CN101900762A - Measuring method of magnetic resistivity of substance under the condition of high voltage - Google Patents
Measuring method of magnetic resistivity of substance under the condition of high voltage Download PDFInfo
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Abstract
The invention relates to a measuring method of the magnetic resistivity of a substance under the condition of high voltage, belonging to the technical field of measurement of physical quantities. The magnetic resistivity of the substance is measured on diamond anvil cells of a metal film electrode (13) on the basis of the van der pauw resistance measurement method according to the following test steps of: assembling equipment; regulating a magnetic field; carrying out the in-site measurement of magnetic field strength; measuring the magnetic resistivity; and the like. The metal film electrode (13) is deposited on one the used diamond anvil cells; a pressing machine (5) and a spacer (4) are both made of nonmagnetic materials; and only a shaking table (2) is made of steel materials. The invention mainly obtains the technical effect of accurately measuring the magnetoresistance effect of a sample under the condition of the high voltage, establishes a nonmagnetic measurement environment, provides a uniform magnetic field on space for the sample, eliminates the influences of lead resistance and contact resistance and carries out the in-site measurement on the magnetic field strength inside a cavity of the sample; and in addition, the used metal electrode (13) can bear high pressure without being cut easily.
Description
Technical field
The invention belongs to the technical field of physical quantity, particularly the measuring method of magnetic sample resistivity under the condition of high voltage.
Background technology
The application of adamas opposed anvils (DAC) is an important breakthrough in the high-potting field, also be present high pressure research personnel the most general employed high pressure generating apparatus it.The ability of its generation ultra-high pressure condition provides the possibility of more profound understanding material high-pressure property for people.Appearance along with various high energy detecting devicess, realize the research of the multiple physical property of material by DAC technology people, changed the research, electrical properties research of research, magneto-resistor etc. as structure of matter research, RAMAN SPECTRA, fluorescence spectrum research, magnetic variation.Magnetoresistance effect is the research focus of magneto-electronics and association area thereof always, reason is wide technology application, magnetoresistance effect can change into electric signal to the external magnetic field signal, so it is read and write at magnetic, aspects such as magnetic memory device and magnetic sensor have a wide range of applications.Aspect theory research, can obtain electron spin Changing Pattern in the material by the measurement of high pressure magnetoresistance, the mangneto phase transformation of reflection material.Along with the development of theoretical and experimental technique, people recognize the using value that magnetoresistance effect is huge gradually.
Measurement for material resistance under the condition of high voltage has obtained a lot of well experimental results.Yet these experiments all are to finish under relatively low pressure conditions, and highest pressure is no more than 5GPa.The technology of measuring resistance mainly is divided into two classes under the high pressure condition: the one, and the measurement of on big cavity press, carrying out, sample cavity is bigger, wiring easily, but the pressure that big cavity press can produce is lower, and therefore, the pressure of measurement is restricted; The 2nd, the measurement of on the adamas opposed anvils, carrying out, but because sample cavity is small, have only about 100 microns, carry out very difficulty of accurate electrode wiring therein, and electrode is easy to by the cut-out of the anvil face corner angle of diamond anvil, so be difficult to carry out High-Voltage Experimentation.Compare with the resistance measurement under the high pressure, magnetic resistivity in site measurement difficulty under the high pressure is bigger, at first need magnetic field is incorporated in the high-pressure area, sample can be in the environment of high pressure and magnetic field coexistence, its less important realization quantitative measurment promptly becomes the measurement that realizes resistivity from the measurement to resistance.Just because of the restriction on the experimental technique, make under the high pressure that the magnetic resistivity of material is measured a blank that is still so far on the high pressure technique in the adamas opposed anvils.
Summary of the invention:
The technical problem to be solved in the present invention is the method for measurement of species magnetic resistivity under a kind of new condition of high voltage of design, provide uniform and stable magnetic field and ultra-high voltage environment to sample, and introducing membrane electrode tests, effectively get rid of the experimental error that lead resistance and contact resistance bring, utilized the present invention's magnetoresistance effect of measurement of species under condition of high voltage accurately.
A kind of measuring method of condition of high voltage magnetic resistivity of substance under is measured on the adamas opposed anvils based on the metal electrode 13 of vanderburg method resistivity measurement; Following testing procedure is arranged:
1. device assembles: two diamond anvils 1 to employed adamas opposed anvils carry out surface cleaning processing, be individually fixed on two shaking tables 2, afterwards press 5 is carried out centering, leveling processing, make two bottom surface keeping parallelisms of diamond anvil 1 surface and press 5; Sample is placed on by in the sample cavity 12 that diamond anvil 1 surface and pad 4 cavities constitute up and down;
2. regulate magnetic field: the press 5 that assembles is positioned in the electromagnetic field, two bottom surfaces of press 5 are adjusted to is parallel to head surface, to guarantee that magnetic direction is vertical with direction of current in the sample; And make the head surface up and down that generates an electromagnetic field close, but kiss press 5 not;
3. the in site measurement of magnetic field intensity: gaussmeter probe 3 is placed on the position of close sample cavity 12 between the shaking table 2 up and down; Rotation gaussmeter probe 3 when the numerical value of gaussmeter is maximum, fixes gaussmeter probe 3 and carries out the magnetic field intensity measurement;
4. the measurement of magnetic resistivity: the contact conductor of diamond anvil 1 bottom is electrically connected with the electrode of test macro, measures the variation relation of the resistivity of sample under different pressures with magnetic field.
In the measurement of described magnetic resistivity, guarantee the magnetic head contact that the contact conductor discord generates an electromagnetic field, and make press 5 as far as possible, in order to avoid the accuracy that influence is measured away from magnetic head.
In device assembles, the four-column type press that described press 5 can be the BeCu alloy; Described shaking table 2 is steel materials; Described pad 4 is rhenium metal pads.
In device assembles, described adamas opposed anvils wherein adopts the vanderburg legal system to make electrode 13 on diamond anvil 1, and the metal film of making by physics vapour deposition system is as the material of electrode, and thickness of metal film is below 4 microns.Metal film as electrode 13 need be nonmagnetic or have extremely weak diamagnetic metallic film, as copper, aluminium, titanium, rhenium etc.
For guaranteeing carrying out smoothly of magnetic resistance measurement, the present invention has mainly solved following key factor, has obtained the technique effect of the magnetoresistivity effect of accurate measuring samples under condition of high voltage.
1) creates non magnetic measurement environment.What use in the experimentation is the four-column type press of BeCu alloy, and envelope pressure pad sheet is the rhenium metal pad after the precompressed.BeCu alloy and rhenium sheet are not subjected to the magnetization in magnetic field, and having guaranteed to have this condition of stabilizing magnetic field in the magnetic resistance measuring process.
2) provide uniform magnetic field on the space for sample.Because press 5 and pad 4 are no magnetic material, have only shaking table 2 to be steel material, can be by magnetic field magnetisation; Because the distance between the shaking table 2 is very little up and down, help in very little sample cavity 12 zones, producing bigger uniform magnetic field.
3) influence of elimination lead resistance and contact resistance.Generally speaking, the numeric ratio of magnetoresistance is less, and little by little the introducing of error will cause the gross differences of measurement result.Inevitable error in electrical measurement comes from lead resistance and contact resistance, and the present invention has adopted the vanderburg legal system to make electrode, and this method can effectively be got rid of the influence of lead resistance and contact resistance, guarantees the accuracy that magnetic resistance is measured.
4) used electrode can bear high pressure and be difficult for being cut off.Employed electrode material is not a tinsel among the present invention, but the metal film by the physics vapour deposition system made is as electrode material, and film thickness is below 4 microns.Therefore, under high pressure, electrode is not easy to be cut off, and also is not easy deformation.Guaranteed the accuracy that magnetic resistance is measured.Through experimental verification, the used membrane electrode of the present invention is bearing under the pressure of 105GPa and can also normally using, for measurement of species magnetoresistance effect under the ultra-high pressure condition provides condition.
5) can carry out in site measurement to the magnetic field intensity in the sample cavity.
Description of drawings
Fig. 1 is the diagrammatic cross-section of mounting equipment of the present invention.
Fig. 2 is the synoptic diagram of assembling back diamond anvil among Fig. 1.
Fig. 3 is the up and down Distribution of Magnetic Field figure when diverse location and different magnetic field intensity between the shaking table of the present invention.
The magnetic resistivity of β boron sample was with the variation relation curve in magnetic field when Fig. 4 was the 1.37GPa of embodiment 3.
The resistivity of B sample was with the variation relation curve in magnetic field when Fig. 5 was the 17.65GPa of embodiment 3
Embodiment
The structure and the performance of embodiment 1 accompanying drawings mounting equipment of the present invention
In Fig. 1,1 is two diamond anvils of adamas opposed anvils, and 2 is shaking table, selects steel to make shaking table, and 3 are the gaussmeter probe, and 4 is pad, selects the rhenium metal sheet to make pad, and 5 is press, preferably the four-column type press of BeCu alloy.
Among Fig. 2,4 is pad, and 12 is sample cavity, is made of up and down diamond anvil 1 surface and pad 4 cavities, and 13 is electrode, can be the metal material electrode, and 14 is protective seam, and A, B, C, D are contact conductor.At the adamas opposed anvils surface deposition of a diamond anvil 1 metal electrode 13 of isolating mutually wherein; The distribution of every strip electrode 13 is that anvil face from diamond anvil 1 is to the side; the protective seam 14 that deposition is arranged on the electrode 13; protective seam 14 can be the adamas insulation course; but electrode 13 is exposed in the termination of anvil face; the position of exposed termination is in the sample cavity 12 of adamas opposed anvils; electrode 13 is exposed in the termination of diamond anvil 1 side simultaneously, is connected to contact conductor A, B, C, D on the exposed termination.
Because the centre bit of shaking table 2 is equipped with the bellmouth of a diameter 1mm, therefore, the magnetic field that is obtained between the shaking table 2 is not fully evenly.Be the accuracy that magnetic resistivity is measured, inventor's independent measurement the Distribution of Magnetic Field between the shaking table, as shown in Figure 3.As can be seen, the bellmouth at shaking table 2 centers that is to say that sample is to be in the highly uniform magnetic field, thereby has guaranteed the accuracy that magnetic resistance is measured the almost not influence of even distribution in magnetic field.
The test process that embodiment 2 is concrete
The first step: employed two diamond anvils 1 are carried out surface cleaning processing, after therein one go up the plating layer of metal film, through whirl coating, exposure, photoetching, a series of step of chemical corrosion, finish metal electrode 13 based on the resistance measurement of vanderburg method.At last, (contact conductor A, B, C, D) draws electrode from the bottom of diamond anvil 1 with lead, in order to measuring.
Second step: two diamond anvils 1 are individually fixed in up and down on two shaking tables 2, afterwards to press 5 carry out centering, leveling is handled.
The 3rd step: packaged sample.
The 4th step: press 5 is positioned in the magnetic field, will guarantees magnetic direction vertical with direction of current in the sample (promptly will with entire electrode or diamond anvil Surface Vertical) in this process.Magnetic field is to be produced by the magnetic head of a pair of electromagnet, and it is parallel that two head surfaces remain, and the direction in magnetic field is then perpendicular to two head surfaces.On the other hand, two bottom surfaces of diamond anvil 1 surface and press 5 are parallel.Therefore, be parallel to head surface, just can guarantee that magnetic direction is vertical with direction of current as long as two bottom surfaces of press 5 are adjusted to.In the adjustment process, make as far as possible that up and down head surface is close, with till the kiss press 5 not.
The 5th step: the in site measurement of sample cavity 12 internal magnetic field intensity.The in site measurement of the magnetic field intensity in the sample cavity 12 is an insoluble problem always, and the present invention has well solved this problem.As seen from Figure 3, the magnetic field around the sample cavity 12 in the 10cm scope still can keep even when magnetic field intensity is very high.Therefore, needn't the measuring samples chamber magnetic field in 12, just can obtain the interior magnetic field intensity of sample cavity 12 but measure magnetic field around the diamond anvil 1.Like this, just can carry out in site measurement to the magnetic field in the sample cavity 12 at any one time.
The 6th step: it is vertical all the time with magnetic field to embezzle the probe 3 that guarantees gaussmeter in the magnetic field intensity measuring process, and survey is only real magnetic field intensity like this.At first, the probe 3 of gaussmeter is placed on the position that is suitable for measuring, rotating detector when the numerical value of gaussmeter is maximum, illustrate that probe 3 is vertical with magnetic field gently, and at this moment, fixing pops one's head in 3 just can measure.
The 7th step: contact conductor A, B, C, the D of the bottom of diamond anvil 1 are connected with the test lead electrode of constant current source and high-sensitivity digital milivoltmeter, carry out the magnetic resistivity measurement.To guarantee the contact of lead-in wire discord magnetic head in the measuring process, and make press 5 as far as possible, in order to avoid the accuracy that influence is measured away from magnetic head.
The research of embodiment 3 boron high pressure magnetoresistances
Step according to embodiment 2 is measured β boron sample resistivity and magnetic field intensity respectively under 1.37GPa and 17.65GPa pressure.
The data in Fig. 4 shows when being 1.37GPa β boron sample resistivity and magnetic field and resistivity are with the variation relation in magnetic field.Along with the increase in magnetic field, resistivity rises rapidly, and when magnetic field was increased to 3000Oe, resistivity began to descend fast.
The data of β boron magnetic sample resistivity that Fig. 5 shows when being 17.65GPa and magnetic field intensity and resistivity are with the variation relation of magnetic field intensity.During low magnetic field intensity, the magnetic resistivity variation tendency does not become, but magneto-resistor slowly increases along with the increase in magnetic field under the High-Field.
Test figure line as can be seen from Fig. 4 and Fig. 5, magnetic resistivity is along with the variation in magnetic field obviously is divided into two parts.In low (less than 3000Oe) scope, magnetic resistivity suddenly rises along with the increase of pressure, and magnetic resistivity and magnetic field are the almost relation of symmetry.This trend does not change along with the variation of pressure is significant.After magnetic field was greater than 3000Oe, magneto-resistor with the variation tendency of pressure significant change had taken place: at low pressure conditions following (1.37GPa), magnetic resistivity descends along with the increase in magnetic field; When pressure was increased to 17.65GPa, magneto-resistor slowly increased along with the increase of pressure.
The transmission mechanism that occurs extreme value explanation material inside on the change curve of magneto-resistor with magnetic field changes.1997, people such as Verbanck found bigger positive magnetoresistance effect in non magnetic Cr/Ag/Cr film.And find increase with the Ag layer thickness, the relation in magneto-resistor and magnetic field has departed from classical parabolic relation, when they thought that the mean free path of conduction electron is greater than the thickness of Ag, the main cause that produces magneto-resistor was that the scattering of conduction electron on the Ag interface causes.For β boron, crystal boundary in the charged particle transport under the magnetic field, play a part one important.Under lower magnetic field, owing to being subjected to Lorentz force in magnetic field, ELECTRON OF MOTION changes movement locus, and its effective mean free path is reduced, cause the increase of resistance.Along with the 3000Oe that is increased in magnetic field, saturated phenomenon appears in magneto-resistor.After magnetic field further increases,, descend with the magnetic field increase during high pressure, but speed all significantly slows down because the magnetic resistivity form of expression different along with pressure has increases with magnetic field during low pressure.Showing as normal magnetic resistance during low pressure, is unusual magnetic resistance during high pressure.Under the normal condition, positive magnetoresistance and electronic spin are irrelevant substantially.For polycrystal Beta boron sample, show unusual magnetoresistance under the high pressure and can be summed up as crystal boundary under the high pressure and reform and to have reduced the scattering of crystal boundary charge carrier.
Claims (4)
1. the measuring method of a condition of high voltage magnetic resistivity of substance under is measured on the adamas opposed anvils based on the metal electrode (13) of vanderburg method resistivity measurement; Following testing procedure is arranged:
1. device assembles: two diamond anvils (1) to employed adamas opposed anvils carry out surface cleaning processing, be individually fixed on two shaking tables (2), afterwards press (5) is carried out centering, leveling processing, make two bottom surface keeping parallelisms of diamond anvil (1) surface and press (5); Sample is placed on by in the sample cavity (12) that diamond anvil (1) surface and pad (4) cavity constitute up and down;
2. regulate magnetic field: the press (5) that assembles is positioned in the electromagnetic field, two bottom surfaces of press (5) are adjusted to is parallel to head surface, to guarantee that magnetic direction is vertical with direction of current in the sample; And make the head surface up and down that generates an electromagnetic field close, but kiss press (5) not;
3. the in site measurement of magnetic field intensity: gaussmeter probe (3) is placed on the position of close sample cavity (12) between the shaking table (2) up and down; Rotation gaussmeter probe (3) when the numerical value of gaussmeter is maximum, fixes gaussmeter probe (3) and carries out the magnetic field intensity measurement;
4. the measurement of magnetic resistivity: the contact conductor of diamond anvil (1) bottom is electrically connected with the electrode of test macro, measures the variation relation of the resistivity of sample under different pressures with magnetic field.
2. according to the measuring method of the described condition of high voltage magnetic resistivity of substance under of claim 1, it is characterized in that, in the measurement of described magnetic resistivity, guarantee the magnetic head contact that the contact conductor discord generates an electromagnetic field, and make press away from magnetic head.
3. according to the measuring method of claim 1 or 2 described condition of high voltage magnetic resistivity of substance under, it is characterized in that in device assembles, described press (5) is the four-column type press of BeCu alloy; Described shaking table (2) is a steel material; Described pad (4) is the rhenium metal pad.
4. according to the measuring method of claim 1 or 2 described condition of high voltage magnetic resistivity of substance under, it is characterized in that, in device assembles, described adamas opposed anvils, wherein a diamond anvil (1) is gone up and is adopted the vanderburg legal system to make electrode (13), the metal film of making by physics vapour deposition system is as the material of electrode, and thickness of metal film is below 4 microns, is nonmagnetic or has extremely weak diamagnetic metallic film as the metal film of electrode (13).
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104596835A (en) * | 2015-01-25 | 2015-05-06 | 吉林大学 | Inner-condensing diamond anvil cell pressing machine |
| CN105540558A (en) * | 2016-01-26 | 2016-05-04 | 吉林大学 | Nitrogen polymer and preparation method thereof |
| CN106093129A (en) * | 2016-06-03 | 2016-11-09 | 石家庄铁道大学 | Application VDP method test column soil body resistivity or water content affect collimation method |
| CN107449714A (en) * | 2017-07-25 | 2017-12-08 | 重庆科技学院 | A kind of application method of dynamic magnetic field experimental provision |
| CN107884728A (en) * | 2017-10-20 | 2018-04-06 | 金华职业技术学院 | A kind of method that magnet-optical medium film physical property is measured under the conditions of cryogenic high pressure |
| CN108745204A (en) * | 2018-08-09 | 2018-11-06 | 吉林师范大学 | The polycrystalline diamond anvil and preparation method thereof of optic test can be achieved |
| CN112147414A (en) * | 2020-09-27 | 2020-12-29 | 中国科学院地球化学研究所 | Method for measuring resistivity of metallic iron under ultrahigh pressure |
| CN112147415A (en) * | 2020-09-27 | 2020-12-29 | 中国科学院地球化学研究所 | Method for measuring resistivity of metal iron sheet at high temperature and high pressure |
| CN112415055A (en) * | 2020-10-10 | 2021-02-26 | 牡丹江师范学院 | Comprehensive in-situ electric transport measurement method based on diamond anvil cell |
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| US4776223A (en) * | 1987-02-06 | 1988-10-11 | The United States Of America As Represented By The United States Department Of Energy | Double bevel construction of a diamond anvil |
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| CN104596835B (en) * | 2015-01-25 | 2017-05-10 | 吉林大学 | Inner-condensing diamond anvil cell pressing machine |
| CN104596835A (en) * | 2015-01-25 | 2015-05-06 | 吉林大学 | Inner-condensing diamond anvil cell pressing machine |
| CN105540558A (en) * | 2016-01-26 | 2016-05-04 | 吉林大学 | Nitrogen polymer and preparation method thereof |
| CN106093129A (en) * | 2016-06-03 | 2016-11-09 | 石家庄铁道大学 | Application VDP method test column soil body resistivity or water content affect collimation method |
| CN106093129B (en) * | 2016-06-03 | 2019-03-08 | 石家庄铁道大学 | The influence collimation method of column soil body resistivity or water content is tested using VDP method |
| CN107449714B (en) * | 2017-07-25 | 2023-02-21 | 重庆科技学院 | Application method of dynamic magnetic field experimental device |
| CN107449714A (en) * | 2017-07-25 | 2017-12-08 | 重庆科技学院 | A kind of application method of dynamic magnetic field experimental provision |
| CN107884728A (en) * | 2017-10-20 | 2018-04-06 | 金华职业技术学院 | A kind of method that magnet-optical medium film physical property is measured under the conditions of cryogenic high pressure |
| CN107884728B (en) * | 2017-10-20 | 2024-01-30 | 金华职业技术学院 | Method for measuring physical properties of magneto-optical medium film under low-temperature high-pressure condition |
| CN108745204A (en) * | 2018-08-09 | 2018-11-06 | 吉林师范大学 | The polycrystalline diamond anvil and preparation method thereof of optic test can be achieved |
| CN108745204B (en) * | 2018-08-09 | 2023-10-20 | 吉林师范大学 | Polycrystalline diamond anvil capable of realizing optical test and preparation method thereof |
| CN112147414A (en) * | 2020-09-27 | 2020-12-29 | 中国科学院地球化学研究所 | Method for measuring resistivity of metallic iron under ultrahigh pressure |
| CN112147414B (en) * | 2020-09-27 | 2021-10-01 | 中国科学院地球化学研究所 | Method for measuring resistivity of metallic iron under ultrahigh pressure |
| CN112147415B (en) * | 2020-09-27 | 2021-09-24 | 中国科学院地球化学研究所 | Method for measuring resistivity of metal iron sheet at high temperature and high pressure |
| CN112147415A (en) * | 2020-09-27 | 2020-12-29 | 中国科学院地球化学研究所 | Method for measuring resistivity of metal iron sheet at high temperature and high pressure |
| CN112415055B (en) * | 2020-10-10 | 2023-06-13 | 牡丹江师范学院 | Comprehensive in-situ electric transport measurement method based on diamond anvil cell |
| CN112415055A (en) * | 2020-10-10 | 2021-02-26 | 牡丹江师范学院 | Comprehensive in-situ electric transport measurement method based on diamond anvil cell |
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Application publication date: 20101201 |