CN102418069A - Epitaxial Ti0.53Cr0.47N film material with low-temperature magneto-resistance effect, and preparation method thereof - Google Patents
Epitaxial Ti0.53Cr0.47N film material with low-temperature magneto-resistance effect, and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an epitaxial Ti0.53Cr0.47N film material with a low-temperature magneto-resistance effect, and a preparation method thereof. The epitaxial film material is Ti0.53Cr0.47N. Under a temperature of 5K and a magnetic field of 50kOe, the magneto-resistance is 6%. According to the invention, a DPS-II ultra-high-vacuum target-facing magnetron sputtering machine produced by Shenyang Scientific Instrument Manufacturing Center of Chinese Academy of Sciences is adopted; a substrate material is an MgO (100) single crystal wafer; a pair of Ti targets with a purity of 99.99% are arranged on a faced target head, wherein one end serves as an N pole of magnetic line of force, and the other end serves as an S pole of the magnetic line of force; Cr sheets are uniformly arranged on the surfaces of the Ti targets; conditions such as vacuum pumping, pre-sputtering, temperature adjusting, and current and voltage controlling are selected; and an epitaxial Ti0.53Cr0.47N film sample grown on the MgO substrate material is prepared. The film provided by the invention has a low-temperature magneto-resistance effect. The adopted method is simple and practicable, and is beneficial for the popularization in industrialized productions.
Description
Technical field
The present invention relates to the spintronics material technology, particularly a kind of novel ferromagnetic material and preparation method who has than high spinning polarizability more specifically, is a kind of Ti with low temperature magneto-resistance effect
0.53Cr
0.47N epitaxial thin film material and preparation method.
Background technology
In recent years, owing to have great application prospect in the magnetic information storage with aspect reading, the spintronics material receives much concern.Nobel Prize in physics in 2007 has been authorized initiator Albert Fert and two professors of Peter Gr ü nberg of spintronics.Now, the electric current that how to obtain high spin-polarization remains one of the hot issue in spintronics field.Obtain the way that high-spin injects and mainly contain the electrode materials of selecting high spinning polarizability, the ferromagnetic substance with high spinning polarizability that particularly can be combined with each other with semiconductor material.
First principle calculates and shows Fe
3O
4, La
1-xA
xMnO
3(LAMO, A are alkaline earth element Ca, Sr and Ba etc.), CrO
2, material such as NiMnSb energy band structure between metal and isolator, be called as semi-metallic.For a spin direction, the energy band structure of semi-metallic has Special metallic features, near Fermi surface, has certain density of states(DOS); And to another kind of spin direction, its energy band structure has the isolator characteristic, near Fermi surface density of states(DOS) be zero or electronics be localization.Therefore, theoretically, semi-metallic should have 100% spin polarizability.But up to now, for Fe
3O
4Material does not obtain high spin polarizability experimentally, does not know Fe yet
3O
4Whether has the semi-metal characteristic, especially at ambient temperature.LAMO and CrO
2The Tc of material is all lower, can not satisfy requirement of actual application.The structure more complicated of Heusler alloy, price is also somewhat expensive, is not easy preparation, and is unfavorable for actual production.Therefore, seeking the novel ferromagnetic electrode material with high spinning polarizability is the key factor and research focus that further develops the spintronics device.
The titanium nitride crystal belongs to isometric system, face-centred cubic structure, its lattice parameter a=0.42173nm.Titanium nitride membrane has excellent machinery, heat, electricity and antiseptic property, because hardness is high, frictional coefficient is low, is widely used as the wear-resisting modified layer of mould, cutter etc.; Because resistance to wear, antiseptic property is good, fusing point is high, high-temperature stability is good, is widely used in aerospace component such as aircraft and rocket; Since conduction, good heat conductivity, the blocking layer of doing commonly used in microelectronic.If magnetic element is doped in the titanium nitride system, if can obtain promptly have the material that magnetic has conduction, will promote the new purposes of titanium nitride material.
At present; The employing pulse laser sediment method that has only Japanese people such as K.Inumaru to go up report at APPLIED PHYSICS LETTERS 91,152501 (2007) in the experiment report both domestic and external prepares finds the magneto-resistor phenomenon in the adulterated TiN epitaxial film of high-Cr; They have also found same phenomenon in the adulterated TiN sosoloid of high-Cr of having reported the preparation of employing chemical process on the PHYSICAL REVIEW B 78,052406 (2008) for comparative study.But the Tc of sample is lower than room temperature, can not reach requirement of actual application.In addition, many in the practical application is main with thin-film material, and the preparation method adopts sputtering method more.But up to the present in the world not about adopting sputtering method to prepare the relevant report of Cr doped Ti N epitaxial film.
Summary of the invention
From the angle of suitability for industrialized production, need to use sputtering method to prepare sample; Need the sample of preparation to have higher spin polarizability from practical application.The present invention promptly from above two purposes, has developed reactive magnetron sputtering method and has prepared Ti
0.53Cr
0.47The N epitaxial film, and observe the low temperature magneto-resistance effect, prove to have higher spin polarizability.
The epitaxial thin film material with low temperature magneto-resistance effect of the present invention's preparation, material is Ti
0.53Cr
0.47N is that 5K and magnetic field are under the 50kOe in temperature, and magneto-resistor is 6%.
Ti
0.53Cr
0.47The preparation method of N epitaxial thin film material, method is following:
The present invention is at preparation Ti
0.53Cr
0.47During the N epitaxial film, the base material that is adopted is MgO (a 100) single-chip.
Concrete preparation method of the present invention realizes through following steps:
Ti
0.53Cr
0.47The preparation method of N epitaxial thin film material, method is following:
1) the DPS-III type ultrahigh vacuum(HHV) subtend target magnetic control sputtering coating equipment that adopts scientific instrument development center, Chinese Academy of Sciences Shenyang to produce; Base material is MgO (a 100) single-chip; The a pair of purity of installation is 99.99% Ti target on the target head of subtend, a N utmost point as magneticline of force, and the other end is the S utmost point; Ti target thickness is 4mm, and diameter is 60mm; In order to mix Cr, evenly place the Cr sheet on the surface of Ti target, the area of Cr sheet is 6mm
2, the quantity of Cr sheet is 200, obtaining Cr in the sample through composition analysis is 47% with respect to the atomic percentage conc of Cr and Ti atomicity summation; Distance between two targets is 80mm, and the axis of target and the distance that is placed with between the specimen holder of MgO base material are 80mm;
2) the MgO base material is removed surface impurity through hyperacoustic mode after, the MgO base material is installed on the substrate frame at midperpendicular place of subtend target line;
3) unlatching DPS-III ultrahigh vacuum(HHV) subtend target magnetic control sputtering coating equipment successively starts the one-level mechanical pump and the secondary molecular pump vacuumizes, and vacuum tightness is superior to 6 * 10 at the bottom of the back of the body of sputtering chamber
-6Pa;
4) feeding purity to Vakuumkammer is 99.999% Ar and N
2Mixed gas, vacuum tightness is remained on 1Pa, wherein the flow of Ar gas is 50sccm, N
2The flow of gas is 50sccm;
5) MgO base material temperature is risen to 550 ℃ with 10 ℃/second speed;
6) open shielding power supply, on a pair of Ti target, apply the electric current of 0.2A and the volts DS of 800V, sputter is 10 minutes in advance, waits sputtering current and voltage stable;
7) plate washer of opening on the substrate frame begins sputter, MgO base material stationkeeping;
8) after sputter finishes, close the plate washer on the substrate frame, close shielding power supply then, stop to feed sputter gas Ar and N
2, open slide valve fully, continue to vacuumize, and MgO base material temperature is reduced to room temperature with the rate of temperature fall of 5 ℃/min, close vacuum system then.Charging into purity to Vakuumkammer is 99.999% nitrogen, opens Vakuumkammer, takes out epitaxially grown Ti on the MgO base material
0.53Cr
0.47The N film sample.
Ti involved in the present invention
0.53Cr
0.47The N epitaxial film has using value on the spintronics device; For example in magnetic RAM, can be used as spin injecting material layer, and the present invention adopt reactive sputtering be industry go up method, the target of producing thin-film material select simple and the target rate of utilization than advantages such as height.
Be the embodiment of confirming that the present invention is best, we have carried out X-ray diffraction to prepared film of the present invention, the measurement of magnetic property and electronic transport characteristic.
Fig. 1 has provided the Ti for preparing among the present invention
0.53Cr
0.47The X-ray diffraction spectrum of N epitaxial film.As can be seen from the figure, Ti has only appearred
0.53Cr
0.47The diffraction peak of N (200) and (400), interpret sample are epitaxially grown film sample.
Fig. 2 has provided the Ti for preparing among the present invention
0.53Cr
0.47The magnetzation curve of N epitaxial film under 15K.As can be seen from the figure, sample shows as ferromegnetism.
Fig. 3 has provided the Ti of the present invention's preparation
0.53Cr
0.47The resistivity of N epitaxial film is with the variation of temperature relation curve.As can be seen from the figure, at the high temperature place, the resistivity of sample reduces along with the reduction of temperature, occurs at the 120K place changing, and at the low temperature place, the phenomenon that resistivity raises along with the reduction of temperature occurs.
Fig. 4 has provided the Ti of the present invention's preparation
0.53Cr
0.47Magneto-resistor under the 5K of N epitaxial film is with the variation relation curve of externally-applied magnetic field.As can be seen from the figure, the magneto-resistor of sample is 6%, and under the magnetic field of 50kOe, does not still reach capacity.
Ti with other method preparation
0.53Cr
0.47The method of N epitaxial film is compared, and prepared film of the present invention has the low temperature magneto-resistance effect, and the method that is adopted is simple and practical, helps the popularization on industrial production.Specific as follows:
Because the main method that present suitability for industrialized production is adopted is a sputtering method; The reactive sputtering that the present invention adopted; With people such as K.Inumaru at APPLIED PHYSICS LETTERS 91; 152501 (2007) and PHYSICAL REVIEW B 78,052406 (2008) pulsed laser depositions of going up report compare with chemical process, on suitability for industrialized production, have clear superiority.
Description of drawings
Fig. 1 has provided the Ti for preparing among the present invention
0.53Cr
0.47The X-ray diffraction spectrum of N epitaxial film.
Fig. 2 has provided the Ti for preparing among the present invention
0.53Cr
0.47The magnetzation curve of N epitaxial film under 15K.
Fig. 3 has provided the Ti of the present invention's preparation
0.53Cr
0.47The resistivity of N epitaxial film is with the variation of temperature relation curve.
Fig. 4 has provided the Ti of the present invention's preparation
0.53Cr
0.47Magneto-resistor under the 5K of N epitaxial film is with the variation relation curve of externally-applied magnetic field.
Embodiment
Structure and property analysis according to we carry out sample prepared among the present invention prepare Ti with subtend target response sputtering method below
0.53Cr
0.47The preferred forms of N epitaxial film is at length explained:
1, the DPS-III type ultrahigh vacuum(HHV) subtend target magnetic control sputtering coating equipment that adopts scientific instrument development center, Chinese Academy of Sciences Shenyang to produce; Base material is MgO (a 100) single-chip; The a pair of purity of installation is 99.99% Ti target on the target head of subtend, a N utmost point as magneticline of force, and the other end is the S utmost point; Ti target thickness is 4mm, and diameter is 60mm; In order to mix Cr, evenly place the Cr sheet on the surface of Ti target, the area of Cr sheet is 6mm
2, the quantity of Cr sheet is 200, obtaining Cr in the sample through composition analysis is 47% with respect to the atomic percentage conc of Cr and Ti atomicity summation; Distance between two targets is 80mm, and the axis of target and the distance that is placed with between the specimen holder of MgO base material are 80mm;
2, the MgO base material is removed surface impurity through hyperacoustic mode after, the MgO base material is installed on the substrate frame at midperpendicular place of subtend target line;
3, unlatching DPS-III ultrahigh vacuum(HHV) subtend target magnetic control sputtering coating equipment successively starts the one-level mechanical pump and the secondary molecular pump vacuumizes, and vacuum tightness is superior to 6 * 10 at the bottom of the back of the body of sputtering chamber
-6Pa;
4, feeding purity to Vakuumkammer is 99.999% Ar and N
2Mixed gas, vacuum tightness is remained on 1Pa, wherein the flow of Ar gas is 50sccm, N
2The flow of gas is 50sccm;
5, MgO base material temperature is risen to 550 ℃ with 10 ℃/second speed;
6, open shielding power supply, on a pair of Ti target, apply the electric current of 0.2A and the volts DS of 800V, sputter is 10 minutes in advance, waits sputtering current and voltage stable;
7, the plate washer of opening on the substrate frame begins sputter, MgO base material stationkeeping;
8, after sputter finishes, close the plate washer on the substrate frame, close shielding power supply then, stop to feed sputter gas Ar and N
2, open slide valve fully, continue to vacuumize, and MgO base material temperature is reduced to room temperature with the rate of temperature fall of 5 ℃/min, close vacuum system then.Charging into purity to Vakuumkammer is 99.999% nitrogen, opens Vakuumkammer, takes out epitaxially grown Ti on the MgO base material
0.53Cr
0.47The N film sample.
We have carried out X-ray diffraction to prepared film of the present invention, the measurement of magnetic property and electronic transport characteristic, result such as Fig. 1,2,3,4 said.
Claims (2)
1. the epitaxial thin film material that has the low temperature magneto-resistance effect is characterized in that epitaxial thin film material is Ti
0.53Cr
0.47N is that 5K and magnetic field are under the 50kOe in temperature, and magneto-resistor is 6%.
2. the preparation method of the epitaxial thin film material of claim 1 is characterized in that method is following:
1) the DPS-III type ultrahigh vacuum(HHV) subtend target magnetic control sputtering coating equipment that adopts scientific instrument development center, Chinese Academy of Sciences Shenyang to produce; Base material is MgO (a 100) single-chip; The a pair of purity of installation is 99.99% Ti target on the target head of subtend, a N utmost point as magneticline of force, and the other end is the S utmost point; Ti target thickness is 4mm, and diameter is 60mm; In order to mix Cr, evenly place the Cr sheet on the surface of Ti target, the area of Cr sheet is 6mm
2, the quantity of Cr sheet is 200, obtaining Cr in the sample through composition analysis is 47% with respect to the atomic percentage conc of Cr and Ti atomicity summation; Distance between two targets is 80mm, and the axis of target and the distance that is placed with between the substrate frame of MgO substrate are 80mm;
2) the MgO base material is removed surface impurity through hyperacoustic mode after, the MgO base material is installed on the substrate frame at midperpendicular place of subtend target line;
3) unlatching DPS-III ultrahigh vacuum(HHV) subtend target magnetic control sputtering coating equipment successively starts the one-level mechanical pump and the secondary molecular pump vacuumizes, and vacuum tightness is superior to 6 * 10 at the bottom of the back of the body of sputtering chamber
-6Pa;
4) feeding purity to Vakuumkammer is 99.999% Ar and N
2Mixed gas, vacuum tightness is remained on 1Pa, wherein the flow of Ar gas is 50sccm, N
2The flow of gas is 50sccm;
5) MgO base material temperature is risen to 550 ℃ with 10 ℃/second speed;
6) open shielding power supply, on a pair of Ti target, apply the electric current of 0.2A and the volts DS of 800V, sputter is 10 minutes in advance, waits sputtering current and voltage stable;
7) plate washer of opening on the substrate frame begins sputter, MgO base material stationkeeping;
8) after sputter finishes, close the plate washer on the substrate frame, close shielding power supply then, stop to feed sputter gas Ar and N
2, open slide valve fully, continue to vacuumize, and MgO base material temperature is reduced to room temperature with the rate of temperature fall of 5 ℃/min, close vacuum system then.Charging into purity to Vakuumkammer is 99.999% nitrogen, opens Vakuumkammer, takes out epitaxially grown Ti in the MgO substrate
0.53Cr
0.47The N film sample.
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|---|---|---|---|
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009101462A (en) * | 2007-10-23 | 2009-05-14 | Mitsubishi Materials Corp | Surface-coated cutting tool |
| CN101497986A (en) * | 2009-03-13 | 2009-08-05 | 天津大学 | Apparatus for preparing extension ferriferrous oxide film by facing-target reactive sputtering and operation method |
| US20090242385A1 (en) * | 2008-03-28 | 2009-10-01 | Tokyo Electron Limited | Method of depositing metal-containing films by inductively coupled physical vapor deposition |
| CN101736303A (en) * | 2009-12-11 | 2010-06-16 | 天津大学 | Preparation method of chromium-doped titanium nitride magnetic semiconductor polycrystal film |
| CN101914751A (en) * | 2010-09-03 | 2010-12-15 | 天津大学 | Preparation method of epitaxy Fe4N film by reactive sputtering with facing targets |
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2011
- 2011-10-24 CN CN 201110325753 patent/CN102418069B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009101462A (en) * | 2007-10-23 | 2009-05-14 | Mitsubishi Materials Corp | Surface-coated cutting tool |
| US20090242385A1 (en) * | 2008-03-28 | 2009-10-01 | Tokyo Electron Limited | Method of depositing metal-containing films by inductively coupled physical vapor deposition |
| CN101497986A (en) * | 2009-03-13 | 2009-08-05 | 天津大学 | Apparatus for preparing extension ferriferrous oxide film by facing-target reactive sputtering and operation method |
| CN101736303A (en) * | 2009-12-11 | 2010-06-16 | 天津大学 | Preparation method of chromium-doped titanium nitride magnetic semiconductor polycrystal film |
| CN101914751A (en) * | 2010-09-03 | 2010-12-15 | 天津大学 | Preparation method of epitaxy Fe4N film by reactive sputtering with facing targets |
Non-Patent Citations (1)
| Title |
|---|
| K.INUMARU ET AL: "Ferromagnetic CrxTi1-xN solid solution nitride thin films grown by pulsed laser deposition and their magnetoresistance", 《APPLED PHYSICS LETTERS》 * |
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