CN101593523A - A kind of L1 0The preparation method of type super-high density magnetic record metallic film - Google Patents
A kind of L1 0The preparation method of type super-high density magnetic record metallic film Download PDFInfo
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- CN101593523A CN101593523A CNA2008101137769A CN200810113776A CN101593523A CN 101593523 A CN101593523 A CN 101593523A CN A2008101137769 A CNA2008101137769 A CN A2008101137769A CN 200810113776 A CN200810113776 A CN 200810113776A CN 101593523 A CN101593523 A CN 101593523A
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Abstract
A kind of L1
0The preparation method of type super-high density magnetic record metallic film belongs to magnetic recording, storage and information reproduction record field.Preparation method's existence condition harshness of existing magnetic record metal thin film, to the equipment requirements height, problems such as production cost height.The present invention mainly contains the alloy firm of ferromagnetic metal A (Fe, Co or Ni) and noble metal B (Pt, Pd, Ag or Au) by the preparation of electrochemical co-deposition method, the atom content of control A is 50%, and The high temperature anneal obtains the superlattice structure (L1 of vertical direction
0Type) super-high density magnetic record metallic film.Prepared film of the present invention has the coercive force of monadic magnetocrystalline anisotropy (K), superelevation and good physical and chemical stability, has potential application prospect in microelectronics field of storage and super-high density magnetic recording material.
Description
Technical field
The invention belongs to magnetic recording, storage and information reproduction record field, be specifically related to a kind of L1
0The preparation method of type (superlattice structure) super-high density magnetic record metallic film.
Background technology
Along with progress of science and technology, the especially develop rapidly of information industry, communication industry, people are more and more higher for the magnetic recording property requirement of magnetic material, and much the magnetic recording property of traditional magnetic material can not satisfy the Time Technology demand for development.As everyone knows, in order to realize high density recording on recording medium, the diameter of the magnetic-particle in the recording sheet must reduce as far as possible, and zone between crystal grain is provided between those magnetic-particles, slackening intergranular magnetic coupling, thereby reduce the noise of this words information on sub-road.In addition, because the desired heat energy of reverse magnetization direction is directly proportional with the cube volume of each magnetic-particle, therefore, the magnetic-particle volume reduces, and its heat energy drag also decreases, and its recording density is restricted.
In order to satisfy the demand for development of current era, people expect to develop a kind of magnetic material with high magnetic recording property always.Since the nineties in 20th century, directly one of solution to the problems described above is to increase the magnetic anisotropy energy (Ku) that keeps the main body magnetic recording thin film of information along direction of magnetization.At present, people are devoted to research and develop the perpendicular magnetic recording method, replace the longitudinal magnetic recording method that present product was adopted with expectation.Superlattice film is owing to have big magnetic anisotropy energy, and the coercive force advantages of higher has become the focus of current research.Usually, superlattice film is to form laminated film by artificial alternately laminated two types film, and each in these two kinds of films all has the thickness of atomic size, and contains a kind of element that another kind of film contains that is different from.Communique JP-A67322/1993 discloses a kind of vertical magnetized film of the Co/Pt of employing superlattice film, and has proposed a kind of stacked circulation that reduces superlattice film, so that also can obtain the method for vertical magnetized film when ferromagnetism Co content is relatively very high in film.This superlattice film forms by using separate equipment to come vacuum moulding machine mainly to contain the material alternating deposit that Co or Fe etc. have ferromagnetic metal and contain noble metals such as Pt or Pd in the main body substrate respectively.In order to overcome this preparation method's mode of deposition harshness, the equipment requirements height, shortcomings such as production cost height, adopting the electrochemical deposition method preparation mainly to contain alloy firm that Co or Fe etc. have ferromagnetic metal and contain noble metals such as Pt or Pd becomes and solves one of important research direction of current increase magnetic recording density.
Summary of the invention
The object of the invention is to provide a kind of L1 in microelectronics field of storage and the super-high density magnetic recording material that is applied to
0The preparation method of type (superlattice structure) super-high density magnetic record metallic film.
The present invention utilizes the electrochemical co-deposition preparation mainly to contain the alloy firm of ferromagnetic metal A and noble metal B, and the atom content of control ferromagnetic metal is 50%, and The high temperature anneal obtains the superlattice structure (L1 of vertical direction
0Type) super-high density magnetic record metallic film.Concrete steps are as follows:
1) electrolyte solution of preparation two metal ion species:
1. the soluble-salt solution that with concentration is 0.01～0.5mol/l ferromagnetic metal A joins in the complexing agent solution that concentration is 0.03～3mol/l, the amount ratio of metal salt solution and complexing agent solution is 1: 1～3, obtain the complex solution of metal A, pH value with the ammoniacal liquor regulator solution is 6～10, the water-bath heating for dissolving;
2. the pH value that adds the ammoniacal liquor regulator solution in concentration is the soluble-salt solution of expensive metal B of 0.1～2.5mol/l is 6～10, the water-bath heating for dissolving;
1. and 2. 3. after two kinds of solution of preparation press the mol ratio mixing in 1: 1 of metal ion A and B with step, be 6～10, prepare the electrolyte solution that contains two metal ion species with the pH value of ammoniacal liquor regulator solution;
2) substrate is handled by electrochemical polish or chemically polishing surface;
3) will be through step 2) substrate handled is as negative electrode, platinum electrode as anode and direct supply and the electrolytic tank that contains the electrolyte solution that contains two metal ion species that step 1) makes in 3. form electro-deposition system;
4) electrodeposition process carries out under 25～90 ℃ constant temperature, adopts galvanostatic method, and current density is controlled at 10～100mA/cm
2, sedimentation time 1～10min;
5) sample that step 4) is made is in 600～800 ℃ of The high temperature anneal 3～5 hours, the L1 that obtains having vertical direction
0Type super-high density magnetic record metallic film.
Wherein, the ferromagnetic metal A of step 1) described in 1. is selected from Fe, Co or Ni; Described complexing agent is selected from ammonium tartrate, EDTA, succinic acid, malonic acid or citric acid; The noble metal B of step 1) described in 2. is selected from Pt, Pd, Ag or Au; Step 2) substrate described in is selected from Copper Foil, monocrystalline MgO sheet or monocrystalline silicon piece.Regulate the alloy firm that cathode-current density obtains containing different component in the step 4), the difference of component makes the structure difference of nanotube in the alloy.
Usually, electrochemical deposition method prepares alloy firm does not need high annealing can have higher coercive force and magnetic recording density.Yet, when by behind the The high temperature anneal alloy firm, realize the transformation of its face-centered cubic (fcc) to center of area four directions (fct) structure, make it have the superlattice structure (L1 of vertical direction
0Type), thus realize coercive force that it has monadic magnetocrystalline anisotropy (K), superelevation and good physical and chemical stability.These advantages make it have potential application prospect in microelectronics field of storage and super-high density magnetic recording material.
The present invention has the following advantages:
1. by preparation method of the present invention, conveniently, controllably prepare the superlattice structure (L1 of vertical direction
0Type) alloy firm of super-high density magnetic record bi-component, thereby realize coercive force that it has monadic magnetocrystalline anisotropy (K), superelevation and good physical and chemical stability, make it in microelectronics field of storage and super-high density magnetic recording material, have potential application prospect.
2. the present invention utilizes different complexing agents and metallic ion to form complex respectively, and it is close mutually to make that standard electrode potential differs the sedimentation potential of two metal ion species in solution of 1～1.4V, finally realizes the codeposition of metal alloy.
3. by changing the thickness of sedimentation time scalable emtal alloy film.In addition, by regulating the emtal alloy film that cathode-current density can obtain different component.
The invention will be further described below in conjunction with embodiment.
Embodiment
Embodiment 1
1) electrolyte solution of preparation two metal ion species:
1. the ammonium tartrate solution that adds the 0.03mol/l of 30ml in the beaker of 50ml is then with the CoCl of the 0.015mol/l of 10ml
2.6H
2O solution is poured in the ammonium tartrate solution, and 60 ℃ of stirring in water bath obtain the purple troubled liquor, splash into 5% ammoniacal liquor and make its dissolving, and the pH value of regulator solution is 9;
2. the 0.35mol/l H that in the beaker of 50ml, adds 10ml
2PtCl
6.6H
2O solution, 95 ℃ of heated and stirred obtain yellow-brownish solution to resolution of precipitate, and the pH value that splashes into 5% ammoniacal liquor regulator solution is 9;
3. with step 1. and 2. the solution of preparation mix, the pH value of the ammoniacal liquor regulator solution with 5% is 9;
2) the substrate monocrystalline silicon piece is handled by chemically polishing surface, and then the ion sputtering gilding layer is about 10m;
3) with step 2) substrate handled is as negative electrode, platinum electrode as anode and direct supply and the electrolytic tank that contains the electrolyte solution that 3. step 1) make form a cover electro-deposition system;
4) electrodeposition process carries out under 60 ℃ constant temperature, adopts galvanostatic method, and current density is controlled at 50mA/cm
2, sedimentation time 3min;
5) sample that step 4) is made obtains the superlattice structure (L1 of vertical direction 700 ℃ of The high temperature anneal 3.5 hours
0Type) super-high density magnetic record Co-Pt alloy firm.
Embodiment 2
1) electrolyte solution of preparation two metal ion species:
1. the ammonium tartrate solution that adds the 0.03mol/l of 10ml in the beaker of 50ml is then with the CoCl of the 0.015mol/l of 10ml
2.6H
2O solution is poured in the ammonium tartrate solution, and 60 ℃ of stirring in water bath obtain the purple troubled liquor, splash into 5% ammoniacal liquor and make its dissolving, and the pH value of regulator solution is 9;
2. add the 0.35mol/l dinitroso diammonia platinum solution of 10ml in the beaker of 50ml, 95 ℃ of heated and stirred obtain yellow-brownish solution to resolution of precipitate, and the pH value that splashes into 5% ammoniacal liquor regulator solution is 9;
3. with step 1. and 2. the solution of preparation mix, the pH value of the ammoniacal liquor regulator solution with 5% is 9;
2) copper clad laminate is passed through the electrochemical polish surface treatment;
3) with step 2) substrate handled is as negative electrode, platinum electrode as anode and direct supply and the electrolytic tank that contains the electrolyte solution that 3. step 1) make form a cover electro-deposition system;
4) electrodeposition process carries out under 80 ℃ constant temperature, adopts galvanostatic method, and current density is controlled at 80mA/cm
2, sedimentation time 1min;
5) sample that step 4) is made obtains the superlattice structure (L1 of vertical direction at 700 ℃ of The high temperature anneal 5h
0Type) super-high density magnetic record Co-Pt alloy firm.
Embodiment 3
1) electrolyte solution of preparation two metal ion species:
1. the ammonium tartrate solution that in the beaker of 50ml, adds the 0.1mol/l of 30ml, then the copperas solution of the 0.2mol/l of 10ml is poured in the ammonium tartrate solution, stirred, obtain faint yellow colloid, splash into strong aqua and make its dissolving, and the pH value of regulator solution is 8.5;
2. the citric acid solution that adds the 0.05mol/l of 30ml in the beaker of 50ml adds the 0.1mol/l palladium bichloride of 10ml then, and heated and stirred obtains yellow-brownish solution to resolution of precipitate, and the pH value of strong aqua regulator solution is 8.5;
3. with step 1. and 2. the solution of preparation mix, add the 0.5mol/l ammonium chloride solution of 10ml again, and be 8.5 with the pH value of strong aqua regulator solution;
2) monocrystalline MgO sheet is handled by chemically polishing surface, and then the ion sputtering gilding layer is about 10m;
3) with step 2) substrate handled is as negative electrode, platinum electrode as anode and direct supply and the electrolytic tank that contains the electrolyte solution that 3. step 1) make form a cover electro-deposition system;
4) electrodeposition process carries out under 60 ℃ constant temperature, adopts galvanostatic method, and current density is controlled at 30mA/cm
2, sedimentation time 8min;
5) sample that step 4) is made obtains the superlattice structure (L1 of vertical direction at 750 ℃ of The high temperature anneal 4.5h
0Type) super-high density magnetic record Fe-Pd alloy firm.
Claims (5)
1, a kind of L1
0The preparation method of type super-high density magnetic record metallic film is characterized in that, may further comprise the steps:
1) electrolyte solution of preparation two metal ion species:
1. the soluble-salt solution that with concentration is the ferromagnetic metal A of 0.01～0.5mol/l joins in the complexing agent solution that concentration is 0.03～3mol/l, the amount ratio of metal salt solution and complexing agent solution is 1: 1～3, obtain the complex solution of metal A, pH value with the ammoniacal liquor regulator solution is 6～10, the water-bath heating for dissolving;
2. the pH value that adds the ammoniacal liquor regulator solution in concentration is the soluble-salt solution of noble metal B of 0.1～2.5mol/l is 6～10, the water-bath heating for dissolving;
1. and 2. 3. after two kinds of solution of preparation press the mol ratio mixing in 1: 1 of metal ion A and B with step, be 6～10, prepare the electrolyte solution that contains two metal ion species with the pH value of ammoniacal liquor regulator solution;
2) substrate is handled by electrochemical polish or chemically polishing surface;
3) will be through step 2) substrate handled is as negative electrode, platinum electrode as anode and direct supply and the electrolytic tank that contains the electrolyte solution that contains two metal ion species that step 1) makes in 3. form electro-deposition system;
4) electrodeposition process carries out under 25～90 ℃ constant temperature, adopts galvanostatic method, and current density is controlled at 10～100mA/cm
2, sedimentation time 1～10min;
5) sample that step 4) is made is in 600～800 ℃ of The high temperature anneal 3～5 hours, the L1 that obtains having vertical direction
0Type super-high density magnetic record metallic film.
2, method according to claim 1 is characterized in that, the ferromagnetic metal Λ of step 1) described in 1. is selected from Fe, Co or Ni.
3, method according to claim 1 is characterized in that, the complexing agent of step 1) described in 1. is selected from ammonium tartrate, EDTA, succinic acid, malonic acid or citric acid.
4, method according to claim 1 is characterized in that, the noble metal B of step 1) described in 2. is selected from Pt, Pd, Ag or Au.
5, method according to claim 1 is characterized in that step 2) described in substrate be selected from Copper Foil, monocrystalline MgO sheet or monocrystalline silicon piece.
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| CN 200810113776 CN101593523B (en) | 2008-05-30 | 2008-05-30 | Method for preparing L10 type ultrahigh density magnetic record metal thin film |
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|---|---|---|---|
| CN 200810113776 CN101593523B (en) | 2008-05-30 | 2008-05-30 | Method for preparing L10 type ultrahigh density magnetic record metal thin film |
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| CN101593523A true CN101593523A (en) | 2009-12-02 |
| CN101593523B CN101593523B (en) | 2011-02-02 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103205787A (en) * | 2013-04-22 | 2013-07-17 | 南通万宝实业有限公司 | Preparation method of metal permanent magnet thin film with multi-layer thin film structure |
| CN107604408A (en) * | 2017-08-25 | 2018-01-19 | 洛阳师范学院 | A kind of bismuth ferrite thin film and preparation method thereof |
| CN110029377A (en) * | 2019-05-15 | 2019-07-19 | 东南大学 | A kind of long-wave band blacker-than-black is composite porous and preparation method thereof |
| CN110651337A (en) * | 2017-05-17 | 2020-01-03 | 株式会社电装 | Magnetic material comprising FeNi ordered alloy and method for producing the same |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1111212C (en) * | 1999-11-22 | 2003-06-11 | 北京理工大学 | Electrochemical deposition process to prepare hard film |
| JP2006269690A (en) * | 2005-03-23 | 2006-10-05 | Fujitsu Ltd | Soft magnetic thin film and magnetic recording head |
-
2008
- 2008-05-30 CN CN 200810113776 patent/CN101593523B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103205787A (en) * | 2013-04-22 | 2013-07-17 | 南通万宝实业有限公司 | Preparation method of metal permanent magnet thin film with multi-layer thin film structure |
| CN110651337A (en) * | 2017-05-17 | 2020-01-03 | 株式会社电装 | Magnetic material comprising FeNi ordered alloy and method for producing the same |
| CN110651337B (en) * | 2017-05-17 | 2023-02-17 | 株式会社电装 | Magnetic material comprising FeNi ordered alloy and method for producing the same |
| CN107604408A (en) * | 2017-08-25 | 2018-01-19 | 洛阳师范学院 | A kind of bismuth ferrite thin film and preparation method thereof |
| CN107604408B (en) * | 2017-08-25 | 2019-11-08 | 洛阳师范学院 | A kind of bismuth ferrite thin film and preparation method thereof |
| CN110029377A (en) * | 2019-05-15 | 2019-07-19 | 东南大学 | A kind of long-wave band blacker-than-black is composite porous and preparation method thereof |
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Granted publication date: 20110202 Termination date: 20190530 |