CN101572096A - Method for optimizing L1<0>-FePt film microstructure - Google Patents
Method for optimizing L1<0>-FePt film microstructure Download PDFInfo
- Publication number
- CN101572096A CN101572096A CNA2009100742725A CN200910074272A CN101572096A CN 101572096 A CN101572096 A CN 101572096A CN A2009100742725 A CNA2009100742725 A CN A2009100742725A CN 200910074272 A CN200910074272 A CN 200910074272A CN 101572096 A CN101572096 A CN 101572096A
- Authority
- CN
- China
- Prior art keywords
- fept film
- former
- film
- fept
- high strength
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Thin Magnetic Films (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
Abstract
The invention discloses a method for optimizing an L1<0>-FePt film microstructure, which adopts a high-pressure technology in the annealing process of a room temperature prepared FePt film in an original state, and the characteristic that high pressure can promote the nucleation of an L1<0> ordered domain and inhibit the growth of the L1<0> ordered domain is utilized; the size of the L1<0> ordered domain in the FePt film is reduced to near 10nm, and the size uniformity of the L1<0> ordered domain is significantly enhanced. The invention reduces the grain size of the FePt film, and effectively optimizes the microstructure of the L1<0>-FePt film. The method adopts the technological parameters: annealing temperature is 400 to 700 DEG C, annealing time is 2 to 200 min, pressure is 0.2 to 1 GPa, and vacuum is p less than 10<-3>Pa. The invention provides basis for the application and the development of the L1<0>-FePt film which is used as magnetic recording material of super-high density.
Description
Technical field
The present invention relates to the magnetic recording media field, specially refer to a kind of optimization method of the most rising super-high density magnetic recording media microstructure.
Background technology
The develop rapidly of digitizing technique needs to transmit, write down a large amount of information.Has L1
0The FePt film of ordered structure is owing to have extra high magnetic anisotropy constant (K
u=(4-7) * 10
7Erg/cm
3Thereby) have minimum super paramagnetic critical dimension (2-3nm) and become super-high density magnetic recording media material of new generation.Theoretical prophesy, the magnetic recording density of this dielectric material can surpass 1TB/in
2L1
0The microstructure of-FePt film has fundamental influence to the raising of its magnetic recording density and magnetic property, for the recording density that realizes superelevation and high signal to noise ratio (S/N ratio) L1
0-FePt film need have the extra fine crystallite dimension (＜10nm) and grain size be evenly distributed.And the FePt film for preparing under the room temperature has face-centred cubic structure (A1 structure), does not have the magnetic recording function, must it be taken place by the A1 structure to L1 through high annealing (generally being higher than 500 ℃)
0The transformation of ordered structure.Studies show that this process of ordering mainly is subjected to L1 in the FePt film
0Domain growth is controlled in order, and so the annealing of high-temperature will inevitably cause the thick, inhomogeneous of the domain of order, thereby can cause L1
0The abnormality growth of-FePt film crystal grain, finally cause the FePt film to have thick crystallite dimension (20-50nm) and grain size distribution inhomogeneous.Though much orderings that under lower temperature, has promoted the FePt film of research work success, owing to promote FePt film L1
0A lot of methods of ordering all pass through to promote L1
0Domain growth is finished in order, thereby thick, the inhomogeneous key issue that also always is restriction FePt film as application of super-high density magnetic recording media material and development of crystallite dimension.
Summary of the invention
The object of the present invention is to provide a kind of optimization L1
0The method of-FePt film microstructure, this invention utilize high pressure energy to promote L1 by adopt high pressure technique in FePt film annealing process
0Domain of order forming core also suppresses the characteristics of its growth, greatly reduces the crystallite dimension and the L1 of FePt film
0Domain of order size, and significantly improved the homogeneity of this Size Distribution.Effective optimization L1
0The microstructure of-FePt film.
Optimization L1 provided by the present invention
0The processing step that method adopted of-FePt microstructure is:
1, at room temperature, adopting the DC magnetron sputtering system growth components scope on the Si of autoxidation substrate with electromagnet is Fe: Pt=40: 60～60: 40 the former primary state FePt film with unordered A1 structure.
2, prepared former primary state FePt film is faced down put in the high strength graphite sleeve pipe, fill cubic boron nitride and do pressure transmitting medium, after sealing with the graphite capping, with this high strength graphite sleeve pipe that FePt film is housed pack into an internal diameter size equal the graphite bush diameter by in interior former and the former that outer female die set becomes, load onto two to the roof pressure head in high strength graphite sleeve pipe both sides.Be close to placement one temperature thermocouple 9 on the interior former of high strength graphite sleeve pipe, in order to the annealing temperature of in site measurement film, a temperature control thermopair is placed in the position near former on pressure head, in order to the annealing temperature of control FePt film 4.
3, the above-mentioned grinding tool that graphite bush and pressure head are housed is contained in the Gleeble-3500 hot modeling test machine vacuum cavity, fixes with jig, the vacuum of vacuum cavity is evacuated to p＜10
-3Pa, by jig by hot modeling test machine to the FePt film 0.2～1GPa that exerts pressure.
4, in the process of pressurization, anneal for FePt film rising temperature to 400～700 ℃, annealing time is 2min～200min; Its temperature is reduced to room temperature, lay down pressure, take out the FePt film.
The invention has the beneficial effects as follows: in the process of FePt film ordering annealing, adopt high pressure technique, because high pressure has the FePt of promotion film L1
0Domain of order forming core also suppresses the effect of its growth, thereby can reduce this film L1
0The size of the domain of order and improve the homogeneity of its Size Distribution; Inhibited owing to high pressure again to atom diffusion, thereby can effectively reduce the crystallite dimension of FePt film, thus improve L1
0The microstructure of-FePt film.The present invention can prepare crystallite dimension tiny (near 10nm) L1 uniformly
0-FePt film.
Description of drawings
Fig. 1 is a kind of optimization L1
0The high pressure annealing device synoptic diagram of-FePt film microstructure method;
Fig. 2 is L1 behind the high pressure annealing
0The size of the domain of order and the degree of order are with the variation relation of pressure;
Fig. 3 is transmission electron microscope dark field image and the bright field image photo and the Size Distribution collection of illustrative plates of FePt film after high pressure (a) and (b) and normal pressure (c), (d) anneal down.
In Fig. 1,1. jig, 2. temperature control thermopair, 3. high strength graphite sleeve pipe, the 4.FePt film, 5. pressure head, 6. in former, 7. outer former, 8. boron nitride pressure transmitting medium, 9. temperature thermocouple, 10. vacuum cavity.
Embodiment
At room temperature, employing magnetron sputtering technique growth components ratio on the Si of autoxidation substrate is 1: 1 a former primary state FePt film 4.To this FePt film at the enterprising horizontal high voltage annealing experiment of Gleeble-3500 hot modeling test machine.Experimental provision as shown in Figure 1.These FePt film 4 faces are placed in the high strength graphite sleeve pipe 3 down, fill cubic boron nitride 8 and do pressure transmitting medium, after sealing with the graphite capping, this high strength graphite sleeve pipe 3 that FePt film 4 is housed internal diameter size of packing into is equaled to load onto two to roof pressure head 5 in high strength graphite sleeve pipe 3 both sides in the former of being made up of interior former 6 and outer former 7 of graphite bush diameter.Adopt these two the pressure head on top vertically put on FePt film 4 surfaces by high strength graphite cover 3 with pressure.Pressure calculates by the load of pressure head 5.Be close to placement one temperature thermocouple 9 on the interior former of high strength graphite sleeve pipe, in order to the annealing temperature of in site measurement film, a temperature control thermopair is placed in the position near former on pressure head, in order to the annealing temperature of control FePt film 4.The above-mentioned grinding tool that high strength graphite cover 3 and pressure head 5 are housed is contained in the vacuum cavity 10 of Gleeble-3500 hot modeling test machine, and fixing with jig 1, vacuum cavity 10 vacuum are evacuated to p＜10
-3Pa, by jig 1 by hot modeling test machine to the FePt film 1GPa that exerts pressure.600 ℃ of annealing temperatures, annealing time 30min.
Experimental result shows: L1 behind the 1GPa high pressure annealing
0The size d=24nm[that the size d=12nm of the domain of order is significantly less than the normal pressure annealing back domain of order sees Fig. 2 and Fig. 3 (a), (c)], the (see figure 2) but the degree of order is more or less the same.1GPa high pressure annealing sample L1
0The size of the domain of order is significantly than the even size distribution [seeing Fig. 3 (a), (c) illustration] of normal pressure annealing specimen.And behind the 1GPa high pressure annealing, the FePt film has more tiny, uniform crystallite dimension [see Fig. 3 (b) and (d)].
Claims (1)
1. optimize L1 for one kind
0The method of-FePt film microstructure is characterized in that: the processing step of described method is:
A. at room temperature, adopting the DC magnetron sputtering system growth components scope on the Si of autoxidation substrate with electromagnet is Fe: Pt=40: 60～60: 40 the former primary state FePt film (4) with unordered A1 structure;
B. prepared former primary state FePt film (4) face is put in the high strength graphite sleeve pipe (3) down, fill cubic boron nitride (8) and do pressure transmitting medium, after sealing with the graphite capping, this high strength graphite sleeve pipe (3) internal diameter of packing into is equaled to load onto two to roof pressure head (5) in high strength graphite sleeve pipe (3) both sides in the former of being made up of interior former (6) and outer former (7) of high strength graphite sleeve pipe (3) diameter; Place temperature thermocouple (9) on the interior former of high strength graphite sleeve pipe being close to, in order to the annealing temperature of in site measurement film, temperature control thermopair (2) is placed in the position near former on pressure head, in order to the annealing temperature of control FePt film (4).
C. the above-mentioned grinding tool that high strength graphite sleeve pipe (3) and pressure head (5) are housed is contained in the Gleeble-3500 hot modeling test machine vacuum cavity (10), fixing with jig (1), vacuum cavity (10) vacuum is evacuated to p＜10
-3Pa, by jig (1) by hot modeling test machine to the FePt film 0.2～1GPa that exerts pressure.
D. in the process of pressurization, anneal for FePt film (4) rising temperature to 400～700 ℃, annealing time is 2min～200min; Its temperature is reduced to room temperature, lay down pressure, take out FePt film (4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100742725A CN101572096B (en) | 2009-04-29 | 2009-04-29 | Method for optimizing L1<0>-FePt film microstructure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100742725A CN101572096B (en) | 2009-04-29 | 2009-04-29 | Method for optimizing L1<0>-FePt film microstructure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101572096A true CN101572096A (en) | 2009-11-04 |
| CN101572096B CN101572096B (en) | 2011-08-10 |
Family
ID=41231428
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100742725A Expired - Fee Related CN101572096B (en) | 2009-04-29 | 2009-04-29 | Method for optimizing L1<0>-FePt film microstructure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101572096B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112305009A (en) * | 2020-11-06 | 2021-02-02 | 北京石油化工学院 | Resistance type high-temperature pressure thermal simulation test device and test method |
| CN112962122A (en) * | 2021-02-01 | 2021-06-15 | 浙江工业大学 | Preparation method of high-coercivity B-doped FePt film |
-
2009
- 2009-04-29 CN CN2009100742725A patent/CN101572096B/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112305009A (en) * | 2020-11-06 | 2021-02-02 | 北京石油化工学院 | Resistance type high-temperature pressure thermal simulation test device and test method |
| CN112305009B (en) * | 2020-11-06 | 2024-01-19 | 北京石油化工学院 | Resistance type high-temperature pressure thermal simulation test device and test method |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101572096B (en) | 2011-08-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Schryvers et al. | Unit cell determination in CuZr martensite by electron microscopy and X-ray diffraction | |
| CN109437920B (en) | Nanometer/submicron structure wBN superhard material, wBN-cBN superhard composite material, preparation method and cutter | |
| CN101572096B (en) | Method for optimizing L1<0>-FePt film microstructure | |
| Ener et al. | Twins–A weak link in the magnetic hardening of ThMn12-type permanent magnets | |
| Zhang et al. | Superelasticity and Serration Behavior in Small‐Sized NiMnGa Alloys | |
| Castle et al. | High coercivity, anisotropic, heavy rare earth-free Nd-Fe-B by Flash Spark Plasma Sintering | |
| Cui et al. | Effects of alignment on the magnetic and mechanical properties of sintered Nd–Fe–B magnets | |
| CN101476055A (en) | Preparation of fully dense massive anisotropic nanocrystalline SmCo5 magnet | |
| CN104961464A (en) | Carbon-based composite with high rebound resilience and high heat conductivity coefficient along thickness direction and preparation method of carbon-based composite | |
| CN104694889A (en) | Preparation method of CdTe sputtering target material | |
| CN111945027B (en) | Method for strengthening GNPs/Ti composite material interface combination by directional growth of TiBw | |
| Hollenberg et al. | Effect of fast neutron irradiation on the structure of boron carbide | |
| Or et al. | Dynamic magnetomechanical properties of Terfenol-D/epoxy pseudo 1-3 composites | |
| Li et al. | Shear band mediated ω phase transformation in Nb single crystals deformed at 77 K | |
| Van Rooyen et al. | The influence of annealing temperature on the strength of TRISO coated particles | |
| Zuo et al. | Strong textured SmCo5 nanoflakes with ultrahigh coercivity prepared by multistep (three steps) surfactant-assisted ball milling | |
| Gao et al. | Coercivity enhancement in sintered Nd-Fe-B magnets by large mass rotating diffusion with Tb strips | |
| CN111962024B (en) | Preparation method of SmCo perpendicular magnetic anisotropic film | |
| Preston et al. | Effect of powder morphology on the microstructure and mechanical property gradients in stainless steels induced by thermal gradients in spark plasma sintering | |
| Wang et al. | Fe-50Ni alloy with ordered L10 structure prepared by cubic pressing | |
| Duenas et al. | Experimental results for magnetostrictive composites | |
| Mohan et al. | Nonstoichiometric FePt Nanoclusters for Heated Dot Magnetic Recording Media | |
| Luo et al. | Superplastic forging for sialon-based nanocomposite at ultralow temperature in the electric field | |
| Mikaili Agah et al. | The effect of electron flow on coercivity and remanence of FePt nanocomposites under heat treatment | |
| Hsiao et al. | Effect of annealing process on strain-induced crystallographic orientation of FePt thin films |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110810 Termination date: 20140429 |