CN102735509A - Preparation method of transmission electron microscope observation sample of magnetic liquid in magnetic field - Google Patents
Preparation method of transmission electron microscope observation sample of magnetic liquid in magnetic field Download PDFInfo
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- CN102735509A CN102735509A CN2012102047094A CN201210204709A CN102735509A CN 102735509 A CN102735509 A CN 102735509A CN 2012102047094 A CN2012102047094 A CN 2012102047094A CN 201210204709 A CN201210204709 A CN 201210204709A CN 102735509 A CN102735509 A CN 102735509A
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Abstract
The invention relates to a preparation method of a transmission electron microscope observation sample of a magnetic liquid in a magnetic field. According to the invention, a certain amount of the magnetic liquid is dispersed in a solvent, such that a mixed liquid is formed; the mixed liquid is subjected to ultrasonic oscillation for approximately 15min, such that the magnetic liquid is uniformly dispersed and is suspended in the solvent, and a transparent dispersion liquid is formed; the dispersion liquid is placed in a transverse magnetic field and a longitudinal magnetic field; according to the testing requirements of the transverse magnetic field and the longitudinal magnetic field, a copper screen position is determined with the assistance of coordinate lines; the copper screen is immersed in the dispersion liquid, and is stood for 1min; the copper screen is drawn back, and is dried on a sealing membrane. Because of the high adsorption capacity of the magnetic particles, a single-layer magnetic particle chain structure is picked up by the copper screen, such that the transmission electron microscope observation sample of the magnetic liquid in the transverse magnetic field or the longitudinal magnetic field is prepared. The sample is delivered to a transmission electron microscope observation room, and the distribution state and arrangement condition of the magnetic particles in the transverse magnetic field or the longitudinal magnetic field can be observed.
Description
Technical field
The invention belongs to electron microscope technology of preparing and material analysis field, the preparation method of the transmission electron microscope specimen of magnetic liquid in a kind of magnetic field is provided, be applicable to the various magnetic liquids of magnetic-particle diameter about 10nm in the observation magnetic field.
Background technology
Magnetic liquid is a kind of magnetic material of ultra paramagnetic, and the single domain magnetic-particle that surfactant is coated about diameter 10nm is dispersed in a kind of solid-liquid two phase colloidal solution that form in the carrier fluid.Magnetic liquid is different from traditional magnetic material, has both had the magnetic of solid, has the flowability of liquid again, often shows unique physicochemical characteristics, has a wide range of applications in ore dressing, sealing and field such as lubricated.It is documented 1 cm
3Magnetic liquid in comprise 10
18Magnetic-particle, the distribution of magnetic-particle plays a part crucially in the magnetic field to the application of magnetic liquid, understands therefore that the distribution situation of magnetic-particle is vital in the magnetic field.
Transmission electron microscope (Transmission electron microscopy; Write a Chinese character in simplified form TEM) be the important method of research nano material micromechanism; But because transmission electron microscope is the high vacuum electronic optical instrument; And magnetic liquid generally with machinery oil, white oil etc. as carrier fluid, therefore can not directly magnetic liquid be put into the electron microscopic sample chamber and observe.At present, the someone utilizes the flowability of magnetic liquid, and magnetic liquid is made in magnetic field does not have mobile magnetic fluid film earlier, makes spray carbon with vacuum coater again and handles, and sprays one deck gold at last again, processes magnetic liquid electron microscopic sample.Though this method is feasible, but the preparation process is loaded down with trivial details, and magnetic-particle exposure duration in air is longer; Oxidized easily; And the overlapping situation of magnetic-particle is more serious, and the distribution situation of magnetic-particle in surface topography that can not the actual response magnetic-particle and the magnetic field is shown in accompanying drawing 2.Have only the surperficial appearance that partly can see magnetic-particle on the edge of in the accompanying drawing 2, other position is because the overlapping distribution situation that can not differentiate magnetic-particle of magnetic-particle.For guaranteeing the distribution situation of magnetic-particle in the real magnetic reaction fields of TEM picture ability, must guarantee that magnetic-particle is not overlapping, reaches a gratifying TEM resolution.
Summary of the invention
Given this, the technical matters that the present invention will solve provides the preparation method of magnetic liquid transmission electron microscope observation sample in a kind of magnetic field, to obtain the better transmission electron microscope high resolution picture of distribution situation.
The preparation method of magnetic liquid transmission electron microscope observation sample in the magnetic field: a certain amount of magnetic liquid is scattered in the solvent; According to the quality quality adjusting magnetic liquid of magnetic liquid and the dilution ratio of solvent; Assurance adds that mixed liquor is transparent behind the magnetic liquid; About 15 minutes of this mixed liquor of sonic oscillation evenly disperses magnetic liquid and is suspended in the solvent, forms a transparent testing sample dispersion liquid.Provide one have a gradient transverse magnetic field and longitudinal magnetic field, dispersion liquid is placed in transverse magnetic field or the longitudinal magnetic field, according to the test needs of transverse magnetic field and longitudinal magnetic field; Utilize coordinate line to regulate the copper mesh position; Copper mesh immersed leave standstill 1 minute in the dispersion liquid, again with the copper mesh pull-up, because the adsorbability of magnetic-particle is very strong; The chain structure of magnetic-particle in magnetic field " picked up " by copper mesh, and is attached to copper mesh.With copper mesh be placed on seal on the film dry; So far the transmission electron microscope test sample preparation of magnetic liquid in transverse magnetic field or longitudinal magnetic field finishes; Send into the transmission electron microscopy observation chamber, promptly can be observed the distribution and the arranging situation of magnetic-particle in transverse magnetic field or the longitudinal magnetic field.Solvent can be selected the solvent of various magnetic liquids for use, and preferred alcohol or acetone or ether not only do not react with magnetic-particle, also are convenient to recycle, and environment is not polluted.
The invention has the advantages that: provide in a kind of very simple magnetic field the magnetic liquid transmission electron microscope with the preparation method of sample; Solved the overlapping serious problem of magnetic-particle; Avoided that magnetic liquid is oxidized in spray carbon, process such as gold-plated is polluted, really the distribution situation of magnetic-particle in the magnetic reaction fields.This technology is suitable for preparing magnetic liquid tem specimen in the magnetic field, and its important feature is not need the complicated sample technology of preparing, does not damage the micromechanism of sample, does not have to pollute and introduce the problem of illusion, and cost is low, uses very extensive.
Description of drawings
The device synoptic diagram that Fig. 1 (a) uses for magnetic liquid transmission electron microscope observation sample preparation methods in the magnetic field of the present invention;
Fig. 1 (b) is the coordinate of transverse magnetic field mobile platform setting in the device of the present invention's use and the synoptic diagram of copper mesh position;
In the device that Fig. 1 (c) uses for the present invention at the square opening bottle synoptic diagram of transverse magnetic field;
The coordinate that is provided with above the longitudinal magnetic field solenoid in the device of Fig. 1 (d) for the present invention's use and the synoptic diagram of copper mesh position;
Fig. 2 is the existing transmission electron microscope photo that magnetic liquid is positioned over the magnetic fluid film for preparing in the magnetic field;
Fig. 3 is the transmission electron microscope photo of magnetic liquid magnetic-particle when not applying magnetic field;
The transmission electron microscope photo of magnetic liquid magnetic-particle when Fig. 4 (a), 4 (b), 4 (c) are respectively 0.2A, 0.6A, 1.0A for transverse magnetic field of the present invention applies electric current;
Fig. 5 (a) and 5 (b) are magnetic induction density and the magnetic induction Gradient distribution curve map of transverse magnetic field under 0.2A, 0.6A, 1.0A electric current;
The transmission electron microscope photo of magnetic liquid magnetic-particle when Fig. 6 (a), 6 (b), 6 (c) are respectively 0.2A, 0.6A, 1.0A for longitudinal magnetic field of the present invention applies electric current;
Fig. 7 (a) and 7 (b) are magnetic induction density and the magnetic induction Gradient distribution curve map of longitudinal magnetic field under 0.2A, 0.6A, 1.0A electric current.
Embodiment
To combine accompanying drawing and specific embodiment that the preparation method of tem specimen provided by the invention is done further detailed description below.
The preparation method of tem specimen provided by the invention mainly comprises following step:
The first step: shown in Fig. 1 (a), designed magnetic liquid transmission electron microscope observation sample preparation apparatus in the magnetic field, this device mainly is made up of transverse magnetic field, longitudinal magnetic field and upgrade-system.
Upgrade-system is to be used for the position of up-down adjustment copper mesh in dispersion liquid.It mainly consists of the following components, base 1, holder 2, up-down guide pillar 3, web joint 4, motor cabinet 5, stepper motor 6, joint pin 7, gripper clamp 8.Web joint 4 can carry out 360 ° of rotations around up-down guide pillar (borded pile) 3, can move up and down along the up-down guide pillar and regulate, and is convenient to the gripper clamp clamping and copper mesh and in transverse magnetic field and longitudinal magnetic field system, adjust the position up and down.Transverse magnetic field uses different gripper clamp 8 respectively with longitudinal magnetic field, and the horizontal saliva of folder mouth of gripper clamp 8 is flat in the transverse magnetic field, copper mesh is parallel to liquid level puts into dispersion liquid; The vertical clamping copper mesh 15 of the folder mouth of gripper clamp is put into dispersion liquid 16 with copper mesh 15 perpendicular to liquid level in the longitudinal magnetic field.
Distance between two solenoids 12 of transverse magnetic field system is 5cm, and coil diameter is 10cm, and 12 pairs of hearts of two solenoids are placed in parallel on the mobile platform 13, and mobile platform 13 can be finely tuned through rotating handwheel 14; The coordinate line that the 1cm grid of even scale is arranged on the mobile platforms in the middle of two solenoids is convenient to accurately locate the position of copper mesh 10, shown in Fig. 1 (b); Shown in Fig. 1 (c), wide is 5cm to the transverse magnetic field of customization, grows tall to be 6cm with square opening bottle 9, and two ribs of square opening bottle indicate scale, and square opening bottle 9 is placed between two solenoids 12 of transverse magnetic field system, is convenient to accurately place copper mesh 10 and holds dispersion liquid 11.
Longitudinal magnetic field solenoid 17 diameters are 10cm, are positioned on the mobile platform 18, and mobile platform 18 can be finely tuned through rotating handwheel 19; The coordinate line that the 1cm grid of even scale is arranged in the solenoid end is convenient to accurately locate the copper mesh position, shown in Fig. 1 (d); The longitudinal magnetic field of customization uses square opening bottle length and width to be 5cm, and height is 1cm, and the high coordinate scale that indicates of square opening bottle holds dispersion liquid, above the square opening bottle longitudinal magnetic field solenoid 17.
Second step: magnetic liquid is scattered in the solvent; According to the quality quality adjusting magnetic liquid of magnetic liquid and the dilution ratio of solvent; Assurance adds that mixed liquor is transparent behind the magnetic liquid; About 15 minutes of this mixed liquor of sonic oscillation evenly disperses magnetic liquid and is suspended in the solvent, forms a testing sample dispersion liquid.
Solvent is chosen as absolute ethyl alcohol in this example; The low molecular weight solvent that also can select other to volatilize fully; Like acetone, ether etc.; This solvent only plays the effect of even dispersion magnetic liquid, and therefore in preparation transmission electron microscope specimen process, this solvent does not react with magnetic liquid.Mixed liquor vibrated in the sonic oscillation appearance about 10 minutes in this example, can also disperse this mixed liquor with additive method, but as adopting also dispersing and mixing liquid of mechanical raking.
The 3rd step: with gripper clamp copper mesh 10,15 is clipped,, copper mesh is moved to position to be measured, shown in Fig. 1 (b) and Fig. 1 (d) through regulating web joint 4, joint pin 7 and mobile platform 13/18.
In transverse magnetic field, copper mesh is horizontal positioned at the core center place, regulate the copper mesh position according to coordinate line after; Gripper clamp is risen, and the square opening bottle that will hold dispersion liquid (the dispersion liquid height is 5cm) moves into mobile platform, puts the position well according to coordinate line; The gripper clamp that at the uniform velocity descends is treated that copper mesh has just immersed and is promptly stopped the gripper clamp motion in the dispersion liquid, leaves standstill 1 minute; With the copper mesh pull-up, because the adsorbability of magnetic-particle is very strong, the chain structure of magnetic-particle " is picked up " by copper mesh fast.Copper mesh is placed on seals on the film dryly, so far the transmission electron microscope test sample preparation of magnetic liquid in transverse magnetic field finishes, and sends into the transmission electron microscopy observation chamber, promptly can be observed the distribution and the arranging situation of magnetic-particle in the transverse magnetic field.
In longitudinal magnetic field, copper mesh 15 is placed perpendicular to iron core at the core center place, regulate the copper mesh position according to coordinate line after; Gripper clamp is risen; The square opening bottle that holds dispersion liquid is moved into mobile platform, and the dispersion liquid height is 5mm, guarantees just submergence copper mesh of dispersion liquid; Avoid that other magnetic linkage influences measurement result in the dispersion liquid, and guarantee to measure at the strongest iron core place of magnetic induction density.Other measuring process and transverse magnetic field are similar, treat that copper mesh has just immersed promptly to stop gripper clamp motion in the dispersion liquid, leave standstill 1 minute, and fast with the copper mesh pull-up, because the adsorbability of magnetic-particle is very strong, the chain structure of magnetic-particle " is picked up " by copper mesh.Copper mesh is placed on seals on the film dryly, so far the transmission electron microscope test sample preparation of magnetic liquid in transverse magnetic field finishes, and sends into the transmission electron microscopy observation chamber, promptly can be observed the distribution and the arranging situation of magnetic-particle in the longitudinal magnetic field.
Make an explanation in the face of other accompanying drawing in the description of drawings down.
Fig. 2 is for being positioned over magnetic liquid in the prior art transmission electron microscope photo of the magnetic fluid film for preparing in the magnetic field; Have only the surperficial appearance that partly can see magnetic-particle on the edge of, other position is because the overlapping distribution situation that can not differentiate magnetic-particle of magnetic-particle.The magnetic-particle TEM picture of making time spent amplification 500K for no externally-applied magnetic field of the present invention shown in Figure 3; Can see the micromechanism of magnetic-particle among the figure clearly; Each particle is a single magnetic domain; The director circle ball of black is a magnetic-particle, and appearance coats the unimolecular layer surfactant of one deck grey, prevents that magnetic-particle group from gathering collection.Fig. 3 shows that no externally-applied magnetic field does the time spent, and magnetic-particle is random even distribution in carrier fluid, and explaining is not having externally-applied magnetic field to do the time spent, and magnetic liquid is in a kind of stable state of low energy.
With left solenoid core center is initial point, and the core center line is the y axle, sets up rectangular coordinate system.Fig. 4 (a), 4 (b) and 4 (c) are for to apply under the electric current of 0.2A, 0.6A and 1.0A to solenoid respectively, the TEM picture of magnetic-particle in different transverse magnetic fields.In order to study the influence of magnetic field and gradient thereof, use PG-5 type gaussmeter to measure coil magnetic induction density on every side in the experiment to the magnetic-particle arrangement architecture.Fig. 5 (a) flows down the axial magnetic induction density change curve along y for different electric, and magnetic pole place magnetic induction density is maximum, and magnetic pole two ends magnetic induction density is symmetrical distribution.Use origin software that the magnetic induction density curve is carried out match, ask partial derivative can get the change curve of magnetic induction gradient to matched curve again.In 0 < y < 1.25cm zone; Magnetic field gradient
; Magnetic induction gradient and magnetic induction density are in the opposite direction; For studying conveniently;
taken absolute value, and Fig. 5 (b) flows down the axial magnetic induction gradient along y for different electric.Fig. 4 (a), 4 (b) and 4 (c) are found that relatively magnetic-particle is line of collimation catenation structure along magnetic direction in the transverse magnetic field, and along with the increase of coil current, the magnetic field around the coil strengthens gradually, and more magnetic-particle is assembled and arrangement along magnetic direction.Fig. 4 (a) is for amplifying the TEM picture of 200K, two line of collimation catenations of clear demonstration structure among the figure; Fig. 4 (b) and 4 (c) are respectively the TEM picture that amplifies 200K and 300K, and along with magnetic field, magnetic pole place strengthens, collection gathers in more magnetic-particle group, forms the magnetic linkage of a black; Along with distance increases, magnetic linkage is tapered.This mainly is that magnetic field, magnetic pole place and magnetic field gradient weaken gradually along with distance increases, and fewer and feweri along the magnetic-particle that magnetic direction is assembled, magnetic linkage attenuates.
With the solenoid core center is initial point, and a certain radius is the y axle, sets up rectangular coordinate system.Fig. 6 (a), 6 (b) and 6 (c) amplify the magnetic-particle TEM picture of 80K for for to apply under the electric current of 0.2A, 0.6A and 1.0A to solenoid respectively in different longitudinal magnetic fields.Fig. 7 (a) flows down the axial magnetic induction density change curve along y for different electric, and hub of a spool place magnetic induction density is maximum, and magnetic induction density is symmetrical distribution along y axle both sides; Along with increasing magnetic induction density, distance reduces gradually.In 0 < y < 3.00cm zone; Magnetic induction gradient
; Magnetic induction gradient and magnetic induction density are in the opposite direction; For studying conveniently;
taken absolute value; Can get different electric and flow down axial magnetic induction gradient, shown in Fig. 7 (b) along y.Fig. 5 and Fig. 6 are relatively found, be line of collimation catenation structure along the magnetic direction magnetic-particle, along with the increase of coil current, the magnetic field around the coil strengthens gradually, and more magnetic-particle is assembled and arrangement along magnetic direction; Most of magnetic-particle all accumulates in the strongest hub of a spool in magnetic field, and along with hub of a spool magnetic field continues to strengthen, magnetic-particle has formed group's clustering architecture, and group's clustering architecture flocks together and forms the long magnetic linkage of a black; The edge
yThe edge that direction of principal axis magnetic field is more weak, the magnetic-particle of gathering is less, and the marginal portion then is that single magnetic-particle is lined up a long-chain.Examining the long magnetic linkage of line of collimation black that group's clustering architecture forms among Fig. 6 (c) finds; Magnetic linkage edge magnetic particle clusters comparatively dense; Magnetic-particle group in magnetic linkage center is bunch more sparse, and this mainly is because the line of collimation catenation structure of magnetic-particle except that receiving influence of magnetic field, also receives the influence of magnetic field gradient; Can see the edge from Fig. 7 (b)
yAxle forward, magnetic field gradient weaken after strengthening earlier gradually, and the line of collimation catenation structure of this and magnetic-particle is one to one.
Arrangement architecture research through to magnetic-particle in longitudinal magnetic field and the transverse magnetic field can get, and magnetic-particle is line of collimation catenation structure along magnetic direction; When magnetic field and magnetic field gradient were more weak, single magnetic-particle was arranged in the line of collimation long-chain; Along with the increase of magnetic field and magnetic field gradient, magnetic-particle has formed group's clustering architecture, and group's clustering architecture flocks together and forms the long magnetic linkage of a black.
Magnetic liquid transmission electron microscope preparation method has the following advantages in the magnetic field provided by the present invention.The first, the inventive method is comparatively simple, directly dispersion liquid is positioned in the magnetic field, regulates the copper mesh position, can be prepared into the transmission electron microscopy observation sample.The second, dual-use of the present invention both can have been measured the arrangement architecture of magnetic-particle in the transverse magnetic field, also can measure the arrangement architecture of magnetic-particle in the longitudinal magnetic field.The 3rd; The invention solves and use transmission electron microscope can not study the problem of magnetic-particle arrangement architecture in the magnetic field; And the method through " dragging for " magnetic-particle has solved the overlapping serious problem of magnetic-particle; Avoided in spray carbon, process such as gold-plated magnetic liquid exposure duration in air longer, oxidized easily, really the distribution situation of magnetic-particle in the magnetic reaction fields.
The above; Be merely the preferable embodiment of the present invention; But protection scope of the present invention is not limited thereto; Any technician who is familiar with the present technique field is equal to replacement or change according to technical scheme of the present invention and inventive concept thereof in the technical scope that the present invention discloses, all should be encompassed within protection scope of the present invention.
Claims (3)
1. magnetic liquid transmission electron microscope observation sample preparation methods in the magnetic field is scattered in magnetic liquid and forms mixed liquor in the solvent, with this mixed liquor of sonic oscillation about 15 minutes; Magnetic liquid is evenly disperseed and be suspended in the solvent, form transparent dispersion liquid, dispersion liquid is placed in transverse magnetic field or the longitudinal magnetic field; Test needs according to transverse magnetic field or longitudinal magnetic field; Utilize coordinate to confirm the position of copper mesh, copper mesh is immersed leave standstill 1 minute in the dispersion liquid, again with the copper mesh pull-up; Utilize the adsorbability of magnetic-particle; The chain structure of magnetic-particle in magnetic field picked up by copper mesh, copper mesh is placed on seals dry evaporating solvent on the film, prepares the transmission electron microscope specimen of magnetic liquid in transverse magnetic field or longitudinal magnetic field.
2. like magnetic liquid transmission electron microscope observation sample preparation methods in the said magnetic field of claim 1; It is characterized in that: dispersion liquid is contained in respectively in two square opening bottles of coordinate sign; Again one of them square opening bottle being put into transverse magnetic field has between two solenoids (12) of coordinate sign, and another square opening bottle wherein is put into above the solenoid (17) of longitudinal magnetic field.
3. magnetic liquid transmission electron microscope observation sample preparation methods as in claim 1 or the 2 said magnetic fields time, it is characterized in that: solvent is ethanol or acetone or ether.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103792121A (en) * | 2014-02-10 | 2014-05-14 | 河北钢铁股份有限公司邯郸分公司 | Preparation method for metallurgical powdered test sample |
| CN106769162A (en) * | 2017-02-20 | 2017-05-31 | 广西大学 | A kind of transmission electron microscope magnetic sample preprocessor |
| CN108490221A (en) * | 2018-03-23 | 2018-09-04 | 山东大学 | A kind of preparation method for transmission electron microscope observation sample of magnetic material |
| CN108956227A (en) * | 2018-07-03 | 2018-12-07 | 中山大学 | A kind of preparation method of the liquid nanometer particulate samples for transmission electron microscope analysis |
| CN109804235A (en) * | 2016-11-30 | 2019-05-24 | 国立研究开发法人产业技术综合研究所 | Target substance detection device and target substance detection method |
| CN114088496A (en) * | 2021-11-25 | 2022-02-25 | 内蒙古工业大学 | Device for preparing transmission electron microscope powder sample |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103792121A (en) * | 2014-02-10 | 2014-05-14 | 河北钢铁股份有限公司邯郸分公司 | Preparation method for metallurgical powdered test sample |
| CN109804235A (en) * | 2016-11-30 | 2019-05-24 | 国立研究开发法人产业技术综合研究所 | Target substance detection device and target substance detection method |
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| CN108490221A (en) * | 2018-03-23 | 2018-09-04 | 山东大学 | A kind of preparation method for transmission electron microscope observation sample of magnetic material |
| CN108956227A (en) * | 2018-07-03 | 2018-12-07 | 中山大学 | A kind of preparation method of the liquid nanometer particulate samples for transmission electron microscope analysis |
| CN114088496A (en) * | 2021-11-25 | 2022-02-25 | 内蒙古工业大学 | Device for preparing transmission electron microscope powder sample |
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