CN102418069B - 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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- CN102418069B CN102418069B CN 201110325753 CN201110325753A CN102418069B CN 102418069 B CN102418069 B CN 102418069B CN 201110325753 CN201110325753 CN 201110325753 CN 201110325753 A CN201110325753 A CN 201110325753A CN 102418069 B CN102418069 B CN 102418069B
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- 239000000463 material Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 230000000694 effects Effects 0.000 title claims abstract description 9
- 230000005291 magnetic effect Effects 0.000 claims abstract description 30
- 238000004544 sputter deposition Methods 0.000 claims abstract description 17
- 239000000758 substrate Substances 0.000 claims abstract description 14
- 239000010408 film Substances 0.000 claims description 28
- 239000007789 gas Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 239000010409 thin film Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000007747 plating Methods 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 4
- 239000008186 active pharmaceutical agent Substances 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 230000006641 stabilisation Effects 0.000 claims description 3
- 238000011105 stabilization Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 2
- 238000001755 magnetron sputter deposition Methods 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- 239000010936 titanium Substances 0.000 description 31
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000009987 spinning Methods 0.000 description 4
- 238000005546 reactive sputtering Methods 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 230000002421 anti-septic effect Effects 0.000 description 2
- 238000001311 chemical methods and process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012552 review Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910005811 NiMnSb Inorganic materials 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 239000003302 ferromagnetic material Substances 0.000 description 1
- 229910001291 heusler alloy Inorganic materials 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000004807 localization Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
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- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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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 magnetic electricresistance effect
0.53Cr
0.47N epitaxial thin film material and preparation method.
Background technology
In recent years, owing to have huge application prospect at 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, the 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 metallic character, has certain density of states(DOS) near Fermi surface; 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 Curie temperature of material is all lower, can not satisfy the requirement of practical application.The complicated structure of Heusler alloy, price are also somewhat expensive, are not easy preparation, and are unfavorable for actual production.Therefore, seeking the Novel iron magnetic pole material with high spinning polarizability is key factor and the study hotspot 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 the aerospace component such as aircraft and rocket; Because conduction, good heat conductivity are commonly used for the blocking layer in microelectronic.If magnetic element is doped in the titanium nitride system, if obtain namely have the material that magnetic has conduction, will promote the new purposes of titanium nitride material.
At present, the people such as K.Inumaru that only have Japan in the experiment both domestic and external report prepare in the TiN epitaxial film that high-Cr mixes at the employing pulse laser sediment methods of APPLIED PHYSICS LETTERS 91,152501 (2007) upper reports and find the magneto-resistor phenomenon; They have also found same phenomenon in the TiN sosoloid of having reported the high-Cr doping of adopting the chemical process preparation on the PHYSICAL REVIEW B 78,052406 (2008) for comparative study.But the Curie temperature of sample is lower than room temperature, can not reach the requirement of practical application.In addition, be main mainly with thin-film material in the practical application, 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 prepare sample with sputtering method; The sample that needs to prepare from practical application has higher spin polarizability.The present invention namely 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 magnetic electricresistance effect, prove to have higher spin polarizability.
The epitaxial thin film material with low temperature magnetic electricresistance 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 as follows:
The present invention is at preparation Ti
0.53Cr
0.47During the N epitaxial film, the base material that adopts is MgO (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 as follows:
1) the DPS-III type ultrahigh vacuum(HHV) subtend targets magnetic sputtering film plating machine that adopts scientific instrument development center, Chinese Academy of Sciences Shenyang to produce, base material is MgO (100) single-chip, at the target head of subtend a pair of purity being installed is 99.99% Ti target, N utmost point as magnetic line of force, the other end is the S utmost point; Ti target thickness is 4mm, and diameter is 60mm; In order to mix Cr, place the Cr sheet at the surface uniform of Ti target, the area of Cr sheet is 6mm
2, the quantity of Cr sheet is 200, obtaining Cr in the sample by 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 by 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 targets magnetic sputtering film plating machine successively starts the one-level mechanical pump and the secondary molecular pump vacuumizes, until the back end vacuum tightness of sputtering chamber is better than 6 * 10
-6Pa;
4) passing into purity to vacuum chamber is 99.999% Ar and N
2Mixed gas, at 1Pa, wherein the flow of Ar gas is 50sccm, N with vacuum keep
2The flow of gas is 50sccm;
5) MgO base material temperature is risen to 550 ℃ with 10 ℃/second speed;
6) open shielding power supply, apply the electric current of 0.2A and the volts DS of 800V at a pair of Ti target, pre-sputter 10 minutes waits sputtering current and voltage stabilization;
7) plate washer of opening on the substrate frame begins sputter, and MgO base material position is fixed;
8) after sputter finishes, close the plate washer on the substrate frame, then close shielding power supply, stop to pass into sputter gas Ar and N
2, open slide valve fully, continue to vacuumize, and MgO base material temperature is down to room temperature with the rate of temperature fall of 5 ℃/min, then close vacuum system.Being filled with purity to vacuum chamber is 99.999% nitrogen, opens vacuum chamber, 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 at the spintronics device, for example in magnetic RAM, can be used as spin injecting material layer, and the present invention adopt reactive sputtering be method, the target of industrial production thin-film material select simple and the target rate of utilization than advantages of higher.
For confirming the embodiment of the best of the present invention, we have carried out X-ray diffraction to the 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 variation with temperature relation curve of N epitaxial film.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 does not still reach capacity under the magnetic field of 50kOe.
Ti with other method preparation
0.53Cr
0.47The method of N epitaxial film is compared, and the prepared film of the present invention has the low temperature magnetic electricresistance effect, and the method simple practical that adopts is conducive to the popularization on industrial production.Specific as follows:
Because the main method that present suitability for industrialized production adopts is sputtering method, reactive sputtering of the present invention, with the people such as K.Inumaru at APPLIED PHYSICS LETTERS 91,152501 (2007) and PHYSICAL REVIEW B 78, the pulsed laser deposition of 052406 (2008) upper report is compared with chemical process, has clear superiority in suitability for industrialized production.
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 variation with temperature relation curve of N epitaxial film.
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
To structure and property analysis that sample prepared among the present invention carries out, the below prepares Ti with the facing targets reactive sputtering method according to us
0.53Cr
0.47The preferred forms of N epitaxial film is described in detail:
1, the DPS-III type ultrahigh vacuum(HHV) subtend targets magnetic sputtering film plating machine that adopts scientific instrument development center, Chinese Academy of Sciences Shenyang to produce, base material is MgO (100) single-chip, at the target head of subtend a pair of purity being installed is 99.99% Ti target, N utmost point as magnetic line of force, the other end is the S utmost point; Ti target thickness is 4mm, and diameter is 60mm; In order to mix Cr, place the Cr sheet at the surface uniform of Ti target, the area of Cr sheet is 6mm
2, the quantity of Cr sheet is 200, obtaining Cr in the sample by 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 by 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 targets magnetic sputtering film plating machine successively starts the one-level mechanical pump and the secondary molecular pump vacuumizes, until the back end vacuum tightness of sputtering chamber is better than 6 * 10
-6Pa;
4, passing into purity to vacuum chamber is 99.999% Ar and N
2Mixed gas, at 1Pa, wherein the flow of Ar gas is 50sccm, N with vacuum keep
2The flow of gas is 50sccm;
5, MgO base material temperature is risen to 550 ℃ with 10 ℃/second speed;
6, open shielding power supply, apply the electric current of 0.2A and the volts DS of 800V at a pair of Ti target, pre-sputter 10 minutes waits sputtering current and voltage stabilization;
7, the plate washer of opening on the substrate frame begins sputter, and MgO base material position is fixed;
8, after sputter finishes, close the plate washer on the substrate frame, then close shielding power supply, stop to pass into sputter gas Ar and N
2, open slide valve fully, continue to vacuumize, and MgO base material temperature is down to room temperature with the rate of temperature fall of 5 ℃/min, then close vacuum system.Being filled with purity to vacuum chamber is 99.999% nitrogen, opens vacuum chamber, 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 the prepared film of the present invention, the measurement of magnetic property and electronic transport characteristic, and the result is as described in Fig. 1,2,3,4.
Claims (1)
1. the epitaxial thin film material that has the low temperature magnetic electricresistance 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%;
The preparation method is as follows:
1) the DPS-III type ultrahigh vacuum(HHV) subtend targets magnetic sputtering film plating machine that adopts scientific instrument development center, Chinese Academy of Sciences Shenyang to produce, base material is MgO (100) single-chip, at the target head of subtend a pair of purity being installed is 99.99% Ti target, N utmost point as magnetic line of force, the other end is the S utmost point; Ti target thickness is 4mm, and diameter is 60mm; In order to mix Cr, place the Cr sheet at the surface uniform of Ti target, the area of Cr sheet is 6mm
2, the quantity of Cr sheet is 200, obtaining Cr in the sample by 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 by 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 targets magnetic sputtering film plating machine successively starts the one-level mechanical pump and the secondary molecular pump vacuumizes, until the back end vacuum tightness of sputtering chamber is better than 6 * 10
-6Pa;
4) passing into purity to vacuum chamber is 99.999% Ar and N
2Mixed gas, at 1Pa, wherein the flow of Ar gas is 50sccm, N with vacuum keep
2The flow of gas is 50sccm;
5) MgO base material temperature is risen to 550 ° of C with the speed of 10 ° of C/ seconds;
6) open shielding power supply, apply the electric current of 0.2A and the volts DS of 800V at a pair of Ti target, pre-sputter 10 minutes waits sputtering current and voltage stabilization;
7) plate washer of opening on the substrate frame begins sputter, and MgO base material position is fixed;
8) after sputter finishes, close the plate washer on the substrate frame, then close shielding power supply, stop to pass into sputter gas Ar and N
2, open slide valve fully, continue to vacuumize, and MgO base material temperature is down to room temperature with the rate of temperature fall of 5 ° of C/min, then close vacuum system.Being filled with purity to vacuum chamber is 99.999% nitrogen, opens vacuum chamber, takes out epitaxially grown Ti in the MgO substrate
0.53Cr
0.47The N film sample.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110325753 CN102418069B (en) | 2011-10-24 | 2011-10-24 | Epitaxial Ti0.53Cr0.47N film material with low-temperature magneto-resistance effect, and preparation method thereof |
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|---|---|---|---|
| CN 201110325753 CN102418069B (en) | 2011-10-24 | 2011-10-24 | Epitaxial Ti0.53Cr0.47N film material with low-temperature magneto-resistance effect, and preparation method thereof |
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| CN102418069A CN102418069A (en) | 2012-04-18 |
| CN102418069B true CN102418069B (en) | 2013-05-29 |
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