CN102543637A

CN102543637A - Preparation method of in situ double-tilt electronic microscope sample rod

Info

Publication number: CN102543637A
Application number: CN2012100051305A
Authority: CN
Inventors: 王乙潜; 谭金山; 梁文双; 杜庆田
Original assignee: Qingdao University
Current assignee: Qingdao University
Priority date: 2012-01-10
Filing date: 2012-01-10
Publication date: 2012-07-04
Anticipated expiration: 2032-01-10
Also published as: CN102543637B

Abstract

The invention belongs to the technical field of material analysis and testing, and relates to a manufacturing method of an in situ double-tilt electronic microscope sample rod for which an electric field and a light signal can be added externally; the method comprises the following steps that: first, three independent channels are arranged in a hollow copper bar of a sample rod based on an existing single-title electronic microscope sample rod in an insulated and closed way; the three independent channels are respectively distributed to a horizontal transmission rod, a lead and an optical fiber and are insulated and sealed; the sample rod tilts rotationally along a Y axis through a stepper motor which is arranged outside the sample rod and is connected with the horizontal transmission rod; then an electric field terminal is arranged on a sample cup and is more than 10cm away from an optical axis, so that the concentration of charge and the affection of the imaging quality are prevented; then an optical fiber fixed column is arranged on the sample cup, metal is sprayed onto the surface of a transmitting optical fiber and the optical fiber is connected in, and a laser led-in sample is formed into an in situ transmission double-tilt sample rod; and according to the preparation method of the in situ double-tilt electronic microscope sample rod, a design idea is novel, the used equipment and technologies are mature, the manufacturing cost is low, the market blank is filled, experimental needs are met, and the practicality and test results are good.

Description

The preparation method of the two electron microscopic sample bars that incline of a kind of original position

Technical field:

The invention belongs to the material analysis technical field of measurement and test, but relate to the preparation method of the two sample for use in transmitted electron microscope bars that incline of original position of a kind of extra electric field and light signal, prepare the electron microscopic sample occasion when being used for specimen.

Background technology:

Growing along with the progress of modern measuring technology and material science research, the research of original position electron micrology becomes one of main direction of electron micrology development, emerges a large amount of achievements in research in recent years.Many tame Electronic Speculum production firm has released the specimen holder that is used for original position research separately one after another, growing research demand even expedited the emergence of the High-tech company (like famous Nanofactory company etc.) with the various original position specimen holders of the special manufacturing.Current but what can buy through market is small manipulation, variable warm area added electric field (comprising electric signal measurement) mostly, can add the original position specimen holder of (survey) power.The technology of preparing of these specimen holders and can handling comparative maturity, the research that makes the original position electron micrology analyze is also mainly concentrated in these areas.Some laboratories can be made the extra electric field specimen holder by oneself both at home and abroad, but majority is a uniclinal at present.This mainly is because the tumbler of design and the two specimen holders that incline of making is faced with a lot of technical barriers for general laboratory.Original position uniclinal specimen holder can satisfy the demand of much sample being carried out original position research; But must under specific crystal orientation, carry out the situation that home position observation is studied to sample for some; Just turned turtle, but therefore normally bought the two specimen holders that incline of added electric field original position that some specialized companies make.Have many good qualities than homemade specimen holder though purchase ready-made specimen holder, cost an arm and a leg, thereby be difficult to it is transformed, to adapt to the special requirement in the experiment.In addition, light signal is imported on the sample is individual relatively stubborn problem always.The progress of optical fiber and micro lens technology, but many seminar have begun to design the original position specimen holder of lead-in light signal, but also do not have ripe commodity available at present.Prosperous day by day along with ferroelectric material and nanometer photoelectronic material research, but will be more strong to the demand of added electric field and light signal original position specimen holder.The two specimen holders that incline of original position of added electric field and light signal are developed in success not only can fill up the blank of domestic and international this specimen holder, and under the situation that does not change the transmission electron microscope agent structure, uses less cost just can widen the function of existing device.

Summary of the invention:

The objective of the invention is to overcome the shortcoming that prior art exists; Widening the existing equipment function with less cost is basic demand; But seek to design the two specimen holders that incline of original position transmission electron microscope that a kind of simple and practical process prepares added electric field and light signal; To adapt to the research demand of new material, solar cell and clean energy resource, especially ferroelectric material and nanometer photoelectronic material.

To achieve these goals; The present invention opens up three independently seal channels earlier in the hollow cavity of specimen holder on the basis of existing uniclinal specimen holder, distribute to horizontal drive link, lead and optical fiber respectively; Again at outside stepper motor and the drive link interlock mutually of installing of specimen holder; Wire binding post and optical fiber fixed leg are installed on specimen cup then, and the lens fiber of lead-in conductor and surperficial metal spraying constitutes the two specimen holders that incline of original position transmission electron microscope; Its concrete processing step comprises:

(1) the two specimen holder designs of inclining of original position: on the basis of existing uniclinal electron microscopic sample bar; Insulating enclosed type is opened up three independently passages in the hollow copper bar of specimen holder, and three autonomous channels are distributed to horizontal drive link, lead and optical fiber respectively and carried out insulated enclosure; Utilization is installed in the stepper motor that the specimen holder outside links to each other with horizontal drive link and realizes that specimen holder verts along the Y axle;

(2) the electric field assembly is installed: the electric field binding post is installed on the specimen cup and makes it apart from more than the optical axis 10cm, influence image quality to avoid accumulation;

(3) optical fiber inserts: the optical fiber fixed leg is installed on specimen cup, with inserting behind the metal spraying of lens fiber surface, laser is imported in the sample, constitute the two specimen holders that incline of original position transmission electron microscope.

The present invention compared with prior art, its mentality of designing is novel, use equipment and technology maturation, low cost of manufacture is filled a hole in the market, and satisfies the experiment needs, practicality and result of the test are good.

Description of drawings:

Fig. 1 is the side-looking structural principle sketch map of the electron microscopic sample bar front end that the present invention relates to.

Fig. 2 is the plan structure principle schematic of the electron microscopic sample bar front end that the present invention relates to.

Fig. 3 is binding post and the sample wire bonds structural principle sketch map that the present invention relates to.

Embodiment:

Below through embodiment and combine accompanying drawing to be described further.

Embodiment:

The processing step of present embodiment comprises the two specimen holder designs of inclining of original position, the electric field assembly is installed and optical fiber inserts; Wherein the two specimen holder designs of inclining of original position are on the basis of existing uniclinal electron microscopic sample bar; In the hollow copper bar of specimen holder, open up three independently seal channels; Distribute to horizontal drive link 1, lead 9 and optical fiber respectively; And with the transmission electron microscope special sealing ring horizontal drive link 1 is sealed, optical fiber and lead 9 are used epoxy sealing respectively, the end view and the vertical view of the two specimen holder front ends that incline of original position are as depicted in figs. 1 and 2 respectively; The X axle of specimen holder verts and realizes by the angle measurement platform of Electronic Speculum itself; The Y axle verts and moves through stepper motor or horizontal drive link 1 along continuous straight runs of external rotating device drive; The right-hand member of pushing direction selector bar 2 moves downward; And then the driving specimen cup rotates counterclockwise positive and negative the verting of realization Y axle under the deboost of spring 8 along B axle 7; It is to be installed on the specimen cup electric field binding post and away from optical axis that the electric field assembly is installed, as shown in Figure 2, when sample is done two verting when moving; Applying between lead 9 and the sample of electric field does not have relative motion, helps the firm connection of lead 9, avoids the influence of the accumulation of lead 9 outer surfaces and binding post 4 to the electron beam patterning quality simultaneously; Because binding post 4 is less; And the lead between the sample 9 is difficult to welding, considers that wire binding post 4 bottoms are insulator, adopts thread platinum to do the top; Directly be wound into the top with the line of sample and get final product, the sample end is with elargol bonding (as shown in Figure 3); It is that optical fiber fixed leg 5 (as depicted in figs. 1 and 2) are installed on specimen cup that optical fiber inserts; Can directly import to laser on the sample inserting binding post 4 behind the metal spraying of lens fiber surface; Do two verting when moving when sample, do not have relative motion between fiber tip and the sample, and luminous range, angle can not change; Improved the accuracy of illumination; Adopt lens fiber (fiber end face is a sphere, can play the effect of condenser lens) to guarantee that light beam has certain convergence, thereby improve the light intensity on the sample; And optical fiber surface is carried out metal spraying handle the influence that can weaken accumulation.The agent structure of the electron microscopic sample bar front end of present embodiment preparation comprises horizon bar 1, direction selector bar 2, A axle 3, binding post 4, optical fiber fixed leg 5, B axle 6, specimen cup 7, spring 8, lead 9, platinum 11, insulator 10 and sample 12; Its actual fabrication process and the product that forms can be realized the object of the invention through detecting, and reach the designing requirement of expection.

Claims

1. the preparation method of the two electron microscopic sample bars that incline of an original position is characterized in that processing step comprises: