CN1124624C - Process for manufacturing MPP core forming powder and process for manufacturing MPP core using the powder - Google Patents

Process for manufacturing MPP core forming powder and process for manufacturing MPP core using the powder Download PDF

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CN1124624C
CN1124624C CN94118159A CN94118159A CN1124624C CN 1124624 C CN1124624 C CN 1124624C CN 94118159 A CN94118159 A CN 94118159A CN 94118159 A CN94118159 A CN 94118159A CN 1124624 C CN1124624 C CN 1124624C
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powder
magnetic core
manufacturing
molybdenum
iron
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CN1118925A (en
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裵光煜
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Chang Sung Co
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Samsung Electro Mechanics Co Ltd
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Abstract

The invention relates to a process for manufacturing an MPP core forming powder and a process for manufacturing the MPP core using the MPP core forming powder, in which the MPP core forming powder can be directly manufactured from melts. The process for manufacturing a powder for an MPP core (moly permalloy powder core) includes the steps of: melting an alloy composed of, 1.6-4.0% by weight of Mo, 78-83% by weight of Ni, and the balance of Fe; and manufacturing a powder by spouting a fluid into the flow of the melts. As the MPP core forming material is manufactured directly from the melts, the workability and productivity are improved, and the yield and the forming density can be also improved, as well as improving the frequency characteristics of the MPP core.

Description

Molybdenum ferronickel magnetic core manufacturing method of power and make the method for this magnetic core with this powder
The present invention relates to be used in and contain molybdenum strong magnet nickel alloy powder magnetic core (below be called the MPP magnetic core be Moly Permal-loy Powder Core) in SMPS (Switching Power Supply) and DC (direct current) converter etc.Especially, the present invention relates to make the formation of MPP magnetic core and form the method that powder is made the MPP magnetic core with manufacturing method of power and with the MPP magnetic core, MPP magnetic core shaping powder can directly be made from melt in the middle of this.
In general, the MPP magnetic core is used on SMPS and the DC converter etc., and it has high permeability and small frequency loss, so use the product of this magnetic core, energy loss can reduce, and small product size can reduce.
Usually, the MPP magnetic core is to make according to the technical process of Fig. 1, will be described in detail below.Promptly, at first in a stove such as electric furnace etc., melt by nickel (Ni) alloy that molybdenum (Mo) and iron (Fe) are formed in order to produce the MPP magnetic core.Form the ingot of certain size then.
The molybdenum that the alloy that manufacturing MPP core material is used should have the 1.6-4.0% weight ratio, the nickel of 78-83% weight ratio, other is an iron.By alloy is heated in electric furnace more than 1500 ℃, 1 hour with on carry out the fusing of alloy.
Then, in the above described manner the ingot of Xing Chenging be heated to 500 ℃ with on carry out 3 roads or more multiple tracks hot rolling, produce the band that width is about 60 inches with this.Then by using cold medium such as water to come band is quenched.
Quenching Treatment is the disordered state in order to make ensuing fragmentation carry out easily and form atomic arrangement in material.The Quenching Treatment condition is controlled by above-mentioned requirements.With disintegrating machine it is crushed to the certain granules size through the band that quenches then, and makes it pass through mesh screen, will make MPP magnetic core shaping powder greater than the particle removal of certain size.
The average particle size particle size that the MPP magnetic core of general extensive employing is shaped with powder is about 50 μ m, and when the powder of this size was screened, screen cloth was selected 120 orders, so that should be removed above 120 purpose particles.Mica is mixed in the powder after the screening, then mixture is put into the temperature that hydrogen reducing atmosphere is heated to 1170-1400.And under this temperature, keep more than 1 hour.Afterwards mixture is cooled to 300 ℃ in stove.Again mixture is cooled to room temperature.
Above-described annealing is in order to eliminate residual stress and distortion in the powder, so will suitably control annealing conditions.
Having carried out heat treated powder in the above described manner and coated with pottery, so that make the particle insulation, is the magnetic core of required form with powder forming then.
Here, for reduce the frictional force between particle and the particle and be pressed body and mould between frictional force, in above-mentioned powder, sneak into the zinc stearate (Zn-Stearate) below 1% before being shaped.
Remove the burr that forms in the mold pressing then, moulded body is heated to about 1170 temperature in reducibility gas hydrogen afterwards.And keep in stove, cooling off then more than 0.6 hour, anneal with this.Check magnetic afterwards,,, thereby finish the manufacturing of MPP magnetic core at its surface-coated polyester etc. for the characteristic of protecting magnetic core is not subjected to the influence of humidity and outside atmosphere.
Above-described annealing is stress and the distortion that remains in the moulded body in order to eliminate, thereby should control annealing conditions by this requirement.
The commonsense method of above-described MPP magnetic core manufacturing comprises too many complex process step, and the result has reduced operating efficiency, has improved production cost, and has reduced productivity ratio.
Commonsense method is to obtain the shaping of MPP magnetic core by pulverizing to use powder, thereby particle has irregular polyhedral shape.As a result, mold pressing density is very low, causes the permeability of MPP magnetic core to reduce.
In addition, in the occasion of commonsense method, powder particle has sharp comer, and ceramic coated is inhomogeneous as a result.In other words, be exactly that the dielectric film of powder particle is inhomogeneous.Thereby make the frequency characteristic of MPP magnetic core trouble occur.
In addition, in order to make smaller size smaller and, to need higher manufacturing technology than the product of light weight.Study energetically for this reason.
For adapting to the needs of this situation, the present inventor has done research for many years to the MPP magnetic core shaping powder that has good characteristic with straightforward procedure manufacturing more, and has invented the method for directly making MPP magnetic core shaping powder from melt.
Simultaneously, directly the method for producing powder from melt is known as atomization (atomizing), and this method never is applied to functional material MPP magnetic core aspect, and only is applied to other field, as is used for structural member material aspect such as auto parts.
Yet,, also only be applied to simple metal, and be not applied to alloy even in the field of having used.
The reason that is not applied to alloy is that if alloy is fused and directly produce powder from this melt, then powder particle does not have uniform formation, and the part of element is by segregation.This fact is also confirmed by present inventor's research.The segregation degree of alloying component is that the inhomogeneities of powder particle tissue changes with the kind and the oxidation characteristic of alloying component.
Particularly, inhomogeneous if alloying component becomes, promptly a certain component segregation also can make permeability significantly reduce, and causes that energy loss increases.Thereby, if direct method with alloy melt production MPP magnetic core powder is applied to functional material, then require powder to have uniform formation.
Therefore, the purpose of this invention is to provide the method for directly producing MPP magnetic core shaping powder from melt.
Another object of the present invention provides and is used to produce the method that particle has the MPP magnetic core shaping powder of sphere or regular polyhedron.
A further object of the invention provides the method for producing the uniform MPP magnetic core of particle alloying component shaping powder.Even powder is directly produced by alloy melt.
It is simple that another object of the present invention provides production process, the MPP magnetic core that permeability height and frequency loss are little.
In order to achieve the above object, the present invention is used to produce a kind of molybdenum ferronickel magnetic core manufacturing method of power that is used to make, and it is characterized by to comprise step: fusing is by 1.6-4.0 weight % molybdenum, 78-83 weight % nickel, alloy that all the other constitute for iron; And, water is sprayed into this melt-flow make powder by being 800~300psi and to spray into flow rate be 110~380 liters/minute to spray into pressure.
The invention provides a kind of method of making molybdenum ferronickel magnetic core, it is characterized by and comprise step: the molybdenum of fusing 1.6~4.5 weight %, the nickel of 78~83 weight % and all the other are the alloy of iron; By with spray into pressure be 800-3000psi and spray into flow velocity be the 110-380 liter/minute, water is sprayed into said alloy melt stream to produce powder; With the above-mentioned powder of ceramic coating, magnetic core then is shaped; The magnetic core that has been shaped is carried out annealing in process, then, check the magnetic of shaping magnetic core.
Describe most preferred embodiment of the present invention in detail referring now to accompanying drawing.Can make above-mentioned purpose of the present invention and other advantage will become more obvious like this, in the accompanying drawings:
Fig. 1 is the technical process block diagram of the common production method of MPP magnetic core.
Fig. 2 is MPP core production technical process method figure of the present invention.
Fig. 3 is with nitrogen (N 2) melt spray and the particles of powder size distribution plot produced.
Fig. 4 is water melt spray and the size distribution plot of the powder particle produced.
Fig. 5 is the curve chart of the inductance of the MPP magnetic core of the inventive method manufacturing and the MPP magnetic core that commonsense method is made with frequency change.
When preparation melt of the present invention, preferably, at first nickel is added and fusing, add then The Fe-Mo alloy also makes its fusing, adds Fe and fusing again, perhaps adds iron and fusing, again Add iron-molybdenum alloy and fusing. Perhaps, add simultaneously iron-molybdenum alloy and iron and fusing. Treat Carry out again alloying after the composition of final powder metallurgy is complete, make alloy melt.
Comprise nickel, the ratio that adds of the one-tenth branch of iron-molybdenum alloy and iron is like this control, namely Final powder metallurgy composition is: the molybdenum of 1.6-4.0%, and the nickel of 78-83%, all the other are iron.
When nickel was melted, heating-up temperature preferably was chosen to be 1600-1650 ℃. Such limit Scope processed former because: if temperature is lower than 1600 ℃, nickel not exclusively melts, and if temperature Be higher than 1650 ℃, melt may be oxidized. Fusing time preferably surpasses one hour, in order to fill Fractional melting.
When iron-molybdenum alloy being joined the nickel melt, and when melting therein, preferably fusing Temperature should be 1650-1700 ℃. Reason is in above-mentioned occasion, if temperature is lower than 1650 ℃, Ni can not melt fully, and if temperature is higher than 1700 ℃, melt may be by oxygen Change, also uneconomical. For reaching fully fusing, fusing time is preferably above one hour.
For iron-molybdenum alloy, general any iron-molybdenum alloy all can. But preferably adopt iron: 40-70% and molybdenum: 60-30%, as adopting iron: 40% and molybdenum: 60% alloy, then better.
When iron being added when melting in the nickel melt, fusion temperature preferably with the melting of iron-molybdenum alloy It is identical to change temperature.
Iron-molybdenum alloy and iron are added the nickel melt and with its fusing after, carry out the alloying place Reason, the melt temperature of nickel, iron-molybdenum alloy and iron is risen to 1700-1750 ℃, is preferably in this Kept one hour or more under the temperature. Reason is, and is if temperature is lower than 1700 ℃, not only former The diffusion velocity of son etc. becomes very slow so that prolong alloying time, and poor fluidity, the result Be difficult to powder from melt. If temperature is higher than 1750 ℃, melt potential evaporation and melt Possible oxidation.
In order fully to carry out alloying, alloying time is preferably 1 hour or more.The purity of metallic nickel and alloyed iron-molybdenum alloy is high more good more, preferably surpasses 99.9%.
Melt through alloy treatment forms powder with the fluid gunite.Be that fluid is sprayed onto in the melt-flow, the fluid drop that sprays into is collided melt-flow, thereby make melt form powder.Fluid can adopt inert gas such as argon or nitrogen or water.Determine that according to the shape of desired powder particle size, powder particle and the atomic arrangement of powder fluid sprays into condition, and injection conditions is with different variation of kind of fluid.
When adopting inert gas such as argon gas or nitrogen, particle is spherical in shape.When adopting water, particle is the polyhedron-shaped of rule.
When fluid adopted inert gas such as argon or nitrogen, expulsion pressure was preferably 50-1200psi (pound/inch 2), flow is preferably 1-14m 3/ min (cubic meter/minute).When fluid adopts water, spray into pressure and be preferably 800-30000psi.Flow is preferably 110-380L/min (rise/minute).
If it is too low to spray into pressure, then the powder particle diameter increases, and coating of particles is irregular.On the other hand, if it is too high to spray into pressure, then particle has spherical shape, but that particle diameter becomes is too little.Thereby be that above-mentioned scope is suitably to spray into pressure.
If flow is too little, melt can not harden fully so, thereby, be difficult to obtain the unordered of atom.On the other hand, if flow is too big, it is inhomogeneous that powder becomes.Thereby flow should be in above-mentioned scope.
Occasion using nitrogen preferably makes-183 ℃ liquid nitrogen, and makes the occasion of water, even 25 ℃ water does not have influence yet.
Resemble top describedly, spray into condition as spraying into pressure and spraying into flow, can obtain different particle sizes, sphere or regular polyhedron shape and atomic arrangement unordered by suitable adjustment.
The particle that desired powder size distributes and should have following size :-100 to+230 orders of 10-15% percentage by weight ,-230 to+325 orders of 25-35% weight ratio, and-325 orders of 45-65% weight ratio.
If the powder of the Zhi Zaoing MPP magnetic core that is used to be shaped in the above described manner then preferably is controlled at the content of carbon and is less than 100PPM (10 -6) content of oxygen is limited in and is less than 200PPm.Surpass the occasion of above-mentioned level at the content of carbon and oxygen, powder should should be reduced processing under hydrogeneous reducing atmosphere.Reduction is handled to be preferably under the 700-800 ℃ of temperature and is carried out more than one hour.
The manufacture method of MPP magnetic core is described according to the process drawing of Fig. 2 now.
At first, by the 1.6-4.0% molybdenum, the nickel of 78-83%, all the other alloys of forming for iron and unavoidable impurities melt as stated above and carry out alloy treatment.Then a fluid is sprayed into melt-flow so that make powder.Here, desirable powder particle size distributes and comprises-100 to+230 orders of 10-15% weight ratio ,-230 to+325 orders of 25-35% weight ratio, and-325 orders of 45-65% weight ratio.When magnetic core was shaped, the shaping density of the distribution of particle size and magnetic core was closely related.If particle size distribution range departs from mutually with above-mentioned scope, may reduce shaping density, thereby, should obtain above-mentioned particle size distribution by adjusting the fluid condition of spraying into.In last art particle size distribution, wish that average particle size particle size is that-100 to+230 purpose scopes are 90 μ m ,-230 to+325 purpose scopes are 70 μ m ,-325 purpose scopes are 45 μ m.In addition, the fluid condition of spraying into should be suitably determines by this way, the grain shape and the atomic arrangement of the MPP magnetic core that can obtain to be suitable for to be shaped.
If the content of carbon and oxygen surpasses 100PPm and 200PPm respectively, powder must reduce processing under hydrogeneous reducing atmosphere so.Reduction is handled under the temperature that is preferably in 700-800 ℃ and is carried out more than 1 hour.
Behind the coating powders, it is configured as required magnetic core in normal way.Preferably powder is put into shaping dies, under the forming pressure of about 240000psi, suppress with forcing press.
Under this condition,, in powder, preferably sneak into the zinc stearate below 1% in order to reduce the friction that is molded between body and shaping dies and the friction between the powder particle.
Then, magnetic is checked in the annealed processing of the magnetic core of formation.Afterwards, not influenced by humidity and outside atmosphere in order to protect the magnetic core characteristic, coating polyester or epoxy resin etc. are finished the production of MPP magnetic core with this on the magnetic core surface.
Carrying out above-mentioned annealing is in order to eliminate residual mechanical stress and distortion, should to control annealing for this purpose.Be preferably under the 530-740 ℃ of temperature and in hydrogeneous reducing atmosphere, anneal more than 0.6 hour.
The thickness of epoxy coating is preferably 50-200 μ m.
Now describe the present invention in detail by embodiment.
(example 1)
With 1.8kg (kilogram) purity is 99.9% the nickel induction furnace of packing into, then, is heated to 1610 ℃ and melts it.And then temperature risen to 1685 ℃, add the alloy that 1kg is made up of 40% iron-60% molybdenum afterwards.This mixture kept melting in 1 hour 10 minutes under said temperature close.Purity with 0.4kg is 99.9% iron adding and melts then.Melt risen to 1710 ℃ of temperature and under this temperature, kept 1 hour, thereby finish the preparation of melt.
Zhi Bei melt freely drips in the above described manner, simultaneously sprays into pressure and 9m with 90PSi 3/ minute flow spray into-183 ℃ nitrogen, make powder thus.Check particle size, the result is shown in Fig. 3 a.
Shown in Fig. 3 a, when directly making powder, can obtain the powder that having of 65-75% is suitable for the particle size distribution of MPP magnetic core with melt.
(example 2 and example 3)
As the occasion of example 1, fluid adopts nitrogen, makes powder with the same way as with example 1, and that just uses 1250PSi in the example 2 sprays into pressure and 9m 3/ minute flow, that uses 45PSi in the example 3 sprays into pressure and 9m 3/ minute flow.Check particle size distribution then, in result shown in Fig. 3 b.Also show the powder of under example 1 condition, making among Fig. 3 b.
Shown in Fig. 3 b,, obtain the powder that is suitable for the MPP magnetic core of 40-50% so only if it is too high or too low to spray into pressure.Efficient is relatively poor.
(example 4)
To make powder with example 1 same way as, just fluid adopts water, and spraying into pressure is 1900PSi, and flow is 150 liters/minute.Detect particle size distribution, the result is shown in Fig. 4 a.
Shown in Fig. 4 a, when when melt directly makes powder, can obtain the powder that having of 70%-90% is suitable for the particle size distribution of MPP magnetic core, explanation thus, this method efficient height.
(example 5)
To make powder with the same mode of example 1, just fluid adopts water, and spraying into pressure is 750PSi, and flow is 150 liters/minute.Then, check particle size distribution, in result shown in Fig. 4 b.
Shown in Fig. 4 b, too low if fluid sprays into pressure, obtain the powder that having of 40%-50% is suitable for the particle size distribution of MPP magnetic core so only.
(example 6)
According to the method for example 1, use powder, and, they are applied with pottery under similarity condition according to the ordinary powder that the regular grind method is made with the alloy manufacturing of sample ingredient.Use 200 then, the forming pressure of the 000PSi magnetic core that is shaped is measured the density of magnetic core then.
According to measured result, magnetic core density reaches 91% of solid density made in accordance with the present invention, and only reaches 87% of solid density according to the magnetic core density of commonsense method manufacturing.
Thereby, in occasion of the present invention, with 200, the low forming pressure of 000PSi, magnetic core also can obtain high density, thereby can prolong the life expectancy of mould, can prevent the damage to ceramic coating simultaneously.
(example 7)
According to example 1 make and powder with 50 μ m average particulate diameters with ceramic coated machine ceramic coated.Add 0.5% zinc stearate, use 240 then, the forming pressure of 000PSi is used the finishing die magnetic core that is shaped.
Then, under hydrogeneous reducing atmosphere, magnetic core remained on 670 ℃ of ten minutes next hours of temperature, magnetic core is annealed.The coating of using epoxy resin coating 100 μ m then is on the magnetic core surface.Inductance measuring is with the variation of frequency, and measurement result is illustrated by Fig. 5.
Fig. 5 shows powder of making by the regular grind method and the powder of making by the inventive method, and the two makes magnetic core under the same conditions, and its its inductance is with the variation of frequency.
As shown in Figure 5, by the MPP magnetic core of the present invention's manufacturing and the MPP magnetic core of making by commonsense method, the permeability of the two much at one.On frequency characteristic, MPP magnetic core of the present invention is better than common MPP magnetic core.
The reason why MPP magnetic core of the present invention is better than commonsense method is that the shape of powder particle is not sharp-pointed, and the ceramic coating of powder particle is uniformly, still can hold uniform coating when magnetic core is shaped.
As mentioned above, the present invention can directly make MPP magnetic core powder from melt by spraying into fluid.Therefore, simplified manufacture process, the result has improved machinability and productivity ratio greatly.In addition, the powder of varying particle size distribution and the powder of sphere or regular polyhedron grain shape can be made by the proper transformation fluid condition of spraying into.As a result, not only having improved the rate of finished products of powder and the frequency characteristic of shaping density but also MPP magnetic core also can improve greatly.

Claims (14)

1. one kind is used to make molybdenum ferronickel magnetic core manufacturing method of power, it is characterized by to comprise step:
Fusing is by the molybdenum of 1.6-4.0 weight %, the nickel of 78-83 weight %, the alloy that all the other constitute for iron; And
By being 800~300psi and to spray into flow velocity be 110~380 liters/minute, water is sprayed into this melt-flow make powder to spray into pressure.
2. manufacturing molybdenum ferronickel magnetic core manufacturing method of power as claimed in claim 1, the step of melted alloy wherein comprises fusing nickel, adds iron-molybdenum alloy and iron, carries out Alloying Treatment.
3. the method for the manufacturing of manufacturing molybdenum ferronickel magnetic core powder as claimed in claim 2, wherein said iron-molybdenum alloy consists of 40-70% iron, and 60-30% molybdenum.
4. the method for the manufacturing of manufacturing molybdenum ferronickel magnetic core powder as claimed in claim 2, wherein the fusion temperature of nickel is 1600-1650 ℃, and the fusion temperature of iron-molybdenum alloy and iron is 1650-1700 ℃, and the alloying temperature is 1700-1750 ℃.
5. the method for the manufacturing of manufacturing molybdenum ferronickel magnetic core powder as claimed in claim 4, wherein the fusing time of the fusing time of nickel and iron-molybdenum alloy and iron and alloying time were respectively more than 1 hour.
6. the method for the manufacturing of manufacturing molybdenum ferronickel magnetic core powder as claimed in claim 1, wherein the particles of powder distribution of sizes comprises that 10~15 weight % are that-100~+ 230 orders, 25~35 weight % are that-230~+ 325 orders, 45~65 weight % are-325 orders.
7. the method for the manufacturing of manufacturing molybdenum ferronickel magnetic core powder as claimed in claim 6, wherein-100 the average particulate diameter to+230 order scopes is 90 μ m, the average particulate diameter of-230 to+325 order scopes is 70 μ m, and the average particulate diameter of-325 order scopes is 45 μ m.
8. as the method for the manufacturing of each described manufacturing molybdenum ferronickel magnetic core powder of claim 1 to 5, wherein said powder reduces processing in reducing atmosphere.
9. the method for the manufacturing of manufacturing molybdenum ferronickel magnetic core powder as claimed in claim 8, wherein said reducing atmosphere is hydrogeneous, and said reduction treatment temperature is 700~800 ℃.
10. method of making molybdenum ferronickel magnetic core is characterized by and comprises step:
The nickel of molybdenum, 78~83 weight % of fusing 1.6~4.5 weight % and all the other are the alloy of iron;
By with spray into pressure be 800-3000psi and spray into flow velocity be the 110-380 liter/minute, water is sprayed into said alloy melt stream to produce powder;
With the above-mentioned powder of ceramic coating, magnetic core then is shaped;
The magnetic core that has been shaped is carried out annealing in process, then, check the magnetic of shaping magnetic core.
11. the method for manufacturing molybdenum ferronickel magnetic core as claimed in claim 10, above-mentioned particles of powder distribution of sizes comprise that 10~15 weight % are-100 to+230 orders, 25~35 weight % are-230 to+325 orders, and 45~65 weight % are-325 orders.
12. the method for manufacturing molybdenum ferronickel magnetic core as claimed in claim 11, wherein-100 the average particulate diameter to+230 order scopes is 90 μ m, and the average particulate diameter of-230 to+325 order scopes is 70 μ m, and the average particulate diameter of-325 order scopes is 45 μ m.
13. as the method for each described manufacturing molybdenum ferronickel magnetic core of claim 10 to 12, wherein powder reduces processing under reducing atmosphere.
14. manufacturing molybdenum ferronickel magnetic core as claimed in claim 13 method, wherein said reducing atmosphere is hydrogeneous, the temperature that reduction is handled is 700~800 ℃.
CN94118159A 1994-06-17 1994-11-07 Process for manufacturing MPP core forming powder and process for manufacturing MPP core using the powder Expired - Fee Related CN1124624C (en)

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KR1019940013719A KR970003124B1 (en) 1993-06-30 1994-06-17 Process for manufacturing mpp core forming powder and process for manufacturing mpp core using the powder
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6074601A (en) * 1983-09-30 1985-04-26 Nippon Ferrite Ltd Dust core
JPS6289802A (en) * 1985-10-16 1987-04-24 Hitachi Metals Ltd Production of fe-ni alloy green compact magnetic core

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6074601A (en) * 1983-09-30 1985-04-26 Nippon Ferrite Ltd Dust core
JPS6289802A (en) * 1985-10-16 1987-04-24 Hitachi Metals Ltd Production of fe-ni alloy green compact magnetic core

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