CN103771850B - Preparation process of uQ-MnZn soft-magnetic ferrite with ultralow value and high loss - Google Patents
Preparation process of uQ-MnZn soft-magnetic ferrite with ultralow value and high loss Download PDFInfo
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 39
- 238000005516 engineering process Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000005469 granulation Methods 0.000 claims abstract description 12
- 230000003179 granulation Effects 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 238000001514 detection method Methods 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 17
- 239000002994 raw material Substances 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 13
- 238000000748 compression moulding Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000009826 distribution Methods 0.000 claims description 6
- 239000003595 mist Substances 0.000 claims description 6
- 238000007493 shaping process Methods 0.000 claims description 6
- 238000003801 milling Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 238000009472 formulation Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 239000007790 solid phase Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- 238000007669 thermal treatment Methods 0.000 claims description 4
- 238000000889 atomisation Methods 0.000 claims description 3
- 238000012790 confirmation Methods 0.000 claims description 3
- 238000007689 inspection Methods 0.000 claims description 3
- 238000011160 research Methods 0.000 claims description 3
- 230000035939 shock Effects 0.000 claims description 3
- 238000001694 spray drying Methods 0.000 claims description 3
- 239000007858 starting material Substances 0.000 claims description 3
- 238000007740 vapor deposition Methods 0.000 claims description 3
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 claims 1
- 229910010413 TiO 2 Inorganic materials 0.000 claims 1
- 238000004891 communication Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000005507 spraying Methods 0.000 abstract 1
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- 229910000831 Steel Inorganic materials 0.000 description 3
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229910003641 H2SiO3 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
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- 230000004927 fusion Effects 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000011656 manganese carbonate Substances 0.000 description 1
- 235000006748 manganese carbonate Nutrition 0.000 description 1
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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Abstract
The invention discloses a characteristic of a uQ-MnZn soft-magnetic ferrite material with ultralow value and high loss and a preparation process thereof, relating to the technical field of the key manufacturing technology of the soft-magnetic ferrite. The manufacturing process comprises the following steps of (1) powdery material: (1.1) formula of the powdery material; and (1.2) technology for controlling the water content of the powdery material; (2) spraying granulation; (3) presintering; (4) mixed-grinding granulation; (5) forming; (6) sintering; (7) detection; and (8) vacuum coating. The preparation process disclosed by the invention has the advantages that uQ product is increased from about 650 thousands on the existing industry and market to about 1 million, so that the performance of the MnZn soft-magnetic ferrite material is excellent; the high-uQ-MnZn material can meet various technologies such as high-end communication, satellite navigation, electromagnetic interference resistance, electromagnetic compatibility, missile guidance, identification of friend or foe and electronic countermeasures, and meet all the requirements of customers, so that the cost is reduced.
Description
Technical field:
The present invention relates to a kind of method of ultralow value loss height μ Q-MnZn soft magnetic ferrite characteristic and preparation technology thereof, belong to soft magnetic ferrite high-end technology field.
Background technology:
Soft magnetic ferrite is widely used in the numerous areas such as household electrical appliance, network communication, automotive electronics, space flight military project national defence.In recent years, its Application Areas also deepens continuously, and also constantly increases the performance requirement of soft magnetic ferrite, strengthens.
Originally high μ Q material and overlapping, the fusion mutually of high Bs material of low magnetic flux density (light current) and high magnetic flux density (forceful electric power) is respectively used to, occur comprising the comprehensive individual type material of high u material, be not only applicable to IT electronics but also be applicable to power electronics.Its principal feature is two high, two low, two wide, i.e. high Bs, high DC stacked; Low-loss, low harmonics distortion; Wideband, wide temperature.
As shown in Figure 1, the Making programme of prior art is:
(1) formula of material: confirm the purity of raw material, granularity and particle shape, specific surface area, homogeneity, the fill characteristic of powder, impurity content and the index such as kind, moisture content, adjusted by the mode such as thermal treatment and vibratory milling and control raw and auxiliary material containing assorted and granularity and distribution, control ratio surface-area and raw material solid phase reactive behavior.
(2) ball millings: adopt roller ball mill, ball-milling medium is steel ball, processing condition are by weight steel ball: raw material: deionized water=3: control at 1: 1, Ball-milling Time 4 ~ 7 hours.
(3) pre-burning: select 800-950 DEG C of calcined temperature, soaking time 5-7 hour.
(4) secondary ball milling: its processing condition, by weight as a reference, make steel ball: raw material: deionized water=4: 1: 0.5 ~ 0.8 controls, sand milling time 2-3 hour.
(5) granulation: ensure particle good sphericity, even particle size distribution, mobility of particle is good.
(6) shaping: mould compression moulding, pressure when controlling shaping and product density and substance.
(7) false burning: increase product density.
(8) sinter: by the magnetic core of compacting sintering 20-24 hour, sintering temperature controls within the scope of 1360-1400 DEG C, ensures product over-all properties.
(9) detect: test product being carried out to the magnetic property such as characteristic, inductance value.
(10) apply: apply on magnetic core surface, magnetic core surface insulation performance is increased.
The shortcoming of prior art: the comprehensive μ Q of MnZn soft magnetic ferrite material cannot be made to reach more than 800,000, and its technique is loaded down with trivial details, and energy consumption is not reached the effect of energy-saving and emission-reduction.
Summary of the invention:
For the problems referred to above, the technical problem to be solved in the present invention is to provide a kind of ultralow value loss height μ Q-MnZn soft magnetic ferrite characteristic and preparation technology thereof.
One of the present invention ultralow value loss height μ Q-MnZn soft magnetic ferrite characteristic and preparation technology thereof, its Making programme is as follows:
(1), powder:
(1.1), powder formulation: except the purity of raw material, outside the detection confirmation of granularity and particle shape, on the ratio formula of material, set up raw and auxiliary material database, determine raw-material purity, granularity, specific surface area, homogeneity, the fill characteristic of powder, impurity content and kind, the indexs such as moisture content, set up starting material Check and Inspection system, establish examinaing method and standard, adjusted by the mode such as thermal treatment and vibratory milling and control raw and auxiliary material containing assorted and granularity and distribution thereof, control ratio surface-area and raw material solid phase reactive behavior, thus for the variant production requirement that different client proposes, make high μ Q material,
(1.2), powder water content technology: adopt advanced equipment namely to be carried out control and the research of water content by high-pressure atomization principle, reach the zone of reasonableness of water content;
(2), mist projection granulating: adopt spray drying granulation technique, granular size evenly, consistence is better, and powder particles size can control within the scope of 3-5 μm;
(3), pre-burning: adopt 800 DEG C of-820 DEG C of calcined temperatures, soaking time is 4-5 hour;
(4), mix grinding granulation: after mist projection granulating carries out pre-burning, try again granulation process;
(5), shaping: particular manufacturing craft compression moulding, pressure when controlling supplied materials water content, compression moulding and product density and substance, meet compact density at 3.0-3.5g/cm
3;
(6), sinter: sinter the whole cycle at 20-22 hour.Sintering temperature controls within the scope of 1100-1150 DEG C, and the time is 2.5-3.5 hour;
(7), detect: test product being carried out to characteristic, inductance value ,-25 DEG C-+125 DEG C positive and negative temperature shock magnetic properties;
(8), vacuum coat: adopt vacuum vapor deposition paint-on technique to develop, the proof voltage of product is punctured and can reach >=1800V, the highlyest can reach >=3000V; Coat thickness is strict controlled in 0.002mm.
Beneficial effect of the present invention is: make MnZn soft magnetic ferrite material μ Q product bring up to about 1,000,000, thus make material property more superior, better meet all requirements in client, broader applications, in every profession and trade, reduce costs.
Accompanying drawing illustrates:
For ease of illustrating, the present invention is described in detail by following concrete enforcement and accompanying drawing.
Fig. 1 is the Making programme figure in background technology;
Fig. 2 is Making programme figure of the present invention.
Embodiment:
For making the object, technical solutions and advantages of the present invention clearly understand, below by the specific embodiment shown in accompanying drawing, the present invention is described.But should be appreciated that, these describe just exemplary, and do not really want to limit the scope of the invention.In addition, in the following description, the description to known features and technology is eliminated, to avoid unnecessarily obscuring concept of the present invention.
As shown in Figure 2, this embodiment is by the following technical solutions: its Making programme is:
(1), powder:
(1.1), powder formulation: except the purity of raw material, outside the detection confirmation of granularity and particle shape, on the ratio formula of material, set up raw and auxiliary material database, determine raw-material purity, granularity, specific surface area, homogeneity, the fill characteristic of powder, impurity content and kind, the indexs such as moisture content, set up starting material Check and Inspection system, establish examinaing method and standard, adjusted by the mode such as thermal treatment and vibratory milling and control raw and auxiliary material containing assorted and granularity and distribution thereof, control ratio surface-area and raw material solid phase reactive behavior, thus for the variant production requirement that different client proposes, make high μ Q material.
In current raw material ratio database, from soft magnetic ferrite crystalline structure, grain growing, compactness and the impact of macroscopical magnetic properties that finally shows, the existing batching of part and the following subordinate list of formulation ratio:
Composition table | Fe2O3 | MnCO3 | ZnO | TiO2 | CaCO3 | H2SiO3 | Ho2O3 |
Example one | 51.00 | 38.00 | 10.00 | 0.60 | 0.32 | 0.05 | 0.03 |
Example two | 51.50 | 37.50 | 9.90 | 0.70 | 0.32 | 0.04 | 0.04 |
Example three | 52.00 | 37.00 | 9.80 | 0.80 | 0.32 | 0.03 | 0.05 |
Example four | 52.50 | 36.50 | 9.70 | 0.90 | 0.32 | 0.02 | 0.06 |
Example five | 53.00 | 36.00 | 9.60 | 1.00 | 0.32 | 0.01 | 0.07 |
(1.2), powder water content technology: moisture content is one of critical control point of product, and moisture is overweight, can cause product adhesion in compression moulding process, cause density to reduce, cause difficulty to shaping; Hypohydration, easily cause product ftracture and internal fissure, reduce product performance, its moisture needs the content remaining on 0.8 ‰, therefore control moisture and Homogeneous Aqueous amount most important.
Adopt advanced equipment namely to be carried out control and the research of water content by high-pressure atomization principle, reach the zone of reasonableness of water content, promote the high-performance of material, reach the object obtaining excellent high μ Q material.
(2), mist projection granulating: adopt spray drying granulation technique, granular size evenly, consistence is better, and powder particles size can control within the scope of 3-5 μm; Particle good sphericity, even particle size distribution, mobility of particle is good, is conducive to the densification of product.
(3), pre-burning: adopt 800 DEG C of-820 DEG C of calcined temperatures, soaking time 4-5 hour, improve density, make solid state reaction complete, be conducive to the electromagnetic performance improving sample.
(4), mix grinding granulation: after mist projection granulating carries out pre-burning, try again granulation process, both ensure that powder mixed effect, again reduced the energy.
(5), shaping: particular manufacturing craft compression moulding, pressure when controlling supplied materials water content, compression moulding and product density and substance, meet compact density at 3.0-3.5g/cm3, consistence is good, for next step sintering is laid a solid foundation.
(6), sinter: adopt at present state-of-the-art bell-jar agglomerating plant in the world, improve sintering atmosphere and technique, optimize sintering temperature, explore the impact of sintering condition on grain-size, homogeneity, phase structure phase composite, sintering temperature, time and Ferrite Material electromagnetic performance relation.
Sinter the whole cycle at 20-22 hour.Sintering temperature controls within the scope of 1100-1150 DEG C, and the time ensures 3 hours, improves homogeneity of product and stability with this, ensures product high comprehensive performance.Summary makes the sintering time of product shorten 20%, reduces production cost.
(7), detect: test product being carried out to characteristic, inductance value ,-25 DEG C-+125 DEG C positive and negative temperature shock magnetic properties.
(8), vacuum coat: adopt advanced vacuum vapor deposition paint-on technique to develop, the proof voltage of product is punctured can reach >=more than 1800V, the highlyest can reach more than 3000V.Coat thickness is strict controlled in 0.002mm, avoided the thin material that causes to lose de-protected insulation layer effect, blocked uply also cause the insulation layer in winding process to break, naked effect, or affect the dimensional problem that client uses.
This embodiment brings up to about 1,000,000 by making μ Q product by about 650,000 on current industry, market, thus make MnZn soft magnetic ferrite material performance more superior, this high μ Q-MnZn material can better meet in every technology such as high-end communication, satellite-navigation, electromagnetism interference, electromagnetic compatibility technology, missile guidance, enemy and we's identification, electronic countermeasure, be satisfied with all requirements of client, thus reduce costs.
This embodiment break soft magnetic ferrite high stable, low-loss height μ Q material μ Q product about 600,000 situation, μ Q product is made to bring up to about 1,000,000, thus make material property more superior, better meet all requirements in client, broader applications are in every profession and trade, requirement especially to soft magnetic ferrite in high-end communication or aerospace, defense technology, reduce this type of high performance material situation of dependence on import, impel industry development and the spare part such as network filter and transformer cost is declined.
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (1)
1. the preparation technology of ultralow value loss height μ Q-MnZn soft magnetic ferrite, is characterized in that: its Making programme is as follows:
(1), powder:
(1.1), powder formulation: except the purity of raw material, outside the detection confirmation of granularity and particle shape, on the ratio formula of material, set up raw and auxiliary material database, determine raw-material purity, granularity, specific surface area, homogeneity, the fill characteristic of powder, impurity content and kind, moisture content, set up starting material Check and Inspection system, establish examinaing method and standard, by thermal treatment and vibratory milling adjustment and control raw and auxiliary material containing assorted and granularity and distribution thereof, control ratio surface-area and raw material solid phase reactive behavior, thus for the variant production requirement that different client proposes, make high μ Q material, material prescription content is Fe
2o
3: 51%, MnCO
3: 38%, ZnO:10%, TiO
2: 0.6%, CaCO
3: 0.32%, H
2siO
3: 0.05%, Ho
2o
3: 0.03%,
(1.2), powder water content technology: adopt advanced equipment namely to be carried out control and the research of water content by high-pressure atomization principle, reach the zone of reasonableness of water content, moisture content accounts for 0.8 ‰;
(2), mist projection granulating: adopt spray drying granulation technique, granular size evenly, consistence is better, and powder particles size controls within the scope of 3-5 μm;
(3), pre-burning: adopt 800 DEG C of-820 DEG C of calcined temperatures, soaking time is 4-5 hour;
(4), mix grinding granulation: after mist projection granulating carries out pre-burning, try again granulation process;
(5), shaping: particular manufacturing craft compression moulding, pressure when controlling supplied materials water content, compression moulding and product density and substance, meet compact density at 3.0-3.5g/cm
3;
(6), sinter: sinter the whole cycle at 20-22 hour, sintering temperature controls within the scope of 1100-1150 DEG C, and the time is 2.5-3.5 hour;
(7), detect: test product being carried out to characteristic, inductance value ,-25 DEG C-+125 DEG C positive and negative temperature shock magnetic properties;
(8), vacuum coat: adopt vacuum vapor deposition paint-on technique to develop, the proof voltage of product is punctured and can reach >=1800V, be up to 3000V; Coat thickness is strict controlled in 0.002mm.
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PCT/CN2014/085174 WO2015106568A1 (en) | 2014-01-14 | 2014-08-26 | Preparation process for mnzn soft ferrite having ultra-low value loss and high uq |
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CN104891980A (en) * | 2015-04-24 | 2015-09-09 | 马鞍山科信咨询有限公司 | Soft magnetic ferrite material suitable for power supply and preparation method thereof |
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