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CN1265185C - Organic light-emitting diode electron microscope test piece and manufacturing method thereof - Google Patents

Organic light-emitting diode electron microscope test piece and manufacturing method thereof Download PDF

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Publication number
CN1265185C
CN1265185C CN 03148265 CN03148265A CN1265185C CN 1265185 C CN1265185 C CN 1265185C CN 03148265 CN03148265 CN 03148265 CN 03148265 A CN03148265 A CN 03148265A CN 1265185 C CN1265185 C CN 1265185C
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electron microscope
emitting diode
light emitting
organic light
test piece
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CN 03148265
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CN1566918A (en
Inventor
蔡和廷
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Huaxing Optoelectronic International Hong Kong Co ltd
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AU Optronics Corp
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Abstract

An organic light emitting diode electron microscope test piece and a manufacturing method thereof. Firstly, an organic light emitting diode sample is provided, wherein the organic light emitting diode sample at least comprises a substrate, a first electrode layer, an organic layer and a second electrode layer. Then, a protective layer is formed on the surface of the sample. Then, the organic light emitting diode sample is cut to obtain an organic light emitting diode sample slice with a specific thickness, so as to increase the probability that organic material molecules of the organic layer are hit by an electron beam emitted by the transmission electron microscope, thereby generating diffraction imaging and obtaining an image of the test piece.

Description

Organic Light Emitting Diode electron microscope test piece and preparation method thereof
Technical field
The present invention relates to a kind of electron microscope test piece, particularly about a kind of Organic Light Emitting Diode electron microscope test piece and preparation method thereof.
Background technology
Along with the progress of material science, microstructure is very huge in the influence in nature of material itself, so the character of desire understanding material itself, just good microscopic analysis technology and instrument must be able to be arranged.General optical microscope, be subject to factors such as optical wavelength, aberration, enlargement ratio is limited, based on more powerful demand, new " micro-" equipment is slowly development just, electron microscope is exactly one of them, and the signal that utilizes electronics and material effect to be produced is identified the electron-optical arrangement of film micro area structure, microtexture, chemical analysis, chemical bonded refractory and electron distributions situation.
Electron microscope (Electron Microscope, EM) generally be meant and utilize the electromagnetic field deviation, the principle of focused electron and electronics and material scattering that effect produces is studied the exact instrument of material structure and microtexture, the electron microscope of a class wherein, transmission electron microscope (Transmission ElectronMicroscope, be called for short TEM), be to pass test piece by electronics, again through the lens enlarge-effect of electromagnetic lens system, and obtain powerful image, many application are arranged on material science, such as: difference row is theoretical, point defect, implanting ions, membrane structure, electronic package failure analysis etc., but the limit of its application, do not lie in the restriction on the resolution of machine own, and be difficulty in the test piece preparation, for the observation of TEM, test piece needs enough thin districts, the good electron penetrance just can be arranged to obtain enough resolution.
Organic Light Emitting Diode (Organic Light Emitting Diode, OLED) basic structure is formed, please refer to shown in Figure 1, comprise: a metallic cathode 12, a transparent anode 14, a transparency carrier 16 and an organic layer 10, wherein the organic material in the organic layer 10 more comprises an electron transfer layer 101, a luminescent layer 102 and a hole transmission layer 103.The principle of luminosity of Organic Light Emitting Diode is by applying a voltage to above-mentioned metallic cathode 12 and transparent anode 14, order about electronics and hole and fixation phenomenon again takes place at organic layer 10, this again the fixation phenomenon energy of emitting will excite the organic material molecule, and then generation luminescence phenomenon, come out by transparency carrier 16 radiation again, become a self luminous display module.In known techniques, the control of each organic material thickness can only be controlled according to the quartz (controlled) oscillator of board on the line in the organic layer 10, is not that actual amount records and knows, so way is not accurately controlled the thickness of each layer.
If when desiring to observe the structure of each organic material layer in the organic layer 10 with transmission electron microscope (TEM), its specimen preparation is down auxiliary focused ion beam (Focus Ion Beam), can prepare thickness of test piece less than the film below 0.1 micron, and under traditional idea, as long as it is thinner that test piece can be ground, its resolution just better, but for Organic Light Emitting Diode, when thickness of test piece less than below 0.1 micron the time, as shown in Figure 2, the level of each organic material and structure can not be told by transmission electron microscope in the organic layer 10, under the ordering about of traditional concept, only can be with test piece wear down again, its result still can't tell the level and the structure of organic material from transmission electron microscope.In view of this, the present invention proposes a kind of specimen preparation method of Organic Light Emitting Diode electron microscope, makes clearly to distinguish the structure and the level of each organic material in the organic layer under electron microscope.
Summary of the invention
Technical matters to be solved by this invention provides a kind of method for making of electron microscope test piece, a kind of Organic Light Emitting Diode electron microscope test piece and preparation method thereof particularly is provided, make to obtain clearly test piece image when doing test piece observes, help the structure analysis of organic material.
Organic Light Emitting Diode electron microscope test piece that provides of the present invention and preparation method thereof is realized by following technical scheme.
The method for making of a kind of Organic Light Emitting Diode electron microscope test piece, be used for the observation of electron microscope, pass this test piece generation by this electron microscope ejected electron bundle and penetrate and the diffraction phenomenon, obtain the image of this test piece, it is characterized in that comprising at least the following step:
One Organic Light Emitting Diode sample is provided, wherein this Organic Light Emitting Diode sample comprises a substrate, one first electrode layer, an organic layer and a second electrode lay at least, this first electrode layer is to be positioned on this substrate, this organic layer is to be positioned on this first electrode layer, and this second electrode lay is to be positioned on this organic layer;
Form the surface of a protective seam in this sample; And
This Organic Light Emitting Diode sample is carried out a cutting program, obtain the thin slice of this Organic Light Emitting Diode sample.
The method for making of described Organic Light Emitting Diode electron microscope test piece is characterized in that: the thickness of above-mentioned thin slice is between 0.2 micron to 0.3 micron.
The method for making of described Organic Light Emitting Diode electron microscope test piece is characterized in that: above-mentioned cutting process is to carry out with focused ion beam.
The method for making of described Organic Light Emitting Diode electron microscope test piece is characterized in that: the thickness of above-mentioned protective seam is between 2 microns to 3 microns.
The method for making of described Organic Light Emitting Diode electron microscope test piece is characterized in that: above-mentioned protective seam is a platinum.
The method for making of described Organic Light Emitting Diode electron microscope test piece is characterized in that: above-mentioned protective seam is a tungsten.
The method for making of described Organic Light Emitting Diode electron microscope test piece is characterized in that: above-mentioned with focused ion beam this sample to be carried out cutting process be the program that comprises a rough lumber.
The method for making of described Organic Light Emitting Diode electron microscope test piece is characterized in that: more comprise the program of frittering.
The method for making of described Organic Light Emitting Diode electron microscope test piece is characterized in that: more comprise the program that an essence is cut.
The method for making of described Organic Light Emitting Diode electron microscope test piece is characterized in that: above-mentioned electron microscope is a transmission electron microscope.
The present invention also provides a kind of Organic Light Emitting Diode electron microscope test piece that is used for said method, the usefulness that is used for the observation of electron microscope, pass this test piece generation by this electron microscope ejected electron bundle and penetrate and the diffraction phenomenon, obtain the image of this test piece, it is characterized in that comprising at least:
One substrate;
One first electrode layer is to be positioned on this substrate;
One organic layer is to be positioned on this first electrode layer;
One the second electrode lay is to be positioned on this organic layer; And
One protective seam is to be made on this second electrode lay;
Wherein the thickness of this test piece is between 0.2 micron to 0.3 micron, and the probability in order to the organic material molecule that increases this organic layer is got to by electron beam is produced the diffraction imaging.
The test piece of described Organic Light Emitting Diode electron microscope is characterized in that: above-mentioned protective seam is to be formed on this second electrode lay with focused ion beam.
The test piece of described Organic Light Emitting Diode electron microscope is characterized in that: the thickness of above-mentioned protective seam is between 2 microns to 3 microns.
The test piece of described Organic Light Emitting Diode electron microscope is characterized in that: above-mentioned protective seam is a platinum.
The test piece of described Organic Light Emitting Diode electron microscope is characterized in that: above-mentioned protective seam is a tungsten.
The test piece of described Organic Light Emitting Diode electron microscope is characterized in that: above-mentioned electron microscope is to be transmission electron microscope.
The invention provides the method for making of a kind of Organic Light Emitting Diode electron microscope test piece, can be used for the usefulness of the observation of electron microscope, pass the test piece generation by transmission electron microscope ejected electron bundle and penetrate and the diffraction phenomenon, obtain the image of test piece.At first, provide an Organic Light Emitting Diode sample, wherein this Organic Light Emitting Diode sample comprises a substrate, one first electrode layer, an organic layer and a second electrode lay in regular turn.Then, form a coat of metal in sample surfaces.Subsequently, the Organic Light Emitting Diode sample is carried out the cutting process of focused ion beam, wherein this cutting process comprises the rough lumber carried out in regular turn, fritters and smart step of cutting, to obtain the thin slice of thickness between 0.2 micron to 0.3 micron, the probability that the organic material molecule of organic layer of so being increased is got to by electron beam is produced the diffraction imaging.
The specimen preparation method of Organic Light Emitting Diode electron microscope of the present invention has following advantage:
(1) by design of the present invention, each hierarchical structure of organic material can clearly be observed out by transmission electron microscope in the Organic Light Emitting Diode (OLED).
(2) when each hierarchical structure of organic material can be by identification clearly, the thickness of each level of affirmation that can be clear and definite, rather than rely on the adjustment of other objective parameter as the time of evaporation organic material, is inferred the actual (real) thickness of organic material layer.
(3) after obtaining accurate organic material layer actual (real) thickness value, to help structural analysis, more because Organic Light Emitting Diode is an autoluminescence assembly, the wherein generation of the more directly related light source of organic material layer, by design of the present invention, can accurately adjust the thickness of each organic layer, and then obtain optimized illumination effect.
By following detailed description in conjunction with the accompanying drawings, can understand the plurality of advantages of foregoing and the present invention easily.
Description of drawings
Fig. 1 is the basic block diagram of Organic Light Emitting Diode.
Fig. 2 is according to the resulting Organic Light Emitting Diode cross-sectional view of known techniques figure.
Fig. 3 is the Organic Light Emitting Diode electron microscope specimen preparation method flow diagram of the preferred embodiment according to the present invention.
Fig. 4 is the cutting synoptic diagram according to the Organic Light Emitting Diode sample of the embodiment of the invention.And
Fig. 5 is according to the resulting Organic Light Emitting Diode cross-sectional view of embodiment of the invention figure.
Embodiment
The invention provides the method for making of a kind of Organic Light Emitting Diode electron microscope test piece.In the present invention, when making that by the thickness of controlling test piece transmission electron microscope ejected electron Shu Yu passes test piece, generation penetrates and the diffraction phenomenon, and then obtain the image of desire observation test piece, make each layer structure of organic material of Organic Light Emitting Diode can be under electron microscope clearly identification come out, will be very helpful with research for the analysis of the structure of Organic Light Emitting Diode.Below enumerate a preferred embodiment now with explanation the present invention, right those who are familiar with this art know that all this only is one for example, and are not in order to limit invention itself.The detailed description of relevant this preferred embodiment is as follows.
As shown in Figure 3, be the Organic Light Emitting Diode electron microscope specimen preparation method flow diagram of preferred embodiment according to the present invention.Shown in step 201, one Organic Light Emitting Diode sample at first is provided, wherein the Organic Light Emitting Diode sample is to comprise a substrate, one first electrode layer, an organic layer and a second electrode lay, more comprise an electron transfer layer, a luminescent layer and a hole transmission layer in the organic layer, but, each layer structure in the above-mentioned organic layer only is an explanation for example, is not in order to limit scope of the present invention.
Then, shown in step 202, form protective seam in the surface of Organic Light Emitting Diode sample.This protective seam is to use platinum (Pt) or tungsten metal materials such as (W), with focused ion beam (Focus Ion Beam, FIB) in Organic Light Emitting Diode sample surfaces place, formation thickness is about the metallic film between 2 microns to 3 microns, its role is to: on the one hand can the sampling stability of structure, avoid when the high-energy cutting step of back segment, causing the collapse of sample structure; On the other hand also can be as the usefulness of sign, in order to observation.
Next, as described in step 203, being cut with the thin slice that the OLED sample becomes a predetermined thickness, please be the cutting synoptic diagram according to the Organic Light Emitting Diode sample of the embodiment of the invention simultaneously with reference to Fig. 4.At first; side in the Organic Light Emitting Diode sample 20 that is coated with protective seam; utilize focused ion beam to carry out the rough lumber of big electric current (coarse milling) earlier; fritter (intermediate milling) with the focused ion beam of middle electric current again, carry out the program that essence is cut (fine milling) with little electric current more at last.Then in the opposite side of the Organic Light Emitting Diode sample 20 that is coated with protective seam, the step of carry out rough lumber more in regular turn, fritter, essence being cut is to form the thin slice of thickness between 0.2 micron to 0.3 micron.Cutting hole 2031,2032,2033 shown in the figure promptly be respectively via rough lumber, fritter, essence cuts the formed cutting of step hole.
Then, shown in step 204, take off this Organic Light Emitting Diode thin slice.Please also refer to Fig. 4, Organic Light Emitting Diode sample 20 two ends are linked to the part of sample body, utilize focused ion beam, so promptly finish the making of electron microscope test piece in to separate.When carrying out the cross-sectional view of test piece, this Organic Light Emitting Diode thin slice is placed earlier on the carbon film, the carbon film that again this is had the Organic Light Emitting Diode thin slice is put on the copper mesh, to carry out the observation of test piece.
As shown in Figure 5, be cross-sectional view figure according to the test piece of embodiment of the invention made, by among the figure as can be known, each layer structure in the organic layer 10 comprises electron transfer layer 103, luminescent layer 102 and hole transmission layer 101, control the thickness (between 0.2 micron to 0.3 micron) of test piece by the present invention, make with the Organic Light Emitting Diode test piece when carrying out the observation of transmission electron microscope, the probability that the organic material molecule of increase organic layer is got to by electron microscope institute ejected electron bundle, produced the diffraction imaging, made that the structure of each level can be via clearly identification of electron microscope.
Though the present invention illustrates as above with preferred embodiments, so it is not only to terminate in the foregoing description in order to limit the present invention's spirit with the invention entity.Be with, the modification of being done in not breaking away from spirit of the present invention and scope all should be included in the claim scope.

Claims (14)

1, the method for making of a kind of Organic Light Emitting Diode electron microscope test piece, be used for the observation of electron microscope, pass this test piece generation by this electron microscope ejected electron bundle and penetrate and the diffraction phenomenon, obtain the image of this test piece, it is characterized in that comprising at least the following step:
One Organic Light Emitting Diode sample is provided, wherein this Organic Light Emitting Diode sample comprises a substrate, one first electrode layer, an organic layer and a second electrode lay at least, this first electrode layer is to be positioned on this substrate, this organic layer is to be positioned on this first electrode layer, and this second electrode lay is to be positioned on this organic layer;
Form the surface of a protective seam in this sample; And
With focused ion beam this Organic Light Emitting Diode sample is carried out a cutting program, obtain the thin slice of this Organic Light Emitting Diode sample, the thickness of this thin slice is between 0.2 micron to 0.3 micron.
2, the method for making of Organic Light Emitting Diode electron microscope according to claim 1 test piece is characterized in that: the thickness of above-mentioned protective seam is between 2 microns to 3 microns.
3, the method for making of Organic Light Emitting Diode electron microscope according to claim 1 test piece, it is characterized in that: above-mentioned protective seam is a platinum.
4, the method for making of Organic Light Emitting Diode electron microscope according to claim 1 test piece, it is characterized in that: above-mentioned protective seam is a tungsten.
5, the method for making of Organic Light Emitting Diode electron microscope according to claim 1 test piece is characterized in that: above-mentioned with focused ion beam this sample to be carried out cutting process be the program that comprises a rough lumber.
6, the method for making of Organic Light Emitting Diode electron microscope according to claim 5 test piece is characterized in that: more comprise the program of frittering.
7, the method for making of Organic Light Emitting Diode electron microscope according to claim 6 test piece is characterized in that: more comprise the program that an essence is cut.
8, the method for making of Organic Light Emitting Diode electron microscope according to claim 1 test piece, it is characterized in that: above-mentioned electron microscope is a transmission electron microscope.
9, a kind of Organic Light Emitting Diode electron microscope test piece is used for the usefulness of the observation of electron microscope, passes this test piece by this electron microscope ejected electron bundle and produces and penetrate and the diffraction phenomenon, obtains the image of this test piece, it is characterized in that comprising at least:
One substrate;
One first electrode layer is to be positioned on this substrate;
One organic layer is to be positioned on this first electrode layer;
One the second electrode lay is to be positioned on this organic layer; And
One protective seam is to be made on this second electrode lay;
Wherein the thickness of this test piece is between 0.2 micron to 0.3 micron, and the probability in order to the organic material molecule that increases this organic layer is got to by electron beam is produced the diffraction imaging.
10, Organic Light Emitting Diode electron microscope according to claim 9 test piece is characterized in that: above-mentioned protective seam is to be formed on this second electrode lay with focused ion beam.
11, Organic Light Emitting Diode electron microscope according to claim 9 test piece is characterized in that: the thickness of above-mentioned protective seam is between 2 microns to 3 microns.
12, Organic Light Emitting Diode electron microscope according to claim 9 test piece is characterized in that: above-mentioned protective seam is a platinum.
13, Organic Light Emitting Diode electron microscope according to claim 9 test piece is characterized in that: above-mentioned protective seam is a tungsten.
14, Organic Light Emitting Diode electron microscope according to claim 9 test piece is characterized in that: above-mentioned electron microscope is to be transmission electron microscope.
CN 03148265 2003-06-30 2003-06-30 Organic light-emitting diode electron microscope test piece and manufacturing method thereof Expired - Lifetime CN1265185C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 03148265 CN1265185C (en) 2003-06-30 2003-06-30 Organic light-emitting diode electron microscope test piece and manufacturing method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 03148265 CN1265185C (en) 2003-06-30 2003-06-30 Organic light-emitting diode electron microscope test piece and manufacturing method thereof

Publications (2)

Publication Number Publication Date
CN1566918A CN1566918A (en) 2005-01-19
CN1265185C true CN1265185C (en) 2006-07-19

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Effective date of registration: 20180427

Address after: Hongkong Chinese Tsuen Tai Chung Road No. 8 TCL industrial center 13 floor

Patentee after: Huaxing Optoelectronic International (Hong Kong) Co.,Ltd.

Address before: Hsinchu, China Taiwan Science Park

Patentee before: AU OPTRONICS Corp.

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Granted publication date: 20060719