CN102509768B - Fe3O4 (ferroferric oxide)/p-Si (p-type silicon) structure capable of regulating and controlling magneto-resistance effect with current and preparation method for same - Google Patents
Fe3O4 (ferroferric oxide)/p-Si (p-type silicon) structure capable of regulating and controlling magneto-resistance effect with current and preparation method for same Download PDFInfo
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- CN102509768B CN102509768B CN201110339932.5A CN201110339932A CN102509768B CN 102509768 B CN102509768 B CN 102509768B CN 201110339932 A CN201110339932 A CN 201110339932A CN 102509768 B CN102509768 B CN 102509768B
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- 230000000694 effects Effects 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 230000001105 regulatory effect Effects 0.000 title claims abstract 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title abstract 11
- 230000001276 controlling effect Effects 0.000 title abstract 3
- 239000000758 substrate Substances 0.000 claims abstract description 56
- 239000013078 crystal Substances 0.000 claims abstract description 26
- 230000005291 magnetic effect Effects 0.000 claims abstract description 22
- 238000004544 sputter deposition Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000007747 plating Methods 0.000 claims description 6
- 230000004907 flux Effects 0.000 claims description 4
- 239000003595 mist Substances 0.000 claims description 4
- 230000005307 ferromagnetism Effects 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 230000006641 stabilisation Effects 0.000 claims description 3
- 238000011105 stabilization Methods 0.000 claims description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 230000005294 ferromagnetic effect Effects 0.000 abstract description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 4
- 229910052710 silicon Inorganic materials 0.000 abstract 3
- 239000010703 silicon Substances 0.000 abstract 3
- 239000013077 target material Substances 0.000 abstract 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract 1
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 230000033228 biological regulation Effects 0.000 description 7
- 238000001816 cooling Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 238000001451 molecular beam epitaxy Methods 0.000 description 2
- 238000001420 photoelectron spectroscopy Methods 0.000 description 2
- 229910005811 NiMnSb Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910001291 heusler alloy Inorganic materials 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000004807 localization Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000005546 reactive sputtering Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
The invention relates to a Fe3O4 (ferroferric oxide)/p-Si (p-type silicon) structure capable of regulating and controlling magneto-resistance effect with current and a preparation method for the same. The Fe3O4/p-Si structure is structurally characterized in that Fe3O4 grows on a p-type silicon single crystal substrate, and the maximum magneto-resistance value of the hetero-structure can reach 40% at the temperature of 100K, in a 50kOe magnetic field and within the current range of 1mA. The preparation method includes the steps of employing a three-target adjustable ultrahigh vacuum magnetron sputtering coating machine produced by SKY Technology Development Co., Ltd. Chinese Academy of Sciences (SKY), and mounting a Fe (ferrum) target with 99.99% purity on a ferromagnetic target, wherein a target material is 2mm in thick, the diameter of the target material is 60mm, and the distance between the target and a substrate support is 10cm; mounting the p-type silicon single crystal substrate on the substrate support above a target head; and obtaining a Fe3O4 sample which grows on the p-type silicon single crystal substrate by controlling conditions such as vacuum degree, sputtering gas, current, voltage, sputtering time and the like. The hetero-structure prepared by the method has large magneto-resistance effect in low current, and the method which is a reactive magnetron sputtering method is simple, practical and beneficial to popularization on industrial production.
Description
Technical field
The present invention relates to a kind of Fe with electric current regulation and control magneto-resistance effect
3O
4/ p-Si structure and preparation method more specifically, are a kind of Fe that can regulate and control by current strength magneto-resistance effect
3O
4/ p-Si heterostructure 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, material and the semi-conducting material that how will have high spinning polarizability are combined with each other, and it is the problem that people will solve that generation has than large magnetic resistance effect.
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 band structure between metal and insulator, be called as semi-metallic.For a spin direction, the band structure of semi-metallic has metallic character, has certain density of states near Fermi surface; And to another kind of spin direction, its band structure has the insulator characteristic, near Fermi surface the density of states be zero or electronics be localization.Therefore, theoretically, semi-metallic should have 100% spin polarizability.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.Fe
3O
4Material has the characteristics such as Curie temperature height, resistivity and semiconductor coupling, therefore with Fe
3O
4Be combined with each other as ferromagnetic layer and semiconductor and can obtain to have the composite material of magneto-resistance effect.
At present, the people such as Wang that only have China in the experiment both domestic and external report in the employing laser molecular beam epitaxy methods of APPLIED PHYSICS LETTERS 92,012122 (2008) upper reports at the N-shaped Si Fe that grown
3O
4Layer, and the maximum magnetic flux resistance value that measures under the magnetic field of 50kOe is 6%.It is that the p-type Si substrate of 2 Ω cm has prepared Fe in resistivity in the situation that substrate is not heated that the people such as Mi adopt magnetron sputtering methods at the upper report of JOURNAL OF APPLIED PHYSICS 107,103922 (2010)
3O
4Layer, and under the electric current of the magnetic field of 90kOe and 100mA, observed 30% magnetoelectricity resistance.
The people such as Mi are that the electric current longitudinal stream is crossed this structure in the magneto-resistance effect of JOURNAL OF APPLIED PHYSICS 107,103922 (2010) upper reports, and namely electric current is from Fe
3O
4Flow to Si.In addition, be main mainly with low current in the practical application, can save the energy like this; And need high magnetoelectricity resistance, improve the sensitivity of device, thereby result of study above-mentioned can not satisfy the requirement of practical application.
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 magneto-resistance effect, and needs the electric current of generation magneto-resistance effect less, is conducive to so energy-conservation.The present invention has developed the Fe with electric current regulation and control magneto-resistance effect namely from above two purposes
3O
4/ p-Si structure, and under reduced-current, observed than large magnetic resistance effect, simultaneously this magneto-resistance effect is magneto-resistance effect in the face, namely electric current is at Fe
3O
4Flow through in the aspect, rather than vertically by this structure.
A kind of Fe with electric current regulation and control magneto-resistance effect of the present invention
3O
4/ p-Si structure is at the p-type Si single crystal substrates Fe that grows
3O
4This heterostructure is under the 100K temperature, under the 50kOe magnetic field, in the current range of 1mA, and the maximum magnetic flux resistance value can reach 40%.Observed 30% magnetoelectricity resistance under the electric current of the magnetic field of 90kOe and 100mA, this result is higher than used magnetic field among the present invention, current strength is large, but the magnetoelectricity resistance is but low than result of the present invention.
Fe with electric current regulation and control magneto-resistance effect of the present invention
3O
4/ p-Si structure, the base material that adopts is that resistivity is p-type Si (100) single-chip of 0.02 Ω cm, the resistivity of the p-type Si that uses here (100) single-chip than people such as Mi at JOURNAL OF APPLIED PHYSICS 107, the resistivity of the p-type Si that uses on 103922 (2010) (100) single-chip is hanged down 2 orders of magnitude, and in preparation process, substrate being heated, thereby Fe
3O
4Crystallization degree improve.
Concrete steps are as follows:
1) the adjustable superhigh vacuum magnetron sputtering film-plating machine of three targets that adopts scientific instrument development center, Chinese Academy of Sciences Shenyang to produce, at ferromagnetism target head a purity being installed is 99.99% Fe target, and the thickness of target is 2mm, and diameter is 60mm; Distance between target and the substrate frame is 10cm;
2) p-type Si single crystal substrates material is removed surface impurity by hyperacoustic mode after, p-type Si single crystal substrates is installed on the substrate frame that is positioned at target head top;
3) the adjustable superhigh vacuum magnetron sputtering film-plating machine of unlatching three targets successively starts the one-level mechanical pump and the secondary molecular pump vacuumizes, until the back end vacuum degree of sputtering chamber is better than 8 * 10
-6Pa;
4) the back end vacuum degree when sputtering chamber is better than 8 * 10
-6During Pa, passing into purity to vacuum chamber is 99.999% Ar and O
2Mist, wherein the flow of Ar gas is 100sccm, O
2The flow of gas is 2.4sccm, with vacuum keep at 1Pa;
5) p-type Si single crystal substrates temperature is risen to 500 ℃ with 10 ℃/second speed;
6) until base reservoir temperature reach 500 ℃ and stable after, open the stepping motor of control substrate frame rotation, make substrate frame and be installed in p-type Si single crystal substrates on the substrate frame with the rotational speed of per minute 2 circles;
7) open shielding power supply, apply the electric current of 0.2A and the direct voltage of 350V at the Fe target, pre-sputter 10 minutes waits sputtering current and voltage stabilization;
8) plate washer of opening substrate frame below begins sputter, and in the sputter procedure, p-type Si single crystal substrates remains on 500 ℃, and always with the rotational speed of 2 circles each second;
9) sputter was closed the plate washer of substrate frame below after 15 minutes, then closed shielding power supply, stopped to pass into sputter gas Ar and O
2, open slide valve fully, continue to vacuumize, turn off the stepping motor of control substrate frame rotation, and p-type Si single crystal substrates temperature is down to room temperature with the rate of temperature fall of 5 ℃/min, then close vacuum system; After system cools, being filled with purity to vacuum chamber is 99.999% nitrogen, until the air pressure in the sputtering chamber reaches a standard atmospheric pressure, stops to pass into nitrogen, opens vacuum chamber, takes out the Fe that grows on the p-type Si single crystal substrates
3O
4Sample.
The Fe of the magneto-resistance effect with electric current regulation and control involved in the present invention
3O
4/ p-Si structure has using value at the spintronics device, can substitute existing magnetic metal material and conduct spin injection source material.
With other Fe
3O
4The performance of/Si structure is compared with the preparation method: the prepared heterostructure of the present invention has than large magnetic resistance effect under little electric current; The method that adopts is reactive magnetron sputtering method, and is simple and practical, is conducive to the popularization on industrial production.Compared with prior art:
1, 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 Wang at APPLIED PHYSICS LETTERS 92, the employing laser molecular beam epitaxy method of 012122 (2008) upper report is compared, and has clear superiority in industrial production;
2, the present invention under the magnetic field of 50kOe, be lower than and measure magnetoelectricity resistance in 40% the face under the electric current of 1mA, than people such as Mi at JOURNAL OF APPLIED PHYSICS 107, longitudinal magnetoresistance effect under the 100mA of 103922 (2010) upper reports has more actual application value, and is more energy-conservation in application process.
Description of drawings
Fig. 1 has provided the Fe for preparing among the present invention
3O
4The X-ray diffraction spectrum of/p-Si structure.
Fig. 2 has provided the Fe for preparing among the present invention
3O
4The photoelectron spectroscopy figure of Fe 2p in the/p-Si structure.
Fig. 3 has provided the Fe of the present invention's preparation
3O
4The null field cooling curve of/p-Si structure and extra show cooling curve.
Fig. 4 has provided the Fe of the present invention's preparation
3O
4The temperature of/p-Si structure is that 100K and magnetic field are that magneto-resistor under the 50kOe is with the variation relation curve of impressed current.
Fig. 5 has provided Fe of the present invention
3O
4The electronic transport feature measurement schematic diagram of/p-Si structure.
Embodiment
According to structure and the property analysis that we carry out sample prepared among the present invention, the below will have the Fe of electric current regulation and control magneto-resistance effect
3O
4The preferred forms of/p-Si structure is described in detail: the way of electrode allows electric current at Fe exactly
3O
4Flow through in the face, namely at Fe
3O
4Four electrodes are arranged on the layer:
1, the adjustable superhigh vacuum magnetron sputtering film-plating machine of three targets that adopts scientific instrument development center, Chinese Academy of Sciences Shenyang to produce, at ferromagnetism target head a purity being installed is 99.99% Fe target, and the thickness of target is 2mm, and diameter is 60mm; Distance between target and the substrate frame is 10cm;
2, p-type Si single crystal substrates material is removed surface impurity by hyperacoustic mode after, p-type Si single crystal substrates is installed on the substrate frame that is positioned at target head top;
3, the adjustable superhigh vacuum magnetron sputtering film-plating machine of unlatching three targets successively starts the one-level mechanical pump and the secondary molecular pump vacuumizes, until the back end vacuum degree of sputtering chamber is better than 8 * 10
-6Pa;
4, the back end vacuum degree when sputtering chamber is better than 8 * 10
-6During Pa, passing into purity to vacuum chamber is 99.999% Ar and O
2Mist, at 1Pa, wherein the flow of Ar gas is 100sccm, O with vacuum keep
2The flow of gas is 2.4sccm; Until the sample preparation end, and after stopping sputter, just can stop in sputtering chamber, to pass into Ar and O
2Mist;
5, finish the 4th) after the step, p-type Si single crystal substrates temperature is risen to 500 ℃ with 10 ℃/second speed;
6, until base reservoir temperature reach 500 ℃ and stable after, open the stepping motor of control substrate frame rotation, make substrate frame and be installed in p-type Si single crystal substrates on the substrate frame with the rotational speed of per minute 2 circles; Until after the sample preparation end, just can stop the substrate frame rotation;
7, open shielding power supply, apply the electric current of 0.2A and the direct voltage of 350V at the Fe target, pre-sputter 10 minutes waits sputtering current and voltage stabilization;
8, the plate washer of opening substrate frame below begins sputter, and in the sputter procedure, p-type Si single crystal substrates remains on 500 ℃, and always with the rotational speed of 2 circles each second;
9, sputter was closed the plate washer of substrate frame below after 15 minutes, then closed shielding power supply, stopped to pass into sputter gas Ar and O
2, open slide valve fully, continue to vacuumize, turn off the stepping motor of control substrate frame rotation, and p-type Si single crystal substrates temperature is down to room temperature with the rate of temperature fall of 5 ℃/min, then close vacuum system; After system cools, being filled with purity to vacuum chamber is 99.999% nitrogen, until the air pressure in the sputtering chamber reaches a standard atmospheric pressure, stops to pass into nitrogen, opens vacuum chamber, takes out the Fe that grows on the p-type Si single crystal substrates
3O
4Sample.
We have carried out X-ray diffraction to prepared sample, x-ray photoelectron power spectrum, the measurement of magnetic property and electronic transport characteristic.
Fig. 1 has provided the Fe of preparation
3O
4The X-ray diffraction spectrum of/p-Si structure.As can be seen from the figure, diffraction maximum all comes from Fe
3O
4And Si (400), illustrate that the sample of preparation is the polycrystalline Fe that does not have oriented growth
3O
4Film.
Fig. 2 has provided the Fe of preparation
3O
4The photoelectron spectroscopy figure of Fe 2p in the/p-Si structure.As can be seen from the figure, Fe
2+Characteristic peak be positioned at 709 and 723eV, cause Fe 2p
1/2With Fe 2p
3/2The broadening at peak, the Fe at the 719eV place
3+The feature satellites, these two characteristics further specify us and are prepared as Fe
3O
4Sample.
Fig. 3 has provided the Fe of preparation
3O
4Null field cooling curve under the 300Oe magnetic field of/p-Si structure and extra show cooling curve.As can be seen from the figure, significant change appears in the magnetization of sample near 116K, and the Verwey transition temperature that the sample that we prepare is described is 116K, and this proves that further the sample that we prepare is near stoichiometric Fe
3O
4Sample.
Fig. 4 has provided the Fe of preparation
3O
4The temperature of/p-Si structure is that 100K and magnetic field are that magneto-resistor under the 50kOe is with the variation relation curve of impressed current.As can be seen from the figure, this heterostructure is under the 100K temperature, under the 50kOe magnetic field, in the current range of 1mA, and the maximum magnetic flux resistance value can reach 40%.
Fig. 5 has provided Fe
3O
4The electronic transport feature measurement schematic diagram of/p-Si structure.It is the standard four-end method that this figure has provided the electrode connection of measuring magneto-resistance effect among the present invention, and electrode is Ag.
Claims (1)
1. one kind has the Fe that electric current is regulated and control magneto-resistance effect
3O
4/ p-Si structure is characterized in that in resistivity be the p-type Si single crystal substrates of the 0.02 Ω cm Fe that grows
3O
4This structure is under the 100K temperature, under the 50kOe magnetic field, in the current range of 1mA, and the maximum magnetic flux resistance value can reach 40%; The preparation method is as follows:
1) the adjustable superhigh vacuum magnetron sputtering film-plating machine of three targets that adopts scientific instrument development center, Chinese Academy of Sciences Shenyang to produce, at ferromagnetism target head a purity being installed is 99.99% Fe target, and the thickness of target is 2mm, and diameter is 60mm; Distance between target and the substrate frame is 10cm;
2) p-type Si single crystal substrates material is removed surface impurity by hyperacoustic mode after, p-type Si single crystal substrates is installed on the substrate frame that is positioned at target head top;
3) the adjustable superhigh vacuum magnetron sputtering film-plating machine of unlatching three targets successively starts the one-level mechanical pump and the secondary molecular pump vacuumizes, until the back end vacuum degree of sputtering chamber is better than 8 * 10
– 6Pa;
4) the back end vacuum degree when sputtering chamber is better than 8 * 10
– 6During Pa, passing into purity to vacuum chamber is 99.999% Ar and O
2Mist, wherein the flow of Ar gas is 100sccm, O
2The flow of gas is 2.4sccm, with vacuum keep at 1Pa;
5) p-type Si single crystal substrates temperature is risen to 500 ℃ with 10 ℃/second speed;
6) until base reservoir temperature reach 500 ℃ and stable after, open the stepping motor of control substrate frame rotation, make substrate frame and be installed in p-type Si single crystal substrates on the substrate frame with the rotational speed of per minute 2 circles;
7) open shielding power supply, apply the electric current of 0.2A and the direct voltage of 350V at the Fe target, pre-sputter 10 minutes waits sputtering current and voltage stabilization;
8) plate washer of opening substrate frame below begins sputter, and in the sputter procedure, p-type Si single crystal substrates remains on 500 ℃ and always with the rotational speed of 2 circles each second;
9) sputter was closed the plate washer of substrate frame below after 15 minutes, then closed shielding power supply, stopped to pass into sputter gas Ar and O
2, open slide valve fully, continue to vacuumize, turn off the stepping motor of control substrate frame rotation, and p-type Si single crystal substrates temperature is down to room temperature with the rate of temperature fall of 5 ℃/min, then close vacuum system; After system cools, being filled with purity to vacuum chamber is 99.999% nitrogen, until the air pressure in the sputtering chamber reaches a standard atmospheric pressure, stops to pass into nitrogen, opens vacuum chamber, takes out the Fe that grows on the p-type Si single crystal substrates
3O
4Sample.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110339932.5A CN102509768B (en) | 2011-11-01 | 2011-11-01 | Fe3O4 (ferroferric oxide)/p-Si (p-type silicon) structure capable of regulating and controlling magneto-resistance effect with current and preparation method for same |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110339932.5A CN102509768B (en) | 2011-11-01 | 2011-11-01 | Fe3O4 (ferroferric oxide)/p-Si (p-type silicon) structure capable of regulating and controlling magneto-resistance effect with current and preparation method for same |
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|---|---|
| CN102509768A CN102509768A (en) | 2012-06-20 |
| CN102509768B true CN102509768B (en) | 2013-10-30 |
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| CN105552213B (en) * | 2015-12-08 | 2017-12-05 | 山东大学 | A kind of method of regulation and control magneto-resistor ratio |
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Non-Patent Citations (6)
| Title |
|---|
| Electrical transport properties and magnetoresistance of polycrystalline Fe3O4/p-Si heterostructures;W.B.Mi,E.Y.Jiang,H.L.Bai;《J.App.Phys.》;20101231;正文第3部分III.RESULTS AND DISCUSSION * |
| Growth and properties of pulsed laser deposited thin films of Fe3O4 on Si substrates of different orientation;Shailja Tiwari,et al.;《J.Phys.Condens.Matter.》;20071231;全文 * |
| Shailja Tiwari,et al..Growth and properties of pulsed laser deposited thin films of Fe3O4 on Si substrates of different orientation.《J.Phys.Condens.Matter.》.2007, |
| W.B.Mi E.Y.Jiang |
| 宋亚舞.非磁性半导体的异常磁电阻效应研究.《中国优秀硕士学位论文全文数据库》.2008, |
| 非磁性半导体的异常磁电阻效应研究;宋亚舞;《中国优秀硕士学位论文全文数据库》;20081016;全文 * |
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