CN101403098A - Magnetic memory material of compound structure of FePt nano-particle monolayer film and B4C and method of producing the same - Google Patents
Magnetic memory material of compound structure of FePt nano-particle monolayer film and B4C and method of producing the same Download PDFInfo
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- CN101403098A CN101403098A CNA2008101975319A CN200810197531A CN101403098A CN 101403098 A CN101403098 A CN 101403098A CN A2008101975319 A CNA2008101975319 A CN A2008101975319A CN 200810197531 A CN200810197531 A CN 200810197531A CN 101403098 A CN101403098 A CN 101403098A
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Abstract
The invention provides a magnetic recording material compounded by iron-platinum nano-particle self-assembly monofilm and B4C and a preparation method thereof. The preparation method comprises the following steps: the mono-disperse nanometer FePt particles with adjustable grain diameters are spread on an inorganic material substrate to form a self-assembly monofilm structure, a B4C protective layer with thickness of 10-50 nanometers is sputtered on the monofilm by the magnetron sputtering technology, and the B4C protective layer covers and protects the iron-platinum nano-particle monofilm; after high temperature annealing, the complex film magnetic recording material formed by the FePt nano-particles with magnetic phase transition and stable self-assembly is formed. The material has the advantages of good stability, high coercive force, high integration, high repeatability, and the like, which can greatly improve recording density.
Description
Technical field
The present invention relates to a kind of single preparation technology who disperses (standard deviation of particle size＜10%) FePt nanometer unitary film, and in the high temperature annealing phase transition process protection of FePt nanometer and stable method in the unitary film.Belong to field of nanometer technology.
Technical background
In the growing current society of science and technology, people have proposed more and more higher requirement to the storage capacity of information.Particularly comprise music at present, video, the widespread use of multimedia meanses such as high-resolution film often needs magnanimity information is stored.Can only reach per square inch about 40GB based on its recording density of hard disc of computer of the magnetic storage technology manufacturing of routine, can not satisfy the growth requirement of information society fully.Utilize AFC (Anti Ferromagnetically Coupled, the antiferromagnetism coupling) technology of present IBM invention, the storage density of existing hard disk has obtained raising to a certain degree again, reaches the rank of 100GB per square inch.In hard disc of computer, there are the following problems as the storage unit of data to utilize the magnetic particle: along with reducing of unit magnetic recording unit volume, envrionment temperature will cause the disappearance of magnetic, and promptly information loses.The thermostability that improves storage element needs the big magnetocrystalline anisotropy of having of magneticsubstance.The maximum material of present known magnetocrystalline anisotropy constant (Ku) is a ferroplatinum, and its Ku is up to 7 * 10
6Joule/cubic meter
[1], make the FePt particle of size about 3.3 nanometers promptly can in environment, keep big coercive force and good thermostability.Suppose that with single FePt particle as a record cell, the recording density of magnetic storage will reach the theoretic limit so, promptly 40-50T bit/ square inch (1T bit=1024G bit) is higher than existing any storage medium far away.In view of the tempting prospect on its information storage, there are many research groups being devoted to develop magnetic recording material of future generation in the world based on the FePt nano-grain array of long-range order always.
Since the grandson of IBM Corporation in 2000 keeps the identical high-sequential array of developing monodispersed FePt nano particle
[2], become the hot topic selection of following high record density hard disc of computer based on the storage medium of magnetic nanoparticle oldered array
[3]Realize the application of nanometer Fe Pt particle aspect ultrahigh density storage, need overcome two obstacles aspect the magnetic medium layer at present: one, at first need to obtain single dispersion, the uniform nano particle of composition (being generally soft magnetism or super paramagnetic), make it on a large scale substrate (as Si, SiO
2) on be self-assembled into unitary film.And the self-assembly of the FePt nano particle of experimentally realizing at present on (electron microscope copper mesh) among a small circle can't be satisfied application need.Two, the FePt nano-grain array of self-assembly formation need form the Hard Magnetic phase later on through the high temperature annealing phase transformation.And high-temperature annealing process often causes the destruction of intergranular reunion and ordered structure
[4], therefore the process in phase transformation guarantees that the formation and the complete of ordered structure of hard magnetic also are key in application.For overcoming above-mentioned two big obstacles, many in the world research groups have proposed different solutions, but these means can only reduce the particulate accumulation to a certain extent at present, and the particle after the annealing is difficult to be self-assembled into the magnetic array of ordered structure again.The another one research direction is the FePt monolayer of particles film of elder generation in big substrate surface preparation self-assembly, carries out high temperature annealing then and takes place to change mutually.But the monolayer of particles film that obtains does not at present possess long range ordered structure, and the magnetic after the annealing is on the low side, can't reach the requirement of application.Therefore to finally realize the application of FePt nano particle in the super high-density recording hard disk, still need a large amount of experimental studies.
Summary of the invention
The objective of the invention is to be to overcome the deficiencies in the prior art, propose a kind of nanometer Fe-Pt particle self-assembled monolayer and B
4C compound magnetic pipe recording material preparation method guarantees that this material has long range ordered structure and high-coercive force, greatly improves recording density.
The present invention is achieved by the following technical solutions: the dispersed nano FePt particle of adjustable grain is spread over formation self-assembled monolayer membrane structure on the inorganic materials substrate, is the B of 10-50 nanometer by magnetron sputtering technique sputter one layer thickness on unitary film
4The C protective layer behind the high temperature annealing, forms FePt nano particle magnetic phase transition and the stable composite membrane magnetic pipe recording material of self-assembly.
Principle of the present invention is FePt nano particle morphology control, finishing to be handled match the FePt particle single-layer membrane structure of long-range order on the preparation macro-scale with substrate surface; Utilize evaporating deposition technique, select high heat stability, chemically stable inorganic thin film B
4C is as the barrier layer in the high temperature annealing, prevents that FePt in the unitary film from building up and the destruction of ordered structure, finally obtains the FePt/B of high-coercive force
4The C composite membrane.
The concrete grammar step is as follows:
1, monodisperse nanometer Fe-Pt particulate preparation: the Fe (CO) of the methyl ethyl diketone platinum of 0.5 mmole, 2 mmoles
5, 1～4 mmole the oleyl amine mixed dissolution of oleic acid, 1～4 mmole in 20 milliliters of Bian alcohol, stir at the condition of nitrogen gas lower magnetic force.Electric mantle heating then makes solution be warming up to 200 degree with the speed of 5 ℃ of per minutes, and keeps this thermotonus to prepare the monodisperse nanometer Fe-Pt particle solution in 2 hours.
2, the preparation of dispersion liquid, spin coating liquid: after solution is cooled to room temperature, in solution, pour 20～40 milliliters of dehydrated alcohols into, sonic oscillation was poured centrifuge tube into after 5 minutes, carry out centrifugal with 3000-10000 rev/min speed, brown supernatant liquor after centrifugal is outwelled, and black precipitate incorporates in 15 milliliters of hexanes in will managing.Use the same terms centrifugal after adding the equal volume dehydrated alcohol again, the black precipitate that obtains incorporates in 10 milliliters of hexanes, utilizes hexane, alcohol to clean once with identical condition again, and the iron platinum grain is dispersed in the 10ml hexane, forms stable dispersion liquid.The octane that adds 1: 1 volume ratio again mixes as spin coating liquid.
3, prepare iron platinum unitary film with spin-coating method: with size is that 1 * 1 centimetre clean silicon slice placed is on sol evenning machine, slowly drip to an iron platinum spin coating liquid on the silicon chip, left standstill 5～15 seconds, sol evenning machine accelerated to 1 500～2000 rpms in 5 seconds then, kept this rotating speed again 80 seconds, and took out after the solution drying on the silicon chip by the time and preserve.
4, magnetron sputtering B
4C film and high temperature annealing phase transformation: the B that utilizes magnetron sputtering sputter one deck 10～50 nanometers on the FePt unitary film
4The C film.Base vacuum is 2 * 10
-4Pa, air pressure maintains 0.5Pa in the sputter procedure.600～800 ℃ of annealing one hour under vacuum condition of the good film of sputter.
5, detect warehouse-in.
The present invention has good stability, the coercive force height, and the integrated level height, repeatable advantages of higher can greatly improve recording density.
Accompanying drawing and explanation
Fig. 1: FePt monolayer of particles film/B of the present invention
4The composite structure synoptic diagram of C protective layer,
From Fig. 1, be clear that B
4The C protective layer protects the containing of FePt monolayer of particles film.
Fig. 2: FePt particle of the present invention is typical unitary film arrangement mode synoptic diagram on silicon chip,
Wherein (a) FePt spin coating liquid concentration is～2 mg/ml; (b) FePt spin coating liquid concentration is～5 mg/ml; (c) FePt spin coating liquid concentration is～8 mg/ml.
Fig. 3: FePt monolayer of particles film/B of the present invention
4650 ℃ of vacuum annealings of C protective layer composite structure transmission electron microscope view after 1 hour,
(a) low transmission electron microscope vertical view of differentiating wherein finds out that therefrom the FePt particle do not build up behind high temperature annealing, show good thermostability; (b) high-resolution-ration transmission electric-lens sectional view is therefrom found out between the FeP particle by the B about one deck 10 nanometers
4C separates.
Embodiment
The present invention is further described with embodiment below.
Embodiment 1
1, the Fe (CO) of the methyl ethyl diketone platinum of 0.5 mmole, 2 mmoles
5, 1 mmole the oleyl amine mixed dissolution of oleic acid, 1 mmole in 20 milliliters of Bian alcohol, stirring heating under condition of nitrogen gas, make solution be warming up to 200 degree, and keep this thermotonus to prepare the monodisperse nanometer Fe-Pt particle in 2 hours with the speed of 5 ℃ of per minutes.
2, after solution is cooled to room temperature, pour 40 milliliters of dehydrated alcohols in solution, sonic oscillation was poured centrifuge tube into after 5 minutes, carried out centrifugally with 10000 rev/mins speed, and the brown supernatant liquor after centrifugal is outwelled, and black precipitate incorporates in 15 milliliters of hexanes in will managing.Use the same terms centrifugal after adding the equal volume dehydrated alcohol again, the black precipitate that obtains incorporates in 10 milliliters of hexanes, utilizes hexane, alcohol to clean once with identical condition again, and the iron platinum grain is dispersed in the 10ml hexane, forms stable dispersion liquid.The octane that adds 1: 1 volume ratio again mixes as spin coating liquid.
3, be that 1 * 1 centimetre clean silicon slice placed is on sol evenning machine with size, an iron platinum spin coating liquid is slowly dripped on the silicon chip, left standstill 5～15 seconds, all the glue machine accelerated to 1500 rpms in 5 seconds then, kept this rotating speed again 80 seconds, and took out after the solution drying on the silicon chip by the time.
4, utilize the B of magnetron sputtering sputter one deck 10 nanometers on the FePt unitary film
4The C film.Base vacuum is 2 * 10
-4Pa, air pressure maintains 0.5Pa in the sputter procedure.The 650 ℃ of annealing one hour under vacuum condition of the good film of sputter.
5, detect warehouse-in.
Embodiment 2
1, the Fe (CO) of the methyl ethyl diketone platinum of 0.5 mmole, 2 mmoles
5, 2 mmoles the oleyl amine mixed dissolution of oleic acid, 2 mmoles in 20 milliliters of Bian alcohol, stirring heating under condition of nitrogen gas, make solution be warming up to 200 degree, and keep this thermotonus to prepare the monodisperse nanometer Fe-Pt particle in 2 hours with the speed of 5 ℃ of per minutes.
2, after solution is cooled to room temperature, pour 20 milliliters of dehydrated alcohols in solution, sonic oscillation was poured centrifuge tube into after 5 minutes, carried out centrifugally with 5000 rev/mins speed, and the brown supernatant liquor after centrifugal is outwelled, and black precipitate incorporates in 15 milliliters of hexanes in will managing.Use the same terms centrifugal after adding the equal volume dehydrated alcohol again, the black precipitate that obtains incorporates in 10 milliliters of hexanes, utilizes hexane, alcohol to clean once with identical condition again, and the iron platinum grain is dispersed in the 10ml hexane, forms stable dispersion liquid.The octane that adds 1: 1 volume ratio again mixes as spin coating liquid.
3, be that 1 * 1 centimetre clean titanium dioxide silicon chip is placed on the sol evenning machine with size, an iron platinum spin coating liquid is slowly dripped on the silicon chip, left standstill 15 seconds, all the glue machine accelerated to 2000 rpms in 5 seconds then, kept this rotating speed again 80 seconds, and took out after the solution drying on the silicon chip by the time.
4, utilize the B of magnetron sputtering sputter one deck 50 nanometers on the FePt unitary film
4The C film.Base vacuum is 2 * 10
-4Pa, air pressure maintains 0.5Pa in the sputter procedure.The good film of sputter is under vacuum condition (10
-3Pa) annealed one hour for 600 ℃.
5, detect warehouse-in.
Embodiment 3
1, the Fe (CO) of the methyl ethyl diketone platinum of 0.5 mmole, 2 mmoles
5, 4 mmoles the oleyl amine mixed dissolution of oleic acid, 4 mmoles in 20 milliliters of Bian alcohol, stirring heating under condition of nitrogen gas, make solution be warming up to 200 ℃, and keep this thermotonus to prepare the monodisperse nanometer Fe-Pt particle in 2 hours with the speed of 5 ℃ of per minutes.
2, after solution is cooled to room temperature, pour 30 milliliters of dehydrated alcohols in solution, sonic oscillation was poured centrifuge tube into after 5 minutes, and is centrifugal with 3000 rev/mins of speed, and the brown supernatant liquor after centrifugal is outwelled, and black precipitate incorporates in 15 milliliters of hexanes in will managing.Use the same terms after adding the equal volume dehydrated alcohol again, the black precipitate that obtains incorporates in 10 milliliters of hexanes, utilizes hexane, alcohol to clean once with identical condition again, at last the iron platinum grain is dispersed in the 10ml hexane, forms stable dispersion liquid.The octane that adds 1: 1 volume ratio again mixes as spin coating liquid.
3, be that 1 * 1 centimetre clean silicon slice placed is on sol evenning machine with size, an iron platinum spin coating liquid is slowly dripped on the silicon chip, left standstill 10 seconds, all the glue machine accelerated to 1500 rpms in 5 seconds then, kept this rotating speed again 80 seconds, and took out after the solution drying on the silicon chip by the time.
4, utilize the B4C film of magnetron sputtering sputter one deck 20 nanometers on the FePt unitary film.Base vacuum is 2 * 10
-4Pa, air pressure maintains 0.5Pa in the sputter procedure.The 800 ℃ of annealing one hour under vacuum condition of the good film of sputter.
5, detect warehouse-in.
Claims (2)
1, a kind of nanometer Fe-Pt particle self-assembled monolayer and B
4C compound magnetic pipe recording material is characterized in that the dispersed nano FePt particle of adjustable grain is spread over formation self-assembled monolayer membrane structure on the inorganic materials substrate, is the B of 10-50 nanometer by magnetron sputtering technique sputter one layer thickness on unitary film
4The C protective layer behind the high temperature annealing, forms FePt nano particle magnetic phase transition and the stable composite membrane magnetic pipe recording material of self-assembly.
2, a kind of nanometer Fe-Pt particle self-assembled monolayer and B
4The preparation method of C compound magnetic pipe recording material is characterized in that the concrete grammar step is as follows:
1), monodisperse nanometer Fe-Pt particulate preparation: the Fe (CO) of the methyl ethyl diketone platinum of 0.5 mmole, 2 mmoles
5, 1～4 mmole the oleyl amine mixed dissolution of oleic acid, 1～4 mmole in 20 milliliters of Bian alcohol, stir at the condition of nitrogen gas lower magnetic force, heat with electric mantle then, make solution be warming up to 200 degree, and keep this thermotonus to prepare the monodisperse nanometer Fe-Pt particle solution in 2 hours with the speed of 5 ℃ of per minutes;
2), dispersion liquid, the preparation of spin coating liquid: after solution is cooled to room temperature, in solution, pour 20～40 milliliters of dehydrated alcohols into, sonic oscillation was poured centrifuge tube into after 5 minutes, carry out centrifugal with 3000-10000 rev/min speed, brown supernatant liquor after centrifugal is outwelled, black precipitate is dissolved in 15 milliliters of hexanes in will managing, use the same terms centrifugal after adding the equal volume dehydrated alcohol again, the black precipitate that obtains incorporates in 10 milliliters of hexanes, utilize hexane again, alcohol cleans once with identical condition, the iron platinum grain is dispersed in the 10ml hexane, forms stable dispersion liquid, the octane that adds 1: 1 volume ratio again mixes as spin coating liquid;
3), prepare iron platinum unitary film with spin-coating method: with size is that 1 * 1 centimetre clean silicon slice placed is on sol evenning machine, slowly drip to an iron platinum spin coating liquid on the silicon chip, left standstill 5～15 seconds, sol evenning machine accelerated to 1500～2000 rpms in 5 seconds then, kept this rotating speed again 80 seconds, and took out after the solution drying on the silicon chip by the time and preserve;
4), magnetron sputtering B
4C film and high temperature annealing phase transformation: the B that utilizes magnetron sputtering sputter one deck 10～50 nanometers on the FePt unitary film
4C film, base vacuum are 2 * 10
-4Pa, air pressure maintains 0.5Pa in the sputter procedure.600～800 ℃ of annealing one hour under vacuum condition of the good film of sputter;
5), detect warehouse-in.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101787522A (en) * | 2010-04-02 | 2010-07-28 | 南京大学 | Method for preparing ordered magnetic nanoparticle composite film with super-high density |
| CN105234427A (en) * | 2015-11-04 | 2016-01-13 | 中国科学院上海高等研究院 | Platinum alloy nano core-shell cube and preparation method thereof |
| CN110055502A (en) * | 2019-05-07 | 2019-07-26 | 吉林大学 | A kind of preparation method of the adjustable semiconductor boron C film of band gap |
| CN112962122A (en) * | 2021-02-01 | 2021-06-15 | 浙江工业大学 | Preparation method of high-coercivity B-doped FePt film |
-
2008
- 2008-11-05 CN CN2008101975319A patent/CN101403098B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101787522A (en) * | 2010-04-02 | 2010-07-28 | 南京大学 | Method for preparing ordered magnetic nanoparticle composite film with super-high density |
| CN101787522B (en) * | 2010-04-02 | 2011-11-09 | 南京大学 | Method for preparing ordered magnetic nanoparticle composite film with super-high density |
| CN105234427A (en) * | 2015-11-04 | 2016-01-13 | 中国科学院上海高等研究院 | Platinum alloy nano core-shell cube and preparation method thereof |
| CN110055502A (en) * | 2019-05-07 | 2019-07-26 | 吉林大学 | A kind of preparation method of the adjustable semiconductor boron C film of band gap |
| CN110055502B (en) * | 2019-05-07 | 2021-04-13 | 吉林大学 | Preparation method of semiconductor boron-carbon film with adjustable band gap |
| CN112962122A (en) * | 2021-02-01 | 2021-06-15 | 浙江工业大学 | Preparation method of high-coercivity B-doped FePt film |
| CN112962122B (en) * | 2021-02-01 | 2022-03-15 | 浙江工业大学 | Preparation method of high-coercivity B-doped FePt film |
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