.
2, pre-burning: above-mentioned solid mixture is dropped into rotary kiln carry out pre-burning, calcined temperature is 700～1000 ℃, the pre-burning time is 30～60 minutes, the control mixture flow rate is the 2-5 kg/minute, the rotary kiln rotating speed is a 10-20 rev/min of kind, make the red solid mixture that solid phase reaction tentatively take place, and make mixture change black into by redness.
3, coarse crushing: the black mixture that pre-burning is obtained carries out coarse crushing, adopts vibrator, and the pulverizing time is 20～50 minutes, makes granular size, is evenly distributed, and radius is littler.
4, sand milling: will carry out sand milling through the mixture of coarse crushing, and obtain the black paste of fine powder after broken, the whole sand milling time is 30-100 minute.Compound relies on the friction between steel ball and powder particle, powder particle and the powder particle in sand mill, further reduce the average grain diameter of powder particle, the distribution of dwindling grain diameter.The sand milling particle diameter is 0.7-1.5 μ m.
5, spraying: through the slip of sand milling, under 80～100 ℃ temperature by the mist projection granulating tower be sprayed into dry tack free, middle moistening, have good fluidity and a dispersed ellipse grains.
Among the present invention, sand milling can adopt a kind of waterproof pulverization, utilizes pure water as solvent.In sand mill, drop into black powder, additive, pure water and the dispersant of coarse crushing by a certain percentage, the ratio of adding is: black powder 48-68wt%, pure water 30-50wt%, additive 0-1wt%, dispersant 0-1wt%, when sand grinding process finishes soon, drop into glue (polyvinyl alcohol) and defoamer again, the total addition of polyvinyl alcohol and defoamer is 0-1wt%.Dispersant black powder in company with pre-burning when sand milling begins adds, and effect is to prevent the particle conglomeration, improves sand milling efficient.Glue act as the compression moulding of being convenient to the soft magnetic ferrite powder, the foam that produces when adding glue is eliminated in acting as of defoamer.
Manganese-zinc power soft ferrite material powder that the present invention proposes has good physicochemical performance.Press GB through appropriate authority and detect, material property is as follows:
The moisture content of particle is 0.1～0.6%,
Pine dress is than being 1.22～1.45g/cm 3,
Angle of repose is 26 °～30 °.
Cost of manufacture of the present invention is low, and is simple and easy to do, and the iron-manganese power soft ferrite material powder that utilizes the present invention to make is used to make magnetic core, can make magnetic core have littler power consumption, littler caloric value, higher working temperature, saturation induction density height, superior performance.
Embodiment
Embodiment 1
Take by weighing 70wt%Fe 2O 3, 23wt%Mn 3O 4, 7wt%ZnO, wherein iron oxide red adopts homemade Baosteel iron oxide red (performance is referring to table 1).Drop in the vibrator, mixed 25 minutes, go into rotary kiln, pre-burning under 900 ℃ temperature, pre-burning 30 minutes.Go into the vibrator coarse crushing subsequently 30 minutes, dropped in the sand mill fine powder more broken 60 minutes.Add pure water 35wt%, di(2-ethylhexyl)phosphate octanol 0.2wt%, polyvinyl alcohol 0.6wt% and defoamer 0.01wt% in the sand grinding process.And adding additive SiO 20.003wt%, CaCO 30.018wt%, V 2O 50.090wt%, Nb 2O 50.050wt%.Last mist projection granulating obtains the Mn-Zn ferrite powder.
Get this powder 18g with 6000kgf/cm 2Pressure forming, obtain the ring-type formed body of diameter 35.5cm, high 14cm.Insulation sintered the Mn-Zn ferrite cemented body in 4 hours under 1350 ℃ of temperature.
, list in the table 2 as the power consumption under the temperature of table 2 with SY8232 tester test sintered body.
Embodiment 2
Take by weighing 67wt%Fe 2O 3, 24wt%Mn 3O 4, 9%ZnO drops in the ball mill and mixed 20 minutes, pre-burning under 950 ℃ temperature, and the pre-burning time is 35 minutes.Go into the vibrator coarse crushing subsequently 35 minutes, dropped in the sand mill fine powder more broken 50 minutes.Need to add pure water 38wt%, di(2-ethylhexyl)phosphate octanol 0.3wt%, polyvinyl alcohol 0.7wt% and defoamer 0.01wt% in the sand grinding process.And adding additive SiO 20.005wt%, CaCO 30.016wt%, Nb 2O 50.055wt%.Last mist projection granulating obtains the Mn-Zn ferrite powder.
Get this powder 18g with 6000kgf/cm 2Pressure forming, obtain the ring-type formed body of diameter 35.5cm, high 14cm.Sintering processing sintering by identical with embodiment 1 obtains the Mn-Zn ferrite cemented body.
, list in the table 2 as the power consumption under the temperature of table 2 with SY8232 tester test sintered body.
Embodiment 3
Take by weighing 68%Fe 2O 3, 24%Mn 3O 4, 8%ZnO adopts vibrator to mix 30 minutes, pre-burning under 920 ℃ temperature, and the pre-burning time is 38 minutes.Use the vibrator coarse crushing subsequently 30 minutes, dropped in the sand mill fine powder more broken 55 minutes.Need to add pure water 30wt%, di(2-ethylhexyl)phosphate octanol 0.15wt%, polyvinyl alcohol 0.55wt% and defoamer 0.01wt% in the sand grinding process.And adding addition of C aCO 30.015wt%, V 2O 50.086wt%, Nb 2O 50.060wt%.Last mist projection granulating obtains the Mn-Zn ferrite powder.
Get this powder 18g with 6000kgf/cm 2Pressure forming, obtain the ring-type formed body of diameter 35.5cm, high 14cm.Sintering processing sintering by identical with embodiment 1 obtains the Mn-Zn ferrite cemented body.
, list in the table 2 as the power consumption under the temperature of table 2 with SY8232 tester test sintered body.
Embodiment 4
Take by weighing 72wt%Fe 2O 3, 22wt%Mn 3O 4, 8wt%ZnO, wherein iron oxide red adopts homemade Baosteel iron oxide red (performance is referring to table 1).Adopt vibrator to mix pre-burning under 860 ℃ temperature 30 minutes.The pre-burning time is 40 minutes, uses the vibrator coarse crushing subsequently 35 minutes, drops in the sand mill fine powder more broken 45 minutes.Need to add pure water 45wt%, di(2-ethylhexyl)phosphate octanol 0.2wt%, polyvinyl alcohol 0.6wt% and defoamer 0.01wt% in the sand grinding process.And adding additive SiO 20.008wt%, V 2O 50.084wt%, Nb 2O 50.070wt%.Last mist projection granulating obtains the Mn-Zn ferrite powder.
Get this powder 18g with 6000kgf/cm 2Pressure forming, obtain the ring-type formed body of diameter 35.5cm, high 14cm.Sintering processing sintering by identical with embodiment 1 obtains the Mn-Zn ferrite cemented body.
, list in the table 2 as the power consumption under the temperature of table 2 with SY8232 tester test sintered body.
Embodiment 5
Take by weighing 72wt%Fe 2O 3, 23wt%Mn 3O 4, 6%ZnO, wherein iron oxide red adopts homemade Baosteel iron oxide red (performance is referring to table 1).Adopt vibrator to mix pre-burning under 870 ℃ temperature 25 minutes.The pre-burning time is 32 minutes, uses the vibrator coarse crushing subsequently 40 minutes, drops in the sand mill fine powder more broken 30 minutes.Need to add pure water 30wt%, di(2-ethylhexyl)phosphate octanol 0.3wt%, polyvinyl alcohol 0.65wt% and defoamer 0.01wt% in the sand grinding process.And adding additive SiO 20.009wt%, CaCO 30.012wt%, V 2O 50.082wt%.Last mist projection granulating obtains the Mn-Zn ferrite powder.
Get this powder 18g with 6000kgf/cm 2Pressure forming, obtain the ring-type formed body of diameter 35.5cm, high 14cm.Sintering processing sintering by identical with embodiment 1 obtains the Mn-Zn ferrite cemented body., list in the table 2 as the power consumption under the temperature of table 2 with SY8232 tester test sintered body.
By table 2 (for ease of relatively listing the PC40 performance of TDK company in), the soft magnetic ferrite powder power consumption that the present invention as can be seen produced is lower, saturation induction density B sHeight, superior performance.Particularly the high temperature power consumption is starkly lower than the standard of the external well-known TDK of manufacturer, has met or exceeded third generation LPL Ferrite Material standard.In addition, the present invention adopts the iron oxide red of Baosteel low-quality to produce high-quality Mn-Zn power ferrite powder, has the advantage that cost is low, raw material are sufficient, and will promote the development of domestic magnetic industry.
Table 1: each factory adds oxidation iron oxide red physicochemical characteristics
Producer The name of an article ??Fe 2O 3％ ???SiO 2％ ????CL％ ???AL 2O 3％ ??BET/SSA ???m 2/g
Baosteel BS (secondary) ???99.3 ???0.012 ????0.15 ????0.01 ????1.8
Korea S mountain lotus ??SKM-5 ???99.4 ???0.0006 ????0.007 ????0.008 ???3-3.2
Nippon Steel ???TCR ???99.4 ???0.007 ????0.007 ????0.018 ????4-5
The Kawasaki Steel ??KH-CPW ???99.3 ???0.008 ?????- ????0.02 ????4-6
NKK ??NKK-SM ???99.35 ???0.01 ????0.01 ????0.01 ????4-7
Iron is former ??TCR-S ???99.3 ???0.008 ????0.01 ????0.01 ????4-6
Table 2
Test condition: frequency f=100kHz; Magnetic flux density B=200mT
Lot number First northern magnetic permeability μ i Saturation induction density B s???(H＝1194A/m) ???25℃ ???60℃ ???80℃ ???100℃
??TDKPC40 ?2300±25％ ????????510 ???600 ???450 ????/ ????410
Embodiment 1 ????2367 ????????513 ???586 ???445 ???360 ????356
Embodiment 2 ????2340 ????????515 ???590 ???445 ???356 ????358
Embodiment 3 ????2367 ????????514 ???553 ???440 ???368 ????361
Embodiment 4 ????2338 ????????520 ???568 ???442 ???385 ????374
Embodiment 5 ????2336 ????????515 ???589 ???452 ???382 ????376

Claims (6)

1, a kind of manganese-iron power soft ferrite material powder is made up of Fe2O3, Mn3O4, ZnO, it is characterized in that each composition and consumption thereof are as follows:
Fe2O3???58-79wt％
Mn3O4???15-30wt％
ZnO?????5-15wt％，
Auxiliary material 0-7wt%,
Total amount satisfies 100%.
2, manganese according to claim 2-iron power soft ferrite material powder is characterized in that additive is SiO 2, CaCO 3, V 2O 5, Nb 2O 5One or more mixture.
3, manganese according to claim 2-iron power soft ferrite material powder is characterized in that dispersant is the di(2-ethylhexyl)phosphate octanol.
4, manganese according to claim 2-iron power soft ferrite material powder is characterized in that defoamer is that Main Ingredients and Appearance is the compound of polyether-type fatty acid ester.
5, the preparation method of a kind of manganese according to claim 1-iron power soft ferrite material powder is characterized in that concrete steps are as follows:
(1) mix: by claim 1 raw material proportion ingredient, adopt ball mill or vibrator to mix, incorporation time is 10～40 minutes, and mixed powder particle size is controlled at about 1.0-1.5 μ m;
(2) pre-burning: above-mentioned solid mixture is dropped into rotary kiln carry out pre-burning, calcined temperature is 700～1000 ℃, and the pre-burning time is 30～60 minutes, and the control powder flow is the 2-5 kg/minute, and the rotary kiln rotating speed is 10-20 rev/min;
(3) coarse crushing: will go up the black mixture that obtains of step pre-burning and carry out coarse crushing, and adopt vibrator, the pulverizing time is 20～50 minutes;
(4) sand milling: will carry out sand milling through the mixture of coarse crushing, and obtain the black paste of fine powder after broken, the whole sand milling time is 30-100 minute;
(5) spraying:, under 80～100 ℃ temperature,, obtain this product by the granulation tower spraying through the slip of sand milling.
6, the preparation method of manganese according to claim 5-iron power soft ferrite material powder, it is characterized in that sand milling is a kind of waterproof pulverization, utilize pure water as solvent, in sand mill, drop into black powder, additive, pure water and the dispersant of coarse crushing by a certain percentage, the ratio of adding is: black powder 48-68wt%, pure water 30-50wt%, additive 0-1wt%, dispersant 0-1wt%, when sand grinding process finishes soon, drop into glue polyvinyl alcohol and defoamer again, the total addition of polyvinyl alcohol and defoamer is 0-1wt%.
CN 03115906 2003-03-20 2003-03-20 Material powder of manganese-zinc power soft magnet ferrite and its preparation method Expired - Fee Related CN1252743C (en)

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100357220C (en) * 2005-07-15 2007-12-26 上海宝钢天通磁业有限公司 Production of high-frequency and low-consumption Mn-Zn ferrite material
CN100369860C (en) * 2005-08-11 2008-02-20 横店集团东磁有限公司 Mn-Zn ferrite material and production process thereof
CN100567206C (en) * 2006-11-30 2009-12-09 横店集团东磁股份有限公司 Mixing method of particle material for soft magnetic ferrite molding
CN101830691A (en) * 2009-03-13 2010-09-15 中国科学院福建物质结构研究所 Method for synthesizing nano ferrite soft magnetic material
CN101870578A (en) * 2010-04-14 2010-10-27 湖北凯立德新材料有限公司 Wide-temperature manganese zinc ferrite material with high-magnetic conductivity of 12,000 mu i and preparation method thereof
CN102211930A (en) * 2011-05-12 2011-10-12 上海电力学院 Preparation method of nano crystal MnZn ferrite with high saturation magnetization intensity
CN101555133B (en) * 2009-05-15 2012-12-26 上海华源磁业有限公司 Mn-Zn wide-temperature soft magnetic ferrite material and preparation method thereof
CN102108022B (en) * 2009-12-25 2013-01-30 上海宝钢磁业有限公司 Manganese-zinc ferrite material with wide temperature range and low temperature coefficient and preparation method thereof
CN102964118A (en) * 2012-11-07 2013-03-13 浙江通达磁业有限公司 Manganese and zinc series ferrite high-frequency material and method for producing same
CN103172359A (en) * 2013-03-25 2013-06-26 海宁联丰磁业股份有限公司 Manganese zinc power ferrite magnetic powder core and preparation method thereof
CN104529428A (en) * 2015-01-07 2015-04-22 中国人民解放军第二炮兵工程大学 Manganese cerium doped nickel zinc ferrite nano wave absorbing powder and preparation method thereof
CN104529426A (en) * 2014-12-19 2015-04-22 江门安磁电子有限公司 High-Bs low-loss manganese-zinc ferrite material applicable to 120-160 DEG C and manufacturing method thereof
WO2015106568A1 (en) * 2014-01-14 2015-07-23 四川省德阳博益磁性材料有限公司 Preparation process for mnzn soft ferrite having ultra-low value loss and high uq
CN107382301A (en) * 2017-09-14 2017-11-24 上海宝钢磁业有限公司 A kind of preparation method of manganese-zinc ferrite feed powder

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100357220C (en) * 2005-07-15 2007-12-26 上海宝钢天通磁业有限公司 Production of high-frequency and low-consumption Mn-Zn ferrite material
CN100369860C (en) * 2005-08-11 2008-02-20 横店集团东磁有限公司 Mn-Zn ferrite material and production process thereof
CN100567206C (en) * 2006-11-30 2009-12-09 横店集团东磁股份有限公司 Mixing method of particle material for soft magnetic ferrite molding
CN101830691A (en) * 2009-03-13 2010-09-15 中国科学院福建物质结构研究所 Method for synthesizing nano ferrite soft magnetic material
CN101555133B (en) * 2009-05-15 2012-12-26 上海华源磁业有限公司 Mn-Zn wide-temperature soft magnetic ferrite material and preparation method thereof
CN102108022B (en) * 2009-12-25 2013-01-30 上海宝钢磁业有限公司 Manganese-zinc ferrite material with wide temperature range and low temperature coefficient and preparation method thereof
CN101870578B (en) * 2010-04-14 2013-06-05 湖北凯立德新材料有限公司 Wide-temperature manganese zinc ferrite material with high-magnetic conductivity of 12,000 mu i and preparation method thereof
CN101870578A (en) * 2010-04-14 2010-10-27 湖北凯立德新材料有限公司 Wide-temperature manganese zinc ferrite material with high-magnetic conductivity of 12,000 mu i and preparation method thereof
CN102211930A (en) * 2011-05-12 2011-10-12 上海电力学院 Preparation method of nano crystal MnZn ferrite with high saturation magnetization intensity
CN102964118A (en) * 2012-11-07 2013-03-13 浙江通达磁业有限公司 Manganese and zinc series ferrite high-frequency material and method for producing same
CN103172359A (en) * 2013-03-25 2013-06-26 海宁联丰磁业股份有限公司 Manganese zinc power ferrite magnetic powder core and preparation method thereof
WO2015106568A1 (en) * 2014-01-14 2015-07-23 四川省德阳博益磁性材料有限公司 Preparation process for mnzn soft ferrite having ultra-low value loss and high uq
CN104529426A (en) * 2014-12-19 2015-04-22 江门安磁电子有限公司 High-Bs low-loss manganese-zinc ferrite material applicable to 120-160 DEG C and manufacturing method thereof
CN104529426B (en) * 2014-12-19 2016-08-24 江门安磁电子有限公司 For high Bs low waste MnZn ferrite material and the manufacture method thereof of 120～160 DEG C
CN104529428A (en) * 2015-01-07 2015-04-22 中国人民解放军第二炮兵工程大学 Manganese cerium doped nickel zinc ferrite nano wave absorbing powder and preparation method thereof
CN107382301A (en) * 2017-09-14 2017-11-24 上海宝钢磁业有限公司 A kind of preparation method of manganese-zinc ferrite feed powder
CN107382301B (en) * 2017-09-14 2020-08-04 上海宝钢磁业有限公司 Preparation method of manganese-zinc ferrite powder

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