CN101215689A - Method for preparing (002) texture Fe thin film - Google Patents
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- CN101215689A CN101215689A CNA2007101733029A CN200710173302A CN101215689A CN 101215689 A CN101215689 A CN 101215689A CN A2007101733029 A CNA2007101733029 A CN A2007101733029A CN 200710173302 A CN200710173302 A CN 200710173302A CN 101215689 A CN101215689 A CN 101215689A
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Abstract
The invention belongs to the field of information storage technology, in particular to a method for preparing (002) texture Fe film. The invention achieves complete (002) orientation through the mode of heat treatment, first a Fe film whose thickness is 10-50 nanometer is deposited on a glass substrate through the mode of magnetron sputtering, then a sample is annealed in a vacuum environment, the heating mode is that the Fe film is irradiated by a halogen lamp, the annealing temperature is 400-600 DEG C, the time is 10-20 minutes, and the Fe film which is prepared has the complete (002) orientation. Various factors which affect final structure during the state of system researching and preparation of the invention provide complete parameter requirements for preparing the Fe (002) texture magnetic film through the mode of magnetron sputtering. A FePt film is further grown on a (002) texture Fe film, a C shaft of a L10 phase FEPt film is vertical to the surface of the film and becomes into a magnetic storage medium with excellent performance.
Description
Technical field
The invention belongs to technical field of information storage, be specifically related to be used for the preparation method that texture is induced the buffer layer of FePt (001) structural growth.
Technical background
For realizing higher recording density, the magnetic storage technology is converted to perpendicular magnetic recording from the longitudinal recording mode.Usually, this requires the normal direction of the easy magnetizing axis of recording medium film along face.Reduce the recorded bit significantly super paramagnetic effect that becomes, the L1 of high magnetocrystalline anisotropy energy for overcoming
0Phase FePt ordered alloy material becomes the research emphasis of superelevation recording density dielectric material of future generation.Because the easy magnetizing axis of FePt ordered alloy film is along the c direction of principal axis of center of area tetragonal, therefore, L1
0The c of phase FePt film is shaft vertically aligned to need to have become the key issue that solves.
In actual applications, can influence the grain growing of magnetic recording layer by the buffer layer (Underlayer, or Buffer layer) that increase has texture, the orientation of control film, and then improve magnetic recording property, as utilize the Cr layer to control the orientation of CoCrPt film [1].According to existing document, the L1 that c is shaft vertically aligned
0FePt ordered alloy film also can obtain in this way, and the material that adopts is [2] such as CrRu, NiTa/Cr usually.Because the lattice parameter of these materials has less lattice mismatch in FePt, the FePt atom can directly be grown along the lattice point of their lattices; Simultaneously, by the lattice parameter of mixing and can also regulate buffer layer, promote the ordering of film, as mix small Ru in the Cr film of (002) texture, when Ru content was 9at%, it is vertical orientated that the FePt film shows.But the diffusion of Cr in the FePt film can cause degenerating of magnetic property.Therefore seeking new suitable cushioning layer material and structure becomes research emphasis.
Fe is a body-centered cubic structure, and lattice parameter a is 0.2866 nanometer, and the spacing d of diagonal angle atom is 0.4053 nanometer [3].L1
0The FePt ordered alloy is a center of area tetragonal, and lattice parameter a, c are respectively 0.3852 and 0.3713 nanometers, is respectively 5.2% and 9.2% with the mismatch degree of Fe diagonal angle interatomic distance d.Be compared to Cr
91Ru
9About 6.4% mismatch degree can be expected the shaft vertically aligned film of c that the Fe film also can induce.Generally speaking, the Fe film shows the texture of (110), and this is that the energy of (110) face is minimum, the easiest growth because for body-centered cubic structure.But data comparison shows that Fe has the crystalline structure identical with Cr, physicalies such as close lattice parameter, atomic radius.Therefore, careful control growth for Thin Film condition is passed through in our expection, can obtain the film of (002) texture.
Ensuing problem is, how to control the diffusion of Fe in the FePt film? problem hereto, can assign to compensate the diffusion of Fe by the one-tenth of regulating the FePt film, here Fe is not a foreign atom, and the composition of Fe can change in the scope of broad among the FePt.Our experiment show this point.
Be compared to Cr, Fe is ferromagnetic film, and show soft magnetic property, with the Fe of (002) texture as buffer layer, both can induce the growth of FePt (001) orientation crystal grain, can utilize the coupling between Fe and the FePt again, preparation spin-exchange-coupled complex media (ECC), drive the upset of FePt magnetic moment by the magnetization reversal of Fe, thereby reduce the write field of entire structure.
Recently, aspect the magneto-electronics investigation of materials, show very high tunneling magnetoresistance (surpassing 400%) with the magnesium oxide single-crystal film as Fe (001)/MgO (001)/Fe (001) tunnel junction of middle barrier layer, far above using amorphous Al
2O
3Film is as the tunnel junction [4] of barrier layer.Its reason is to have only holosymmetric Δ in crystal barrier when tunnelling takes place
1Electronics in being with just has high tunnelling probability, simultaneously the Δs of most spins
1Energy band and Fermi surface have overlapping, the Δ of minority spin
1Energy band and Fermi surface do not have overlapping, and therefore very high magneto-resistance effect is arranged.This discovery makes the DEVELOPMENT PROSPECT of magnetic random memory (MRAM) become bright.In this tunnel junction, the MgO crystal film is crucial, adopts the method for molecular beam epitaxy and sputter to grow on monocrystalline or texture Fe thin film surface usually, and therefore, preparing high-quality Fe (002) film is the key that obtains the high-performance tunnel junction.The method cost of considering sputter is low, is widely used industrial, so research seems extremely important with the Fe film that the method for sputter prepares (002) texture.
Based on the importance of above two aspects, the present invention proposes and adopt heat treated preparation technology, substrate heating and sputter finish the postheat treatment dual mode when comprising sputter, can prepare the Fe magneticthin film of (002) texture quickly and easily.The present invention has systematically studied influences the factor that Fe film texture forms, and has defined this technology conditions needed.On this basis, the L1 that has prepared the high orientation and the high degree of order
0Phase FePt film.
Reference:
[1]M.L.Plumer，J.Van?Ek，D.Weller，The?Physics?of?Ultrahigh-density?Magnetic?Recording，Berlin；New?York：Springer，2001
[2]R.F.C.Farrow，D.Weller，R.F.Marks，et?al.J.Appl.Phys.1996，79(8)，5967-5969；Chen?J.S.Lim?B.C.Wang?J.P.Appl.Phys.Lett.81，2002，(10)：1848-1850；Xu?Y.F.Chen?J.S.WangJ.P.Appl.Phys.Lett.2002，80(18)：3325-3327；Z.G.Zhang，K.Kang?and?T.Suzuki，Appl.Phys.Lett.2003，83(9)，1785-1787；Maeda?T，IEEE?Trans.on?Magn.2005，41(10)：3331-3333
[3] X ray polycrystalline (powder) diffraction data storehouse (JCPDS:Joint Committee on Powder Diffraction Standards)
[4]S.S.P.Parkin，C.Kaiser，A.Panchula，P.M.Rice，B.Hughes，M.Samant?and?S.H.Yang，Nature?Materials，3，862，S.Yuasa，T.Nagahama，A.Fukushima，Y.Suzuki?and?K.Ando，NatureMaterials，3，868
Summary of the invention
It is simple to the objective of the invention is to propose a kind of preparation process, the method for preparation (200) texture Fe thin film that the preparation difficulty reduces, and the application of film aspect preparation super-high density magnetic storage medium that the inventive method prepares proposed.
The method of preparation (002) texture Fe thin film that the present invention proposes adopts magnetically controlled DC sputtering equipment, and concrete steps are as follows:
(1) deposition Fe film on substrate.
To put into the sputtering chamber of magnetron sputtering equipment through pretreated substrate; The background air pressure of sputtering chamber is dropped to less than 5 * 10
-8The vacuum environment of Torr begins to prepare film; As working gas, feed sputtering chamber with argon gas, make sputtering pressure not be higher than 5.0mTorr; Under an atmospheric pressure value of selecting, between substrate and pure Fe target, add a sputtering power (not limiting), on substrate, deposit the Fe film under the room temperature, thickness is 10nm-50nm;
(2) the Fe film is heat-treated.
After having deposited the Fe film, stop to feed working gas, with sputtering chamber draw back to air pressure less than 5 * 10
-8The vacuum environment of Torr.Open the halogen lamp of sample (Fe film above the substrate) top, sample is carried out irradiated heat, temperature rise rate is controlled between 20 ℃/min～50 ℃/min, and keeps less than 1 * 10
-6The vacuum environment of Torr, annealing temperature are controlled at 400 ℃-600 ℃, specifically decide on the Fe film thickness, and annealing time is 10-20 minute, promptly obtain (200) texture Fe thin film.Annealing is turned off power supply, the film sample naturally cooling after finishing.
Among the present invention, substrate can adopt glass, and the pretreated usual method of substrate is: substrate is put into liquid detergent solution, use ultrasonic about 15 minutes of Ultrasonic Cleaners, use a large amount of deionized water rinsings.Again substrate is put into 1: 1 solution of 98% vitriol oil and hydrogen peroxide and soaked about 15 minutes, use a large amount of washed with de-ionized water.Then cleaned substrate is dried up.Be sent to sputtering chamber.Background air pressure Deng sputtering chamber is reduced to less than 5 * 10
-8Begin to prepare film after the Torr.
Among the present invention, the crystal grain that directly deposits the Fe film that obtains under the room temperature is imperfect, and X-ray diffraction analysis demonstrates these crystal grain and presents faint (110) orientation.By to the further thermal treatment of film, can obtain to have the Fe film of fine (002) texture.Because common vacuum sputtering equipment has the add in-place thermic devices, therefore can be used for film preparation and sample thermal treatment simultaneously.
(200) texture Fe thin film by method for preparing obtains can be used as magnetic recording material L1
0The buffer layer of phase FePt film, thus obtaining to use aspect the preparation super-high density magnetic storage medium.Specific practice is: be prepared into after (002) texture Fe thin film, underlayer temperature is elevated to 480 ℃～520 ℃, the FePt film of growing thereon then.Here method and the control condition of FePt film of growing is the same with the method for common growth FePt film.Experimental result shows L1
0The c axle of phase FePt ordered alloy film is perpendicular to film surface, and the diffusion of Fe atom between Fe buffer layer and FePt film simultaneously makes the composition of FePt in the bilayer film depart from the composition of FePt single thin film.
The structure of film adopts X-ray diffractometer (XRD) to measure, and the appearance of Fe (110) and (200) diffraction peak illustrates the existence of Fe in the film (110) and (200) structure respectively.For the FePt film, (002) is the basic peak of its c axle orientation, all exists in order and in the disordered structure; And (001) peak is the superlattice peaks, only is present in the ordered structure.Therefore, characterize the ordering degree of film usually with the intensity rate S of (001) and (002) diffraction peak.
Description of drawings
Fig. 1 is the diffracting spectrum of Corning Glass/Fe (15nm) film, and wherein (a) and (b) are respectively the XRD figure without annealing and annealed sample.
Fig. 2 is Corning Glass/Fe (10nm, 15nm, 25nm, 50nm) diffracting spectrum of annealing gained sample under differing temps.Wherein, (a1), (a2), (a3), (a4) are that the Fe sample of 10nm is respectively through the XRD figure spectrum after 600 degree, 500 degree, 400 degree, the 300 degree annealing; (b1), (b2), (b3), (b4) are that the Fe sample of 15nm is respectively through the XRD figure spectrum after 600 degree, 500 degree, 400 degree, the 300 degree annealing; (c1), (c2), (c3), (c4) are that the Fe sample of 25nm is respectively through the XRD figure spectrum after 600 degree, 500 degree, 400 degree, the 300 degree annealing; (d1), (d2), (d3), (d4) are that the Fe sample of 50nm is respectively through the XRD figure spectrum after 600 degree, 500 degree, 400 degree, the 300 degree annealing.
Fig. 3 is the diffracting spectrum of Corning Glass/Fe (15nm) film spatter film forming under different capacity.Wherein, (a) and (b), (c), (d) are respectively the XRD figure spectrums of sputtering power sample when being 120W, 95W, 50W, 40W.
Fig. 4 is the diffracting spectrum of Corning Glass/Fe (15nm) film spatter film forming under different air pressure.Wherein, (a) and (b), (c), (d) are respectively the XRD figure spectrums of sputtering pressure sample when being respectively 12.0mTorr, 8.0mTorr, 5.0mTorr, 2.0mTorr.
Fig. 5 is Corning Glass/Fe (15nm)/FePt (7nm) at fixing Pt sputtering power is 40W, changes the X ray diffracting spectrum of sample of the sputtering power preparation of Fe.Wherein, the different sputtering powers of (a) and (b), (c), (d), the corresponding Fe of (e) difference: 20W, 30W, 50W, 60W and 80W.
Embodiment
Further specifically describe the present invention below by embodiment.
Embodiment 1.Corning Glass/Fe (15nm) annealing and unannealed contrast
The CMS-18 multifunctional magnetic control sputtering equipment that computerizeds control prepares Corning Glass/Fe (15nm) sample.Adopt Corning Glass (corning glass) as substrate, sputtering power is 80W, and sputtering pressure 3.0mTorr, Fe film thickness are 15nm.Use the tungsten-iodine lamp irradiation sample at last in a vacuum, 600 ℃ of following in-situ annealing 15 minutes.As shown in Figure 1, (a) and (b) be respectively Fe sample deposition attitude and annealed after XRD figure spectrum.Deposition aspect product have only faint (110) peak, illustrate that its crystal grain step is complete, and present (110) orientation.Sample has only very strong (200) diffraction peak after the annealing, illustrates that prepared polycrystal film realized (002) texture fully.
Embodiment 2.Corning Glass/Fe (10nm, 15nm, 25nm, 50nm) relation of thickness and annealing temperature
The CMS-18 multifunctional magnetic control sputtering equipment that computerizeds control prepare the Fe film sample of different thickness: CorningGlass/Fe (10nm, 15nm, 25nm, 50nm).Adopt Corning Glass as substrate, sputtering power is 70W, and sputtering pressure is 4.0mTorr, and the thickness of controlling the Fe film by the control sputtering time is respectively: 10nm, 15nm, 25nm, 50nm.Use the tungsten-iodine lamp irradiation sample at last in a vacuum, annealed 15 minutes down at 300 ℃, 400 ℃, 500 ℃, 600 ℃ respectively.As shown in Figure 2, (a1), (a2), (a3), (a4) are that the Fe sample of 10nm is composed through the XRD figure after 600 ℃, 500 ℃, 400 ℃, the 300 ℃ annealing respectively.When 300 ℃ of thermal treatment, can't see (110) diffraction peak in the X-ray spectrogram; After annealing temperature was elevated to 400 ℃, (200) peak began to occur, and along with the raising of temperature becomes obviously gradually, and form well (002) texture; (b1), (b2), (b3), (b4) are that the Fe sample of 15nm is composed through the XRD figure after 600 ℃, 500 ℃, 400 ℃, the 300 ℃ annealing respectively.When 300 ℃ of thermal treatment, faint (110) diffraction peak appears in the X-ray spectrogram; Similarly, through having realized (002) texture in 400 ℃ .500 ℃ and 600 ℃ of heat treated Fe films; (c1), (c2), (c3), (c4) are that the Fe sample of 25nm is composed through the XRD figure after 600 ℃, 500 ℃, 400 ℃, the 300 ℃ annealing respectively.It should be noted that heat treated sample under lesser temps (300,400 ℃), demonstrate (110) texture, and all realize completely (200) structure through comparatively high temps (300 ℃, 400 ℃) annealed sample; (d1), (d2), (d3), (d4) are that the Fe sample of 50nm is composed through the XRD figure after 600 ℃, 500 ℃, 400 ℃, the 300 ℃ annealing respectively.The result shows, could realize completely (002) texture at the Fe of 600 ℃ of preparations film.This shows that under identical heat-treat condition, obtaining well, the thermal treatment temp of (002) texture increases along with the thickness of Fe film.
Embodiment 3.Corning Glass/Fe (15nm) changes sputtering power
The CMS-18 multifunctional magnetic control sputtering equipment that computerizeds control prepares Corning Glass/Fe (15nm) under different capacity.Adopt Corning Glass as substrate, sputtering pressure 3.0mTorr, film thickness remains on 15nm, sputter under the room temperature.Deposition is carried out irradiated heat with tungsten-iodine lamp to sample after finishing in a vacuum, anneals 15 minutes down at 600 ℃.As shown in Figure 3, (a) and (b), (c), (d) are respectively the XRD figure spectrums of sputtering power sample when being 120W, 95W, 50W, 40W.The result shows to have only (200) diffraction peak to occur, and shows at the Fe film and has realized completely (002) texture.This shows that preparation of realization (002) texture Fe thin film and sputtering power have nothing to do.
Embodiment 4-Corning Glass/Fe (15nm) changes sputtering pressure
The CMS-18 multifunctional magnetic control sputtering equipment that computerizeds control prepares Corning Glass/Fe (15nm) under different sputtering pressures.Adopt Corning Glass as substrate, sputtering power is 80W, and sputtering pressure is 12.0mTorr, 8.0mTorr, 5.0mTorr, 2.0mTorr, and film thickness remains 15nm, sputter under the room temperature.Use the tungsten-iodine lamp irradiation sample then in a vacuum, annealed 15 minutes down at 600 ℃ respectively.As shown in Figure 4, (a) and (b), (c), (d) are respectively the XRD figure spectrums of sputtering pressure sample when being respectively 12.0 mTorr, 8.0mTorr, 5.0mTorr, 2.0mTorr.When air pressure is not less than 8.0mTorr, (110) and (200) diffraction peak appears in the film that is obtained simultaneously, show the crystal grain that has (110) and (200) orientation in the Fe film simultaneously.And when sputtering pressure was lower than 5.0mTorr, film presented very strong (200) diffraction peak, and (110) diffraction peak is very faint, shows the Fe film that can obtain to have fine (002) texture under this condition.
Embodiment 5.Corning Glass/Fe (15nm)/FePt (7nm)
The CMS-18 multifunctional magnetic control sputtering equipment that computerizeds control has prepared Corning Glass/Fe (15nm).Adopt Corning Glass as substrate, sputtering power is 80W, and sputtering pressure 3.0mTorr, thickness are 15nm.Use the tungsten-iodine lamp irradiation sample then in a vacuum, 600 ℃ of following in-situ annealing 15 minutes.At last, under 500 ℃ condition, by the method for cosputtering, growth FePt film on the Fe film surface, fixedly the sputtering power of Pt is 40W, the sputtering power of Fe changes to 80W from 20W, the departing from of the FePt composition that causes with the diffusion that compensates the Fe atom.Sputtering pressure 5.0mTorr, thickness are 7nm.As shown in Figure 5, (001) of FePt and (002) diffraction peak clearly, and (111) peak is very faint, show obtained to have (001) texture, the c axle is perpendicular to the L1 of film surface
0Phase FePt ordered alloy film.
Claims (2)
1. a method for preparing (002) texture Fe thin film adopts magnetically controlled DC sputtering equipment, and concrete steps are as follows:
(1) deposition Fe film on substrate
To put into the sputtering chamber of magnetron sputtering equipment through pretreated substrate; The background air pressure of sputtering chamber is dropped to less than 5 * 10
-8The vacuum environment of Torr begins to prepare film; As working gas, feed sputtering chamber with argon gas, make sputtering pressure not be higher than 5.0mTorr; Under an atmospheric pressure value of selecting, between substrate and pure Fe target, add a sputtering power, on substrate, deposit the Fe film under the room temperature, thickness is 10nm-50nm;
(2) the Fe film is heat-treated
After having deposited the Fe film, stop to feed working gas, with sputtering chamber draw back to air pressure less than 5 * 10
-8The vacuum environment of Torr is opened the halogen lamp of sample top, and sample is carried out irradiated heat, and temperature rise rate is controlled between 20 ℃/min～50 ℃/min, and keeps less than 1 * 10
-6The vacuum environment of Torr, annealing temperature are controlled at 400 ℃-600 ℃, and annealing time is 10-20 minute, promptly obtain (200) texture Fe thin film.
2. method for preparing magnetic storage medium FePt film is characterized in that (200) texture Fe thin film of utilizing the described method of claim 1 to prepare, as magnetic recording material L1
0The buffer layer of phase FePt film, thus obtaining to use aspect the preparation super-high density magnetic storage medium.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101886243A (en) * | 2010-07-14 | 2010-11-17 | 中国科学院长春应用化学研究所 | Method for preparing iron thin film |
| CN101752158B (en) * | 2008-12-03 | 2011-08-31 | 中国科学院电子学研究所 | Method for improving slow wave component heat dispersion by utilizing nano material |
| CN108642463A (en) * | 2018-06-04 | 2018-10-12 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of preparation method for electrode laminated film before solar cell |
| CN110580938A (en) * | 2019-09-24 | 2019-12-17 | 天津大学 | Method for regulating vapor deposition metal film texture by constructing texture model by texture yield anisotropy |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US5824409A (en) * | 1995-11-13 | 1998-10-20 | Board Of Regents | High coercivity longitudinal recording media and method for its preparation |
| CN1317695C (en) * | 2005-07-06 | 2007-05-23 | 北京科技大学 | Method for improving L10-Fept thin film performance with surface activating agent |
| CN100390865C (en) * | 2006-06-29 | 2008-05-28 | 复旦大学 | Method for directional control growth of L10-FePt |
| CN100510190C (en) * | 2006-11-30 | 2009-07-08 | 复旦大学 | Method for preparing c-shaft vertically aligned L10 phase FePt magnetic recording film |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101752158B (en) * | 2008-12-03 | 2011-08-31 | 中国科学院电子学研究所 | Method for improving slow wave component heat dispersion by utilizing nano material |
| CN101886243A (en) * | 2010-07-14 | 2010-11-17 | 中国科学院长春应用化学研究所 | Method for preparing iron thin film |
| CN101886243B (en) * | 2010-07-14 | 2012-05-30 | 中国科学院长春应用化学研究所 | Method for preparing iron thin film |
| CN108642463A (en) * | 2018-06-04 | 2018-10-12 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of preparation method for electrode laminated film before solar cell |
| CN110580938A (en) * | 2019-09-24 | 2019-12-17 | 天津大学 | Method for regulating vapor deposition metal film texture by constructing texture model by texture yield anisotropy |
| CN110580938B (en) * | 2019-09-24 | 2023-05-26 | 天津大学 | Method for regulating and controlling texture of deposited metal film by utilizing texture yield anisotropy |
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