CN100392775C - Magnetic-particle thin-film material and its preparation method and application - Google Patents
Magnetic-particle thin-film material and its preparation method and application Download PDFInfo
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- CN100392775C CN100392775C CNB2006100130570A CN200610013057A CN100392775C CN 100392775 C CN100392775 C CN 100392775C CN B2006100130570 A CNB2006100130570 A CN B2006100130570A CN 200610013057 A CN200610013057 A CN 200610013057A CN 100392775 C CN100392775 C CN 100392775C
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Abstract
The present invention relates to a magnetic granule film material and a preparation method and application thereof. The magnetic granule film material is prepared by that a magnetic granule film is prepared on a substrate and comprises (NiFe)<x>Ge<1-x>, wherein x is volume percentage of ferronickel alloy granules which account for 0.52 to 0.58%, and the thickness of the film is from 4 to 8 nanometers. The magnetic granule film is prepared by a magnetron sputtering method which comprises the following steps that high-purity argon is led into a vacuum chamber, and then the opening degree of ultra-high vacuum flash board valve is reduced to 20%; radio-frequency power of 25 W is added to a germanium target, and direct current power of 12 to 22 W is added to a ferronickel alloy target according to the requirements of components. The magnetic granule film of the present invention has the characteristics of simple preparation process, low cost, high sensitivity, wide working temperature range, small component size, etc., and therefore, the present invention has a wide application prospect in the fields of aviation, spaceflight, military affairs, etc.
Description
Technical field
The present invention relates to a kind of magnetic-particle thin-film material and its production and application, specifically is not magnetic-particle thin-film material of forming of alloy and germanium and preparation method thereof of a kind of glass with characteristics such as highly sensitive, that preparation technology is simple, preparation cost is low.
Background technology
Seminar from French scientist A.Fert in 1988 has periodically found giant magnetoresistance effect (giant magnetoresistance in the multilayer film at [Fe/Cr], GMR) since, researcher has successively been found giant magnetoresistance effect in membrana granulosa structures such as magnetic metallized multilayer film, [NiO/NiFe/Cu/NiFe/Cu/NiO] isospin valve arrangement and Cu-Co such as [Co/Ag (Ru, Cr)].Wherein, owing to have in the system of giant magnetoresistance effect at the magnetic tunnel-junction of feeromagnetic metal/insulator/feeromagnetic metal formation and the magnetic granular thin film that feeromagnetic metal-insulator constitutes etc., the transport mechanism of electronics is a tunneling effect, its giant magnetoresistance effect be also referred to as usually tunnelling road type magneto-resistor (tunnel magnetoresistance, TMR).
Since giant magnetoresistance effect and the magneto-resistance effect of tunnelling type are found, because it has highfield sensitivity, be widely applied to computer magnetic reading head, Weak magentic-field detection, position probing or the like magneto-dependent sensor spare very soon, relate to ambits such as information technology, medical science, chemistry, biology.Over particularly nearest more than 10 years, the application and development of magnetic resistance material is obtained progress rapidly, receive tangible economic benefit and social benefit.
Currently used magnetic resistance material mostly is spin valve structure, Chinese patent CN 1684145A for example: " magnetoresistance effect film and manufacturing thereof " (application number: CN200410074144.8), CN 1603454A: " a kind of method for preparing spin valve that improves giant magnetoresistance effect " (application number: CN200410067585.5), CN 1591580A: " magnetoresistance effect film; magneto-resistance effect magnetic head and solid-state memory " (application number: CN200410058665.4), CN1595676A: " magneto-resistive effect element; magnetic head; magnetcisuspension hanging component and magnetic reproducing apparatus " (application number: CN200410077156.6), CN 1604355A: " magneto-resistive effect element; magnetic head and magnetic reproducing device " (application number: CN200410083163.7) or the like.The magnetic resistance material of this structure is made up of substrate/resilient coating/ferromagnetic layer/Cu/ ferromagnetic layer/antiferromagnetic/cover layer usually, there is complicated process of preparation, the shortcoming such as stable of the material property that extends influence between layers of material, when particularly it is as device application, need add bias magnetic field, this has further strengthened the volume of device.For overcoming big, the shortcomings such as cost is high, complicated process of preparation of above-mentioned magnetic resistance material volume, must seek a kind ofly have highfield sensitivity, working temperature is wide, volume is little, the simple magnetosensitive sense material of preparation.
Nineteen ninety-five, people such as A.B.Pakhomov [A.B.Pakhomov, X.Yan, B.Zhao.Giant Hall effect inpercolating ferromagnetic granular metal-insulator films.Applied Physical Letters, 1995,67 (23): 3497～3499] reported Ni-SiO
2Etc. the huge enhancing phenomenon of Hall effect in the magnetic metallic particles membrane system, under the temperature of 5K, Ni-SiO
2The unusual Hall resistance rate ρ of film
XyUp to 160 μ Ω cm,,, and this phenomenon called huge Hall effect near the numerical value of semiconductor silicon than high four magnitudes of corresponding simple metal material.Subsequently, people are successively at NiFe-SiO
2, Fe-SiO
2Deng also having found huge Hall effect in the particle film system.These discover, for people provide a kind of novel, are different from the magnetic sensor device material of semi-conducting material and magnetic resistance material.
So-called magnetic-particle thin-film material be by the iron of nanoscale, cobalt, glass not magnetic metal such as alloy be randomly distributed in insulators such as silicon dioxide, or the composite material that constitutes in the semiconductor parents such as silicon, germanium, structural parameters such as the metallic particles yardstick of material, metal volume percentage, film thickness can arbitrarily be controlled as required, belong to typical artificial structure's nano-functional material.Different with the normal Hall effect of semi-conducting material, the Hall effect of magnetic-particle thin-film material comprises two parts, its Hall resistance rate ρ
XyCan be expressed as: ρ
Xy=R
0[H+4 π M (1-D)]+R
S4 π M.First normal Hall effect of representing Lorentz force action on charge carrier, to cause in the formula, D is a demagnetizing factor, this is identical with Hall effect mechanism in nonmagnetic metal or the semiconductor; Second expression is the distinctive attribute of magnetic material by the Hall effect that the magnetic scattering causes, is called as extraordinary Hall effect.When metal volume percentage during at 0.40～0.60, the unusual Hall coefficient of magnetic granular thin film is near the numerical value of semiconductor silicon, and this just provides possibility for the application of magnetic granular thin film in magnetic sensor device.
The Hall resistance R of magnetic granular thin film
HCan be expressed as R
H=V
H/ i=ρ
H/ d=(R
0B+R
sM)/and d, as seen, its Hall resistance and magnetization M are closely related, and are inversely proportional to the thickness of film.[A.B.Pakhomov such as A.B.Pakhomov, X.Yan, B.Zhao.Giant Hall effect in percolating ferromagnetic granular metal-insulator films.Applied Physical Letters, 1995,67 (23): 3497～3499] Ni-SiO of Bao Dao thickness～1 μ m
2Particle film be 0.40～0.60 o'clock at metal volume percentage x, the saturated Hall resistance of its maximum is about～2 Ω, theoretically, when film thickness reduces 100 times, is
The time, its Hall resistance can reach～200 Ω about, far above the sensitivity of some semiconductor silicon or germanium Hall element.But, in most magnetic granular thin films, reduction along with metal volume fraction and film thickness, magnetic-particle super-paramagnetic phenomena occurs in room temperature region, the saturation magnetization of film is reduced, suppressed the increase of Hall resistance, [Thermoremanence and zero-field-cooled/field-cooled magnetization study ofCo such as J.C.Denardin
x(SiO
2)
1-xGranular films, Physical Review B, 2002,65 (6): 054422/1～8] this phenomenon has been carried out detailed argumentation.Therefore, the extraordinary Hall effect of magnetic granular thin film is applied to the senser element material, must guarantees that the magnetization of film is basicly stable under the very little situation of thickness, such film just has the Hall resistance of the bigger numerical that the hall sensing modulator material possesses.
We [Journal of Applied Physics 98 (2005) p086105] have prepared the iron-germanium particle film material of amorphous, and thickness is the Fe of 4.1 nanometers
0.67Ge
0.33The Hall resistance sensitivity of sample is 82V/AT, is the twice with silica-based Hall element of identical input resistance value.But do not relate to concrete preparation technology in the report.
Summary of the invention
An object of the present invention is to provide a kind of magnetic-particle thin-film material, it is different from conventional semiconductor material or magnetic resistance material, iron-germanium particle film the material that also is different from simultaneously non crystalline structure, its Hall resistance sensitivity is up to 100V/AT, and working temperature can expand to-250 ℃ to+200 ℃.Compare with traditional semi-conducting material or magnetic resistance material, material preparation of the present invention is simple, and cost is low, and is highly sensitive, and operating temperature range is wide, and device size is little, thereby uses more extensive.
Another object of the present invention provides a kind of method of making described magnetic-particle thin-film material.
A kind of magnetic-particle thin-film material provided by the invention is to make magnetic granular thin film on substrate, and the composition of magnetic granular thin film mainly is (NiFe)
xGe
1-x, wherein the atomic ratio in the permalloy (dilval) is Ni: Fe=80: 20, and x is the shared percent by volume of the metallic particles of dilval in the material, preferred x=0.52～0.58; Film thickness is in 4～8 nanometers, and preferred film thickness is in 5 nanometers.Described substrate is glass, quartz, monocrystalline silicon, monocrystalline GaAs.
In order accurately to control the composition and the thickness of film, under different iron target sputtering power conditions, the thickness of preparing different iron contents is about (NiFe) of 300 nanometers earlier
xGe
1-xThe particle film material then with the composition of Xray fluorescence spectrometer mensuration material, is determined the thickness of material with the method for transmission electron microscope profile scanning.On this basis, by the sputtering power and the sputtering time of control iron target, accurately control (NiFe) respectively
xGe
1-xThe composition of thin-film material and thickness, thus optimum efficiency obtained.
(NiFe) of the present invention
xGe
1-xThe following step of preparation method's process of magnetic granular thin film:
1) at first, the usefulness photoetching process forms the pattern for nickel deposited iron germanium film on substrate;
2) adopt the superhigh vacuum magnetron sputtering film-plating machine, carrying on the back end vacuum degree less than 3 * 10
-7During Torr, highly purified argon gas is fed vacuum chamber, argon flow amount is 10sccm;
3) drop to 3 * 10 in vacuum degree
-4During Torr, the open degree of ultra high vacuum slide valve is set at 20%; Adjust dilval and inclination angle, two target centers of germanium 30 degree, be set at 25 watts radio-frequency power on the germanium target, be set at 12～20 watts direct current power on the ferronickel target, pre-sputter 20～25 minutes;
4) open the baffle plate of dilval target, germanium target and substrate, dilval target and germanium target are jointly facing to the substrate spatter film forming that is positioned at 12～14 cm height places, top, center, substrate is with 20～25 rev/mins speed Rotating with Uniform, and to set sputtering time be 2 minutes;
5) by the magnetic force rotating shaft sample is delivered to secondary vacuum chamber, take out sample, remove photoresist; And form pattern for depositing electrode with the outside of photoetching process particle film on substrate, and sample is sent into vacuum chamber, prepare the titanium layer of 50 nanometer thickness and the gold layer of 300 nanometer thickness continuously and form electrode, titanium target and gold target all adopt direct current sputtering;
6) by the magnetic force rotating shaft sample is delivered to secondary vacuum chamber, take out sample, remove photoresist; And with photoetching process above particle film on the substrate, form the deposition protective layer pattern; sample is sent into vacuum chamber prepare silicon dioxide layer of protection, the titanium dioxide silicon target adopts radio frequency sputtering, utilizes computer-controlled program; setting sputtering power is 250 watts, and sputtering time is 10 minutes.
The described particle film pattern of step 1) is " ten " font pattern, and the foursquare length of side of pattern center is at 0.3～1.0 μ m, and the length of ledge is 0.2 μ m on foursquare four limits, center.
The outside on four limits of described square particle film forms in order to deposit the rectangular patterns of four electrodes, and each electrode pattern has 0.15 micron lap with four limits of square particle film respectively.
The protective layer of described particle film is a square pattern, and the foursquare length of side covers particle film fully at 0.5～1.2 μ m.
(NiFe) provided by the invention
xGe
1-xMagnetic-particle thin-film material has highfield sensitivity, working temperature is wide, volume is little, prepare simple advantage, can be used to make magneto-dependent sensor spares such as computer magnetic reading head, magnetic random memory, Weak magentic-field detection, position probing.
(NiFe) of the present invention
xGe
1-xMagnetic granular thin film adopts the design of " ten " font, and the dimension of active layer is at 0.3～1.0 micron.
Substrate of the present invention is glass, quartz, monocrystalline silicon, monocrystalline GaAs etc.
A kind of magnetic granular thin film of the present invention is different from conventional semiconductor material and magnetic resistance material, and material of the present invention has advantages such as preparation technology is simple, highly sensitive, operating temperature range is wide, device size is little.
Description of drawings
Fig. 1 is preparation (NiFe)
xGe
1-xThe pattern of magnetic granular thin film and electrode, dash area resist coating not among the figure.Only drawn among the figure and particle film electrodes in contact part.
Fig. 2 is (NiFe)
xGe
1-xMagnetic granular thin film is 0.56 at the shared percent by volume x of the metallic particles of iron, the high resolution transmission electron microscope photo when thickness is 5 nanometers.
Fig. 3 is that thickness is 5 nanometers (NiFe)
0.56Ge
0.44Sensitivity and the temperature relation of magnetic granular thin film sample in Kelvin is 2～480K scope.
Embodiment
Embodiment 1
1, the preparation of active layer pattern.On substrate, form " ten " font pattern with photoetching process for the deposited particles film, as Fig. 1 (a), dash area resist coating not among the figure, the foursquare length of side of pattern center is at 1.0 μ m, and the length of ledge is 0.2 μ m on foursquare four limits, center.
2, feed argon gas under the room temperature.Adopt the DPS-III type superhigh vacuum magnetron sputtering film-plating machine at Shenyang section of Chinese Academy of Sciences instrument center, be better than 3 * 10 in back of the body end vacuum degree
-7During Torr, highly purified argon gas is fed vacuum chamber, argon flow amount is 10sccm.Treat that vacuum degree drops to 3 * 10
-4During the Torr left and right sides, the computer control software that utilizes equipment to carry is set at 20% with the open degree of ultra high vacuum slide valve.
3, pre-sputter.Adjust purity and be about 99.99% dilval target and inclination angle, germanium target center 30 degree, be set at 25 watts radio-frequency power on the germanium target, be set at 15 watts direct current power on the dilval target, pre-sputter 20 minutes.
4, spatter film forming.Open the baffle plate of dilval target, germanium target and quartz substrate, substrate is with 20 rev/mins speed Rotating with Uniform, and the control sputtering time was at 2 minutes, and film thickness is 5 nanometers.
5, preparation electrode.By the magnetic force rotating shaft sample is delivered to secondary vacuum chamber, take out sample, remove photoresist; And form in order to deposit the rectangular patterns of four electrodes with the outside on photoetching process four limits of square particle film on substrate, as Fig. 1 (b), dash area resist coating not among the figure, each electrode pattern have 0.15 micron lap with four limits of square particle film respectively.Sample is sent into vacuum chamber, prepare the titanium layer of 50 nanometer thickness and the gold layer of 300 nanometer thickness continuously and form electrode, titanium target and gold target all adopt direct current sputtering.
6, preparation protective layer.By the magnetic force rotating shaft sample is delivered to secondary vacuum chamber, take out sample, remove photoresist; And above square particle film on the substrate, form in order to deposit the square pattern of protective layer with photoetching process, the foursquare length of side covers particle film fully at 0.5～1.2 μ m.Sample is sent into vacuum chamber prepare silicon dioxide layer of protection 50 nanometers, the titanium dioxide silicon target adopts radio frequency sputtering, utilizes computer-controlled program, and setting sputtering power is 250 watts, and sputtering time is 10 minutes.
Embodiment 2
The model that adopts Muti-technic company to produce is the x-ray photoelectron spectrometer of Physical Electronic spectrometer S600, to (NiFe) of embodiment 1 preparation
xGe
1-xParticle film carries out composition test, and the metal volume fraction that calculates dilval particle in the particle film is 0.56, the consisting of of film: (NiFe)
0.56Ge
0.44
Embodiment 3
Adopting model is that the transmission electron microscope of JEOL 2010F is to embodiment 1 prepared (NiFe)
0.56Ge
0.44Particle film carries out the high resolution transmission electron microscope test, the results are shown in Figure 2.
As can be seen from Figure 2, the yardstick of the dilval particle of polycrystalline is 3 nanometers, and germanium is present in the intergranular bright zone of dilval with the form of amorphous.
Embodiment 4
The physical property measuring instrument PPMS-9 that utilizes U.S. Quantum Design company to produce is in the magnetic field range of ± 2kOe, to (NiFe) with extraordinary Hall effect of embodiment 1 preparation
0.56Ge
0.44Particle film carries out linearity measure in Kelvin is the scope of 2～400K, the results are shown in Figure 3.
Hall resistance sensitivity is the important parameter of particle film, can be expressed as under the unit the action of a magnetic field resistance variations of material production.The size of Hall resistance sensitivity has reflected the detectability of material to externally-applied magnetic field, and sensitivity is high more, and material is strong more to the amplifying power of field signal, and the lower limit in the magnetic field that can survey is more little.As seen from Figure 3, in the temperature range of 30～480K, the Hall resistance sensitivity K of material
HValue is about 100V/AT, and this numerical value is higher than the twice of commercial semiconductor silicon or germanium Hall element magnetic sensitivity, and does not vary with temperature substantially in the temperature range of 20～480K.
(NiFe) of the present invention
xGe
1-xMagnetic-particle thin-film material is different from conventional semiconductor material and magnetic resistance material, also is different from the iron-germanium particle film material of non crystalline structure simultaneously, and its Hall resistance sensitivity is up to 100V/AT, and working temperature can expand to-250 ℃ to+200 ℃.Material preparation process of the present invention is simple, highly sensitive, operating temperature range is wide, device size is little, thereby has broad application prospects in fields such as Aeronautics and Astronautics, military affairs.
Claims (8)
1. a magnetic-particle thin-film material is characterized in that it is to make magnetic granular thin film on substrate, and the composition of magnetic granular thin film is (NiFe)
xGe
1-x, wherein x is the shared percent by volume of metallic particles of dilval, 0.40＜x＜0.60; Ni: Fe=80: 20, atomic ratio; Film thickness 4～8 nanometers; Described substrate is glass, quartz, monocrystalline silicon or monocrystalline GaAs.
2. magnetic-particle thin-film material according to claim 1 is characterized in that x=0.52-0.58.
3. magnetic-particle thin-film material according to claim 1 is characterized in that it is the design of " ten " font, and its Hall resistance sensitivity is up to 100VA/T, and working temperature is at-250 ℃ to+200 ℃.
4. the preparation method of the described magnetic-particle thin-film material of claim 1 is characterized in that it being through following step:
1) at first, the usefulness photoetching process forms the pattern for nickel deposited iron germanium film on substrate;
2) adopt the superhigh vacuum magnetron sputtering film-plating machine, carrying on the back end vacuum degree less than 3 * 10
-7During Torr, highly purified argon gas is fed vacuum chamber, argon flow amount is 10sccm;
3) drop to 3 * 10 in vacuum degree
-4During Torr, the open degree of ultra high vacuum slide valve is set at 20%; Adjust dilval and inclination angle, two target centers of germanium 30 degree, be set at 25 watts radio-frequency power on the germanium target, be set at 12～20 watts direct current power on the ferronickel target, pre-sputter 20～25 minutes;
4) open the baffle plate of dilval target, germanium target and substrate, dilval target and germanium target are jointly facing to the substrate spatter film forming that is positioned at 12～14 cm height places, top, center, substrate is with 20～25 rev/mins speed Rotating with Uniform, and to set sputtering time be 2 minutes;
5) by the magnetic force rotating shaft sample is delivered to secondary vacuum chamber, take out sample, remove photoresist; And form pattern for depositing electrode with the outside of photoetching process particle film on substrate, and sample is sent into vacuum chamber, prepare the titanium layer of 50 nanometer thickness and the gold layer of 300 nanometer thickness continuously and form electrode, titanium target and gold target all adopt direct current sputtering;
6) by the magnetic force rotating shaft sample is delivered to secondary vacuum chamber, take out sample, remove photoresist; And with photoetching process above particle film on the substrate, form the deposition protective layer pattern; sample is sent into vacuum chamber prepare silicon dioxide layer of protection, the titanium dioxide silicon target adopts radio frequency sputtering, utilizes computer-controlled program; setting sputtering power is 250 watts, and sputtering time is 10 minutes.
5. the preparation method of magnetic-particle thin-film material according to claim 4, it is characterized in that the described particle film pattern of step 1) is " ten " font pattern, the foursquare length of side of pattern center is at 0.3～1.0 μ m, and the length of ledge is 0.2 μ m on foursquare four limits, center.
6. the preparation method of magnetic-particle thin-film material according to claim 5, the outside that it is characterized in that four limits of described square particle film forms in order to deposit the rectangular patterns of four electrodes, and each electrode pattern has 0.15 micron lap with four limits of square particle film respectively.
7. the preparation method of magnetic-particle thin-film material according to claim 5, the protective layer that it is characterized in that described particle film is a square pattern, the foursquare length of side covers particle film fully at 0.5～1.2 μ m.
8. the application of the described magnetic-particle thin-film material of claim 1 is characterized in that it is used for making computer magnetic reading head, magnetic random memory, Weak magentic-field detects or the magneto-dependent sensor spare of position probing.
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| CN100555698C (en) * | 2006-11-24 | 2009-10-28 | 中国科学院物理研究所 | A kind of metal multiple layer film hall device and preparation method thereof |
| CN112068044B (en) * | 2020-08-11 | 2021-11-05 | 苏州大学 | Method for visualizing complex magnetic field |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1172332A (en) * | 1996-07-31 | 1998-02-04 | 南京大学 | Granular membrane huge magnetic resistance effect sensor material |
| JP2001036162A (en) * | 1999-07-21 | 2001-02-09 | Hitachi Cable Ltd | Hall element |
| JP2002158226A (en) * | 2000-11-21 | 2002-05-31 | Sharp Corp | Silicon nitride solid surface protective film and its manufacturing method as well as hall element |
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2006
- 2006-01-16 CN CNB2006100130570A patent/CN100392775C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1172332A (en) * | 1996-07-31 | 1998-02-04 | 南京大学 | Granular membrane huge magnetic resistance effect sensor material |
| JP2001036162A (en) * | 1999-07-21 | 2001-02-09 | Hitachi Cable Ltd | Hall element |
| JP2002158226A (en) * | 2000-11-21 | 2002-05-31 | Sharp Corp | Silicon nitride solid surface protective film and its manufacturing method as well as hall element |
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