CN102345104A - Preparation method of colossal magnetoresistance effect Fe-Ti-O amorphous film - Google Patents
Preparation method of colossal magnetoresistance effect Fe-Ti-O amorphous film Download PDFInfo
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- CN102345104A CN102345104A CN2011102875697A CN201110287569A CN102345104A CN 102345104 A CN102345104 A CN 102345104A CN 2011102875697 A CN2011102875697 A CN 2011102875697A CN 201110287569 A CN201110287569 A CN 201110287569A CN 102345104 A CN102345104 A CN 102345104A
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Abstract
A preparation method of a colossal magnetoresistance effect Fe-Ti-O amorphous film adopts an ultra-high vacuum three-target codeposition magnetron sputtering coating machine for the preparation, and comprises the following steps: 1) mounting a Ti target and a Fe target on a target head of the coating machine respectively; 2) mounting a glass substrate on a substrate support; 3) turning on the magnetron sputtering device to vacuumize a sputtering chamber; 4) introducing mixed gas of O2 and Ar into the vacuum chamber to obtain a vacuum degree of 1 Pa of the vacuum chamber; 5) turning on a sputtering direct-current power supply, applying a current and a voltage to the Ti target and the Fe target; 6) opening a baffle plate of the substrate, rotating the substrate support, growing a film on the substrate; 7) after the sputtering is completed, injecting nitrogen into the vacuum chamber to obtain the prepared target product. The advantages of the invention are that: the process method is simple and easy to carry out, and the prepared film has high room-temperature magnetoresistance effect; the production cost is low, and the method is applicable to large-scale popularization and application.
Description
Technical field
Semiconductor material technology of preparing of the present invention, particularly a kind of preparation method of large magnetic resistance effect Fe-Ti-O noncrystalline membrane.
Background technology
In the Fe/Cr magnetoresistance effect, found that (Giant Magnetoresistance, GMR), this work obtained Nobel Prize in physics in 2007 to giant magnetoresistance effect in 1988.After this, in non-homogeneous magnetic system (multilayer film, membrana granulosa, tunnel junction etc.), found many novel physical phenomenons successively, as wear then the type magneto-resistor (Tunnel Magnetoresistance, TMR), huge hall effect, high-coercive force, high-frequency soft magnetic property etc.Therefore, the research of spin correlation electron transport property in the non-homogeneous magnetic system and magnetic property becomes in recent years Materials science and condensed state physics field one of active subject the most.
Non-homogeneous magnetic system; (Giant Magnetoresistance, GMR) research has formed an emerging cross discipline-spintronics (Spintronics) gradually like the giant magnetoresistance effect in magnetoresistance effect, magneticmetal-non-magnetic metal, magneticmetal-isolator particle film system and the MTJ of antiferromagnetic coupling.Spintronics is handled with the existing information of using positive and negative charge and is compared through existing the character of two different states (upper and lower) to be applied in the information processing electron spinning, is expected to the electronic component of realizing that integrated level is high, current consumption is low, processing speed is high.The research of spintronics material and device roughly is divided into three phases, promptly is the research of GMR and the TMR magneto-resistance effect and the device thereof of representative with magnetoresistance effect, membrana granulosa, tunnel junction and Spin Valve; Transport the conceptual phase that performance is an object with spin correlation in magneticsemiconductor and the dilute magnetic semiconductor; Be the applied research stage of target with preparation spintronics device.
People such as Tian Yufeng observe the big positive magneto-resistance effect of low temperature (5K) in the Co-ZnO nanometer particle film; Peak can reach 811%; And the content of Co is closely related in the value of magneto-resistor and the film, but they think that the appearance of positive magneto-resistance effect suppresses relevant [ApplPhysLett92 (2008) 192109.] with the spin Zeeman effect to the transition of spin correlation range.German Research group finds 31% positive magneto-resistor [Thin Solid Films, 2006,515:2549.] during at 5K in the metal-doped ZnO film of 3d.Scientific research group of northeastern Japan university has found low temperature large magnetic resistance phenomenon in the Co-C60 laminated film, maximum can reach 85% [Appl Phys Lett, 2006,89:113118.] under appropriate current.The Liu Yihua professor of department of physics of Shandong University is at Fe-In
2O
3Found the remarkable reinforcing effect [JPhys:Condens Matter, 2003,15:47.] of magneto-resistor in the particle film.Magneto-resistance effect in these new systems will become the candidate material of novel spintronics device.Yet; The physical mechanism of magneto-resistance effect and Changing Pattern thereof is still unclear in these magneticmetal element-semi-conductor systems; Need the further investigation of system to separate bright its microphysics mechanism; Provide fundamental basis for its design, enrich the understanding of people simultaneously magneto-resistance effect at the spintronics device.In former study, do not provide the result of study of magneticmetal element doping titanium deoxid film magneto-resistance effect.
Summary of the invention
The objective of the invention is provides a kind of preparation method of large magnetic resistance effect Fe-Ti-O noncrystalline membrane to above-mentioned technical Analysis, and this process method technology is simple, easy to implement, and the film that makes has higher Investigation on Room-temperature Magnetoresistance; Production cost is low, is suitable for large-scale promotion application.
Technical scheme of the present invention:
A kind of preparation method of large magnetic resistance effect Fe-Ti-O noncrystalline membrane adopts the preparation of ultrahigh vacuum(HHV) three target codeposition magnetron sputtering coaters, and this step is following:
1) a Ti target and Fe target are installed respectively on the target head of coating equipment;
2) with behind the glass basic surface contaminant removal, install on the substrate frame, substrate up, target below, the distance of substrate and target is 13cm;
3) unlatching magnetron sputtering equipment successively starts the one-level mechanical pump and the secondary molecular pump vacuumizes, and vacuum tightness is greater than 8.5 * 10 at the bottom of the back of the body of sputtering chamber
-6Pa;
4) feed O to Vakuumkammer
2With the mixed gas of Ar, make that the vacuum tightness in the Vakuumkammer is 1Pa;
5) open the sputter direct supply, on Ti target Fe target, apply electric current and voltage respectively, sputter is 20 minutes in advance, waits sputtering current and voltage stable;
6) open the baffle plate of substrate, the speed of changeing with PM 2 is simultaneously rotated substrate frame, the titania-doped noncrystalline membrane of growth iron on substrate;
7) growing film was closed the baffle plate of substrate after 15 minutes, and substrate frame stops operating, and closed shielding power supply then, stopped to feed sputter gas Ar and O
2, close vacuum system after continuing to vacuumize half a hour, charging into purity to Vakuumkammer then is 99.999% nitrogen, presses when identical up to the air pressure and the outside atmosphere of Vakuumkammer, opens Vakuumkammer and takes out the target product that makes.
The purity of said Ti target and Fe target is 99.99%, and the thickness of Ti target is 4mm, and the thickness of Fe target is 2.5mm, and the diameter of Ti target and Fe target is 60mm.
Said O
2In the Ar mixed gas, O
2Be 99.999% with the purity of Ar, wherein O
2Flow be 3sccm, the flow of Ar is 100sccm.
Said sputter direct supply applies the electric current of 0.4A and the voltage of 340V on the Ti target, on the Fe target, apply the electric current of 0.3A and the voltage of 320V.
The preparation method of a kind of large magnetic resistance effect Fe-Ti-O noncrystalline membrane involved in the present invention has and has advantages such as suitability for industrialized production compatibility, target selection and preparation condition are simple now, in the preparation of various electronics devices, is with a wide range of applications.
Compare with other method for preparing film, the present invention has the following advantages:
1) the present invention's Fe-Ti-O noncrystalline membrane of adopting sputtering method to prepare to have big Investigation on Room-temperature Magnetoresistance is compared with organism metallochemistry vapour deposition process with pulsed laser deposition commonly used, on suitability for industrialized production, has explicit costs and technical superiority;
2) processing condition are simple, do not need the substrate heating, do not need special base material, on substrate of glass, just can realize, not only from industry, realize that more easily range of application is also wider simultaneously;
3) film has higher Investigation on Room-temperature Magnetoresistance.
Description of drawings
Fig. 1 is the high resolution transmission electron microscope light field image of the Fe-Ti-O noncrystalline membrane of the present invention's preparation.
Fig. 2 for the resistance of the Fe-Ti-O noncrystalline membrane of the present invention preparation with the variation of temperature relation curve.
Fig. 3 for the magneto-resistor of the Fe-Ti-O laminated film of the present invention preparation with externally-applied magnetic field and variation of temperature relation curve (the vertical face in magnetic field).
Embodiment
Embodiment:
The structure and the property analysis that sample prepared among the present invention are carried out according to us; The preferred forms that will have the titania-doped noncrystalline membrane preparation of iron of big Investigation on Room-temperature Magnetoresistance below explains that at length the magnetron sputtering equipment of using among the embodiment is the ultrahigh vacuum(HHV) three target codeposition magnetron sputtering coaters that adopt scientific instrument development center, Chinese Academy of Sciences Shenyang to produce.
A kind of preparation method of large magnetic resistance effect Fe-Ti-O noncrystalline membrane, this step is following:
1) purity being installed on the target head of coating equipment respectively is 99.99% Ti target and 99.99% Fe target, and the thickness of target is respectively 4mm and 2.5mm, and diameter is 60mm;
2) adopt UW to the glass basic surface contaminant removal after, substrate is installed on the substrate frame, substrate up, target below, the distance of substrate and target is 13cm;
3) unlatching magnetron sputtering equipment successively starts the one-level mechanical pump and the secondary molecular pump vacuumizes, and vacuum tightness is greater than 8.5 * 10 at the bottom of the back of the body of sputtering chamber
-6Pa;
4) feeding purity to Vakuumkammer is 99.999% O
2Mixed gas with 99.999% Ar makes that the vacuum tightness in the Vakuumkammer is 1Pa, wherein O
2Flow be 3sccm, the flow of Ar is 100sccm;
5) open the sputter direct supply, on the Ti target, apply the electric current of 0.4A and the voltage of 340V respectively, on the Fe target, apply the electric current of 0.3A and the voltage of 320V, sputter is 20 minutes in advance, waits sputtering current and voltage stable;
6) open the baffle plate of substrate, the speed of changeing with PM 2 is simultaneously rotated substrate frame, the titania-doped noncrystalline membrane of growth iron on substrate;
7) growing film was closed baffle plate, the substrate frame rotation system of substrate after 15 minutes, closed shielding power supply then, stopped to feed sputter gas Ar and O
2, continue to vacuumize, close vacuum system after half a hour, charging into purity to Vakuumkammer is 99.999% nitrogen, presses when identical up to the air pressure and the outside atmosphere of Vakuumkammer, opens Vakuumkammer and takes out sample and get final product.
Be to confirm the embodiment that the present invention is best, we have carried out AFM, resistance with the analysis with the variation relation of externally-applied magnetic field of temperature variation relation and magneto-resistor to the film of the present invention's preparation.
Fig. 1 is the high resolution transmission electron microscope light field image of the Fe-Ti-O noncrystalline membrane of the present invention's preparation.As can be seen from the figure, sample is unordered non-crystalline state, long-range order do not occur.
Fig. 2 for the resistance of the Fe-Ti-O noncrystalline membrane of the present invention preparation with the variation of temperature relation curve.As can be seen from the figure, the resistance of sample shows as the semi-conductor conductive characteristic along with the reduction of temperature raises.
Fig. 3 for the magneto-resistor of the Fe-Ti-O laminated film of the present invention preparation with externally-applied magnetic field and variation of temperature relation curve (the vertical face in magnetic field).As can be seen from the figure, the magnetoelectricity resistance of sample under 3K is greater than 30%, and magneto-resistor is about 8% when 300K.
Claims (4)
1. the preparation method of a large magnetic resistance effect Fe-Ti-O noncrystalline membrane is characterized in that: adopt the preparation of ultrahigh vacuum(HHV) three target codeposition magnetron sputtering coaters, this step is following:
1) a Ti target and Fe target are installed respectively on the target head of coating equipment;
2) with behind the glass basic surface contaminant removal, install on the substrate frame, substrate up, target below, the distance of substrate and target is 13 cm;
3) unlatching magnetron sputtering equipment successively starts the one-level mechanical pump and the secondary molecular pump vacuumizes, and vacuum tightness is greater than 8.5 * 10 at the bottom of the back of the body of sputtering chamber
– 6Pa;
4) feed O to Vakuumkammer
2With the mixed gas of Ar, make that the vacuum tightness in the Vakuumkammer is 1 Pa;
5) open the sputter direct supply, on Ti target Fe target, apply electric current and voltage respectively, sputter is 20 minutes in advance, waits sputtering current and voltage stable;
6) open the baffle plate of substrate, the speed of changeing with PM 2 is simultaneously rotated substrate frame, the titania-doped noncrystalline membrane of growth iron on substrate;
7) growing film was closed the baffle plate of substrate after 15 minutes, and substrate frame stops operating, and closed shielding power supply then, stopped to feed sputter gas Ar and O
2, close vacuum system after continuing to vacuumize half a hour, charging into purity to Vakuumkammer then is 99.999% nitrogen, presses when identical up to the air pressure and the outside atmosphere of Vakuumkammer, opens Vakuumkammer and takes out the target product that makes.
2. according to the preparation method of the said large magnetic resistance effect Fe-Ti-O of claim 1 noncrystalline membrane; It is characterized in that: the purity of said Ti target and Fe target is 99.99%; The thickness of Ti target is 4 mm, and the thickness of Fe target is 2.5 mm, and the diameter of Ti target and Fe target is 60 mm.
3. according to the preparation method of the said large magnetic resistance effect Fe-Ti-O of claim 1 noncrystalline membrane, it is characterized in that: said O
2In the Ar mixed gas, O
2Be 99.999% with the purity of Ar, wherein O
2Flow be 3sccm, the flow of Ar is 100 sccm.
4. according to the preparation method of the said large magnetic resistance effect Fe-Ti-O of claim 1 noncrystalline membrane; It is characterized in that: said sputter direct supply applies the electric current of 0.4 A and the voltage of 340 V on the Ti target, on the Fe target, applies the electric current of 0.3 A and the voltage of 320 V.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105845315A (en) * | 2016-05-06 | 2016-08-10 | 天津理工大学 | Amorphous FeTiO/SiO2/p-Si heterostructure material and preparation method thereof |
| CN110565059A (en) * | 2019-09-10 | 2019-12-13 | 天津大学 | Preparation method and device of titanium oxide-based nano particle composite film with room-temperature tunnel magnetoresistance effect |
| CN111441027A (en) * | 2020-05-28 | 2020-07-24 | 上海大学 | Fe70Nb10B20Surface modification method of amorphous alloy film |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101736303A (en) * | 2009-12-11 | 2010-06-16 | 天津大学 | Preparation method of chromium-doped titanium nitride magnetic semiconductor polycrystal film |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101736303A (en) * | 2009-12-11 | 2010-06-16 | 天津大学 | Preparation method of chromium-doped titanium nitride magnetic semiconductor polycrystal film |
Non-Patent Citations (1)
| Title |
|---|
| 刘晖等: "(Fe3O4)60(TiO2)40薄膜的输运性能研究", 《第四届全国磁性薄膜与纳米磁学会议论文集》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105845315A (en) * | 2016-05-06 | 2016-08-10 | 天津理工大学 | Amorphous FeTiO/SiO2/p-Si heterostructure material and preparation method thereof |
| CN110565059A (en) * | 2019-09-10 | 2019-12-13 | 天津大学 | Preparation method and device of titanium oxide-based nano particle composite film with room-temperature tunnel magnetoresistance effect |
| CN110565059B (en) * | 2019-09-10 | 2021-09-17 | 天津大学 | Preparation method and device of titanium oxide-based nano particle composite film with room-temperature tunnel magnetoresistance effect |
| CN111441027A (en) * | 2020-05-28 | 2020-07-24 | 上海大学 | Fe70Nb10B20Surface modification method of amorphous alloy film |
| CN111441027B (en) * | 2020-05-28 | 2022-01-11 | 上海大学 | Fe70Nb10B20Surface modification method of amorphous alloy film |
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