CN105510194A - Measurement method of diameter-to-thickness ratio of permanent magnetic ferrite powder - Google Patents
Measurement method of diameter-to-thickness ratio of permanent magnetic ferrite powder Download PDFInfo
- Publication number
- CN105510194A CN105510194A CN201510863855.1A CN201510863855A CN105510194A CN 105510194 A CN105510194 A CN 105510194A CN 201510863855 A CN201510863855 A CN 201510863855A CN 105510194 A CN105510194 A CN 105510194A
- Authority
- CN
- China
- Prior art keywords
- permanent
- thickness ratio
- radius
- ferrite powder
- permanent magnetic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 110
- 239000000843 powder Substances 0.000 title claims abstract description 55
- 238000000691 measurement method Methods 0.000 title abstract 5
- 239000002245 particle Substances 0.000 claims abstract description 85
- 238000000034 method Methods 0.000 claims abstract description 59
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000758 substrate Substances 0.000 claims abstract description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000005259 measurement Methods 0.000 claims abstract description 7
- 238000012360 testing method Methods 0.000 claims description 27
- 210000002966 serum Anatomy 0.000 claims description 22
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 239000000523 sample Substances 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- KPLQYGBQNPPQGA-UHFFFAOYSA-N cobalt samarium Chemical compound [Co].[Sm] KPLQYGBQNPPQGA-UHFFFAOYSA-N 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 239000010445 mica Substances 0.000 claims description 3
- 229910052618 mica group Inorganic materials 0.000 claims description 3
- 229910001172 neodymium magnet Inorganic materials 0.000 claims description 3
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 7
- 239000002002 slurry Substances 0.000 abstract description 2
- 235000019441 ethanol Nutrition 0.000 abstract 1
- 239000011268 mixed slurry Substances 0.000 abstract 1
- 238000001132 ultrasonic dispersion Methods 0.000 abstract 1
- BGPVFRJUHWVFKM-UHFFFAOYSA-N N1=C2C=CC=CC2=[N+]([O-])C1(CC1)CCC21N=C1C=CC=CC1=[N+]2[O-] Chemical compound N1=C2C=CC=CC2=[N+]([O-])C1(CC1)CCC21N=C1C=CC=CC1=[N+]2[O-] BGPVFRJUHWVFKM-UHFFFAOYSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 239000008187 granular material Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 241000446313 Lamella Species 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000000007 visual effect Effects 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- AJCDFVKYMIUXCR-UHFFFAOYSA-N oxobarium;oxo(oxoferriooxy)iron Chemical compound [Ba]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O AJCDFVKYMIUXCR-UHFFFAOYSA-N 0.000 description 3
- 229910052712 strontium Inorganic materials 0.000 description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical group [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000276425 Xiphophorus maculatus Species 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Magnetic Means (AREA)
Abstract
The invention relates to a measurement method of the diameter-to-thickness ratio of permanent magnetic ferrite powder. The method at least comprises steps as follows: a to-be-tested sample and ethyl alcohol or acetone are mixed for preparation of slurry, mixed slurry is formed after ultrasonic dispersion and dropped on a substrate located in a magnetic field for orientation, an image of the to-be-tested sample after orientation is cut by a scanning electron microscope, and the diameter-to-thickness ratio of a single particle of the permanent magnetic ferrite powder and/or the diameter-to-thickness ratio of the permanent magnetic ferrite powder are/is calculated by measuring the radial length and the thickness of the single particle of the permanent magnetic ferrite powder in the image. The measurement method is applicable to measurement of the diameter-to-thickness ratio of the permanent magnetic ferrite powder having the smaller size, with the adoption of the measurement method, diameter-to-thickness ratio data of single particles can be obtained, and average data of the to-be-tested sample can also be obtained; the measurement method further has the advantages that the sample is prepared conveniently and quickly, particle orientation is accurate, particle boundaries are clear, data statistics is convenient and the like.
Description
Technical field
The present invention relates to material particle size field tests, particularly relate to a kind of measuring method of granule permanent magnetic ferrite powder radius-thickness ratio.
Background technology
Permanent-magnet ferrite, as a kind of basic function material of electronics industry, has penetrated into the every field of human being's production, life.Obtain a wide range of applications in automobile, motorcycle, televisor, sound equipment, computing machine, communication terminal machine, Medical Instruments etc., it is also an importance of energy development.No matter from the angle of resource, or from the angle of the energy and application, the prospect of permanent-magnet ferrite development is all very wide, and its demand also grows with each passing day.
Most widely used in permanent-magnet ferrite is strontium ferrite and barium ferrite.Strontium ferrite and barium ferrite all belong to hexagonal system structure, and powder particle presents hexagonal plate.Permanent-magnet ferrite also presents magnetocrystalline anisotropy, is easy to magnetize and reaches capacity in the crystalline axis direction perpendicular to hexaplanar, and other direction is then difficult to reach magnetic saturation.The sheet degree of permanent magnetic ferrite powder particle has considerable influence to aspects such as its magnetic property, filling rate and processing characteristics, therefore seems particularly important to the measurement of the powder sheet degree of permanent-magnet ferrite.Wherein, the radius-thickness ratio of permanent-magnet ferrite is the characterizing method of the most datumization of its sheet degree, most statistical significance.
Chinese patent (publication No. is CN104359803A) discloses a kind of flaky powder radius-thickness ratio method of testing based on scanning electron microscope.Powder to be measured and deionized water or alcohols solvent also fully disperse according to finite concentration mixed pulp by this patent; Slurry drops drying in substrate is completed natural air drying orientation; Again orienting piece is placed in liquid nitrogen and carries out freezing brittle failure; Again the orienting piece of brittle failure is placed in vacuum metal spraying; Finally be placed on sample platform of scanning electronic microscope by the orienting piece after metal spraying, observation front is to obtain lamella particle surface information, and measuring frequency section to obtain lamella particle end face information, thus calculates the radius-thickness ratio of flaky powder according to surface information and end face information.Although the method for testing that this patent provides effectively can obtain the thickness of a large amount of platy shaped particle lamella, diameter and more surface, end face shape information.But, at least also there are following two defects in the method for testing that this patent provides: (1) utilizes the method for nature orientation to be suitable for the larger powder of radius-thickness ratio, its under the influence of gravity general with tiling but not erect state be oriented in substrate, for the powder that radius-thickness ratio is less, naturally directed method can not ensure directed state; (2) mode of cryogenic freezing brittle failure is more suitable for large-size particle, for more short grained powder, is difficult to the effect reaching brittle failure.
Chinese patent (notification number is CN103196802B) discloses a kind of measuring method of filler sheet layer material radius-thickness ratio.The measuring method that this patent provides is: washed, put into conductance liquid by sample, the potential of hydrogen of adjustment conductance liquid, by physics and ultrasonic power, sample is dispersed in conductance liquid, electric-resistivity method is utilized microporous pipe to be placed in conductance liquid, each placement electrode in conductance liquid inside and outside microporous pipe, and add predetermined voltage at the two ends of electrode; The lamella radius-thickness ratio obtaining sample is calculated according to the voltage pulse signal between electrode.Although the measuring method precision that this patent provides is high, general applicability is strong, but, what the measuring method provided by this patent was calculated is overall mean values, the data of individual particle cannot be reflected, and the measuring method that this patent provides is without statistical data, cannot reflect the composition of radius-thickness ratio data.
Chinese patent (publication No. is CN103105149A) discloses the characterizing method of a kind of shape powder radius-thickness ratio.The characterizing method that this patent provides is: resin dissolves is obtained resin solution in organic solvent, and is mixed with resin solution by sheet shape powder, after solvent volatilization, by coated good sheet shape powder dispersion; Coated good sheet shape powder is carried out pressing machinery orientation by hot pressing press, and by the device suppressed according to the solidification temperature of resin be cured set time; By bonding for the device stack of solidification, cut off the bonding device of lamination from perpendicular to pressing direction, and fracture is placed in the polishing of metallographic sample preparation machine and prepares metallographic sample; By length and the thickness of each metallographic sample in optical microscope or scanning electron microscopic observation visual field, the ratio of length and thickness is the length-diameter ratio of sheet shape powder, and the mean value of the length-diameter ratio of all shape powder in visual field is for characterizing the length-diameter ratio of sheet shape powder.The characterizing method that this patent provides can make sheet shape powder observe in very wide visual field at the thickness of two-dimensional directional and diameter, and then is characterized.But, also there is following defect in the characterizing method that this patent provides: (1) is difficult to when cutting open through smooth fracture for the powder that size is less, and easily occur resin enwrapped granule, make granule boundary fuzzy, be unfavorable for situation about measuring, adopt the characterizing method that this patent provides, particle is less, because the error measuring the radius-thickness ratio brought is larger; (2) Sample Preparation Procedure of characterizing method that provides of this patent is comparatively loaded down with trivial details, needs with mixed with resin and rolling is cut open again, and the sample size of needs is also larger.
Therefore, a kind of orientation of the ferrite powder particles for reduced size is provided and the method for observing pattern and its radius-thickness ratio of statistical computation becomes problem demanding prompt solution.
Summary of the invention
For the deficiency of prior art, the invention provides a kind of measuring method of permanent magnetic ferrite powder radius-thickness ratio, described method at least comprises the steps: testing sample and ethanol or acetone mixed pulp and form mixed serum after ultrasound wave disperses, described mixed serum is dropped in the substrate be in magnetic field and carry out orientation, described testing sample after completing orientation is by scanning electron microscope cut-away view picture, and calculate the radius-thickness ratio of described single permanent-magnet ferrite particle and/or calculate the radius-thickness ratio of described permanent magnetic ferrite powder by the radical length of permanent-magnet ferrite particle single in measurement image and thickness.
According to a preferred implementation, the radical length of described single permanent-magnet ferrite particle is 20 μm and following.Preferably, the radical length of described single permanent-magnet ferrite particle is 10 μm and following.
According to a preferred implementation, the radius-thickness ratio of described permanent magnetic ferrite powder calculates in the following way: choose radical length and thickness that 30 ~ 70 sharply marginated permanent-magnet ferrite particles also measure described 30 ~ 70 sharply marginated permanent-magnet ferrite particles respectively, namely the average aspect ratio calculating described 30 ~ 70 sharply marginated permanent-magnet ferrite particles obtains the radius-thickness ratio of described permanent magnetic ferrite powder.Preferably, the radical length of permanent-magnet ferrite particle and thickness utilize the test function of specialized image analysis software to carry out measuring.More preferably, specialized image analysis software is SISC-IAS.
According to a preferred implementation, described mixed serum is made as follows: put into ultrasonic cleaning instrument after the ratio being 1: 1 by weight by described testing sample and ethanol or acetone mixes and disperse 10 ~ 20min namely to obtain described mixed serum.Preferably, putting into ultrasonic cleaning instrument after the ratio being 1: 1 by weight by described testing sample and acetone mixes disperses 20min namely to obtain described mixed serum.
According to a preferred implementation, the solvent mixed with described testing sample is not limited to ethanol or acetone, also can be to have better volatile methyl alcohol, isopropyl alcohol, ether, chloroform equal solvent.
According to a preferred implementation, dispersing mode when preparing described mixed serum is not limited to ultrasonic disperse, also can be the mode of mechanical raking dispersion.
According to a preferred implementation, described magnetic field is formed in the following way: place ferrite permanent magnet, samarium cobalt permanent magnet body, Nd-Fe-B permanent magnet or electromagnet in described substrate both sides to form described magnetic field simultaneously.Preferably, the magnet of described substrate both sides is placed by identical direction.
According to a preferred implementation, described orientation process completes in the following way: draw described mixed serum with dropper and described mixed serum is dripped 1 ~ 2 on the substrate, the permanent-magnet ferrite particle dropped in described suprabasil described mixed serum rotates the arrangement of Formation rule under described magnetic fields, after ethanol or acetone volatilization completely, remove described magnetic field and namely complete orientation process.
According to a preferred implementation, described testing sample orientation completed is placed on scanning electron microscope platform, chooses sharply marginated upper strata permanent-magnet ferrite particle and carries out observation and cut-away view picture.
According to a preferred implementation, by described scanning electron microscope cut-away view as time select enlargement factor be 3000 times and more than.
According to a preferred implementation, the instrument of observation is not limited to scanning electron microscope, also can be that optical microscope etc. has the equipment amplifying observing function.
According to a preferred implementation, described substrate is silicon chip, electro-conductive glass or mica sheet.Preferably, described substrate is silicon chip.
According to a preferred implementation, described substrate processes before use as follows: described substrate be immersed in take out after carrying out ultrasonic cleaning in distilled water, ethanol or acetone soln and dry, as subsequent use.
The measuring method of permanent magnetic ferrite powder radius-thickness ratio provided by the invention at least has following advantage:
Measuring method provided by the invention is suitable for orientation that radical length is 20 μm and following small size permanent magnetic ferrite powder particle and morphology observation thereof, by measuring method of the present invention, not only can obtain the radius-thickness ratio data of individual particle, and the average data of permanent magnetic ferrite powder to be measured can be obtained; Measuring method of the present invention also has the advantages such as convenient and swift, the required sample size of sample preparation is few, orientation of particles is accurate, granule boundary is clear, data statistics is convenient.
Accompanying drawing explanation
Fig. 1 is the hexagonal plate structural representation of permanent-magnet ferrite particle of the present invention;
Fig. 2 is the outboard profile of the permanent-magnet ferrite particle under scanning electron microscope;
Fig. 3 is the orientation process schematic diagram of permanent-magnet ferrite particle; With
Fig. 4 is the scanning electron microscope (SEM) photograph of the permanent-magnet ferrite particle after orientation completes.
Reference numerals list
1: the thickness 2 of permanent-magnet ferrite particle: the radical length of permanent-magnet ferrite particle
3: dropper 4: magnet
5: base 6: substrate
Embodiment
Be described in detail below in conjunction with accompanying drawing.
The mentality of designing of the measuring method of a kind of permanent magnetic ferrite powder radius-thickness ratio provided by the invention is as follows: in permanent-magnet ferrite, most widely used strontium ferrite and barium ferrite are hexagonal plate structure, as shown in Figure 1.Wherein, the direction of arrow is the direction of permanent-magnet ferrite easy magnetization, and all the other directions are then difficult to reach magnetic saturation.By orientation process, the arrangement of the permanent-magnet ferrite particle Formation rule in testing sample can be made.Observe under again the permanent-magnet ferrite particle that Formation rule arranges being placed in scanning electron microscope, permanent-magnet ferrite particle side structure clearly can be seen.The side structure of the permanent-magnet ferrite particle that Fig. 2 observes under showing scanning electron microscope.Wherein, what horizontal direction 1 represented is the thickness of permanent-magnet ferrite particle.What vertical direction 2 represented is the radical length of permanent-magnet ferrite particle.The radical length of permanent-magnet ferrite particle is also referred to as the path length of permanent-magnet ferrite particle.To the permanent-magnet ferrite particle under scanning electron microscope, utilize the test function of image analysis software can measure the radical length of permanent-magnet ferrite particle and thickness, then utilize radical length value namely to obtain the radius-thickness ratio of permanent-magnet ferrite particle divided by one-tenth-value thickness 1/10.The measuring method of permanent magnetic ferrite powder radius-thickness ratio provided by the invention at least comprises the steps:
S1: the preparation of substrate.The substrate that the present invention uses is silicon chip, electro-conductive glass or mica sheet.Preferably, the substrate that the present invention uses is silicon chip.Substrate before use, needs to prepare in the following manner: substrate is immersed in taking-up after carrying out ultrasonic cleaning in distilled water, ethanol or acetone soln and dries, as subsequent use.
S2: producing of mixed serum.The raw material that the present invention uses is permanent magnet ferrite powder, and the radical length of its particle is 20 μm and following.Preferably, the ferritic radical length of permanent magnet that the present invention uses is 10 μm and following.Mixed serum is made as follows: the ratio being 1: 1 by weight by testing sample and ethanol or acetone mixes, and mixed solution is put into ultrasonic cleaning instrument dispersion 10 ~ 20min and namely obtains mixed serum.More preferably, putting into ultrasonic cleaning instrument after the ratio being 1: 1 by weight by testing sample and acetone mixes disperses 20min namely to obtain mixed serum.It is very fast that solvent is preferably the evaporation rate of acetone mainly due to acetone.
S3: orientation process.Fig. 3 shows the orientation process schematic diagram of permanent-magnet ferrite particle.As shown in Figure 3, magnet 4 and substrate 6 are positioned on base 5.Substrate 6 is in magnetic field.Magnetic field is formed in the following way: place magnet 4 in the both sides of substrate 6 to form magnetic field simultaneously.Preferably, the south poles direction of the magnet 4 of substrate 6 both sides placement is consistent.Refer again to Fig. 3, the black end of magnet 4 is the arctic of magnet, and the white end of magnet 4 is the South Pole of magnet.Preferably, magnet 4 is one or both in ferrite permanent magnet, samarium cobalt permanent magnet body, Nd-Fe-B permanent magnet or electromagnet.Mixed serum in substrate 6 rotates the arrangement of Formation rule under magnetic fields, and after ethanol or acetone volatilization completely, permanent-magnet ferrite particle not easily rotates owing to not having solvent, removes magnetic field and namely completes orientation process.Method for alignment orientation provided by the invention is accurate, and granule boundary is clear, is convenient to the measurement of permanent-magnet ferrite particle radical length and thickness.
S4: the measurement of radical length and thickness.The substrate being loaded with the testing sample that orientation completes is placed on scanning electron microscope platform, chooses sharply marginated upper strata permanent-magnet ferrite particle and carry out observation and cut-away view picture.Fig. 4 show orientation complete after the scanning electron microscope (SEM) photograph of permanent-magnet ferrite particle.As shown in Figure 4, the radical length of permanent-magnet ferrite particle single in image and thickness are measured and recorded data.Preferably, first get rid of the particle being difficult to see clearly border being in lower floor be blocked in the visual field during measurement, the sharply marginated particle in upper strata is added up one by one.Preferably, by described scanning electron microscope cut-away view as time select enlargement factor be 3000 times and more than.Preferably, the radical length of permanent-magnet ferrite particle and thickness utilize the test function of specialized image analysis software to carry out measuring.More preferably, specialized image analysis software is SISC-IAS.
S5: the calculating of radius-thickness ratio.The calculating of radius-thickness ratio comprises the calculating of single permanent-magnet ferrite radius-thickness ratio and the calculating of permanent magnetic ferrite powder radius-thickness ratio.The radius-thickness ratio of single permanent-magnet ferrite calculates as follows: utilize the radical length value of single the permanent-magnet ferrite recorded namely to obtain its radius-thickness ratio divided by one-tenth-value thickness 1/10.The radius-thickness ratio of permanent magnetic ferrite powder calculates as follows: radical length value and the one-tenth-value thickness 1/10 of adding up 30 ~ 70 sharply marginated permanent-magnet ferrite particles, namely the average aspect ratio calculating these 30 ~ 70 sharply marginated permanent-magnet ferrite particles obtains the radius-thickness ratio of permanent magnetic ferrite powder.
According to a preferred implementation, the calculating of testing sample average aspect ratio, the permanent-magnet ferrite numbers of particles chosen is inaccurate to the reflection of average level very little, The more the better in principle, but consider and too much can increase corresponding workload, generally choose 30 ~ 70 sharply marginated permanent-magnet ferrite particles and carry out statistical computation.
According to a preferred implementation, by scanning electron microscope cut-away view as time can select larger enlargement factor.Preferably, the enlargement factor of selection be 3000 times and more than.By selecting larger enlargement factor, can reduce to measure the error brought.
The measuring method of permanent magnetic ferrite powder radius-thickness ratio provided by the invention, not only can obtain the radius-thickness ratio data of single permanent-magnet ferrite particle, and can obtain the average data of testing sample.Mostly measuring method of the prior art is the mean value measuring testing sample, seldom can measure the radius-thickness ratio of individual particle.On the other hand, measuring method General Requirements measuring object of the prior art is of a size of hundreds of micron or even several millimeters, and radical length size is no more than to the small sized particles of 20 μm, is difficult to use method of the prior art to carry out sample preparation orientation.Such as, in prior art, candidate particles is carried out to the measure of brittle failure, when particle size is larger, the moment that particle is subject to is larger, easily to rupture, and measuring object of the present invention is the particle that radical length size is no more than 20 μm, the radical length size of even most of particle is no more than 10 μm, the difficulty that fracture occurs undersized particle like this increases greatly, needs extra increase measure could realize short grained brittle failure toward contact.Again such as, adopt the measure cut open by particle in prior art, be metallic particles due to what cut open in prior art, hardness is relatively little, plasticity is better, the difficulty cut open is little, and the permanent-magnet ferrite in the present invention is ceramic-like material, and hardness is high, plasticity is poor, belong to hard crisp type, use the measure difficulty cut open to increase, and cut open to as if undersized particle, further increase its difficulty.
Utilize the measuring method of permanent magnetic ferrite powder radius-thickness ratio of the present invention, through the preparation of substrate, mixed serum produce with orientation process after, the substrate being loaded with the testing sample that orientation completes is placed on scanning electron microscope platform, choose sharply marginated 50 upper strata permanent-magnet ferrite particles and carry out observation and cut-away view picture, use the test function of specialized image analysis software SISC-IAS to measure the radical length of 50 permanent-magnet ferrite particles and thickness, and record corresponding radical length value and one-tenth-value thickness 1/10.The data obtained is as shown in table 1 below.
Table 1 survey radical length and the thickness of 50 permanent-magnet ferrite particles
The radical length maximal value of 50 permanent-magnet ferrite particles getting is 12.2 μm, and minimum value is 2.2 μm.The maximum thickness of 50 permanent-magnet ferrite particles getting is 3.9 μm, and minimum value is 0.8 μm.The radius-thickness ratio of each permanent-magnet ferrite particle can be calculated divided by thickness by its radical length.Wherein, radius-thickness ratio has 4, accounting 8% below 2.00.Radius-thickness ratio has 26, accounting 52% between 2.00 ~ 2.99.Radius-thickness ratio has 14, accounting 28% between 3.00 ~ 3.99.Radius-thickness ratio is 4.00 and above have 6, accounting 12%.By calculating the average aspect ratio of 50 permanent-magnet ferrite particles, the average aspect ratio of testing sample can be obtained.By calculating, the average aspect ratio of the present embodiment testing sample is 3.52.
It should be noted that; above-mentioned specific embodiment is exemplary; those skilled in the art can find out various solution under the inspiration of the disclosure of invention, and these solutions also all belong to open scope of the present invention and fall within protection scope of the present invention.It will be understood by those skilled in the art that instructions of the present invention and accompanying drawing thereof are illustrative and not form limitations on claims.Protection scope of the present invention is by claim and equivalents thereof.
Claims (10)
1. a measuring method for permanent magnetic ferrite powder radius-thickness ratio, is characterized in that, described method at least comprises the steps:
Testing sample and ethanol or acetone mixed pulp are formed mixed serum after ultrasound wave disperses, described mixed serum is dropped in the substrate be in magnetic field and carry out orientation, described testing sample after completing orientation by scanning electron microscope cut-away view picture, and is calculated the radius-thickness ratio of described single permanent-magnet ferrite particle and/or is calculated the radius-thickness ratio of described permanent magnetic ferrite powder by the radical length of permanent-magnet ferrite particle single in measurement image and thickness.
2. the measuring method of permanent magnetic ferrite powder radius-thickness ratio as claimed in claim 1, is characterized in that, the radical length of described single permanent-magnet ferrite particle is 20 μm and following.
3. the measuring method of permanent magnetic ferrite powder radius-thickness ratio as claimed in claim 1 or 2, it is characterized in that, the radius-thickness ratio of described permanent magnetic ferrite powder calculates in the following way:
Choose radical length and thickness that 30 ~ 70 sharply marginated permanent-magnet ferrite particles also measure described 30 ~ 70 sharply marginated permanent-magnet ferrite particles respectively, namely the average aspect ratio calculating described 30 ~ 70 sharply marginated permanent-magnet ferrite particles obtains the radius-thickness ratio of described permanent magnetic ferrite powder.
4. the measuring method of permanent magnetic ferrite powder radius-thickness ratio as claimed in claim 1 or 2, it is characterized in that, described mixed serum is made as follows:
Putting into ultrasonic cleaning instrument after the ratio being 1: 1 by weight by described testing sample and ethanol or acetone mixes disperses 10 ~ 20min namely to obtain described mixed serum.
5. the measuring method of permanent magnetic ferrite powder radius-thickness ratio as claimed in claim 1 or 2, it is characterized in that, described magnetic field is formed in the following way:
Place ferrite permanent magnet, samarium cobalt permanent magnet body, Nd-Fe-B permanent magnet or electromagnet to form described magnetic field in described substrate both sides simultaneously.
6. the measuring method of permanent magnetic ferrite powder radius-thickness ratio as claimed in claim 5, it is characterized in that, described orientation process completes in the following way:
Draw described mixed serum with dropper and described mixed serum is dripped 1 ~ 2 on the substrate, the permanent-magnet ferrite particle dropped in described suprabasil described mixed serum rotates the arrangement of Formation rule under described magnetic fields, after ethanol or acetone volatilization completely, remove described magnetic field and namely complete orientation process.
7. the measuring method of permanent magnetic ferrite powder radius-thickness ratio as claimed in claim 1 or 2, it is characterized in that, described testing sample orientation completed is placed on scanning electron microscope platform, chooses sharply marginated upper strata permanent-magnet ferrite particle and carries out observation and cut-away view picture.
8. the measuring method of permanent magnetic ferrite powder radius-thickness ratio as claimed in claim 7, is characterized in that, by described scanning electron microscope cut-away view as time the enlargement factor selected be 3000 times and more than.
9. the measuring method of permanent magnetic ferrite powder radius-thickness ratio as claimed in claim 1 or 2, it is characterized in that, described substrate is silicon chip, electro-conductive glass or mica sheet.
10. the measuring method of permanent magnetic ferrite powder radius-thickness ratio as claimed in claim 9, it is characterized in that, described substrate processes before use as follows:
Described substrate is immersed in take out after carrying out ultrasonic cleaning in distilled water, ethanol or acetone soln and dries, as subsequent use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510863855.1A CN105510194A (en) | 2015-12-01 | 2015-12-01 | Measurement method of diameter-to-thickness ratio of permanent magnetic ferrite powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510863855.1A CN105510194A (en) | 2015-12-01 | 2015-12-01 | Measurement method of diameter-to-thickness ratio of permanent magnetic ferrite powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105510194A true CN105510194A (en) | 2016-04-20 |
Family
ID=55718335
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510863855.1A Pending CN105510194A (en) | 2015-12-01 | 2015-12-01 | Measurement method of diameter-to-thickness ratio of permanent magnetic ferrite powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105510194A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108417331A (en) * | 2018-05-15 | 2018-08-17 | 上海理工大学 | A kind of preparation method of the single gold-coating magnetic nano particle of small scale |
| CN108426905A (en) * | 2018-02-02 | 2018-08-21 | 东华大学 | A kind of simple and easy method of nanometer powder dispersion electron microscopyc sample preparation |
| CN110186738A (en) * | 2018-02-22 | 2019-08-30 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of flakelike powder section sample |
| CN114235649A (en) * | 2021-12-20 | 2022-03-25 | 珠海真理光学仪器有限公司 | Particle diameter-thickness ratio measuring method and device based on laser particle sizer and storage medium |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010066056A (en) * | 2008-09-09 | 2010-03-25 | Dic Corp | Method and program for evaluating particle size distribution, and apparatus for evaluating particle size distribution |
| CN102240805A (en) * | 2011-07-27 | 2011-11-16 | 湖南航天工业总公司 | Method for preparing anisotropic bonded rare-earth permanent magnet |
| CN102700148A (en) * | 2012-05-15 | 2012-10-03 | 东华大学 | Orientation method of carbon nanotubes in molding process of composite materials |
| CN102956339A (en) * | 2012-10-31 | 2013-03-06 | 中国计量学院 | Unidirectional transparent composite magnet and preparation method |
| CN103105149A (en) * | 2013-01-22 | 2013-05-15 | 北矿磁材科技股份有限公司 | Characterization method of flake-shaped powder radius-thickness ratio |
| CN104359803A (en) * | 2014-11-14 | 2015-02-18 | 河南理工大学 | Sheet-shaped powder radius-thickness ratio testing method based on scanning electron microscope |
-
2015
- 2015-12-01 CN CN201510863855.1A patent/CN105510194A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010066056A (en) * | 2008-09-09 | 2010-03-25 | Dic Corp | Method and program for evaluating particle size distribution, and apparatus for evaluating particle size distribution |
| CN102240805A (en) * | 2011-07-27 | 2011-11-16 | 湖南航天工业总公司 | Method for preparing anisotropic bonded rare-earth permanent magnet |
| CN102700148A (en) * | 2012-05-15 | 2012-10-03 | 东华大学 | Orientation method of carbon nanotubes in molding process of composite materials |
| CN102956339A (en) * | 2012-10-31 | 2013-03-06 | 中国计量学院 | Unidirectional transparent composite magnet and preparation method |
| CN103105149A (en) * | 2013-01-22 | 2013-05-15 | 北矿磁材科技股份有限公司 | Characterization method of flake-shaped powder radius-thickness ratio |
| CN104359803A (en) * | 2014-11-14 | 2015-02-18 | 河南理工大学 | Sheet-shaped powder radius-thickness ratio testing method based on scanning electron microscope |
Non-Patent Citations (1)
| Title |
|---|
| 徐健等: "钡铁氧体磁粉颗粒尺度的扫描电镜测量", 《清华大学学报（自然科学版）》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108426905A (en) * | 2018-02-02 | 2018-08-21 | 东华大学 | A kind of simple and easy method of nanometer powder dispersion electron microscopyc sample preparation |
| CN110186738A (en) * | 2018-02-22 | 2019-08-30 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of flakelike powder section sample |
| CN110186738B (en) * | 2018-02-22 | 2021-11-02 | 宁波新材料测试评价中心有限公司 | Preparation method of flaky powder section sample |
| CN108417331A (en) * | 2018-05-15 | 2018-08-17 | 上海理工大学 | A kind of preparation method of the single gold-coating magnetic nano particle of small scale |
| CN114235649A (en) * | 2021-12-20 | 2022-03-25 | 珠海真理光学仪器有限公司 | Particle diameter-thickness ratio measuring method and device based on laser particle sizer and storage medium |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105510194A (en) | Measurement method of diameter-to-thickness ratio of permanent magnetic ferrite powder | |
| Gault et al. | Influence of surface migration on the spatial resolution of pulsed laser atom probe tomography | |
| Yang et al. | Experimental and theoretical evidence for temperature driving an electric-magnetic complementary effect in magnetic microwave absorbing materials | |
| CN108775979A (en) | A kind of high sensitivity pliable pressure sensor and preparation method thereof | |
| Antonets et al. | Nanostructure and conductivity of thin metal films | |
| CN109759034A (en) | A kind of selective fixing means, adsorbed film and the application of trivalent antimony | |
| Zhang et al. | In situ ultrasound acoustic measurement of the lithium-ion battery electrode drying process | |
| CN102735599B (en) | The method measuring cell structure distribution of pores | |
| CN107727886A (en) | A kind of inversion type high speed Electrochemical Atomic Force Microscopy | |
| JP2014149272A (en) | Producing method of thin sample, and observation method of sample | |
| CN108061697B (en) | Method for calculating three-dimensional porosity of soil body | |
| CN107869978A (en) | A kind of method for measuring thickness of electrochemical deposition nano thin-film | |
| CN104808159A (en) | Valid linewidth frequency sweep measurement system and measurement method | |
| CN102435628B (en) | Characterization method for structural morphology of porous electrode material | |
| CN102620642A (en) | Detection method of metal nanometer film thickness | |
| CN103871917A (en) | Method for preparing semiconductor failure analysis sample | |
| Legerstee et al. | Scanning probe microscopy facility for operando study of redox processes on lithium ion battery electrodes | |
| CN114275730B (en) | Magnetic vibrator coupling resonance type micro-nano weighing device and preparation method thereof | |
| CN103884551A (en) | Microscopy characterization and evaluation method of homogeneity of carbon fibers | |
| Daub et al. | Ni nanowires electrodeposited in single ion track templates | |
| CN106093129B (en) | The influence collimation method of column soil body resistivity or water content is tested using VDP method | |
| CN104318096B (en) | A kind of extracting method for granular material intrinsic electromagnetic parameter | |
| Zhang et al. | Multi‐Scale Characterization Techniques for Polymer‐Based Solid‐State Lithium Batteries | |
| CN209495986U (en) | Transmission electron microscope original position electrical testing chip for focused ion beam sample preparation technique | |
| CN112098446B (en) | Characterization method for radius-thickness ratio of flaky powder material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160420 |
|
| RJ01 | Rejection of invention patent application after publication |