CN1450573A - Method for preparing composite nano crystal magnetic recording material - Google Patents
Method for preparing composite nano crystal magnetic recording material Download PDFInfo
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- CN1450573A CN1450573A CN 03116544 CN03116544A CN1450573A CN 1450573 A CN1450573 A CN 1450573A CN 03116544 CN03116544 CN 03116544 CN 03116544 A CN03116544 A CN 03116544A CN 1450573 A CN1450573 A CN 1450573A
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Abstract
This invention relates to a process method for a compound nanometer crystal magnetic recording material characterizing in applying a mechanical alloying method to synthesize pure Fe powder and pure carbon powder into Fe-C compound under constant temperature and pressure then to synthesize Fe-C nm crystal with nm crystal soft magnetic powder into two-phase compound nm crystal magnet recording material with good magnetism, capable of becoming magnetic recording medium better that r-Fe2O3 or magnetized powder adhering magnetic not needing strict conditions of high temperature high pressure and special environment.
Description
Technical field
The present invention relates to a kind of preparation method of composite nanocrystalline magnetic recording material, belong to the magnetic material manufacturing process technology field.
Background technology
The Fe-C based compound has certain advantage in the magnetic material, and at first it has higher saturation magnetic moment σ s=110em μ/g-140em μ/g, and higher coercivity Hc=400-800oe, and these indexs substantially exceed the γ-Fe of existing market supply
2O
3Powder (σ s=70em μ/g, Hc=340oe).It is oxidized that next is that it is difficult for.Though metal iron powder has high saturation magnetic moment σ s=200em μ/g), but its chemical stability is very poor, the surface can generate the very low FeO of σ s in air.The Fe-N alloy also has high saturation and magnetic intensity, and (σ s=190em μ/g), though better than the chemical stability of metal Fe powder, it still can generate the low oxide of σ s on the surface.Therefore the Fe-C system that is difficult for oxidation has than γ-Fe
2O
3Much higher σ s, Hc; Having again than metal iron powder and Fe-N is the good characteristics of chemical stability of alloy, so be a kind of good magnetic recording material.
But since two yuan of based compounds of Fe-C at room temperature Fe-C be immiscible, have the element of the positive heat of mixing, its heat of mixing is 20KJ/M
3Therefore at room temperature, they all are metastable state, to synthesize the uniformly single-phase Fe-C of getting (such as FeC, Fe
3C, Fe
5C
2, Fe
7C
3) be relatively more difficult.In the ordinary course of things, only could synthesize the Fe-C compound under high pressure 3-8Gpa, high temperature 1000-17000C and special atmosphere, this obviously needs higher cost.
Summary of the invention
The purpose of this invention is to provide a kind of mechanical alloying method, at normal temperatures and pressures, produce Fe-C compound and other soft magnet powder chemical combination, generate the composite nanocrystalline magnetic material by certain process.
The preparation method of composite nanocrystalline magnetic recording material of the present invention, it is characterized in that adopting the mechanical alloying method, at normal temperatures and pressures by certain technical process, with original material straight iron powder and the synthetic Fe-C compound of pure carbon powder, with nano-crystalline Fe-C and the synthetic two-phase composite nanocrystalline magnetic recording material of nano-crystal soft-magnetic powdered, its concrete steps are as follows then:
A. raw material are prepared: with putting into the stainless steel jar mill that cleans up after the pure α-Fe powder of certain atomic percent and the graphite C powder;
B. prepare nano-crystalline Fe-C compound powder with high-energy ball milling: by suitable ball powder weight ratio, stainless steel ball not of uniform size is put into ball grinder, and enclose argon gas, with suitable drum's speed of rotation, suitable Ball-milling Time, carry out ball milling, rotating is alternate in the mechanical milling process, finally forms Fe
5C
2Intermetallic compound, its average crystal grain size is 10nm; Take out then Fe
5C
2Compound and purifying 1-2 hour;
C. prepare the nano-crystal soft-magnetic powder with high-energy ball milling: with soft magnetic material α-Fe powder, or Fe-Ni powder or Fe-Co powder grind to form and have crystallite dimension and be the solid solution superfines less than 10nm;
D. prepare the composite nanocrystalline superfines: further mixed nano-crystal Fe
5C
2Compound and α-Fe powder, or Fe-Ni solid-solution powder or Fe-Co solid-solution powder; By suitable ball powder weight ratio, suitable drum's speed of rotation, suitable Ball-milling Time is proceeded ball milling, makes two-phase composite nanocrystalline superfines, i.e. Fe
5C
2/ α-Fe powder;
E. heat treatment: vacuum annealing is carried out in the two-phase composite nanocrystalline magnetic powder of the prepared one-tenth back of sieving under 100-350 ℃ of temperature, annealing time is 30-60 minute, finally makes two-phase composite nanocrystalline magnetic recording material.
In the process of the compound two-phase nanocrystalline magnetic of preparation, if when the amount of soft magnetic powder solid solution FeNi, FeCo is less, the final compound two-phase nanocrystalline magnetic that forms all is Fe
5C
2/ α-Fe powder after heat treatment, forms two-phase composite nanocrystalline Fe
5C
2/ α-Fe magnetic recording material.
The advantage of the inventive method is: prepare the Fe-C magnetic compound with the mechanical alloying method at normal temperatures and pressures owing to adopt, compare with traditional molten alloy, the inventive method has the continuous adjustability of operation composition, can realize alloying to those systems that can not dissolve each other or difficult system of dissolving each other, Jie that originally need could synthesize under high pressure and hot conditions surely is on good terms to be generated at normal temperatures and pressures, therefore it is simple to have preparation technology, the characteristics that can reduce cost.
Embodiment
Embodiment one:
(1) be that drop in the stainless steel jar mill that cleans up 99.8% Fe powder, 99.85% graphite C powder mixing back with purity, Fe is 1: 1 with the atomic percentage ratio of C.
(2) ball powder weight ratio is 25: 1, and stainless steel ball not of uniform size is put into ball grinder and enclosed argon gas, and drum's speed of rotation is 200 rev/mins, and the ball milling time is 255 hours, and in mechanical milling process, rotating is carried out separately.The main Fe of final formation
5C
2Compound between compound metal, its average crystal grain size is 10nm;
(3) in being filled with the glove box of argon gas with single-phase Fe
5C
2Compound powder takes out and purifying 1-2 hour;
(4) sieve with 200-300 purpose mesh screen;
(5) with the Fe that makes
5C
2Carry out vacuum annealing under 300 ℃ of temperature of single-phase magnetic, annealing time is 60 minutes.The Fe that finally obtains
5C
2The magnetic of single-phase magnetic is as shown in the table:
Table 1 Fe
5C
2The magnetic of single-phase composite magnetic powder
Embodiment two:
| Fe 5C 2 | Saturation magnetization σ s (em μ/g) | Coercivity Hc (oe) |
| The preparation attitude | 87.9 | 339 |
| 200 ℃ of annealed state | 92.5 | 434 |
(1) be that drop in the stainless steel jar mill that cleans up 99.8% Fe powder, 99.85% graphite C powder mixing back with purity, Fe is 1: 1 with the atomic percentage ratio of C.
(2) ball powder weight ratio is 25: 1, and stainless steel ball not of uniform size is put into ball grinder and enclosed argon gas, and drum's speed of rotation is 200 rev/mins, and the ball milling time is 255 hours, and in mechanical milling process, rotating is carried out separately.The final Fe that forms
5C
2Intermetallic compound, its average crystal grain size is 10nm;
(3) nanocrystalline solid solution superfines is made with soft magnetic material Fe-Ni powder in same step (1) and (2), and its crystallite dimension is less than 10nm;
(4) mixed nano-crystal Fe
5C
2Compound and Fe-Ni solid-solution powder, its Fe
5C
2The atomic percent of compound and Fe-Ni is 96: 4, i.e. [(Fe
5C
2)
96(Fe-Ni)
4]; Same step (1) and (2) can be made into Fe
5C
2/ α-Fe two-phase composite magnetic powder;
(5) in being filled with the glove box of argon gas, with Fe
5C
2/ α-Fe two-phase composite magnetic powder takes out, and purifying 1-2 hour;
(6) sieve with 200-300 purpose mesh screen;
(7) with the Fe that makes
5C
2Carry out vacuum annealing under/α-300 ℃ of temperature of Fe two-phase composite magnetic powder, annealing time is 60 minutes.The Fe that finally makes
5C
2The magnetic of/α-Fe two-phase composite magnetic powder is as shown in the table:
Table 1 Fe
5C
2The magnetic of/α-Fe two-phase composite magnetic powder
| Fe 5C 2/ α-Fe | Saturation magnetization σ s (em μ/g) | Coercivity Hc (oe) |
| The preparation attitude | 99.5 | 260 |
| 300 ℃ of annealed state | 99.7 | 368 |
In the inventive method, namely in above-described embodiment, the purpose of its annealing process is the internal stress that produces because of ball milling in order to eliminate on the one hand, in order to make material grains more even, more complete, further improves magnetism of material and stability on the other hand.
The inventive method also can be produced other two-phase composite nanocrystalline magnetic material by above-mentioned same step and method, comprises Fe-C based compound: FeC, Fe3C, Fe7C2; Soft magnet powder has: α-Fe powder, Fe-Ni solid-solution powder, Fe-Co solid-solution powder.For example can prepare Fe
5C
2/ α-Fe, Fe
5C
2/ (Fe-Co), Fe
3C/ (Fe-Ni), Fe
3Two composite nanocrystalline Fe of the composition proportion such as C/ (Fe-Co)
5C
2/ α-Fe magnetic material.
Claims (1)
1. the preparation method of a composite nanocrystalline magnetic recording material, it is characterized in that adopting the mechanical alloying method, at normal temperatures and pressures by certain technical process, with original material straight iron powder and the synthetic Fe-C compound of pure carbon powder, with nano-crystalline Fe-C and the synthetic two-phase composite nanocrystalline magnetic recording material of nano-crystal soft-magnetic powdered, its concrete steps are as follows then:
A. raw material are prepared: with putting into the stainless steel jar mill that cleans up after the pure α-Fe powder of certain atomic percent and the graphite C powder;
B. prepare nano-crystalline Fe-C compound powder with high-energy ball milling: by suitable ball powder weight ratio, stainless steel ball not of uniform size is put into ball grinder, and enclose argon gas, with suitable drum's speed of rotation, suitable Ball-milling Time, carry out ball milling, rotating is alternate in the mechanical milling process, finally forms Fe
5C
2Intermetallic compound, its average crystal grain size is 10nm; Take out then Fe
5C
2Compound and purifying 1-2 hour;
C. prepare the nano-crystal soft-magnetic powder with high-energy ball milling: with soft magnetic material α-Fe powder, or Fe-Ni powder or Fe-Co powder grind to form and have crystallite dimension and be the solid solution superfines less than 10nm;
D. prepare the composite nanocrystalline superfines: further mixed nano-crystal Fe
5C
2Compound and α-Fe powder, or Fe-Ni solid-solution powder or Fe-Co solid-solution powder; By suitable ball powder weight ratio, suitable drum's speed of rotation, suitable Ball-milling Time is proceeded ball milling, makes two-phase composite nanocrystalline superfines, i.e. Fe
5C
2/ α-Fe powder;
E. heat treatment: vacuum annealing is carried out in the two-phase composite nanocrystalline magnetic powder of the prepared one-tenth back of sieving under 100-350 ℃ of temperature, annealing time is 30-60 minute, finally makes two-phase composite nanocrystalline magnetic recording material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03116544 CN1242433C (en) | 2003-04-22 | 2003-04-22 | Method for preparing composite nano crystal magnetic recording material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03116544 CN1242433C (en) | 2003-04-22 | 2003-04-22 | Method for preparing composite nano crystal magnetic recording material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1450573A true CN1450573A (en) | 2003-10-22 |
| CN1242433C CN1242433C (en) | 2006-02-15 |
Family
ID=28684199
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03116544 Expired - Fee Related CN1242433C (en) | 2003-04-22 | 2003-04-22 | Method for preparing composite nano crystal magnetic recording material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1242433C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1937121B (en) * | 2006-09-21 | 2010-04-14 | 上海大学 | Method for preparing complex-phase nano crystal permanent-magnet ferrite material |
| CN103030143A (en) * | 2012-08-09 | 2013-04-10 | 北京大学 | Iron carbide particle, and fabrication method and application thereof |
-
2003
- 2003-04-22 CN CN 03116544 patent/CN1242433C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1937121B (en) * | 2006-09-21 | 2010-04-14 | 上海大学 | Method for preparing complex-phase nano crystal permanent-magnet ferrite material |
| CN103030143A (en) * | 2012-08-09 | 2013-04-10 | 北京大学 | Iron carbide particle, and fabrication method and application thereof |
| CN103030143B (en) * | 2012-08-09 | 2015-02-18 | 北京大学 | Iron carbide particle, and fabrication method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1242433C (en) | 2006-02-15 |
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Granted publication date: 20060215 |