CN1331975C - Nano grain iron germanium particle film magnetic sensitive material - Google Patents
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- CN1331975C CN1331975C CNB2005101222363A CN200510122236A CN1331975C CN 1331975 C CN1331975 C CN 1331975C CN B2005101222363 A CNB2005101222363 A CN B2005101222363A CN 200510122236 A CN200510122236 A CN 200510122236A CN 1331975 C CN1331975 C CN 1331975C
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Abstract
The present invention relates to magnetic sensitive materials of nanocrystal iron-germanium granule films, which are used as magnetic sensitive materials of an active layer in Hall elements, and have a general formula of Fe<x>Ge<1-x>, wherein x is the volume percentage of the metal granules of Fe, and is greater than 0.45 and less than 0.60, and the thickness of the film is 4 to 8 nm. The nanocrystal iron-germanium granule film materials of the present invention are different from the traditional semiconductor materials and iron-germanium granule film materials of noncrystalline structure; the sensitivity of Hall resistance reaches 125 V/AT; the operating temperature range can be extended to -250 DEG C to 200 DEG C, and the nanocrystal iron-germanium granule film materials have little thermal drift and zero magnetic field offset. Compared with the traditional semiconductor materials, the magnetic sensitive materials of the present invention have the advantages of simple material preparation, low cost, high sensitivity, wide operating temperature range and small size of elements, and thus, the magnetic sensitive materials have broad application prospects in the fields of aviation, spaceflight, military affairs, etc.
Description
Technical field
The invention belongs to the new function material field, particularly a kind of nano crystal iron-germanium granule magneto sensitive material, it is as the magnetic-sensitive material of active coating in the Hall element.
Background technology
Hall element is a kind of magnetic sensor device that the Hall effect of the active layer material of utilization own is measured magnetic field, active coating, the electrode of being made by semiconductor single crystal material and protect their encapsulation to form.At present, the whole world to the annual requirement of hall device more than 1,000,000,000, detect at brushless machine, gear rotational speed, noncontacting switch, position-sensing switch in the process control, the security device ABS (ABS (Anti-lock Braking System)) of automobile, car engine ignition has regularly obtained on the current/voltage transmitter etc. using widely.Be characterized in contactless sensing, the reliability height in order to detect current/voltage, does not have the loss of insertion, and realize input and output signal isolation fully, do not have overload and damage or the like.At aspects such as the accurate Drawing of the research of magneticsubstance and magnetic measurement apparatus, earth magnetism field pattern, geological prospecting, navigation, Aeronautics and Astronautics crucial purposes is arranged all.
The active layer material of the magnetosensitive sense in the present Hall element generally all adopts semiconductor materials such as silicon, indium antimonide, indium arsenide, arsenic potassium, and the yardstick of element is in the submillimeter magnitude.And, because that characteristic parameters such as the concentration of the current carrier of semiconductor material, mobility vary with temperature is very big, the working temperature of Hall element is restricted, for example, the working temperature of general Hall element is-40 ℃ to+150 ℃.If in wideer temperature range, for example-250 ℃ to+200 ℃ of work, must be used in combination the Hall element of multiple model, the size that this has just further strengthened Hall element also makes the element cost increase greatly.For overcoming big, the shortcomings such as cost is high, complicated process of preparation of semiconductor active layer material volume, must seek a kind ofly have the magnetic field sensitivity close with semiconductor material, working temperature is wide, volume is little, prepare simple equivalent material.
People such as A.B.Pakhomov [A.B.Pakhomov, X.Yan, B.Zhao.Giant Hall effect in percolatingferromagnetic 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 pure metal material.Subsequently, people are successively at NiFe-SiO
2, Fe-SiO
2Deng also having found huge Hall effect in the particle film system.This discovers, for people provide a kind of magnetic-sensitive material as the Hall element active coating except that semiconductor material.
So-called ferromagnetic metal particle film material is to be distributed in isolators such as silicon-dioxide immediately by magnetic metals such as the iron of nanoscale, cobalts, or the matrix material that constitutes in the semi-conductor parents such as silicon, germanium, structural parameter such as the metallic particles yardstick of material, metal volume fraction, film thickness can arbitrarily be controlled as required, belong to typical artificial structure's nano-functional material.Different with the normal Hall effect of semiconductor material, the Hall effect of ferromagnetic metal particle film material comprises two portions, 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 current carrier, to cause in the formula, D is a demagnetizing factor, this is identical with Hall effect mechanism in non-magnetic metal or the semi-conductor; Second expression is the distinctive attribute of magneticsubstance by the Hall effect that the magnetic scattering causes, is called as extraordinary Hall effect.When metal volume per-cent during at 0.45～0.60, the unusual Hall coefficient of ferromagnetic metal particle film is near the numerical value of semiconductor silicon, and this just provides possibility for the application of particle film in Hall element.
The Hall resistance R of magnetic metal particle film
HCan be expressed as R
H=V
H/ i=ρ
H/ d=(R
0B+R
sM)/and d, as seen, Hall resistance in the magnetic granular thin film and specific magnetising moment 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 ferromagneticgranular metal-insulator films.Applied Physical Letters, 1995,67 (23): 3497～3499] Ni-SiO of Bao Dao thickness～1 μ m
2Particle film be 0.45～0.60 o'clock at metal volume per-cent x, the saturated Hall resistance of its maximum is about～2 Ω, theoretically, when film thickness reduces 100 times, when being 100 , its Hall resistance can reach～200 Ω about, far above the sensitivity of some semiconductor silicon or germanium Hall element.But, in most magnetic metal particle 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 andzero-field-cooled/field-cooled magnetization study of Co such as J.C.Denardin
x(SiO
2)
1-xGranular films, Physical ReviewB, 2002,65 (6): 054422/1～8] this phenomenon has been carried out detailed argumentation.Therefore, metallic ferromagnetic extraordinary Hall effect is applied to the senser element material, must guarantees that the specific magnetising moment 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.
Summary of the invention
The purpose of this invention is to provide a kind of nano crystal iron-germanium granule magneto sensitive material, it is different from conventional semiconductor material, nanocrystalline iron-germanium particle film the material that also is different from simultaneously non-crystal structure, its Hall resistance sensitivity is up to 125V/AT, working temperature can expand to-250 ℃ to+200 ℃, and has littler thermal drift, zero magnetic field skew.Compare with traditional semiconductor material, material preparation of the present invention is simple, and cost is low, and is highly sensitive, operating temperature range is wide, and device size is little, thereby uses more extensive.
The general formula of nano crystal iron-germanium granule magneto sensitive material provided by the invention is Fe
xGe
1-x, wherein x is the shared volume percent of metallic particles of iron in the material, 0.45＜x＜0.60, preferred x=0.52～0.58; Film thickness is in 4～8 nanometers, and preferred film thickness is in 5 nanometers.
The following step of preparation method's process of nano crystal iron-germanium granule magneto sensitive material of the present invention:
1) at first, on substrate, form " ten " font pattern with photolithography for the deposited iron germanium film, as Fig. 1 (a), dash area resist coating not among the figure, the foursquare length of side of pattern center is at 0.3～1.0 μ m, and the length of protuberance is 0.2 μ m on foursquare four limits, center.
2) adopt general ultrahigh vacuum(HHV) facing-target magnetron sputtering system coating equipment, earlier highly purified argon gas is fed vacuum chamber;
3) open degree of reduction ultrahigh vacuum(HHV) slide valve is set radio frequency power on the germanium target, and the iron target is set dc power, and the substrate Rotating with Uniform is carried out pre-sputter;
4) open the baffle plate of iron target, germanium target and substrate, iron target d.c. sputtering, the radio-frequency sputtering of germanium target, two target centre bits are set to the inclination angle, and are common facing to the substrate spatter film forming that is positioned at the top, center;
5) by the magnetic force rotating shaft sample is delivered to secondary vacuum chamber, take out sample, remove photoresist material; And form in order to deposit the rectangular patterns of four electrodes with the outside on photolithography four limits of square iron germanium 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 iron germanium film respectively.Sample is sent into vacuum chamber, prepare the titanium layer after 50 nanometers and the gold layer of 300 nanometer thickness continuously and form electrode, titanium target and gold target all adopt d.c. sputtering.
6) by the magnetic force rotating shaft sample is delivered to secondary vacuum chamber, take out sample, remove photoresist material; And form in order to deposit the square pattern of protective layer above square iron germanium film on the substrate with photolithography, the foursquare length of side covers the iron germanium film fully at 0.5～1.2 μ m.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, and setting sputtering power is 200 watts, and sputtering time is 10 minutes.
The following step of preparation method's process of nano crystal iron-germanium granule magneto sensitive material of the present invention:
1) at first, on substrate, form " ten " font pattern with photolithography for the deposited iron germanium film, as Fig. 1 (a), dash area resist coating not among the figure, the foursquare length of side of pattern center is at 0.3～1.0 μ m, and the length of protuberance is 0.2 μ m on foursquare four limits, center.
2) adopt general ultrahigh vacuum(HHV) facing-target magnetron sputtering system coating equipment, be better than 3 * 10 in back of the body end vacuum tightness
-7During Torr, highly purified argon gas is fed vacuum chamber, argon flow amount is 10sccm.
3) drop to 3 * 10 in vacuum tightness
-4During Torr, the open degree of ultrahigh vacuum(HHV) slide valve is set at 20%; Adjust iron and inclination angle, two target central positions of germanium 30 degree, be set at 15 watts radio frequency power on the germanium target, be set at 9 watts dc power on the iron target, pre-sputter 20～25 minutes;
4) open the baffle plate of iron target, germanium target and substrate, iron target and germanium target be jointly facing to the substrate spatter film forming that is positioned at 10～11 cm height places, top, center, and 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 material; And form in order to deposit the rectangular patterns of four electrodes with the outside on photolithography four limits of square iron germanium 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 iron germanium 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 d.c. sputtering.
6) by the magnetic force rotating shaft sample is delivered to secondary vacuum chamber, take out sample, remove photoresist material; And form in order to deposit the square pattern of protective layer above square iron germanium film on the substrate with photolithography, the foursquare length of side covers the iron germanium film fully at 0.5～1.2 μ m.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, and setting sputtering power is 200 watts, and sputtering time is 10 minutes.
Nano crystal iron-germanium granule magneto sensitive material provided by the invention is used for preparing Hall element as the magnetic-sensitive material of active coating.
The ferromagnetic metal particle film active coating of Hall element of the present invention adopts the design of " ten " font, and the dimension of active coating is at 0.3～1.0 micron.
Substrate of the present invention is glass, quartz, silicon single crystal, monocrystalline arsenic potassium etc.
The invention provides a kind of is active coating with the magnetic granular thin film; utilize the miniature Hall element of magneticsubstance extraordinary Hall effect principle work; its working temperature is in-250 ℃ to+200 ℃ scopes; and has a higher sensitivity; the Hall resistance sensitivity of Hall element is up to more than the 125VA/T; near the GaAs Hall element, be silicon and more than 3 times of germanium Hall element with commercialization of identical input resistance numerical value.And in-250 ℃ to+200 ℃ operating temperature range, the linear lag of sample is better than 3/1000ths, and thermal drift is less than 140ppm/K, and zero magnetic field side-play amount is in 5/1000ths.
The present invention is in-250 ℃ to+200 ℃ temperature range, and the sensitivity of material is temperature independent.
Nano crystal iron-germanium particle thin-film material of the present invention is different from conventional semiconductor material, nanocrystalline iron-germanium particle film the material that also is different from simultaneously non-crystal structure, its Hall resistance sensitivity is up to 125V/AT, working temperature can expand to-250 ℃ to+200 ℃, and has littler thermal drift, zero magnetic field skew.Compare with traditional semiconductor material, material preparation process of the present invention is simple, and cost is low.The Hall element volume of making is little, preparation is simple, highly sensitive, operating temperature range is wide, and device size is little, thereby has broad application prospects in fields such as Aeronautics and Astronautics, military affairs.
Description of drawings
Fig. 1 is the pattern of preparation nano crystal iron-germanium particle thin-film active coating and electrode, dash area resist coating not among the figure.
Fig. 2 is that nano crystal iron-germanium particle thin-film is 0.58 at the shared volume percent 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 the Fe of 5 nanometers
0.54Ge
0.46Sensitivity and the temperature relation of iron-germanium particle thin-film sample in Kelvin's temperature is 2～480K scope.
Fig. 4 is that thickness is the Fe of 5 nanometers
0.54Ge
0.46The linear lag of iron-germanium particle thin-film sample and temperature relation.
Embodiment
Embodiment 1
1, the preparation of active coating pattern.On substrate, form " ten " font pattern with photolithography for the deposited iron germanium 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 protuberance is 0.2 μ m on foursquare four limits, center.
2, feed argon gas under the room temperature.Adopt the DPS-III type ultrahigh vacuum(HHV) facing-target magnetron sputtering system coating equipment at Shenyang section of Chinese Academy of Sciences instrument center, be better than 3 * 10 in back of the body end vacuum tightness
-7During Torr, highly purified argon gas is fed vacuum chamber, argon flow amount is 10sccm.Treat that vacuum tightness 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 ultrahigh vacuum(HHV) slide valve.
3, pre-sputter.Adjust purity and be about 99.99% iron and inclination angle, two target central positions of germanium 30 degree, be set at 15 watts radio frequency power on the germanium target, be set at 10 watts dc power on the iron target, pre-sputter 20 minutes.
4, spatter film forming.Open the baffle plate of 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 material; And form in order to deposit the rectangular patterns of four electrodes with the outside on photolithography four limits of square iron germanium 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 iron germanium 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 d.c. sputtering.
6, preparation protective layer.By the magnetic force rotating shaft sample is delivered to secondary vacuum chamber, take out sample, remove photoresist material; And form in order to deposit the square pattern of protective layer above square iron germanium film on the substrate with photolithography, the foursquare length of side covers the iron germanium film fully at 0.5～1.2 μ m.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, and setting sputtering power is 200 watts, and sputtering time is 10 minutes.
Test result:
The shared volume percent x of metallic particles that adopts magnetron sputtering method to prepare iron is 0.58, and thickness is the nano crystal iron-germanium particle thin-film of 5 nanometers, carries out the high resolution transmission electron microscope test, the results are shown in Figure 2.
As can be seen from Figure 2, the polycrystalline particle form of iron about with 6～8 nanometers exists, and germanium is present in the intergranular dark zone of iron with the form of amorphous, forms Fe
0.58Ge
0.42
Embodiment 2
Be set at 9 watts dc power on the iron target, the volume ratio x that other operational condition is tapped a blast furnace with embodiment 1 preparation is 0.54, and thickness is the brilliant iron-germanium particle thin-films of 5 nanos.
The physical properties survey meter PPMS-9 that utilizes U.S. Quantum Design company to produce, in the magnetic field range of ± 2kOe, shared volume percent x is 0.54 to the metallic particles of iron, thickness is the nano crystal iron-germanium particle thin-film of 5 nanometers, having carried out Kelvin's temperature is the sensitivity test of 2～480K, the results are shown in Figure 3.
Sensitivity is the important parameter of Hall element active coating, can be expressed as under the unit the action of a magnetic field resistance change that Hall element produces.The size of sensitivity has reflected the detectivity of Hall element to externally-applied magnetic field, and sensitivity is high more, and transmitter 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 50～400K, the Hall resistance sensitivity K of film
HValue about 125V/AT, this numerical value and semiconductor GaAs Hall element magnetic sensitivity K
H～120V/AT is approaching, and does not vary with temperature substantially.
Embodiment 3
The physical properties survey meter PPMS-9 that utilizes U.S. Quantum Design company to produce, in the magnetic field range of ± 2kOe, to the nano crystal iron-germanium particle thin-film of embodiment 2 preparation, in being the scope of 2～400K, Kelvin's temperature carries out linearity measure, the results are shown in Figure 4.
The linear lag of transmitter is characterizing the measuring accuracy of device to different magnetic field, and in the downfield scope of ± 2kOe, the film sample Hall resistance and the magnetic field that record under each temperature are located along the same line, and resistance and magnetic field show good linear relationship.Be the linear lag of quantificational expression measurement curve, we adopt the method for linear fit, draw the maximum relative error under the differing temps, are shown among Fig. 4.In the measurement temperature range of 2-480K, the linear lag of sample is better than 3/1000ths.
Embodiment 4: the area of the active coating that embodiment 1 is obtained is that 1 μ m * 1 μ m, thickness are the Hall element of 5 nanometers, with the commercial silicon Hall element with identical input resistance numerical value together, measure simultaneously the magnetic field of 500 oersteds at ambient temperature, the Hall resistance sensitivity of this material is 125VA/T, be commercial silicon Hall element Senior Three doubly more than.
Embodiment 5: the area of the active coating that embodiment 1 is obtained is that 1 μ m * 1 μ m, thickness are the Hall element of the present invention of 5 nanometers, with the commercial silicon Hall element with identical input resistance numerical value together, under-250 ℃ the low temperature environment that the physical properties survey meter PPMS-9 that U.S. Quantum Design company produces provides, measure the magnetic field of 1000 oersteds.The sensitivity of commercial silicon Hall element produces bigger variation, is changed to subzero 200 degrees centigrade 49VA/T by the 42VA/T of room temperature, and thermal drift is greater than 800ppm/K; And the Hall resistance sensitivity of hall device of the present invention is 126VA/T, and thermal drift obviously is better than commercial silicon Hall element less than 40ppm/K.
Fe-Ge nano-crystalline granule film is as the Hall element material, working temperature is in-250 ℃ to+200 ℃ scope, its resistance to low temperature is better than commercial semiconductor hall sensor, and advantage such as have highly sensitive, low thermal drift, the linear lag is good, zero magnetic field skew is little has broad application prospects in fields such as Aeronautics and Astronautics, military affairs.
Claims (2)
1, a kind of nano crystal iron-germanium granule magneto sensitive material, the general formula that it is characterized in that it is Fe
xGe
1-x, wherein x is the shared volume percent of metallic particles of iron, 0.45＜x＜0.60, and film thickness is 4～8 nanometers.
2, nano crystal iron-germanium granule magneto sensitive material according to claim 1 is characterized in that x=0.52-0.58.
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| CN1331975C true CN1331975C (en) | 2007-08-15 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1111829A (en) * | 1994-04-11 | 1995-11-15 | 日立金属株式会社 | Magnetic core elemment for antenna, thin-film antena, and card equipped with thin-film antenna |
| US5750273A (en) * | 1995-03-30 | 1998-05-12 | Kabushiki Kaisha Toshiba | Soft magnetic thin film and thin film magnetic element using the same |
| JP2000003875A (en) * | 1998-06-12 | 2000-01-07 | Semiconductor Energy Lab Co Ltd | Semiconductor device and manufacture thereof |
| JP2003264324A (en) * | 2002-03-12 | 2003-09-19 | Alps Electric Co Ltd | Magnetic detecting element |
-
2005
- 2005-12-08 CN CNB2005101222363A patent/CN1331975C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1111829A (en) * | 1994-04-11 | 1995-11-15 | 日立金属株式会社 | Magnetic core elemment for antenna, thin-film antena, and card equipped with thin-film antenna |
| US5750273A (en) * | 1995-03-30 | 1998-05-12 | Kabushiki Kaisha Toshiba | Soft magnetic thin film and thin film magnetic element using the same |
| JP2000003875A (en) * | 1998-06-12 | 2000-01-07 | Semiconductor Energy Lab Co Ltd | Semiconductor device and manufacture thereof |
| JP2003264324A (en) * | 2002-03-12 | 2003-09-19 | Alps Electric Co Ltd | Magnetic detecting element |
Non-Patent Citations (1)
| Title |
|---|
| Fe-Ge非晶薄膜的短程序结构 王文采，陈玉，金属学报，第25卷第1期 1989 * |
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