CN100533610C

CN100533610C - Powder composition, method for making soft magnetic components and soft magnetic composite component

Info

Publication number: CN100533610C
Application number: CNB2004800394525A
Authority: CN
Inventors: L·谢伦; A·阿赫林; L·胡尔特曼; O·安德森
Original assignee: Hoganas AB
Current assignee: Hoganas AB
Priority date: 2003-12-29
Filing date: 2004-12-15
Publication date: 2009-08-26
Anticipated expiration: 2024-12-15
Also published as: AU2004309770A1; ES2655322T3; CA2552142A1; ZA200605385B; TWI394178B; BRPI0418274A; CN1902719A; SE0303580D0; JP2010028131A; JP5138227B2; WO2005064621A1; DK1700319T3; TW200534298A; EP1700319B1; JP2007535134A; AU2004309770B2; RU2006127438A; KR100775179B1; PL1700319T3; RU2326461C2

Abstract

The invention concerns powder compositions consisting of electrically insulated particles of a soft magnetic material of an iron or iron-based powder and 0.1-2% by weight of a lubricant selected from the group consisting of fatty acid amides having 14-22 C atoms. Optionally a thermoplastic binder such as polyphenylene sulphide may be included in the composition. The invention also concerns a method for the preparation of soft magnetic composite components.

Description

The method of powder composition, manufacturing soft magnetic components and soft magnetic composite component

Technical field

The present invention relates to iron-based powder combination.More specifically, the present invention relates to be used for making the powder composition of soft magnetic composite component by powder metallurgy manufacturing approach.These compositions help making the soft magnetic composite component with high density and valuable magnetic property and mechanical performance.

Background technology

Soft magnetic material is used for following purposes: for example, and the core in the inductor, the stator of generator and rotor, adjuster, transducer and transformer core.Traditionally, soft magnetic core, for example rotor in the generator and stator are made by piling up the steel laminated material.Soft magnetism compound (SMC) material is based on the soft magnetism particle that has electric insulation coating layer on each particle (normally iron-based).Use traditional powder metallurgic method with insulating particle compacting (optional), obtain the SMC parts thus with lubricant and/or adhesive.Compare with the method for using the steel laminated material, the material that uses this powder metallurgy technology to make to have the higher SMC element design degree of freedom because the SMC material can carry three-dimensional magnetic flux, and can obtain 3D shape by pressing.

Two key characteristics of iron-core element are its magnetic permeability and core loss characteristics.The magnetic permeability of material is the indication of the ability of its ability that is magnetized or its carrying magnetic flux.Magnetic permeability is meant the ratio of induced flux and magnetizing force or field intensity.When making magnetic material be exposed in the alternating magnetic field, because magnetic hysteresis loss and eddy current loss and produce power loss, core loss.Magnetic hysteresis loss is by for the essential energy consumption of restraining in the iron-core element of residual magnetic force causes, and proportional with the frequency of alternating field.Eddy current loss causes by producing electric current in the iron-core element, and square proportional with the frequency of alternating field, and the electric current in the iron core produces because of the variations of flux that alternating current (AC) condition causes.Therefore for making the eddy current minimum, high resistivity is desirable, and particularly important under higher frequency.For the magnetic hysteresis loss that reduces the core element that is used for the alternating current purposes and improve its magnetic permeability, need heat-treat the parts of compacting usually.

Exploitation has been pointed in the research of the powder metallurgy manufacturing of the magnetic core element of using the coating iron-based powder improved the iron powder composition that some physics and magnetic property can not damage other performance of final element again.Required element function comprises, for example, and by high magnetic permeability, low core loss, high saturation induction, (high density) and the high strength of the frequency range that enlarges.Usually, the component density of increase has improved all these performances.

Required powder property comprises the applicability for compression molding techniques, this means that powder is molded as high density, high strength components easily, and this element ejects from molding equipment easily, and element has level and smooth surface smoothness.

The present invention relates to a kind of novel powder composition, and this powder composition is used to prepare the purposes of soft magnetic composite component with required powder property.This new compositions can be suppressed the element that (and heat treatment) becomes to have desired properties.

The invention still further relates to method and soft magnetic components itself that a kind of manufacturing has the soft magnet base member of excellent element function.

Brief summary of the invention

In brief, powder composition of the present invention is that electric insulation particle and fatty acid amide lubricant by soft magnetic material constitutes.Randomly, there are thermoplastic adhesives in the composition.Method of the present invention comprises the heat treatment of mixing, compacting and optional gained element, has the soft magnet base member of excellent properties thereby produce.

Detailed Description Of The Invention

This powder preferably substantially pure, water-atomized iron powder or iron sponge powder with irregular shape of particle.In this article, term " substantially pure " is meant that the amount that powder should not contain field trash and impurity O, C and N substantially should remain on minimum.Particle mean size is usually less than 300 microns to being higher than 10 microns.The example of these powder is available from ABC 100.30, the ASC100.29 of Sweden Hoganas AB, AT 40.29, ASC 200, ASC 300, NC 100.24, SC 100.26, MH 300, MH 40.28, MH 40.24.

According to a specific embodiment of the present invention, used powder contains than the normal thick particle of situation in the common mold pressing.In the practice, this means that powder does not contain particulate substantially.Term " do not contain particulate substantially " and be meant be less than about 10%, preferably be less than 5% powder particle and have granularity less than 45 microns, this granularity is to record by the method for describing among the SS-EN 24497.Average grain diameter is generally 106 to 425 microns.Greater than 212 microns particle weights usually above 20%.Maximum particle size can be about 2 millimeters.

The size of iron-based particle commonly used distributes according to Gaussian distribution curve in PM industry, and its average grain diameter is 30 to 100 microns, and the particle of about 10-30% is less than 45 microns.Therefore, powder may have the particle size distribution that departs from powder commonly used used according to the present invention.Powder that can be by removing thin part or have the powder that desired particle size distributes by manufacturing and obtain these meal.Yet, the invention is not restricted to meal, also comprise the powder of the mold pressing granularity commonly used that has in the PM industry among the present invention.

The electric insulation layer of powder particle can be made by inorganic material.What particularly be fit to is disclosed insulating barrier type (being incorporated herein by this reference) among the US 6348265, and it relates to the basic powder particle that the iron by the substantially pure of the separator that contains oxygen and phosphorus that contains insulation constitutes.About coating, should especially propose, coating layer thickness may influence the performance of composite component.The powder that contains insulating particle can be used as Somaloy ^TM500 and 550 available from Sweden Hoganas AB.

Lubricant is selected from fatty acid amide used according to the present invention.Particularly suitable acid amides is to contain 12-24, preferred 14-22 carbon atom, the primary amide of the saturated or unrighted acid of 18-22 carbon atom most preferably.Lubricant quantity can be lower than 2 weight % of composition weight, preferably is lower than 1.5 weight %.It is 0.05-1 weight % that lubricant is particularly preferably measured, preferred 0.05 to 0.8, more preferably 0.1 to 0.8 weight %, most preferably 0.1 to 0.5 weight %.Particularly preferred lubricant is stearic amide, oleamide, docosanoic acid acid amides, erucic acid (eurcic acid) acid amides, palmitamide, and stearic amide most preferably.At United States Patent (USP) 6,537, in 389, mention the stearic amide that combines with rapeseed methylester as lubricant, also mention as in thermoplastic resin, the polyphthalamide (polyphatalamide) of the adhesive of compacting soft magnetic powder.

Kollag has the density of about 1-2 gram/cubic centimetre usually, and this compares very low with the iron-based powder density of about 7.8 gram/cubic centimetres.Therefore, in composition, comprise the solid density that the lower lubricant of these density can reduce the compacting element.Therefore, lubricant being kept is important for making high density components on a small quantity.Yet the lubricant of low amount is easy to generate (ejection) problem that ejects.Be surprised to find that the lubricant of the above-mentioned type amount of can hanging down is used under the situation that does not produce the problem of ejecting.

By replacing internal lubricant (promptly adding the lubricant in the iron-based powder mix to) with die wall lubrication (DWL), and be used in combination high pressing pressure, can obtain high green density.Yet when pressing down system insulation iron-based powder at high pressing pressure, a shortcoming of this known method is, destroys the insulating barrier of iron-based powder easily, thereby causes the high core loss under upper frequency.In addition, the use meeting of DWL further increases process complexity, and this can prolong circulation timei and reduce production stability in the industrial environment.

According to the present invention, can use fatty acid amide as the unique additive in insulation iron or the iron-based powder, certainly, for some application, it is favourable adding small amount of thermal plastic resin, especially polyphenylene sulfide (PPS).Term " on a small quantity " this be meant be lower than composition weight 2, preferably be lower than 0.8, more preferably less than 0.6, most preferably be lower than 0.5 weight %.When amount is lower than 0.05 weight %, do not observe any effect of PPS.Particularly, the amount of PPS can not wait between 0.1 to 0.5 weight %, preferred 0.2 to 0.5 or 0.4 weight %.When the good frequency stability of needs, the interpolation of PPS is useful especially.

PPS and stearic combination are known from patent application WO01/22448.The embodiment of this application discloses and can make soft magnetic material by the electric insulation iron-based powder is mixed with PPS and stearic acid.This mixture suppressed at elevated temperatures and with the parts of gained compacting in blanket of nitrogen 260 ℃ of heat treatments, then 285 to 300 ℃ of secondary heat treatment.Be surprised to find that,, can obtain some advantages by using this novel powder compositions (it has comprised fatty acid amide but not corresponding aliphatic acid).For example, have been found that novel powder has unexpected improved greasy property, this make will compacting parts to eject the required energy that ejects from mould lower, can obtain higher density, and can obtain better cross-breaking strength.In addition, pressing step can carry out at ambient temperature.In addition, can make heat treatment easier, disclose the first required heat treatment step because can omit according to WO.

The iron-based magnetic that contains insulating particle and combine with thermoplastic resin has been described in U.S. Patent application 2002/0084440.Opposite with particle of the present invention, known particle also contains rare earth element before these.In addition, the consumption of thermoplastic resin is relatively large, i.e. at least 5 weight %.In addition, the granularity of iron-based powder quite little (as an example, having mentioned 3 microns).Can also comprise the lubricant that is selected from the number of chemical compound.These powder compositions preferably can be used for injection moulding according to stating, extrude, injection compression and injection press be with preparation high-weatherability bonding permanent magnet.

In order to prepare composite component of the present invention, single shaft pressed powder composition in the punch die that mustn't lubricate usually at first, but this powder composition also can use in lubricated punch die.Element with compacting ejects from punch die and optional heat-treating then.

Compacting can be in the temperature of ambient temperature or rising and is carried out under the pressure of the highest 1500MPa.

According to preferred embodiment of the present invention, be compressed in the instrument of appropriate heating and carry out, because not only can improve green density thus and eject performance, can also improve maximum relative permeability.The element function that will press down system at the temperature that raises and low pressing pressure with compare with the element function that the higher pressure pressing pressure presses to identical green density in ambient temperature, Ya Zhi element has higher magnetic permeability at elevated temperatures.For bigger element, may also must improve powder temperature to realize improvement of the present invention.

Heat treatment can be carried out in one or several steps.A step heat treatment of recommending is to carry out between 250 to 550 ℃ 30 minutes to 4 hours in oxygen-containing atmosphere (air).

Another selection is to heat-treat 30 minutes to 3 hours at 250-350 ℃ in air or inert gas, heat treatment 15 minutes to 2 hours between 350 to 550 ℃ in containing oxygen (air) atmosphere then.

When comprising PPS in the composition, recommend to use different slightly heat treatment.For example, in this case, heat treatment can be carried out 30 minutes to 4 hours at 250-350 ℃ in oxygen-containing atmosphere (air).Another selection is to heat-treat 30 minutes to 3 hours at 250-350 ℃ in air or inert gas, then in oxygen-containing atmosphere (air) 300 to 500 ℃ of heat treatments 15 minutes to 2 hours.

Can use different atmosphere, time and temperature to heat-treat to obtain to have the final element of desired properties, this makes this novel powder compositions particularly attractive.

By high pressure (for example being higher than 800MPa) down compacting contain the iron-based insulating powder with coarse grain and the composition of lubricant as mentioned above, then repressed element is heat-treated, obtain the soft magnetic composite component of density 〉=7.5 gram/cubic centimetres, maximum relative permeability μ max 〉=600, coercivity H≤250A/m and electricalresistivity 〉=20 μ Ω m.This element can be used in stator in the engine for example and the rotor elements required high request and uses.

Further set forth the present invention by the following example.

Embodiment 1

Use following material.

Use iron-based water atomised powder as raw material, its particle contains thin inorganic coating (Somaloy ^TM500, can be available from Sweden Hoganas AB).

The PPS powder,

The stearic acid powder, lubricant A,

The stearic amide powder, lubricant B.

According to table 1, with 3 kilograms of basic powder Somaloy ^TM500 mix with PPS and stearic amide or stearic acid.

Table 1. mixture of powders: lubricant and PPS (weight %)

Sample number	PPS	Lubricant
Sample number	PPS	Lubricant	A1	0.60％	0.2％A
A2	0.50％	0.3％A	A1	0.60％	0.2％A
A2	0.50％	0.3％A	A3	0.50％	0.3％B
A4	0.30％	0.3％B	A3	0.50％	0.3％B
A4	0.30％	0.3％B	A5	0.30％	0.4％B
A6	0.30％	0.5％B	A5	0.30％	0.4％B
A6	0.30％	0.5％B	A7	0.1％	0.3％B
A8	0.2％	0.3％B	A7	0.1％	0.3％B
A8	0.2％	0.3％B	A9	-	0.4％B

Mixture of powders is depressed to 45 millimeters of internal diameters, 55 millimeters of external diameters and high 5 millimeters ring-type sample at 800MPa and ambient temperature (room temperature).The ring-type sample that same compacting is 10 millimeters high, and on these samples, measure ejecting force.Ejecting energy is presented in the table 2.The result shows, uses fatty acid amide to obtain the obviously lower energy that ejects.

Table 2. records on the ring-type sample of h=10 millimeter ejects energy

Sample number	PPS	Lubricant	Eject energy (Jiao/square centimeter)
Sample number	PPS	Lubricant	Eject energy (Jiao/square centimeter)	A1	0.60％	0.2％A	52
A2	0.50％	0.3％A	46	A1	0.60％	0.2％A	52
A2	0.50％	0.3％A	46	A3	0.50％	0.3％B	38
A4	0.30％	0.3％B	37	A3	0.50％	0.3％B	38
A4	0.30％	0.3％B	37	A5	0.30％	0.4％B	33
A6	0.30％	0.5％B	30	A5	0.30％	0.4％B	33
A6	0.30％	0.5％B	30	A7	0.10％	0.3％B	41
A8	0.20％	0.3％B	39	A7	0.10％	0.3％B	41
A8	0.20％	0.3％B	39	A9	-	0.4％B	35

After the compacting, with parts 290 ℃ of heat treatments 120 minutes in air.The heat treated ring rotation 25 of gained is changeed.According to standard IEC 60404-6, second edition 2003-06 measures relative AC inductance magnetic permeability with LCR-meter (HP4284A).

Table 3 and 4 has shown the decline of initial permeability (frequency stability).The decline of initial permeability be expressed as 10 and 100kHz under the difference of initial permeability divided by the initial permeability under the 10kHz.Table 3 shows, by the amount of fatty acid amide is increased to 0.5% from 0.3, can obtain better frequency stability.Table 4 shows, uses fatty acid amide to replace corresponding aliphatic acid, can obtain better frequency stability.In addition, table 4 shows that when not using PPS, frequency stability descends more.Yet,, be 95 at the initial permeability of 1kHz according to survey, and A3 is 75 for A9.High initial magnetoconductivity under lower frequency is favourable for some application.

The decline of table 3 initial permeability

	Dμ 10-100kHz(％)
	Dμ 10-100kHz(％)	A4	7.4
A5	5.2	A4	7.4
A5	5.2	A6	4.2

The decline of table 4 initial permeability

	Dμ 10-100kHz(％)
	Dμ 10-100kHz(％)	A2	6.4
A3	3.9	A2	6.4
A3	3.9	A9	20.9

By four point measurement method measured resistivity and be presented in the table 5.From this table, as can be seen, use fatty acid amide to replace corresponding acid, can obtain obviously higher resistivity.

The resistivity of table 5. ring-type sample

Sample number	PPS	Lubricant	Resistivity, resistance coefficient μ Ohm*m
Sample number	PPS	Lubricant	Resistivity, resistance coefficient μ Ohm*m	A2	0.50％	0.3％A	316
A3	0.50％	0.3％B	400	A2	0.50％	0.3％A	316

In addition, at 290 ℃ of heat treatments after 120 minutes in air, the cross-breaking strength TRS of specimen.According to ISO 3995 test TRS.On parts, test TRS at 200 ℃ equally.TRS is presented in the table 6.The sample that contains 0.5%PPS and 0.3% stearic amide (A3) is compared with the sample that contains 0.2%PPS+0.6% stearic acid (A1) with the sample that contains 0.5%PPS and 0.3% stearic acid (A2), all shows obviously higher TRS room temperature (RT) and 200 ℃.For the mixture with low organic substance total content, density is higher, and this causes higher induction and magnetic permeability (μ max).

Table 6. is at the density and the TRS of room temperature and 200 ℃

Sample number	PPS	Lubricant	Density gram/cubic centimetre after the heat treatment	TRS room temperature MPa	TRS 200℃MPa
Sample number	PPS	Lubricant	Density gram/cubic centimetre after the heat treatment	TRS room temperature MPa	TRS 200℃MPa	A1	0.60％	0.2％A	7.18	68	51
A2	0.50％	0.3％A	7.18	46	30	A1	0.60％	0.2％A	7.18	68	51
A2	0.50％	0.3％A	7.18	46	30	A3	0.50％	0.3％B	7.19	81	67
A4	0.30％	0.3％B	7.27	88	73	A3	0.50％	0.3％B	7.19	81	67
A4	0.30％	0.3％B	7.27	88	73	A5	0.30％	0.4％B	7.22	87	73
A6	0.30％	0.5％B	7.17	51	68	A5	0.30％	0.4％B	7.22	87	73
A6	0.30％	0.5％B	7.17	51	68	A7	0.1％	0.3％B	7.35	85	74
A8	0.2％	0.3％B	7.31	84	71	A7	0.1％	0.3％B	7.35	85	74
A8	0.2％	0.3％B	7.31	84	71	A9	-	0.4％B	7.33	87	78

Embodiment 2

Use following material.

Use iron-based water atomised powder as raw material, its particle has phosphorous inorganic shallow layer (Somaloy ^TM500, available from Sweden Hoganas AB).

The PPS powder,

The stearic acid powder, lubricant A,

The stearic amide powder, lubricant B,

The docosanoic acid powder, lubricant C,

The oleamide powder, lubricant D,

Kenolube ^TM。

According to following table 7, with basic powder Somaloy ^TM500 with PPS and mix lubricant.

Table 7. mixture of powders: lubricant and PPS (weight %)

Sample number	PPS	Lubricant
Sample number	PPS	Lubricant	B1	0.50％	0.3％A
B2	0.50％	0.3％B	B1	0.50％	0.3％A
B2	0.50％	0.3％B	B3	0.50％	0.3％C
B4	0.50％	0.3％D	B3	0.50％	0.3％C
B4	0.50％	0.3％D	B5	0.30％	0.3％B
B6	-	0.4％B	B5	0.30％	0.3％B
B6	-	0.4％B	B7	-	0.3％B
B8	0.1％	0.3％B	B7	-	0.3％B
B8	0.1％	0.3％B	B9	0.2％	0.3％B
B10	-	0.4％Kenolube ^TM	B9	0.2％	0.3％B

Mixture of powders is pressed into test-strips according to ISO 3995 under the pressing pressure of 800MPa and ambient temperature.After the compacting, parts are heat-treated in two step heat treatments.The first step was carried out 105 minutes at 290 ℃ in inert nitrogen atmosphere.After this step is at 350 ℃ of heat treatment steps that carry out 60 minutes in air.Cross-breaking strength TRS according to ISO 3995 specimen.

The result of cross-breaking strength test is presented in the table 8.As can be seen from Table 8, the sample made from the mixture of fatty acids acid amides produces enough TRS values.Reach higher density after the heat treatment, this is favourable to induction and magnetic permeability.If PPS content reduces to 0.3% or lower, TRS rises to the above value of 80MPa.Do not contain PPS and contain the sample of stearic amide lubricant even have the above TRS value of 100MPa.The lubricant Kenolube that tradition is used ^TMUse can not produce required cross-breaking strength.

Density under table 8. room temperature and TRS

Embodiment 3

This embodiment shows, compare with the ethylene bis stearamide lubricant with the zinc stearate that generally uses, when using low amount fatty acid amide lubricant of the present invention and being used in combination meal and during high pressing pressure, eject the low ejecting force of acquisition in the process at the compacting element, and obtain to eject the perfect surface smoothness of element.

Meet US 6,348,265 soft magnetism iron-based meal (wherein particle is surrounded by inorganic insulating material) and the mix lubricant of 0.2 weight % with two kilograms according to table 9.The particle size distribution of iron-based meal is presented in the table 10.Mixture E and F are the Comparative Examples that comprises known lubricants.

Table 9

Mixture	Lubricant
Mixture	Lubricant	A	The docosanoic acid acid amides
B	Erucyl amide	A	The docosanoic acid acid amides
B	Erucyl amide	C	Stearmide
D	Oleamide	C	Stearmide
D	Oleamide	E	Zinc stearate
F	Ethylene bis stearamide	E	Zinc stearate

Table 10

Granularity (micron)	Weight %
Granularity (micron)	Weight %	>425	0.1
425-212	64.2	>425	0.1
425-212	64.2	212-150	34.0
150-106	1.1	212-150	34.0
150-106	1.1	106-75	0.3
45-75	0.2	106-75	0.3
45-75	0.2	<45	0

The cylindrical specimen (50 gram) of transferring to the gained mixture in the punch die and under the pressing pressure of 1100MPa, moving and be pressed into 25 millimeters of diameters with the single shaft compacting.Used die materials is traditional tool steel.Ejecting in the process of compacting sample, the record ejecting force.Record eject sample required always eject energy/coating (enveloping) area.Following table 11 has shown and has ejected energy, green density and surface smoothness.

Table 11

Mixture	Eject energy (Jiao/square centimeter)	Green density (gram/cubic centimetre)	Surface smoothness
Mixture	Eject energy (Jiao/square centimeter)	Green density (gram/cubic centimetre)	Surface smoothness	A	90	7.64	Perfect
B	83	7.65	Perfect	A	90	7.64	Perfect
B	83	7.65	Perfect	C	93	7.63	Perfect
D	70	7.67	Can accept	C	93	7.63	Perfect
D	70	7.67	Can accept	E	117	7.66	Unacceptable
F	113	7.64	Perfect	E	117	7.66	Unacceptable

Embodiment 4

The following example shows that the particle size distribution of soft magnet based powders is to ejecting the influence of performance and green density.Use is according to " slightly " powder of embodiment 3." carefully " particle size distribution of powder is listed in the table 12.Use 0.2 weight % stearmide to prepare mixture according to the program of embodiment 3.Mixture based on " carefully " powder is made sample H by mark, and compares with sample C.

Table 12

Granularity (micron)	Weight %
Granularity (micron)	Weight %	>425	0
425-212	0	>425	0
425-212	0	212-150	11.2
150-106	25.0	212-150	11.2
150-106	25.0	106-75	22.8
45-75	26.7	106-75	22.8
45-75	26.7	<45	14.3

According to embodiment 3 used programs mixture is pressed into cylindrical sample.Following table 13 has shown green density and appearance.

Table 13

Mixture	Green density (gram/cubic centimetre)	Surface smoothness
Mixture	Green density (gram/cubic centimetre)	Surface smoothness	C	7.63	Perfect
H	7.53	Can accept	C	7.63	Perfect

As can be seen from Table 13, the composition that contains fine powder produces lower green density and impaired surface smoothness.

Embodiment 5.

This embodiment has compared the known lubricant ethylene bis stearamide (EBS) and the example of lubricant stearmide.Use mixes with EBS and stearmide respectively according to table 14 according to " slightly " powder of embodiment 3.Program according to embodiment 3 prepares sample.

Table 14

Mixture	EBS (weight %)	Stearmide (weight %)
Mixture	EBS (weight %)	Stearmide (weight %)	1	0.20	--
2	0.30	--	1	0.20	--
2	0.30	--	3	0.40	--
4	0.50	--	3	0.40	--
4	0.50	--	5	--	0.10
6	--	0.20	5	--	0.10
6	--	0.20	7	--	0.30

Under 1100MPa, mixture of powders is pressed into 45 millimeters of internal diameters, 55 millimeters of external diameters and high 10 millimeters ring.Ejecting in the process of compacting sample, calculate sample is ejected the required energy/coating area that always ejects from punch die.Following table 15 shown calculate eject energy/area, green density and appearance.

Table 15. ejects energy, green density, appearance

Mixture	Eject energy [Jiao/square centimeter]	Density [gram/cubic centimetre]	Appearance
Mixture	Eject energy [Jiao/square centimeter]	Density [gram/cubic centimetre]	Appearance	1	54	7.65	Unacceptable
2	40	7.61	Can accept	1	54	7.65	Unacceptable
2	40	7.61	Can accept	3	33	7.56	Perfect
4	28	7.51	Perfect	3	33	7.56	Perfect
4	28	7.51	Perfect	5	73	7.67	Can accept
6	38	7.64	Perfect	5	73	7.67	Can accept
6	38	7.64	Perfect	7	37	7.59	Perfect

As can be seen from Table 15, can add and be low to moderate 0.2% novel lubricant, and still can obtain perfect surface smoothness, and for reference lubricant EBS, obtain that perfect surface smoothness is minimum will add 0.4%.

Embodiment 6

This embodiment has compared respectively the magnetic property of realizing similarly ejecting the element that energy value required minimum emollient component stearmide and EBS make with being.Magnetic property after the heat treatment of the element of making by mixture 2 and mixture 6 according to embodiment 5 relatively.

Except that highly being 5 millimeters, according to embodiment 5 compacting ring-type samples.With the green compact sample 300 ℃ of heat treatments 60 minutes in air, then 530 ℃ of heat treatments 30 minutes in air.The ring rotation 100sense that gained is heat treated changes and 100drive changes, and tests in the Brockhaus hysteresisgraph.Following table 16 has shown the sensitivity under the 10kA/m, maximum relative permeability, coercive force H _cWith the core loss under 400Hz, 1T.

Table 16. soft magnet performance

	Sample 2	Sample 6
	Sample 2	Sample 6	Maximum permeability	480	750
The B[T of 10000A/m]	1.58	1.66	Maximum permeability	480	750
The B[T of 10000A/m]	1.58	1.66	Hc[A/m]	218	213
Core loss 400Hz, 1T[W/kg]	78.4	42.1	Hc[A/m]	218	213

As can be seen from Table 16, element soft magnet performance excellence of the present invention.

Embodiment 7

The following example has shown the influence that eject performance and green density of punch die temperature to the compacting sample.In this embodiment, select the primary amide stearmide as amide lubricant of the present invention.According to the program of embodiment 3, in 2 kilograms of soft magnetism electric insulation iron-based meal, add 0.2% stearmide.

Under the pressing pressure of 1100MPa, mixture of powders is pressed into 45 millimeters of internal diameters, 55 millimeters of external diameters and high 10 millimeters ring.Write down ejecting force in the process ejecting of compacting sample.Calculating ejects the required energy/coating area that always ejects with sample from punch die.Following table 17 has shown and has ejected energy, green density and appearance at the sample of different punch die temperatures systems.

Table 17. ejects energy, green density, appearance under different punch die temperature

The punch die temperature (℃)	Eject energy [Jiao/square centimeter]	Green density [gram/cubic centimetre]	Appearance
The punch die temperature (℃)	Eject energy [Jiao/square centimeter]	Green density [gram/cubic centimetre]	Appearance	25	38.4	7.64	Perfect
50	31.5	7.66	Perfect	25	38.4	7.64	Perfect
50	31.5	7.66	Perfect	60	30.6	7.67	Perfect
70	29.3	7.67	Perfect	60	30.6	7.67	Perfect
70	29.3	7.67	Perfect	80	27.5	7.69	Perfect

As can be seen from Table 17, the raising meeting of punch die temperature produces positive impact to ejecting energy and green density.

Embodiment 8

This embodiment has compared the element function of element made in accordance with the present invention and by the performance of the element of DWL compacting.In embodiments of the invention and Comparative Examples, all use " slightly " powder of embodiment 3.Use 0.2 weight % stearmide as the lubricant in the embodiment of the invention, and the gained powder composition is become green density 80 ℃ controlled punch die temperatures is the ring-type sample of 7.6 gram/cubic centimetres.In Comparative Examples, do not use internal lubricant, and use DWL.At ambient temperature the ring-type sample is depressed into the density of 7.6 gram/cubic centimetres.Ring-type sample external diameter is 55 millimeters, 45 millimeters of internal diameters and high 5 millimeters.

After the compacting, heat-treat according to table 18.By 4 method measured resistivity.In hysteresis graph, carry out before the magnetic measurement, ring-type sample rotation 100drive is changeed and the 100sense commentaries on classics.From the loop, obtain the DC performance with 10kA/m.Under 1T with different frequency measurement core losss.In Fig. 1, draw the functional arrangement of core loss/circulation and frequency.

Table 18: magnetic property

Sample	Heat treatment	B _10kA/m	Hc [A/m]	ρ [μΩm]	1T, 400Hz[W/kg] time core loss
Sample	Heat treatment	B _10kA/m	Hc [A/m]	ρ [μΩm]	1T, 400Hz[W/kg] time core loss	The present invention	530 ℃, 30 minutes, air	1.65	192	103	41
The DWL method	Do not have	1.66	305	60	60	The present invention	530 ℃, 30 minutes, air	1.65	192	103	41
The DWL method	Do not have	1.66	305	60	60	The DWL method	530 ℃, 30 minutes, air	1.66	189	3	109

From table 18 and Fig. 1, as can be seen, compare, because lower H with the DWL method _cWith higher resistivity, the present invention produces obviously lower core loss in alternating field.

Embodiment 9

In this embodiment, demonstrate the ferrocart core that can obtain to have the excellent magnetic energy by the present invention.Also demonstrate of the positive impact of the punch die temperature of rising to maximum relative permeability.

With " slightly " powder of embodiment 3 and the mix lubricant of different content and type.Make ring-type sample (OD=55, ID=45, h=5 millimeter) and strip sample (30 * 12 * 6 millimeters) with the process conditions that provide in the table 19.

Measure density by quality and the size of measuring the ring-type sample.By 4 methods measured resistivity on the ring-type sample.In the Brockhaus hysteresisgraph, carry out before the magnetic measurement, ring-type sample rotation 100drive is changeed and the 100sense commentaries on classics.From the loop, obtain μ with 10kA/m _MaxAnd H _cAnd so on the DC performance, simultaneously measure core loss with 1T and 400Hz.On test-strips, measure the cross-breaking strength (TRS) of heat treated parts by three-point bending method.

Table 19: the process conditions of ring-shaped sample

Sample	Lubricant type	Amounts of lubrication (weight %)	Pressing pressure (MPa)	The punch die temperature (℃)	Heat treatment
Sample	Lubricant type	Amounts of lubrication (weight %)	Pressing pressure (MPa)	The punch die temperature (℃)	Heat treatment	1	Stearmide	0.2	1100	25	300 ℃, 45 minutes, air+520 ℃ ^＊, air
2	Stearmide	0.2	1100	80	300 ℃, 45 minutes, air+520 ℃ ^＊, air	1	Stearmide	0.2	1100	25	300 ℃, 45 minutes, air+520 ℃ ^＊, air
2	Stearmide	0.2	1100	80	300 ℃, 45 minutes, air+520 ℃ ^＊, air	3	Stearmide	0.2	800	80	530 ℃, 30 minutes, air
4	Stearmide	0.2	1100	25	530 ℃, 30 minutes, air	3	Stearmide	0.2	800	80	530 ℃, 30 minutes, air
4	Stearmide	0.2	1100	25	530 ℃, 30 minutes, air	5	Stearmide	0.2	1100	80	530 ℃, 30 minutes, air
6	Stearmide	0.1	1100	85	530 ℃, 30 minutes, air	5	Stearmide	0.2	1100	80	530 ℃, 30 minutes, air
6	Stearmide	0.1	1100	85	530 ℃, 30 minutes, air	7	Stearmide	0.3	800	25	300 ℃, 1 hour, air+530 ℃, 30 minutes, air
8	Stearmide	0.3	800	80	300 ℃, 1 hour, air+530 ℃, 30 minutes, air	7	Stearmide	0.3	800	25	300 ℃, 1 hour, air+530 ℃, 30 minutes, air
8	Stearmide	0.3	800	80	300 ℃, 1 hour, air+530 ℃, 30 minutes, air	9	Stearmide	0.3	1100	25	300 ℃, 1 hour, air+530 ℃, 30 minutes, air
10	Stearmide	0.3	1100	80	300 ℃, 1 hour, air+530 ℃, 30 minutes, air	9	Stearmide	0.3	1100	25	300 ℃, 1 hour, air+530 ℃, 30 minutes, air
10	Stearmide	0.3	1100	80	300 ℃, 1 hour, air+530 ℃, 30 minutes, air	11	Erucyl amide	0.2	1100	25	330 ℃, 2 hours, air+530 ℃, 30 minutes, air
12	Erucyl amide	0.2	1100	25	340 ℃, 2 hours, N ₂+ 530 ℃, 30 minutes, air	11	Erucyl amide	0.2	1100	25	330 ℃, 2 hours, air+530 ℃, 30 minutes, air

^*In element, improve temperature to 520 ℃ with about 4 ℃/minute

Table 20: the measurement of element function

Sample	Density (gram/cubic centimetre)	μ _max	Hc (A/m)	Resistivity (μ Ohm*m)	Core loss under 1T400Hz (W/kg)	TRS (MPa)
Sample	Density (gram/cubic centimetre)	μ _max	Hc (A/m)	Resistivity (μ Ohm*m)	Core loss under 1T400Hz (W/kg)	TRS (MPa)	1	7.62	754	209	473	42	93
2	7.63	852	204	230	40	97	1	7.62	754	209	473	42	93
2	7.63	852	204	230	40	97	3	7.60	718	208	103	43	n.a
4	7.62	602	198	591	39	59	3	7.60	718	208	103	43	n.a
4	7.62	602	198	591	39	59	5	7.65	861	178	98	37	68
6	7.71	918	177	66	38	78	5	7.65	861	178	98	37	68
6	7.71	918	177	66	38	78	7	7.49	669	228	574	46	70
8	7.53	880	202	33	48	81	7	7.49	669	228	574	46	70
8	7.53	880	202	33	48	81	9	7.56	672	224	515	44	67
10	7.62	860	203	64	43	76	9	7.56	672	224	515	44	67
10	7.62	860	203	64	43	76	11	7.62	633	192	414	38	54
12	7.68	738	205	614	39	67	11	7.62	633	192	414	38	54

Claims

1. powder composition, it comprises the soft magnetic material particle of iron or iron-based powder and the lubricant of 0.05 to 2 weight %, the soft magnetic material particle of described iron or iron-based powder has electric insulation layer, and described lubricant is selected from the primary amide of the saturated or unsaturated straight chain fatty acid that contains 12-24 carbon atom.

2. according to the composition of claim 1, wherein aliphatic acid contains 14-22 carbon atom.

3. according to the composition of claim 1, it is characterized in that described primary amide is selected from the group of being made up of stearic amide, oleamide, docosanoic acid acid amides, erucyl amide and palmitamide.

4. according to the composition of claim 1, it further comprises polyphenylene sulfide.

5. according to the composition of claim 4, wherein the consumption of polyphenylene sulfide is 0.05-2.0 weight %.

6. according to the composition of claim 3, the amount of wherein said primary amide is 0.05 to 1 weight %.

7. according to the composition of claim 1, wherein electric insulation layer is made by inorganic material.

8. according to the composition of claim 1, wherein iron or iron-based powder are made of the iron of substantially pure.

9. according to the composition of claim 1, the soft magnetic material particle that wherein is less than the described iron of 10 weight % or iron-based powder has the granularity less than 45 microns.

10. according to the composition of claim 9, the soft magnetic material particle that wherein is less than the described iron of 5 weight % or iron-based powder has the granularity less than 45 microns.

11. a method of making soft magnetic components comprises the following steps:

A) with the mix lubricant of soft magnet or iron-based powder and 0.05 to 2 weight %, wherein the particle of soft magnet or iron-based powder is surrounded by electric insulation layer, and described lubricant is selected from the primary amide of the saturated or unsaturated straight chain fatty acid that contains 12-24 carbon atom,

B) compacting said composition, and

C) the gained element is heat-treated, or the gained element is not heat-treated.

12. according to the method for claim 11, wherein compacting is carried out at elevated temperatures.

13., wherein suppress being higher than under the pressing pressure of 800MPa according to the method for claim 11.

14. according to the method for claim 11, wherein heat treatment is carried out at 250 ℃ to 550 ℃.

15. according to the method for claim 14, wherein heat-treat at the highest 350 ℃ earlier, heat-treat at the highest 550 ℃ then.

16. according to the method for claim 11, wherein heat treatment is carried out in air or inert atmosphere.

17. soft magnetic composite component, it comprises the composition of the lubricant of iron-based insulating powder and 0.05 to 2 weight %, then the element of compacting is heat-treated and obtained by compacting, wherein said lubricant is selected from the primary amide of the saturated or unsaturated straight chain fatty acid that contains 12-24 carbon atom, this soft magnetic composite component:

Density 〉=7.5 gram/cubic centimetres,

Maximum relative permeability μ max 〉=600,

Coercivity H≤250A/m

Electricalresistivity 〉=20 μ Ω m.

18. according to the soft magnetic composite component of claim 17, its density 〉=7.6 gram/cubic centimetres.

19. according to the soft magnetic composite component of claim 17, its maximum relative permeability μ max 〉=700.

20. according to each soft magnetic composite component of claim 17 to 19, its electricalresistivity 〉=100 μ Ω m.