CN101705474B - Preparation method of iron nitride film with strong Hall effect - Google Patents
Preparation method of iron nitride film with strong Hall effect Download PDFInfo
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- CN101705474B CN101705474B CN2009102291890A CN200910229189A CN101705474B CN 101705474 B CN101705474 B CN 101705474B CN 2009102291890 A CN2009102291890 A CN 2009102291890A CN 200910229189 A CN200910229189 A CN 200910229189A CN 101705474 B CN101705474 B CN 101705474B
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- 229910001337 iron nitride Inorganic materials 0.000 title claims abstract description 25
- 230000005355 Hall effect Effects 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims description 16
- 239000000758 substrate Substances 0.000 claims abstract description 32
- 239000010409 thin film Substances 0.000 claims abstract description 26
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000004544 sputter deposition Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 239000008186 active pharmaceutical agent Substances 0.000 claims description 3
- 230000005307 ferromagnetism Effects 0.000 claims description 3
- 238000009434 installation Methods 0.000 claims description 3
- 238000007747 plating Methods 0.000 claims description 2
- 239000000356 contaminant Substances 0.000 claims 1
- 238000009776 industrial production Methods 0.000 abstract description 4
- 238000005546 reactive sputtering Methods 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 230000002159 abnormal effect Effects 0.000 abstract 1
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000004098 selected area electron diffraction Methods 0.000 description 3
- 229910001199 N alloy Inorganic materials 0.000 description 2
- 229910001566 austenite Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012552 review Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000005856 abnormality Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- YYXHRUSBEPGBCD-UHFFFAOYSA-N azanylidyneiron Chemical compound [N].[Fe] YYXHRUSBEPGBCD-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 238000005325 percolation Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002463 transducing effect Effects 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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Abstract
本发明涉及一种具有大的异常霍尔效应的氮化铁薄膜的制备方法，采用中科院沈阳科学仪器研制中心生产的KPS450型可调三靶超高真空磁控溅射镀膜机，在强磁性靶头上安装一个纯度为99.99％的Fe靶。靶材的厚度为2.3mm，直径为60mm；靶与基片之间的距离为10cm。开启磁控溅射设备，直至溅射室的背底真空度为8×10-6Pa；向真空室通入纯度为99.999％的Ar和N2的混合气体，将真空度保持在1Pa。在Fei靶上施加0.3A的电流和300V左右的直流电压；完全打开闸板阀，待系统冷却后，向真空室充入纯度为99.999％的氮气，打开真空室，取出样品。由于目前工业化生产所采用的主要方法是溅射法，本发明所采用的反应溅射法，不需要基底加热等附加条件，在工业化生产上具有明显优势。
The invention relates to a method for preparing an iron nitride thin film with a large abnormal Hall effect. The KPS450 adjustable three-target ultra-high vacuum magnetron sputtering coating machine produced by the Shenyang Scientific Instrument Development Center of the Chinese Academy of Sciences is used. A 99.99% pure Fe target is mounted on the head. The thickness of the target is 2.3 mm, and the diameter is 60 mm; the distance between the target and the substrate is 10 cm. Turn on the magnetron sputtering equipment until the back vacuum of the sputtering chamber is 8×10 -6 Pa; feed a mixed gas of Ar and N 2 with a purity of 99.999% into the vacuum chamber to keep the vacuum at 1 Pa. Apply a current of 0.3A and a DC voltage of about 300V to the Fei target; fully open the gate valve, and after the system cools down, fill the vacuum chamber with nitrogen with a purity of 99.999%, open the vacuum chamber, and take out the sample. Since sputtering is the main method used in industrial production at present, the reactive sputtering method adopted in the present invention does not require additional conditions such as substrate heating, and has obvious advantages in industrial production.
Description
Technical field
Patent of the present invention relates to a kind of preparation method with iron nitride thin film of big unusual Hall effect, more specifically, is a kind of preparation method who is applied to the iron nitride thin film with big unusual Hall effect on the electronics device.
Background technology
Successively reported near percolation threshold NiFe-SiO in 1995 and 1996
2, Fe-SiO
2, Ni-SiO
2Huge enhancing phenomenon [J.Appl.Phys., 1996,79 (8): 6140 ~ 6142 etc. hall effect in the magnetic metal one isolator particle film system; Appl.Phys.Lett., 1995,67 (23): 3497 ~ 3499].They find, under the temperature of 5K, and Ni-SiO
2The abnormality of film is the ear electricalresistivity suddenly
XyUp to 160 μ Ω cm,, and this phenomenon called huge hall effect than high four magnitudes of corresponding pure metal material.It is being with a wide range of applications aspect electronics devices such as magnetic transducing device.
Iron nitride thin film has erosion resistance, wear resistance and high advantages such as thermostability, becomes people's research focus.Up to now, because nitrided iron has a lot of phase structures, its magnetic property difference is very big, so people mainly study the magnetic property of iron nitride thin film.Fe-N Alloys has different phase structures in different temperature under the different nitrogen contents.Below 591 ℃, exist three of α, γ ', ε etc. single-phase in the Fe-N Alloys system, it is respectively body-centered cubic (bcc) that iron atom is wherein arranged, face-centered cubic (fcc) and hexagonal solid matter (hcp) structure.At the nitrogen-atoms percentage composition less than 20% o'clock, four phases: the α-Fe of body-centered cubic structure (N) below in the iron nitrogen system, existing, the α '-Fe (N) of body-centered teteragonal (bct) structure, the α " Fe of body-centered structure of the quartet
16N
2γ '-Fe with simple cubic structure
4Four phases such as N.Wherein, α " Fe
16N
2Saturation magnetization the highest, be the focus of people research in the last thirty years.But up to the present, people are less to the electronic transport The Characteristic Study of iron nitride thin film.
At present, have only in the experiment both domestic and external report people such as Y.H.Cheng go up at PHYSICAL REVIEW B 80,174412 (2009) report the preparation of employing sputtering methods be mixed with γ-Fe
2O
3ε-Fe
3Found unusual hall effect among the N, but wherein the resistivity of ear unusually suddenly of report only is 25 μ Ω cm, the Hall resistivity among the present invention (61 μ Ω cm) will be hanged down more than one times.
Summary of the invention
From the angle of suitability for industrialized production, need to use sputtering method to prepare sample, and require preparation condition fairly simple; The sample that needs to prepare from practical application has the big resistivity of ear suddenly.The present invention promptly from above two purposes, has developed reactive magnetron sputtering method and has prepared the iron nitride thin film material, and has the big resistivity of ear suddenly.
The present invention is when the preparation iron nitride thin film, and the base material that is adopted is a glass substrate.
Concrete preparation method of the present invention realizes through following steps:
1, the adjustable three target superhigh vacuum magnetron sputtering film-plating machines of KPS450 type that adopt scientific instrument development center, Chinese Academy of Sciences Shenyang to produce, purity of installation is 99.99% Fe target on ferromagnetism target head.The thickness of target is 2.3mm, and diameter is 60mm; Distance between target and the substrate is 10cm.
2, base material is removed surface impurity by modes such as ultrasonic wave after, substrate is installed on the substrate frame, the distance between target and the substrate is 10cm, substrate frame up, target below;
3, unlatching magnetron sputtering equipment successively starts the one-level mechanical pump and the secondary molecular pump vacuumizes, and vacuum tightness is 8 * 10 at the bottom of the back of the body of sputtering chamber
-6Pa;
4, feeding purity to vacuum chamber is 99.999% Ar (100sccm) and N
2Mixed gas (15sccm) remains on 1Pa with vacuum tightness.
5, open shielding power supply, at electric current that applies 0.3A on the Fei target and the volts DS about 300V, pre-sputter 10 minutes waits sputtering current and voltage stable;
6, the plate washer of opening on the substrate frame begins sputter, and substrate position is fixed.In the sputter procedure, substrate is not heated;
7, 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, close vacuum system then.After treating system cools, charging into purity to vacuum chamber is 99.999% nitrogen, opens vacuum chamber, takes out sample.
Iron nitride thin film involved in the present invention has potential on electronics device uses, and the present invention adopt reactive sputtering be conventional means, the target of industrial production thin-film material select simple and the target rate of utilization than advantages such as height.
Compare with other method with thin-film material of big unusual hall effect; the prepared iron nitride thin film of the present invention has big hall effect; and ear resistivity does not vary with temperature with the slope of the variation relation in magnetic field suddenly under downfield, helps its practical application on electronics device.The method that is adopted is simple and practical, helps the popularization on industrial production.
Unusually suddenly the ear resistivity of the prepared sample of the present invention bigger (61 μ Ω cm) is much larger than the γ-Fe that is mixed with of people such as Y.H.Cheng in PHYSICAL REVIEW B 80,174412 (2009) the last employing sputtering method preparations of reporting
2O
3ε-Fe
3Found among the N that ear resistivity only is 25 μ Ω cm unusually suddenly.So the material among the present invention more helps the application on actual electronics device.
Because the main method that present suitability for industrialized production is adopted is a sputtering method, reactive sputtering of the present invention does not need supplementary condition such as substrate heating, has clear superiority on suitability for industrialized production;
Description of drawings
Fig. 1 has provided the X-ray diffraction spectrum of the iron nitride thin film for preparing among the present invention.
Fig. 2 has provided the transmission electron microscope image of the iron nitride thin film for preparing among the present invention, and illustration is the selected area electron diffraction pattern.
Fig. 3 has provided the resistivity of iron nitride thin film of the present invention's preparation with the variation of temperature relation curve.
Fig. 4 has provided the resistivity of ear suddenly measured under the differing temps of iron nitride thin film of the present invention's preparation variation relation curve with externally-applied magnetic field, illustration be under the upfield suddenly ear resistivity with the variation relation curve of externally-applied magnetic field.
Embodiment
According to structure and property analysis that we carry out sample prepared among the present invention, the preferred forms that below the reactive sputtering method preparation is had the iron nitride thin film of big unusual Hall effect is described in detail:
1, the adjustable three target magnetic control sputtering coating equipments of KPS-I type ultrahigh vacuum(HHV) that adopt scientific instrument development center, Chinese Academy of Sciences Shenyang to produce, purity of installation is 99.99% Fe target on ferromagnetism target head.The thickness of target is 2.3mm, and diameter is 60mm; Distance between target and the substrate is 10cm.
2, base material is removed surface impurity by modes such as ultrasonic wave after, substrate is installed on the substrate frame, the distance between target and the substrate is 10cm, substrate frame up, target below;
3, unlatching magnetron sputtering equipment successively starts the one-level mechanical pump and the secondary molecular pump vacuumizes, and vacuum tightness is 8 * 10 at the bottom of the back of the body of sputtering chamber
-6Pa;
4, feeding purity to vacuum chamber is 99.999% Ar (100sccm) and N
2Mixed gas (15sccm) remains on 1Pa with vacuum tightness.
5, open shielding power supply, at electric current that applies 0.3A on the Fei target and the volts DS about 300V, pre-sputter 10 minutes waits sputtering current and voltage stable;
6, the plate washer of opening on the substrate frame begins sputter, and substrate position is fixed.In the sputter procedure, substrate is not heated;
7, 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, close vacuum system then.After treating system cools, charging into purity to vacuum chamber is 99.999% nitrogen, opens vacuum chamber, takes out sample.
For confirming effect of the present invention, we have carried out X-ray diffraction to prepared film of the present invention, the measurement of transmission electron microscope and electronic transport characteristic.
Fig. 1 has provided the X-ray diffraction spectrum of the iron nitride thin film for preparing among the present invention.As can be seen from the figure, diffraction peak comes from γ respectively " FeN (111) crystal face and ε-Fe
3N (101), (111), (112) and (202) crystal face, contain γ in the interpret sample " FeN and ε-Fe
3Two kinds of phases of N.
Fig. 2 has provided the transmission electron microscope image of the iron nitride thin film for preparing among the present invention, and illustration is the selected area electron diffraction pattern.From MIcrosope image, as can be seen, the amorphous substance of a lot of whites is arranged around the particle, and the particulate distribution of sizes is inhomogeneous.From the selected area electron diffraction pattern, we can see that diffraction ring corresponds respectively to γ " FeN (111) crystal face and ε-Fe
3N (101), (111), (112) and (202) crystal face have further proved the result of X-ray diffraction.
Fig. 3 has provided the resistivity of iron nitride thin film of the present invention's preparation with the variation of temperature relation curve.To find out from figure, the resistivity of sample raises along with the reduction of temperature, shows as semi-conductive conductive characteristic.
Fig. 4 has provided the ear suddenly resistivity measured under the differing temps of iron nitride thin film of the present invention's preparation variation relation curve with externally-applied magnetic field.As can be seen from the figure, the unusual ear resistivity suddenly of the maximum saturation of sample is the 61 μ Ω cms of 3 temperature when being 3K.And in the magnetic field range of+10kOe, the resistivity of ear suddenly of sample is the linear changing relation with externally-applied magnetic field at-10k0e.The slope of this linear relationship is constant in 3K arrives the temperature range of 305K, and that is to say does not have dependency to temperature, and these characteristics help its practical application in this temperature range.Illustration be under the upfield suddenly ear resistivity with the variation relation curve of externally-applied magnetic field.As can be seen from the figure, the saturated resistivity of ear suddenly of sample reduces along with the increase of temperature.
The preparation method of the iron nitride thin film that the present invention proposes with big unusual Hall effect; be described by embodiment; person skilled obviously can be changed or suitably change and combination content as herein described in not breaking away from content of the present invention, spirit and scope, realizes the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.
Claims (1)
1. preparation method with iron nitride thin film of big unusual Hall effect is characterized in that step is as follows:
1) the adjustable three target superhigh vacuum magnetron sputtering film-plating machines of KPS450 type that adopt scientific instrument development center, Chinese Academy of Sciences Shenyang to produce, purity of installation is 99.99% Fe target on ferromagnetism target head; The thickness of target is 2.3mm, and diameter is 60mm; Distance between target and the substrate is 10cm;
2) with behind the substrate material surface contaminant removal, substrate is installed on the substrate frame, the distance between target and the substrate is 10cm, substrate frame up, target below;
3) unlatching magnetron sputtering equipment successively starts the one-level mechanical pump and the secondary molecular pump vacuumizes, and vacuum tightness is 8 * 10 at the bottom of the back of the body of sputtering chamber
-6Pa;
4) feeding purity to vacuum chamber with the speed of 100sccm is 99.999% Ar and to feed purity with the speed of 15sccm be 99.999% N
2Mixed gas, vacuum tightness is remained on 1Pa;
5) open shielding power supply, apply the electric current of 0.3A and the volts DS of 300V on the Fe target, pre-sputter 10 minutes waits sputtering current and voltage stable;
6) plate washer of opening on the substrate frame begins sputter, and substrate position is fixed; In the sputter procedure, substrate is not heated;
7) 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, close vacuum system then; After treating system cools, charging into purity to vacuum chamber is 99.999% nitrogen, opens vacuum chamber, takes out sample;
8) measure the variation relation of the resistivity of ear suddenly of iron nitride thin film with externally-applied magnetic field, the maximum saturation of the iron nitride thin film sample of unusual Hall effect ear resistivity unusually suddenly is 61 μ Ω cm in temperature during for 3K.
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| CN102560352B (en) * | 2010-12-31 | 2014-03-05 | 中国科学院合肥物质科学研究院 | Tungsten sulfide and tungsten nitride composite film material and preparation method thereof |
| CN104451546A (en) * | 2014-11-25 | 2015-03-25 | 天津大学 | Preparation method of doped ferrite material with giant plane Hall effect |
| CN110129736B (en) * | 2019-04-30 | 2021-07-13 | 南开大学 | A kind of Fe/C60 particle thin film Hall effect material and preparation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6410170B1 (en) * | 1999-05-20 | 2002-06-25 | Read-Rite Corporation | High resistivity FeXN sputtered films for magnetic storage devices and method of fabrication |
| CN101003893A (en) * | 2007-01-18 | 2007-07-25 | 天津大学 | Method for preparing polycystalline thin film material of ferroferric oxide |
| CN101497987A (en) * | 2009-03-13 | 2009-08-05 | 天津大学 | Apparatus for preparing polycrystal ferriferrous oxide film by facing-target reactive sputtering and operation method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6410170B1 (en) * | 1999-05-20 | 2002-06-25 | Read-Rite Corporation | High resistivity FeXN sputtered films for magnetic storage devices and method of fabrication |
| CN101003893A (en) * | 2007-01-18 | 2007-07-25 | 天津大学 | Method for preparing polycystalline thin film material of ferroferric oxide |
| CN101497987A (en) * | 2009-03-13 | 2009-08-05 | 天津大学 | Apparatus for preparing polycrystal ferriferrous oxide film by facing-target reactive sputtering and operation method |
Non-Patent Citations (2)
| Title |
|---|
| Y F Chen et al.Structure and magnetic properties of RF sputtered Fe–N films.《JOURNAL OF PHYSICS D: APPLIED PHYSICS》.2007,第37卷(第10期),期刊第1429页右栏第2段至第1430页左栏第1段. * |
| 周剑平.磁控溅射Fe-N单层膜的研究.《金属功能材料》.2000,第7卷(第3期),期刊第26-31页. * |
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