CN104325133B - Nanometer iron powder sintered body containing nano ferriferrous oxide and preparation method thereof - Google Patents
Nanometer iron powder sintered body containing nano ferriferrous oxide and preparation method thereof Download PDFInfo
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- CN104325133B CN104325133B CN201410646653.7A CN201410646653A CN104325133B CN 104325133 B CN104325133 B CN 104325133B CN 201410646653 A CN201410646653 A CN 201410646653A CN 104325133 B CN104325133 B CN 104325133B
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Abstract
The invention discloses a kind of nanometer iron powder sintered body containing nano ferriferrous oxide and preparation method thereof.Nanometer iron powder sintered body is formed by following preparation of raw material by mass percentage: nano ferriferrous oxide powder 80~100%, additive powder 0~20%, described additive powder is containing a kind of powder in C, Al, Si, Mn, Sn, Ni, Co, Cr, Mo, Cu, Nb element or two kinds and two or more composite powders.Its preparation method is, is sufficiently mixed by raw material, then carries out molding, isostatic pressed or vibration moulding, finally in the mixed atmosphere of high-purity hydrogen or high-purity hydrogen and nitrogen, is sintered at 850~1200 DEG C, is incubated 30~300 minutes.Present invention process is simple, realizes the sintering of quick ferrum system composite powder, can manufacture antifriction alloy, high temperature alloy, silicon steel, automobile high-strength parts and other steel for special purposes products, low production cost under relatively low low temperature.
Description
Technical field
The present invention relates to nanometer iron powder sintered body, contain nanometer four in particular to one and aoxidize three
Nanometer iron powder sintered body of ferrum and preparation method thereof.
Background technology
In field of powder metallurgy, metal powder is pressurizeed in metal pattern, after molding, enters
The sintered body that row sinters and makes, can manufacture the Machinery Ministry of complicated shape well with precision
Part.Therefore, require the automobile component of high dimensional accuracy, antifriction alloy, high temperature alloy with
And in the manufacture of other specific use parts, sintered body can be applied widely.
The Chinese invention patent of Publication No. CN101772389A discloses " powder used in metallurgy
Ferrum system mixed-powder and iron powder sintering body ", it is with containing iron-based powder, graphite powder, copper powder
It is raw material with composite oxides, sinters 1000 DEG C of implemented below.Publication No.
The Chinese invention patent of CN101733400A disclose " high-strength composition iron powder and use it
Sintered component ", be with iron powder primary raw material, add a certain amount of Mn, Fe-Mn (grain
Less than 45 microns of footpath), Cu and powdered graphite, more than the fusing point of Cu, 1300 DEG C with
Sintering is realized in lower temperature range.The Chinese utility model of Publication No. CN201141401Y
Patent disclosure " bimetallic bearing of a kind of copper-clad iron powder sintering ", on the surface of steel plate
Upper sintering has the wearing layer of copper-clad iron powder, forms the composite of stacking, and uses this composite wood
Material makes axle sleeve or flat board, and sintering has the rubbing surface that surface is bearing of copper-clad iron powder.
In sum, the research of ferrum system composite powder sintered body, it is concentrated mainly on employing fusing point
Relatively low copper powder is as sintering aid aspect, it is impossible to meet high intensity parts and its
The use of his steel for special purposes product needs.
Summary of the invention
Present invention aim to the deficiency overcome existing for prior art, it is provided that Yi Zhongna
Nanometer iron powder sintered body of meter Han You nano ferriferrous oxide and preparation method thereof.
The fusing point of general material is, under a certain pressure, the solid-state of pure material and liquid are in flat
Temperature during weighing apparatus, say, that under this pressure and melting temperature, pure material is solid-state
Chemical potential and the chemical potential being in a liquid state are equal.For block pure object, its chemical potential is simply
The function of temperature and pressure.
And nano-particle is little due to particle diameter, specific surface free energy is high, therefore its chemical potential ratio is identical
Under the conditions of blocks of solid much higher, result cause its fusing point and sintering temperature be significantly less than with
The blocks of solid of sample material, and the particle diameter of granule is the least, its fusing point and sintering temperature are the lowest.
Such as, the fusing point of bulk Pb is 600K, and the fusing point of 20 nanometer spherical Pb granules reduces
288K, and nano-Ag particles is starting fusing less than 373K, and the fusing point of conventional Ag is high
Reach 1273K.
We are found by experimental study, when the particle diameter of nanometer iron powder is less than 100 nanometer,
Its fusing point can reduce, meanwhile, high-purity hydrogen or high-purity hydrogen and the spy of nitrogen mixture atmosphere
Under the conditions of Shu, after metal-oxide is reduced into simple substance granule, its activity is higher, it is easier to it
His metal or oxide reaction, sintering.Utilize this principle to design, produce multiple gold
Belong to sintered powder, to meet high intensity parts and the use of other steel for special purposes products
Need.
For achieving the above object, the nanometer containing nano ferriferrous oxide designed by the present invention
Iron powder sintering body, it forms by following preparation of raw material by mass percentage: nanometer four aoxidizes
Three iron powder 80~100%, additive powder 0~20%, described additive powder is for containing
A kind of powder in C, Al, Si, Mn, Sn, Ni, Co, Cr, Mo, Cu, Nb element
End or two kinds and two or more composite powders.
Preferably, the nanometer iron powder sintered body containing nano ferriferrous oxide by following by quality
The preparation of raw material of percentage ratio forms: nano ferriferrous oxide powder 90~95%, graphite powder
0.05~0.5%, Al powder 1.0~5.0%, Si powder 1.0~5.0%, Mn powder 1.0~4.5%.
Preferably, the nanometer iron powder sintered body containing nano ferriferrous oxide by following by quality
The preparation of raw material of percentage ratio forms: nano ferriferrous oxide powder 80~95%, Ni powder 5~
20%, Co powder 0~10%.
Preferably, the nanometer iron powder sintered body containing nano ferriferrous oxide by following by quality
The preparation of raw material of percentage ratio forms: nano ferriferrous oxide powder 80~90%, Ni powder 5~
15%, Cr powder 5~15%, Mn powder 0~5%.
Preferably, the nanometer iron powder sintered body containing nano ferriferrous oxide by following by quality
The preparation of raw material of percentage ratio forms: nano ferriferrous oxide powder 90~95%, Al powder 1.0~
1.5%, Si powder 2.0~5.0%, Mn powder 1.0~3.5%, Sn powder 0.1~1.0%, Cu
Powder 0.2~0.8%.
Preferably, the nanometer iron powder sintered body containing nano ferriferrous oxide by following by quality
The preparation of raw material of percentage ratio forms: nano ferriferrous oxide powder 80~90%, graphite powder
0.1~0.5%, Mn powder 1.0~3.5%, Cr powder 5~15%, Mo powder 2~8%.
In the present invention, the mean diameter of described nano ferriferrous oxide powder is less than 80 nanometers,
Purity more than 98%.The mean diameter of described additive powder is less than 10 microns, purity 99%
Above.
The preparation method of the above-mentioned nanometer iron powder sintered body containing nano ferriferrous oxide: first
Raw material is sufficiently mixed, then carries out molding, isostatic pressed or vibration moulding, finally high-purity
In the mixed atmosphere of hydrogen or high-purity hydrogen and nitrogen, at sintering temperature 850~1200 DEG C
It is sintered, is incubated 30~300 minutes.
In the mixed atmosphere of the present invention, hydrogen volume percent concentration is 20~99%, nitrogen
Concentration of volume percent is 1~80%.
Found by experimental study, when the particle diameter of nano ferriferrous oxide powder is received less than 80
Meter Shi, its fusing point can reduce, meanwhile, in high-purity hydrogen or high-purity hydrogen and the mixing of nitrogen
Under the specific condition of atmosphere, nano ferriferrous oxide powder reduction become fe after its activity relatively
, even there is liquid phase in height, it is easier to reacts with other metals or oxide, sinters, profit
Can design by this principle, produce various metals sintered powder.
The beneficial effects of the present invention is: use technique scheme, present invention process is simple,
Under relatively low low temperature, realize the sintering of quick ferrum system composite powder, antifriction alloy, height can be manufactured
Temperature alloy, silicon steel, automobile high-strength parts and other steel for special purposes products, produce
With low cost.
Detailed description of the invention
In order to preferably explain the present invention, below in conjunction with specific embodiment, the present invention is made into one
The detailed description of step, but they do not constitute restriction to the present invention.
Embodiment 1
The composition of raw materials of the nanometer iron powder sintered body containing nano ferriferrous oxide, by quality hundred
Proportion by subtraction is: nano ferriferrous oxide powder 89.5%, additive powder 10.5%;Wherein,
Additive powder is graphite powder 0.5%, Al powder 1.5%, Si powder 5.0%, Mn powder 3.5%.
Preparation method: first nano ferriferrous oxide powder and additive powder are carried out fully
Mixing, then carries out compression molding, finally in high-purity hydrogen atmosphere, in sintering temperature 900
It is sintered at DEG C, temperature retention time 120 minutes.
Embodiment 2
The composition of raw materials of the nanometer iron powder sintered body containing nano ferriferrous oxide, by quality hundred
Proportion by subtraction is: nano ferriferrous oxide powder 95%, additive powder 5%;Wherein, add
Thing powder is graphite powder 0.1%, Al powder 2.0%, Si powder 1.4%, Mn powder 1.5%.
Preparation method: first nano ferriferrous oxide powder and additive powder are carried out fully
Mixing, then carries out compression molding, finally in high-purity hydrogen atmosphere, in sintering temperature 950
It is sintered at DEG C, temperature retention time 30 minutes.
Embodiment 3
The composition of raw materials of the nanometer iron powder sintered body containing nano ferriferrous oxide, by quality hundred
Proportion by subtraction is: nano ferriferrous oxide powder 94%, additive powder 6%;Wherein, add
Thing powder is graphite powder 0.3%, Al powder 1.5%, Si powder 2.2%, Mn powder 2.0%.
Preparation method: first nano ferriferrous oxide powder and additive powder are carried out fully
Mixing, then carries out compression molding, finally in high-purity hydrogen and nitrogen mixture atmosphere, and hydrogen
Air volume percent concentration is 90%, and nitrogen concentration of volume percent is 10%, in sintering temperature
It is sintered at spending 900 DEG C, temperature retention time 30 minutes.
Embodiment 4
The raw material of the nanometer iron powder sintered body containing nano ferriferrous oxide is 100% nanometer four
Fe 3 O powder.
Preparation method: nano ferriferrous oxide powder is carried out compression molding, at high-purity hydrogen
In atmosphere, it is sintered at sintering temperature 850 DEG C, temperature retention time 120 minutes.
Embodiment 5
The raw material of the nanometer iron powder sintered body containing nano ferriferrous oxide is 100% nanometer four
Fe 3 O powder.
Preparation method: nano ferriferrous oxide powder is carried out compression molding, at high-purity hydrogen
With in nitrogen mixture atmosphere, hydrogen volume percent concentration is 70%, nitrogen percent by volume
Concentration is 30%, is sintered at sintering temperature 900 DEG C, temperature retention time 120 minutes.
Embodiment 6
The composition of raw materials of the nanometer iron powder sintered body containing nano ferriferrous oxide, by quality hundred
Proportion by subtraction is: nano ferriferrous oxide powder 85%, additive powder 15%;Wherein, add
Thing powder is Ni powder 5%, Co powder 10%.
Preparation method: first nano ferriferrous oxide powder and additive powder are carried out fully
Mixing, then carries out vibration moulding, finally in high-purity hydrogen, in sintering temperature 1000
It is sintered at DEG C, temperature retention time 300 minutes.
Embodiment 7
The composition of raw materials of the nanometer iron powder sintered body containing nano ferriferrous oxide, by quality hundred
Proportion by subtraction is: nano ferriferrous oxide powder 80%, additive powder 20%;Wherein, add
Thing powder is Ni powder 20%.
Preparation method: first nano ferriferrous oxide powder and additive powder are carried out fully
Mixing, then carries out isostatic pressing, finally in high-purity hydrogen, in sintering temperature 1050
It is sintered at DEG C, temperature retention time 120 minutes.
Embodiment 8
The composition of raw materials of the nanometer iron powder sintered body containing nano ferriferrous oxide, by quality hundred
Proportion by subtraction is: nano ferriferrous oxide powder 80%, additive powder 20%;Wherein, add
Thing powder is Ni powder 10%, Co powder 10%.
Preparation method: first nano ferriferrous oxide powder and additive powder are carried out fully
Mixing, then carries out compression molding, finally in high-purity hydrogen and nitrogen mixture atmosphere, and hydrogen
Air volume percent concentration is 50%, and nitrogen concentration of volume percent is 50%, in sintering temperature
It is sintered at spending 1100 DEG C, temperature retention time 60 minutes.
Embodiment 9
The composition of raw materials of the nanometer iron powder sintered body containing nano ferriferrous oxide, by quality hundred
Proportion by subtraction is: nano ferriferrous oxide powder 80%, additive powder 20%;Wherein, add
Thing powder is Ni powder 15%, Cr powder 5%, Mn powder 5%.
Preparation method: first nano ferriferrous oxide powder and additive powder are carried out fully
Mixing, then carries out compression molding, finally in high-purity hydrogen atmosphere, in sintering temperature 1050
It is sintered at DEG C, temperature retention time 120 minutes.
Embodiment 10
The composition of raw materials of the nanometer iron powder sintered body containing nano ferriferrous oxide, by quality hundred
Proportion by subtraction is: nano ferriferrous oxide powder 80%, additive powder 20%;Wherein, add
Thing powder is Ni powder 5%, Cr powder 15%.
Preparation method: first nano ferriferrous oxide powder and additive powder are carried out fully
Mixing, then carries out vibration moulding, in high-purity hydrogen and nitrogen mixture atmosphere, and hydrogen
Long-pending percent concentration is 40%, and nitrogen concentration of volume percent is 60%, in sintering temperature
It is sintered at 1100 DEG C, is incubated 60 minutes.
Embodiment 11
The composition of raw materials of the nanometer iron powder sintered body containing nano ferriferrous oxide, by quality hundred
Proportion by subtraction is: nano ferriferrous oxide powder 95%, additive powder 5%;Wherein, add
Thing powder is Al powder 1.0%, Si powder 2.0%, Mn powder 1.0%, Sn powder 0.6%, Cu
Powder 0.4%.
Preparation method: first nano ferriferrous oxide powder and additive powder are carried out fully
Mixing, then carries out compression molding, finally in high-purity hydrogen atmosphere, in sintering temperature 1150
It is sintered at DEG C, temperature retention time 60 minutes.
Embodiment 12
The composition of raw materials of the nanometer iron powder sintered body containing nano ferriferrous oxide, by quality hundred
Proportion by subtraction is: nano ferriferrous oxide powder 80%, additive powder 20%;Wherein, add
Thing powder is graphite powder 0.5%, Mn powder 2.5%, Cr powder 15%, Mo powder 2%.
Preparation method: first nano ferriferrous oxide powder is fully mixed with additive powder
Close, then carry out compression molding, finally in high-purity hydrogen atmosphere, in sintering temperature 1050
It is sintered at DEG C, temperature retention time 120 minutes.
Claims (4)
1. the nanometer iron powder sintered body containing nano ferriferrous oxide, it is characterised in that
It is formed by following preparation of raw material by mass percentage:
Nano ferriferrous oxide powder 90~95%, graphite powder 0.05~0.5%, Al powder 1.0~
5.0%, Si powder 1.0~5.0%, Mn powder 1.0~4.5%;
Or, nano ferriferrous oxide powder 80~95%, Ni powder 5~20%, Co powder 0~
10%;
Or, nano ferriferrous oxide powder 80~90%, Ni powder 5~15%, Cr powder 5~
15%, Mn powder 0~5%;
Or, nano ferriferrous oxide powder 90~95%, Al powder 1.0~1.5%, Si powder 2.0~
5.0%, Mn powder 1.0~3.5%, Sn powder 0.1~1.0%, Cu powder 0.2~0.8%;
Or, nano ferriferrous oxide powder 80~90%, graphite powder 0.1~0.5%, Mn
Powder 1.0~3.5%, Cr powder 5~15%, Mo powder 2~8%.
Nanometer iron powder containing nano ferriferrous oxide the most according to claim 1 burns
Knot body, it is characterised in that: the mean diameter of described nano ferriferrous oxide powder is less than 80
Nanometer, purity more than 98%.
3. the Nanoscale Iron containing nano ferriferrous oxide according to claim 1
The preparation method of compact, it is characterised in that: first raw material is sufficiently mixed, then enters
Row molds, isostatic pressed or vibration moulding, finally at high-purity hydrogen or high-purity hydrogen and nitrogen
In mixed atmosphere, it is sintered at sintering temperature 850~1200 DEG C, is incubated 30~300
Minute.
Nanometer iron powder containing nano ferriferrous oxide the most according to claim 3 burns
The preparation method of knot body, it is characterised in that: in described mixed atmosphere, hydrogen volume percentage ratio
Concentration is 20~99%, and nitrogen concentration of volume percent is 1~80%.
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CN1057800A (en) * | 1991-07-08 | 1992-01-15 | 孔凯旋 | Spongy iron heat diffusion body and manufacture method thereof |
CN1532965A (en) * | 2003-03-25 | 2004-09-29 | 勇 张 | Activated iron electrode |
CN101246773A (en) * | 2007-02-12 | 2008-08-20 | 北京有色金属研究总院 | High-efficiency soft magnetic material and method for producing the same |
CN101772389A (en) * | 2007-08-03 | 2010-07-07 | 株式会社神户制钢所 | Powder used in metallurgy iron is mixed-powder and iron powder sintered body |
CN102603198A (en) * | 2012-03-07 | 2012-07-25 | 南京工业大学 | Inorganic electromagnetic-wave absorbing material and preparation method thereof |
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2014
- 2014-11-14 CN CN201410646653.7A patent/CN104325133B/en active Active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1057800A (en) * | 1991-07-08 | 1992-01-15 | 孔凯旋 | Spongy iron heat diffusion body and manufacture method thereof |
CN1532965A (en) * | 2003-03-25 | 2004-09-29 | 勇 张 | Activated iron electrode |
CN101246773A (en) * | 2007-02-12 | 2008-08-20 | 北京有色金属研究总院 | High-efficiency soft magnetic material and method for producing the same |
CN101772389A (en) * | 2007-08-03 | 2010-07-07 | 株式会社神户制钢所 | Powder used in metallurgy iron is mixed-powder and iron powder sintered body |
CN102603198A (en) * | 2012-03-07 | 2012-07-25 | 南京工业大学 | Inorganic electromagnetic-wave absorbing material and preparation method thereof |
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