CN101206945A - Method of preparing multi-component high-frequency thin ferromagnetic film material with component gradient - Google Patents

Method of preparing multi-component high-frequency thin ferromagnetic film material with component gradient Download PDF

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CN101206945A
CN101206945A CNA2007100098480A CN200710009848A CN101206945A CN 101206945 A CN101206945 A CN 101206945A CN A2007100098480 A CNA2007100098480 A CN A2007100098480A CN 200710009848 A CN200710009848 A CN 200710009848A CN 101206945 A CN101206945 A CN 101206945A
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target
sputter
main material
film material
ferromagnetic
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李山东
杜正恭
刘美梅
王大伟
李培友
程唤龄
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Fujian Normal University
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Fujian Normal University
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Abstract

The invention relates to a method for preparing a high-frequency ferromagnetic film material with component gradient under the room temperature condition. The invention adopts the proposal that in a vacuum thin film gradient sputtering device, a ferromagnetic material is adopted as a main material target and arranged below a sputtered base plate; simple substances, oxides, nitrides, borides, carbides or phosphides are taken as adulterants to be arranged at the position outwards deviated from the center of the base plate, during the sputtering, the components of the main material target form an even film on the base plate, and the components of an adulterant target form a film provided with the components of the adulterants and distributed in gradient form along a certain direction. The invention adopts the design that the main material target is rightly opposite and the adulterant target is eccentric, the graded distribution of the components of the adulterants is realized, and the purpose that the uniaxial anisotropy is obtained is attained. The saturation magnetization (Ms) of the prepared film material is 8 to 25 kG, the equivalent field (Hk) of the uniaxial anisotropy, etc. is 50 to 400 Oe or higher, and the self-resonant frequency is close to 3G Hz or higher.

Description

A kind of preparation method with multicomponent high-frequency thin ferromagnetic film material of component gradient
Technical field
The present invention relates to a kind of preparation method of high-frequency thin ferromagnetic film material, particularly at ambient temperature a kind of, promptly possess the preparation method of the multicomponent high-frequency thin ferromagnetic film material with component gradient of high uniaxial anisotropy without heat treatment.
Technical background
When the ripe gradually development in communications market, relevant IC uses especially and constantly grows up, and has had increasing manufacturer to improve the application percentage of system's single crystalline chip (SOC).On real product is made, be not that various spare parts all are suitable for integrated processing procedure.Wherein inductance element occupies bigger area, and the past can't be designed into it in integrated circuit always.In recent years, the application of high-frequency thin ferromagnetic film material makes inductance element participate in the integrated possibility that becomes.At present, high-frequency thin ferromagnetic film material and planar inductor integration technology are widely used in (T.Sato, E.Komai, K.Yamasawa, T.Hatanai, A.Makino, IEEE Trans.on Magn., 33 (1997) 3310-3312 in the integrated processing procedure of passive device; V.Korenivski and R.B.vanDover, J.Appl.Phys., 82 (1997) 5247-5254; K.Ikeda, K.Kobayashi, K.Ohta, R.Kondo, T.Suzuki, and M.Fujimoto, IEEE Trans.on Magn., 39 (1997) 3057-3061).Because the adding of ferromagnetic thin film material can improve the inductance value and the quality factor of inductance coil, thereby plays reduced volume, improve the effect of usefulness.At present, be used widely at aspects such as DC-DC transducer, filter, adjuster, phase-shifters (C.S.Kim, S.Bae, H.J.Kim, S.E.Nam, H.J.Kim, IEEE Trans.on Magn., 37 (2001) 2894-2896 of ferromagnetic inductance; M.Yamaguchi, K.Yamada, andK.H.Kim, IEEE Trans.on Magn., 42 (2006) 3341-3343; Y.Hayakawa, A.Makino, H.Fujimori, and A.Inoue, J.Appl.Phys., 81 (1997) 3747-3752; B.Orlando, A.-S.Royer, and B.Viala, IEEE Trans.on Magn., 42 (2001) 3371-3373).In these applications, the high-frequency iron magnetic property of ferromagnetic thin film becomes the key factor of integrated processing procedure.The general requirement of these ferromagnetic materials has high saturation magnetization, uniaxial anisotropy and big resistivity, therefore, generally select the ferromagnetic material of iron cobalt-based and so on for use, and utilize the 300-600 ℃ of magnetic-field heat treatment under the condition, the high-frequency iron magnetic membrane material material (S.Jin that has uniaxial anisotropy with generation, W.Zhu, R.B.van Dover, T.H.Tiefel, V.Korenivski, and L.H.Chen, Appl.Phys.Lett., 70 (1997) 3161-3163; L.H.Chen, Y.H.Shih, K.A.Ellis, S.Jm, R.B.van Dover, and T.J.Klemmer, IEEE Trans.on Magn., 36 (2000) 3418-3420; I.Fergen, K.Seemann, A.v.d.Weth, A.Sch ü ppen, J.Magn.Magn.Mater., 242-245 (2002) 146-151).Heat treatment under so higher temperature has not only increased manufacturing cost, the more important thing is with traditional Si basis set to become metallization processes incompatible, cause the impaired of other element, even it is impossible that preparation process is become.
Summary of the invention
The invention provides a kind of problem that can solve the above multi-element film material preparation of ternary simultaneously and become compatible two aspects of metallization processes with the Si basis set, obtained under the room temperature preparation conditioned disjunction varying temperature environment, and promptly possessed the preparation method of high uniaxial anisotropy and the ferromagnetic thin-film material of high frequency without heat treatment.This method is integrated for ferromagnetic thin film and other element, realizes that integrated processing procedure is highly beneficial, thereby has solved a ferromagnetic film and the incompatible difficult problem of other element processing procedure in the traditional handicraft.
The present invention realizes by following concrete technical scheme: in vacuum film gradient sputter equipment, adopting ferromagnetic material is the main material target, places by under the substrate of sputter; Simultaneously, be the alloy target material with element simple substance, oxide, nitride, boride, carbide or phosphide, place the position of outwards departing from substrate center, carry out the sputter reaction, prepare a kind of multicomponent high-frequency thin ferromagnetic film material with component gradient.On this substrate, form the film of equal Uniform during sputter from the composition of main material target, form the film that has alloy composition distribution gradient along a certain direction from the composition of alloy target.
The ferromagnetic material that is used for the main material target described in the present invention is metal ferromagnetic material, nonmetal ferromagnetic material or oxide ferromagnetic material.Wherein: the metal ferromagnetic material is the alloy ferromagnetic material that Fe, Co or Ni elemental metals ferromagnetic material or Fe, Co or Ni metal and other magnesium-yttrium-transition metal, rare-earth metals form; Oxide, nitride, boride, carbide or the phosphide ferrimagnet of nonmetal ferrimagnet for further constituting by above-mentioned metal ferromagnetic material or alloy ferromagnetic material.
The metal material that is used to mix the thing target of the present invention is: Hf, Zr, Nb, Ta, Ru, Re, V, Mo, W, Cr or Al; Nonmetallic materials are mixed the thing target: Si, B or C; Oxide mixes the thing target: Al 2O 3, SiO 2, TiO 2, Ta 2O 5, V 2O 5, Nd 2O 3, HfO 2, ZrO 2Or Cr 2O 3Nitride material mixes the thing target: AlN, NbN, Ni 3N, TaN, ZrN or HfN; Boride material mixes the thing target: FeB, NiB or CoB; Carbide material mixes the thing target: Fe 3C, SiC, TaC or HfC; Phosphide material mixes the thing target: Fe 2P, Ni 5P 4Or CoP.
During the sputter reaction, vacuum cavity carries out sputter under the protection that charges into argon gas, argon oxygen gas mixture or argon nitrogen mixture gas, and sputter power and reaction sputter time are respectively: sputter power reacts 20～180 minutes sputter time between 10-350W.Utilize this method not only can on substrate, form the uniform film of composition to the material sputter of main material target, can obtain to have the high-frequency thin ferromagnetic film material of alloy target composition, distribution gradient along a certain direction.
Film gradient sputter equipment described in the present invention, constitute by electronic control system, target stand system, sputter substrate system, target stand system and sputter substrate system are in the vacuum cavity, be correspondingly set up and down, electronic control system is connected with target stand system, sputter substrate system respectively with power lead by holding wire.
Be provided with in the electronic control system of the present invention substrate temperature controller, rotational speed governor, main material target and alloy target radio-frequency power controller, gas flow controller, be positioned at water-cooled heter temperature auto-controller, the sputtering time controller of the substrate temperature that can raise on the substrate, and send line by holding wire, lead with target stand, vacuum orifice and gas injection port, the radio-frequency power power supply of stepping motor, main material target and alloy target respectively and link to each other.
Target stand of the present invention system is made up of 1～4 main material target stand, 1 alloy target stand, the fixed head that is used for fixing target stand.
Sputter substrate of the present invention system is made of the substrate of the stepping motor of controllable rotation speed, circular rotation sputter sample disc, sputter and the heater changing device that is positioned at the substrate top.
The present invention can also be on the basis of above-mentioned gradient sputter, by feeding argon oxygen or argon nitrogen mixture gas realization response sputter, to obtain to contain oxygen or nitrogenous gradient film material.
During preparation, be affixed on the bottom surface of circular rotation sputter sample disc by the substrate of sputter.When being rotated by the substrate oblong of sputter rotation sputter sample disc, moving 90 degree (3 main material targets and the alloy targets of revolution, being 90 degree central angles distributes) will just in time make by the substrate of sputter be positioned at the main material target directly over, and when turning to the alloy target, it is corresponding to be the misalignment shape by the substrate of sputter and alloy target.This main material target over against, and the design of alloy target off-centre, make that be uniform by sample on the substrate of sputter from the composition of main material target everywhere, and rotate the composition distribution gradient of the radial direction generation of sputter sample disc, thereby realize the Gradient distribution of alloy composition from the alloy target along circle.
The present invention has utilized the variation of concentration of dopant gradient, causes magnetic thin film inside to form the graded of stress along the concentration of dopant gradient direction, and then retrains magnetic moment direction, reaches the purpose that obtains uniaxial magnetic anisotropy.According to the amount difference of alloy, prepared high-frequency thin ferromagnetic film material, its saturation magnetization (M s) be worth at 8～25kG uniaxial anisotropy equivalent field (H k) 50～400Oe, or higher, self-resonant frequency is near 3GHz or higher.
In the multicomponent high-frequency thin ferromagnetic film material with component gradient of the present invention, it is M that their composition is expressed general formula xD yR zWherein: M is the composition combination from the main material target, x=50～99; D is the composition combination from the alloy target, y=1～50; R is O or the N composition that obtains from oxygen or nitrogen reactive sputtering, z=0～60; X+y+z=100.When z=0, represent to have only the gradient sputter under the argon shield, when z ≠ 0th, the reactive sputtering under expression argon oxygen or the argon nitrogen mixed gas atmosphere.Above numerical value is atomic percentage.
Table 1:
D value (mm) Fe(at.％) Co(at.％) Al(at.％) O(at.％)
2.5 36.38 42.55 3.29 17.78
7.5 37.64 42.08 3.00 17.28
12.5 39.63 42.05 2.50 15.83
17.5 38.91 42.69 2.43 15.97
22.5 38.92 43.70 2.29 15.09
27.5 40.11 43.10 2.06 14.73
32.5 40.72 42.86 1.90 14.52
37.5 40.85 43.25 1.81 14.10
42.5 40.04 44.48 1.74 13.74
47.5 40.72 44.03 1.65 13.60
Table 1 is (Fe 5Co 5) x-(Al 2O 3) yHave in the multicomponent high-frequency thin ferromagnetic film material of component gradient Fe, Co, Al, O in the doping system in each component distributing situation of sample diverse location.D value representation measurement point on film sample 16 length directions leaves the distance of the most close alloy target one end in the table.
Table 2:
D value (mm) Hf(at.％) Co(at.％) Fe(at.％)
0 14.02 23.35 62.63
3 13.55 23.48 62.97
6 12.83 23.57 63.6
9 11.97 23.69 64.34
12 11.25 23.84 64.91
15 10.67 24.03 65.3
18 10.13 24.21 65.66
21 9.76 24.29 65.95
24 9.36 24.41 66.23
27 9.07 24.5 66.43
30 8.77 24.59 66.64
Table 2 is (Fe 7Co 3) x-Hf yHave in the high-frequency thin ferromagnetic film material of component gradient Fe, Co and Hf in the doping system in each component distributing situation of sample diverse location.D value representation measurement point on film sample 16 length directions leaves the distance of the most close alloy target one end in the table.
Table 3:
D value (mm) Fe(at.％) Co(at.％) Hf(at.％) N(at.％)
10 44.24 19.22 14.71 21.82
15 45.40 19.20 13.20 22.20
20 46.20 20.60 11.30 21.90
25 48.45 20.74 10.87 19.94
30 49.60 20.84 9.12 20.44
35 49.25 22.12 8.81 19.82
40 51.50 22.00 7.90 18.60
45 51.95 22.52 7.61 17.92
50 51.70 21.24 7.11 19.94
Table 3 is (Fe 7Co 3) x-Hf yN zHave in the high-frequency thin ferromagnetic film material of component gradient Fe, Co, H f and N in the doping system in each component distributing situation of sample diverse location.D value representation measurement point on film sample 16 length directions leaves the distance of the most close alloy target one end in the table.
Table 4:
D value (mm) Zr(at.％) B(at.％) Co(at.％) Fe(at.％)
0 20.92 2.67 20.75 55.66
3 20.22 2.68 20.94 56.16
6 19.15 2.69 21.13 57.03
9 17.67 2.72 21.42 58.19
12 16.8 2.72 21.62 58.86
15 16 2.73 21.86 59.41
18 15.02 2.74 22.16 60.08
21 14.57 2.75 22.26 60.42
24 14.12 2.76 22.39 60.73
27 13.54 2.76 22.55 61.15
30 13.13 2.77 22.66 61.44
33 12.66 2.77 22.84 61.73
36 12.23 2.78 23.32 61.67
39 11.97 2.78 23.2 62.05
42 11.66 2.78 23.34 62.22
45 11.37 2.79 23.48 62.36
Table 4 is (Fe 7Co 3) x-Zr yB zHave in the high-frequency thin ferromagnetic film material of component gradient Fe, Co, Zr and B in the doping system in each component distributing situation of sample diverse location.D value representation measurement point on film sample 16 length directions leaves the distance of the most close alloy target one end in the table.
Accompanying drawing and description of drawings
Fig. 1 is a film gradient sputter equipment structural representation of the present invention.
Composition from the alloy target when Fig. 2 is sputter forms the film profile that has the distribution of alloy component gradient along a certain direction on this substrate.
Fig. 3 is (Fe 5Co 5) x-(Al 2O 3) ySystem Al component content is with the variation relation of position.
Fig. 4 is (Fe 5Co 5) x-(Al 2O 3) yThe VSM curve of system typical sample when the preparation attitude.
Fig. 5 is (Fe 5Co 5) x-(Al 2O 3) yThe magnetic spectrum figure of system typical sample when the preparation attitude.
Fig. 6 is (Fe 7Co 3) x-Hf yThe Hf composition is with the variation relation of position in the system sample.
Fig. 7 is (Fe 7Co 3) x-Hf yThe typical magnetic hysteresis loop of system gradient film.
Fig. 8 is (Fe 7Co 3) x-Hf yThe typical magnetic spectrum curve of system gradient film.
Fig. 9 is (Fe 7Co 3) x-Hf yN zHf component distributing in the reactive sputtering system sample.
Figure 10 is (Fe 7Co 3) x-Hf yN zThe typical magnetic hysteresis loop of reactive sputtering system gradient film.
Figure 11 is (Fe 7Co 3) x-Hf yN zThe typical magnetic spectrum curve of reactive sputtering system gradient film.
Figure 12 is (Fe 7Co 3) x-Zr yB zSystem gradient film Zr component distributing.
Among Fig. 1, among Fig. 1, the 1st, the associated electrical control system such as rf control unit in the film gradient sputter equipment, this electronic control system includes rf control unit, gas flow controller, the sputtering time controller of rotational speed governor, main material target and alloy target, and they are connected with controlled part by wire respectively; The 2nd, the alloy target; The 3rd, the target stand of alloy target is used for fixedly alloy target 2; The 4th, the target stand fixed head with liftable function; The 5th, the liftable screw rod that links to each other with the target stand fixed head is by screw rod 5 adjustable target seats 4 and by the distance between the substrate of sputter; The 6th, by the bleeding point of electronic control system 1 control; The 7th, target stand 4 recirculating cooling water systems, cold water is lower inlet opening extremely, enters by hose to be positioned at the hollow in the form of a ring cooling chamber of target stand, and by the upper water-out hole out, reduces the temperature of target stand with this; The 8th, the target stand of main material target; The 9th, the main material target; The 10th, by the substrate of sputter; The 11st, for fixing by the circular rotating sputter sample disc of sputter substrate 9; The 12nd, be positioned at the heater of substrate top, be used for the rising substrate temperature, to realize the alternating temperature sputter; The 13rd, by the air inlet of the injected protective gas of gas flow-control in the electronic control system 1, by he can be in the vacuum cavity pass into argon gas, argon oxygen gas mixture or argon nitrogen mixture gas; The 14th, vacuum cavity; The 15th, by the stepper motor of electronic control system 1 medium speed controller control.
Among Fig. 2, the 10th, by the sputter substrate; The 16th, possess the ferromagnetic thin-film material layer of high uniaxial anisotropy and high frequency.
Fig. 3～12 reflected Related Component content in the different systems with VSM curve when the preparation attitude of the variation relation of position, typical sample, typical hysteresis curve, sample the magnetic spectrum figure during in the preparation attitude etc. Digital proof gradient sputtering method can obtain good high-frequency soft magnetic performance among the figure, such as the resonant frequency of higher anisotropy field and 5.5 GHz. And the material of the corresponding system of reporting in the document, the poor performance that the material property that does not adopt gradient sputter preparation method to obtain obtains than the method illustrates that this preparation method has larger advantage. S and E are respectively that film sample is the most close and away from the site of an end of alloy target among Fig. 3, Fig. 6, Fig. 9, Figure 12.
Embodiment
In order further to understand technology side of the present invention scheme, the present invention is made specific description with by way of example.Present embodiment is only as to the further understanding of invention scheme, and not as the restriction of claim.
Embodiment 1
Preparation (Fe) x-(Nd) yO zThin-film material
Three main material target Fe and an alloy target Nd are put respectively on main material target target stand and alloy target target stand according to position shown in Figure 1, be 90 degree central angles between the target stand and arrange.To be fixed in circular rotation sputter sample disc 11 bottom surfaces by the substrate 10 of sputter, and with the corresponding arrangement of 90 degree central angles.Startup vacuumizes control system, when the background vacuum pressure is lower than 5 * 10 -6Behind the Torr, feed the mist two-way gas of high-purity Ar gas and Ar/O=10/1, the Ar throughput is 50sccm, and Ar/O mixed gas flow 5sccm starts circular rotation sputter sample disc 11 during vacuum chamber operating pressure 5.8mTorr, and rotating speed is made as 40 rev/mins.The sputtering power of main material target Fe and alloy target Nd is set to 80 and 30W respectively, and sputtering time is 80 minutes, can obtain (Fe) x-(Nd) yO zThe high-frequency thin ferromagnetic film material of system.
Embodiment 2
Preparation (Fe) x-(Nd 2O 3) yThin-film material
With reference to embodiment 1 described way, be the main material target with Fe, with Nd 2O 3Be the alloy target.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 20sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 2.8mTorr, and rotating speed is made as 30 rev/mins.Main material target Fe and alloy target Nd 2O 3Sputtering power be set to 160 and 170W respectively, sputtering time is 160 minutes, can obtain (Fe) x-(Nd 2O 3) yThe high-frequency thin ferromagnetic film material of system.
Embodiment 3
Preparation (Co) x-(Nd) yN zThin-film material
With reference to embodiment 1 described way, be that main material target, Nd are the alloy target with Co.Vacuum pressure is lower than 5 * 10 in vacuum cavity -6Behind the Torr, feed the mist two-way gas of high-purity Ar gas and Ar/N=10/1, the Ar throughput is 50sccm, and Ar/N mixed gas flow 10sccm starts circular rotation sputter sample disc during vacuum chamber operating pressure 6.0mTorrr, and rotating speed is made as 50 rev/mins.The sputtering power of main material target Co and alloy target Nd is set to 80 and 130W respectively, and sputtering time is 60 minutes, can obtain (Co) x-(Nd) yN zThe high-frequency thin ferromagnetic film material of system.
Embodiment 4
Preparation (Fe) x-(Sm) yN zThin-film material
With reference to embodiment 1 described way, be the main material target with Fe, be the alloy target with Sm.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed the mist two-way gas of high-purity Ar gas and Ar/N=10/1, the Ar throughput is 50sccm, Ar/N mixed gas flow 5sccm, start circular rotation sputter sample disc during vacuum chamber operating pressure 5.8mTorr, rotating speed is made as 40 rev/mins, and the sputtering power of main material target Fe and alloy target Sm is set to 80 and 20W respectively, sputtering time is 130 minutes, can obtain (Fe) x-(Sm) yN zThe high-frequency thin ferromagnetic film material of system.
Embodiment 5
Preparation (Fe 5Co 5) x-(Al 2O 3) yThin-film material
With reference to embodiment 1 described way, with Fe 5Co 5Be main material target, Al 2O 3For alloy target, single crystalline Si are substrate.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 20sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 2.8mTorr, and rotating speed is made as 20 rev/mins, main material target Fe 5Co 5With alloy target Al 2O 3Sputtering power all be set to 60W, sputtering time is 130 minutes, can obtain (Fe 5Co 5) x-(Al 2O 3) yThe high-frequency thin ferromagnetic film material of system.
Embodiment 6
Preparation (Fe 7Co 3) x-Hf yThin-film material
With reference to embodiment 1 described way, with Fe 7Co 3Be main material target, Hf yBe the alloy target.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 20sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 2.8mTorr, and rotating speed is made as 20 rev/mins, main material target Fe 7Co 3Be set to 160 and 180W respectively with the sputtering power of alloy target Hf, sputtering time is 120 minutes, can obtain (Fe 7Co 3) x-Hf yThe high-frequency thin ferromagnetic film material of system.
Embodiment 7
Preparation (Fe 7Co 3) xHf yN zThin-film material
With reference to embodiment 1 described way, with Fe 7Co 3For main material target, Hf are the alloy target.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed the mist two-way gas of high-purity Ar gas and Ar/N=10/1, the Ar throughput is 50sccm, Ar/N mixed gas flow 10sccm, start circular rotation sputter sample disc during vacuum chamber operating pressure 6.0mTorr, rotating speed is made as 30 rev/mins, main material target Fe 7Co 3Be set to 180 and 220W respectively with the sputtering power of alloy target Hf, sputtering time is 180 minutes, can obtain (Fe 7Co 3) x-Hf yN zThe high-frequency thin ferromagnetic film material of system.
Embodiment 8
Preparation (Fe 7Co 3) x-Zr yB zThe system thin-film material
With reference to embodiment 1 described way, be provided with two main material targets, with Fe 7Co 3For principal component, with Zr is the alloy target.When the background vacuum pressure is lower than 5 * 10 -6Behind the Torr, feed high-purity Ar gas, the Ar throughput is 25sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 3.0mTorr, and rotating speed is made as 50 rev/mins.Two main material target, one the sputtering power of alloy target Zr are set to 80,80 and 60W respectively, and sputtering time is 40 minutes, can obtain (Fe 7Co 3) x-Zr yB zThe high-frequency thin ferromagnetic film material of system.
Embodiment 9
Preparation (Fe 5Co 5) x-(AlN) yThin-film material
With reference to embodiment 1 described way, be provided with three main material targets and an alloy target, with Fe 5Co 5For the main material target, with AlN is the alloy target.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 30sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 3.2mTorr, and rotating speed is made as 40 rev/mins.Main material target Fe 5Co 5Be set to 80 and 120W respectively with the sputtering power of alloy target AlN, sputtering time is 80 minutes, can obtain (Fe 5Co 5) x-(AlN) yThe high-frequency thin ferromagnetic film material of system.
Embodiment 10
Preparation (Fe 7Co 3) xC yThin-film material
With reference to embodiment 1 described way, be provided with the target stand of four main material targets and an alloy target, be 72 degree central angles and arrange, with main material target Fe 7Co 3Put respectively on main material target and alloy target target stand with alloy target C.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 20sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 2.8mTorr, and rotating speed is made as 40 rev/mins.Main material target Fe 7Co 3Be set to 80 and 140W respectively with the sputtering power of alloy target C, sputtering time is 150 minutes, can obtain (Fe 7Co 3) xThe high-frequency thin ferromagnetic film material of-C system.
Embodiment 11
Preparation (Fe 5Co 5) x-(TaC) yThe system thin-film material
With reference to embodiment 1 described way, present embodiment is provided with the target stand of four main material targets and an alloy target, is 72 degree central angles and arranges, with main material target Fe 5Co 5Put respectively on main material target and alloy target target stand with alloy target TaC.Substrate is fixed in circular rotation sputter sample disc bottom surface, and with the corresponding arrangement of 72 degree central angles.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 30sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 3.2mTorr, and rotating speed is made as 30 rev/mins.Main material target Fe 5Co 5Be set to 60 and 220W respectively with the sputtering power of alloy target TaC, sputtering time is 60 minutes, can obtain (Fe 5Co 5) x-(TaC) yThe high-frequency thin ferromagnetic film material of system.
Embodiment 12
Preparation (Fe 7Co 3) x-(CoP) yThin-film material
With reference to embodiment 1 described way, present embodiment is provided with the target stand of three main material targets and an alloy target, is 90 degree central angles and arranges.With main material target Fe 7Co 3Put respectively on the target stand of main material target and alloy target with alloy target CoP.Substrate is fixed in ground under the circular rotation sputter sample disc, and with the corresponding arrangement of 90 degree central angles.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 30sccm, starts circular rotation sputter sample disc during vacuum cavity operating pressure 3.2mTorr, and rotating speed is made as 30 rev/mins.Main material target Fe 7Co 3Be set to 60 and 80W respectively with the sputtering power of alloy target CoP, sputtering time is 70 minutes, can obtain (Fe 7Co 3) x-(CoP) yThe high-frequency thin ferromagnetic film material of system.
Embodiment 13
Preparation (Fe 5Ni 5) x-(SiO 2) yThin-film material
With reference to embodiment 1 described way, present embodiment is provided with two main material targets and an alloy target, is 120 degree central angles and arranges, and the main material target is Fe 5Ni 5, the alloy target is SiO 2Substrate is fixed in ground under the circular rotation sputter sample disc, and with the corresponding arrangement of 120 degree central angles.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 20sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 2.8mTorr, and rotating speed is made as 20 rev/mins.Main material target Fe 5Ni 5With alloy target SiO 2Sputtering power be set to 160 and 280W respectively, sputtering time is 40 minutes, can obtain (Fe 5Ni 5) x-(SiO 2) yThe high-frequency thin ferromagnetic film material of system.
Embodiment 14
Preparation (Fe 5Ni 5) xB yThin-film material
With reference to embodiment 1 described way, present embodiment is provided with two main material targets and an alloy target, is 120 degree central angles and arranges, and the main material target is Fe 5Ni 5, the alloy target is B, puts respectively on the target stand of main material target and alloy target.Substrate is fixed in ground under the circular rotation sputter sample disc, and with the corresponding arrangement of 120 degree central angles.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 20sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 2.8mTorr, and rotating speed is made as 40 rev/mins.Main material target Fe 5Ni 5Be set to 60 and 80W respectively with the sputtering power of alloy target B, sputtering time is 80 minutes, can obtain (Fe 5Ni 5) x-B yThe high-frequency thin ferromagnetic film material of system.
Embodiment 15
Preparation (Fe 5Ni 5) x-(FeB) yThin-film material
With reference to embodiment 1 described way, present embodiment is provided with four main material targets and an alloy target, is 72 degree central angles and arranges, and the main material target is Fe 5Ni 5, the alloy target is FeB, puts respectively on the target stand of main material target and alloy target.Substrate is fixed in ground under the circular rotation sputter sample disc, and with the corresponding arrangement of 72 degree central angles.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 30sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 3.2mTorr, and rotating speed is made as 40 rev/mins.Main material target Fe 5Ni 5All be set to 280W with the sputtering power of alloy target FeB, sputtering time is 30 minutes, can obtain (Fe 5Ni 5) x-(FeB) yThe high-frequency thin ferromagnetic film material of system.
Embodiment 16
Preparation (Fe 7Ni 3) x-Ta yThin-film material
With reference to embodiment 1 described way, present embodiment is provided with a main material target and an alloy target, is 180 degree central angles and arranges, and the main material target is Fe 7Ni 3, the alloy target is Ta, puts respectively on the target stand of main material target and alloy target.Substrate is fixed in ground under the circular rotation sputter sample disc, and with the corresponding arrangement of 180 degree central angles.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 20sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 2.8mTorr, and rotating speed is made as 20 rev/mins.Main material target Fe 7Ni 3All be set to 260W with the sputtering power of alloy target Ta, sputtering time is 60 minutes, can obtain (Fe 7Ni 3) x-Ta yThe high-frequency thin ferromagnetic film material of system.
Embodiment 17
Preparation (Fe 7Ni 3) x-(ZrN) yThin-film material
With reference to embodiment 1 described way, present embodiment is provided with two main material targets and an alloy target, is 120 degree central angles and arranges, and the main material target is Fe 7Ni 3, the alloy target is ZrN, puts respectively on the target stand of main material target and alloy target.Substrate is fixed in ground under the circular rotation sputter sample disc, and with the corresponding arrangement of 120 degree central angles.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 20sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 2.8mTorr, and rotating speed is made as 20 rev/mins.Main material target Fe 7Ni 3Be set to 40 and 100W respectively with the sputtering power of alloy target ZrN, sputtering time is 80 minutes, can obtain (Fe 7Ni 3) x-(ZrN) yThe high-frequency thin ferromagnetic film material of system.
Embodiment 18
Preparation (Fe 6Ni 4) x-Al yN zThin-film material
With reference to embodiment 1 described way, present embodiment is provided with two main material targets and an alloy target, is 120 degree central angles and arranges, and the main material target is Fe 6Ni 4, the alloy target is AlN, puts respectively on the target stand of main material target and alloy target.Substrate is fixed in ground under the circular rotation sputter sample disc, and with the corresponding arrangement of 120 degree central angles.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed the mist two-way gas of high-purity Ar gas and Ar/N=10/1, the Ar throughput is 50sccm, and Ar/N mixed gas flow 10sccm starts circular rotation sputter sample disc during vacuum chamber operating pressure 6.0mTorr, and rotating speed is made as 10 rev/mins.Main material target Fe 6Ni 4Be set to 50 and 80W respectively with the sputtering power of alloy target AlN, sputtering time is 60 minutes, can obtain (Fe 6Ni 4) x-Al yN zThe high-frequency thin ferromagnetic film material of system.
Embodiment 19
Preparation (Fe 4Co 4Ni 2) x-(V 2O 5) yThin-film material
With reference to embodiment 1 described way, present embodiment is provided with four main material targets and an alloy target, is 72 degree central angles and arranges, and the main material target is Fe 4Co 4Ni 2, the alloy target is V 2O 5, put respectively on the target stand of main material target and alloy target.Substrate is fixed in ground under the circular rotation sputter sample disc, and with the corresponding arrangement of 72 degree central angles.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 20sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 2.8mTorr, and rotating speed is made as 20 rev/mins.Main material target Fe 4Co 4Ni 2With alloy target V 2O 5Sputtering power be set to 60 and 120W respectively, sputtering time is 60 minutes, can obtain Fe 4Co 4Ni 2) x-(V 2O 5) yThe high-frequency thin ferromagnetic film material of system.
Embodiment 20
Preparation (Fe 4Co 4Ni 2) x-(Nb) yThin-film material
With reference to embodiment 1 described way, present embodiment is provided with three main material targets and an alloy target, is 90 degree central angles and arranges, and the main material target is Fe 4Co 4Ni 2, the alloy target is Nb, puts respectively on the target stand of main material target and alloy target.Substrate is fixed in ground under the circular rotation sputter sample disc, and with the corresponding arrangement of 90 degree central angles.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 30sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 3.2mTorr, and rotating speed is made as 12 rev/mins.Main material target Fe 4Co 4Ni 2Be set to 70 and 80W respectively with the sputtering power of alloy target Nb, sputtering time is 50 minutes, can obtain (Fe 4Co 4Ni 2) x-(Nb) yThe high-frequency thin ferromagnetic film material of system.
Embodiment 21
(Fe 4Co 4Ni 2) x(B) ySystem
Preparation (Fe 4Co 4Ni 2) x-B yThin-film material
With reference to embodiment 1 described way, present embodiment is provided with three main material targets and an alloy target, is 90 degree central angles and arranges, and the main material target is Fe 4Co 4Ni 2, the alloy target is B, puts respectively on the target stand of main material target and alloy target.Substrate is fixed in ground under the circular rotation sputter sample disc, and with the corresponding arrangement of 90 degree central angles.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 30sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 3.2mTorr, and rotating speed is made as 30 rev/mins.Main material target Fe 4Co 4Ni 2Be set to 60 and 280W respectively with the sputtering power of alloy target B, sputtering time is 60 minutes, can obtain (Fe 4Co 4Ni 2) x-B yThe high-frequency thin ferromagnetic film material of system.
Embodiment 22
(Fe 4Co 4Ni 2) x(HfN) ySystem
Preparation (Fe 4Co 4Ni 2) x-(HfN) yThin-film material
With reference to embodiment 1 described way, present embodiment is provided with four main material targets and an alloy target, is 72 degree central angles and arranges, and the main material target is Fe 4Co 4Ni 2, the alloy target is HfN, puts respectively on the target stand of main material target and alloy target.Substrate is fixed in ground under the circular rotation sputter sample disc, and with the corresponding arrangement of 72 degree central angles.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 30sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 3.2mTorr, and rotating speed is made as 40 rev/mins.Main material target Fe 4Co 4Ni 2Be set to 80 and 160W respectively with the sputtering power of alloy target HfN, sputtering time is 45 minutes, can obtain (Fe 4Co 4Ni 2) x-(HfN) yThe high-frequency thin ferromagnetic film material of system.
Embodiment 23
Preparation (Fe 4Co 4Ni 2) x-(Ni 5P 4) yThin-film material
With reference to embodiment 1 described way, present embodiment is provided with four main material targets and an alloy target, is 72 degree central angles and arranges, and the main material target is Fe 4Co 4Ni 2, the alloy target is Ni 5P 4, put respectively on the target stand of main material target and alloy target.Substrate is fixed in ground under the circular rotation sputter sample disc, and with the corresponding arrangement of 72 degree central angles.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 30sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 3.2mTorr, and rotating speed is made as 40 rev/mins.Main material target Fe 4Co 4Ni 2With alloy target Ni 5P 4Sputtering power all be set to 60W, sputtering time is 40 minutes, can obtain (Fe 4Co 4Ni 2) x-(Ni 5P 4) yThe high-frequency thin ferromagnetic film material of system.
Embodiment 24
(Fe 82Nd 10B 8) x(Nd) y(O) zSystem
Preparation (Fe 4Co 4Ni 2) x-(Nd) y(O) zThin-film material
With reference to embodiment 1 described way, present embodiment is provided with four main material targets and an alloy target, is 72 degree central angles and arranges, and the main material target is Fe 82Nd 10B 8, the alloy target is Nd, puts respectively on the target stand of main material target and alloy target.Substrate is fixed in ground under the circular rotation sputter sample disc, and with the corresponding arrangement of 72 degree central angles.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed the mist two-way gas of high-purity Ar gas and Ar/O=10/1, the Ar throughput is 50sccm, and Ar/O mixed gas flow 5sccm starts circular rotation sputter sample disc during vacuum chamber operating pressure 5.8mTorr, and rotating speed is made as 40 rev/mins.Main material target Fe 82Nd 10B 8Be set to 100 and 20W respectively with the sputtering power of alloy target Nd, sputtering time is 40 minutes, can obtain (Fe 4Co 4Ni 2) x-(Nd) y(O) zThe high-frequency thin ferromagnetic film material of system.
Embodiment 25
Preparation (NiFe 2O 4) x-(B) yThin-film material
With reference to embodiment 1 described way, present embodiment is provided with four main material targets and an alloy target, is 72 degree central angles and arranges, and the main material target is NiFe 2O 4, the alloy target is B, puts respectively on the target stand of main material target and alloy target.Substrate is fixed in ground under the circular rotation sputter sample disc, and with the corresponding arrangement of 72 degree central angles.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 30sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 3.2mTorr, and rotating speed is made as 40 rev/mins.Main material target NiFe 2O 4Be set to 60 and 180W respectively with the sputtering power of alloy target B, sputtering time is 100 minutes, can obtain (NiFe 2O 4) x-(B) yThe high-frequency thin ferromagnetic film material of system.
Embodiment 26
Preparation (CoFe 2O 4) x-(C) yThin-film material
With reference to embodiment 1 described way, present embodiment is provided with two main material targets and an alloy target, is 120 degree central angles and arranges, and the main material target is CoFe 2O 4, the alloy target is C, puts respectively on the target stand of main material target and alloy target.Substrate is fixed in ground under the circular rotation sputter sample disc, and with the corresponding arrangement of 120 degree central angles.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 30sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 3.2mTorr, and rotating speed is made as 10 rev/mins.Main material target CoFe 2O 4Be set to 200 and 180W respectively with the sputtering power of alloy target C, sputtering time is 120 minutes, can obtain (CoFe 2O 4) x-(C) yThe high-frequency thin ferromagnetic film material of system.
Embodiment 27
Preparation (NiMn) x-(Sb) yThin-film material
With reference to embodiment 1 described way, present embodiment is provided with two main material targets and an alloy target, is 120 degree central angles and arranges, and the main material target is NiMn, and the alloy target is Sb, puts respectively on the target stand of main material target and alloy target.Substrate is fixed in ground under the circular rotation sputter sample disc, and with the corresponding arrangement of 120 degree central angles.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 20sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 2.8mTorr, and rotating speed is made as 20 rev/mins.The sputtering power of main material target NiMn and alloy target Sb all is set to 80W, and sputtering time is 60 minutes, can obtain (NiMn) x-(Sb) yThe high-frequency thin ferromagnetic film material of system.
Embodiment 28
Preparation (CoMn) x-(Sb) yThin-film material
With reference to embodiment 1 described way, present embodiment is provided with a main material target and an alloy target, is 180 degree central angles and arranges, and the main material target is CoMn, and the alloy target is Sb, puts respectively on the target stand of main material target and alloy target.Substrate is fixed in ground under the circular rotation sputter sample disc, and with the corresponding arrangement of 180 degree central angles.Be lower than 5 * 10 at the background vacuum pressure -6Behind the Torr, feed high-purity Ar gas, flow is 20sccm, starts circular rotation sputter sample disc during vacuum chamber operating pressure 2.8mTorr, and rotating speed is made as 20 rev/mins.The sputtering power of main material target CoMn and alloy target Sb is set to 120 and 60W respectively, and sputtering time is 60 minutes, can obtain (CoMn) x-(Sb) yThe high-frequency thin ferromagnetic film material of system.

Claims (7)

1. the preparation method with multicomponent high-frequency thin ferromagnetic film material of component gradient is characterized in that in vacuum film gradient sputter equipment, and adopting ferromagnetic material is the main material target, places by under the substrate of sputter; With element simple substance, oxide, nitride, boride, carbide or phosphide is the alloy target material, places the position of outwards departing from substrate center, carries out the sputter reaction, prepares a kind of multicomponent high-frequency thin ferromagnetic film material with component gradient.
2. the preparation method with multicomponent high-frequency thin ferromagnetic film material of component gradient according to claim 1 is characterized in that described ferromagnetic material is meant metal ferromagnetic material, nonmetal ferromagnetic material or oxide ferromagnetic material.
3. the preparation method with multicomponent high-frequency thin ferromagnetic film material of component gradient according to claim 2 is characterized in that described metal ferromagnetic material is meant the alloy ferromagnetic material that forms into Fe, Co or Ni elemental metals ferromagnetic material or Fe, Co or Ni metal and other magnesium-yttrium-transition metal, rare-earth metals.
4. the preparation method with multicomponent high-frequency thin ferromagnetic film material of component gradient according to claim 2 is characterized in that oxide, nitride, boride, carbide or phosphide ferrimagnet that described nonmetal ferrimagnet or oxide ferromagnetic material further constitute for the alloy ferromagnetic material that is formed by Fe, Co or Ni elemental metals ferromagnetic material or Fe, Co or Ni metal and other magnesium-yttrium-transition metal, rare-earth metals.
5. the preparation method with multicomponent high-frequency thin ferromagnetic film material of component gradient according to claim 1 is characterized in that described mixing in the thing target material, and metal material is: Hf, Zr, Nb, Ta, Ru, Re, V, Mo, W, Cr or Al; Nonmetallic materials are: Si, B or C; Oxide is: Al 2O 3, SiO 2, TiO 2, Ta 2O 5, V 2O 5, Nd 2O 3, HfO 2, ZrO 2Or Cr 2O 3Nitride is: AlN, NbN, Ni 3N, TaN, ZrN or HfN; Boride is: FeB, NiB or CoB; Carbide is: Fe 3C, SiC, TaC or HfC; Phosphide is: Fe 2P, Ni 5P 4Or CoP.
6. the preparation method with multicomponent high-frequency thin ferromagnetic film material of component gradient according to claim 1 is characterized in that described alloy target material places the position of outwards departing from substrate center.
7. the preparation method with multicomponent high-frequency thin ferromagnetic film material of component gradient according to claim 1; when it is characterized in that described sputter reacts; vacuum cavity carries out sputter under the protection that charges into argon gas, argon oxygen gas mixture or argon nitrogen mixture gas; sputter power between 10-350W, 20～180 minutes sputter time.
CNA2007100098480A 2007-11-20 2007-11-20 Method of preparing multi-component high-frequency thin ferromagnetic film material with component gradient Pending CN101206945A (en)

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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
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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
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
CN102683003A (en) * 2012-05-03 2012-09-19 中国科学院宁波材料技术与工程研究所 Method for preparing single-shaft magnetic anisotropy thin film
CN103714942B (en) * 2013-12-27 2016-08-17 青岛大学 A kind of automatic biasing heterogeneous body microwave ferromagnetic thin film material and preparation method thereof
CN103646749A (en) * 2013-12-27 2014-03-19 青岛大学 Quasi-isotropy microwave ferromagnetic multilayer film and preparation method thereof
CN103714942A (en) * 2013-12-27 2014-04-09 青岛大学 Self-biased non-homogeneous microwave ferromagnetic thin film material and preparation method thereof
CN103646749B (en) * 2013-12-27 2015-10-14 青岛大学 A kind of quasi-isotropic microwave ferromagnetic multilayer film and preparation method thereof
CN105448463A (en) * 2016-01-14 2016-03-30 青岛大学 Optical mold ferromagnetic resonance enhancing multilayer film and preparation method of optical mold ferromagnetic resonance enhancing multilayer film
CN105448463B (en) * 2016-01-14 2017-12-22 青岛大学 A kind of multilayer film of optical mode ferromagnetic resonance enhancing and preparation method thereof
CN107895623A (en) * 2016-01-14 2018-04-10 青岛大学 A kind of multilayer film of optical mode ferromagnetic resonance enhancing
CN107895624A (en) * 2016-01-14 2018-04-10 青岛大学 A kind of multilayer film of optical mode ferromagnetic resonance enhancing
CN107895624B (en) * 2016-01-14 2020-01-10 青岛大学 Multilayer film with enhanced optical mode ferromagnetic resonance
CN105872937A (en) * 2016-04-29 2016-08-17 梧州恒声电子科技有限公司 Glue injecting production line for loudspeaker
CN115475745A (en) * 2022-10-26 2022-12-16 鞍钢集团北京研究院有限公司 Preparation process and coating method of vanadium oxide rare earth double-doped ferrite magnetic composite film slurry
CN115475745B (en) * 2022-10-26 2023-10-20 鞍钢集团北京研究院有限公司 Preparation process and coating method of vanadium oxide rare earth double-doped ferrite magnetic composite film slurry

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