CN103868777A - Preparation method for transmission electron microscope sample - Google Patents
Preparation method for transmission electron microscope sample Download PDFInfo
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- CN103868777A CN103868777A CN201410126975.9A CN201410126975A CN103868777A CN 103868777 A CN103868777 A CN 103868777A CN 201410126975 A CN201410126975 A CN 201410126975A CN 103868777 A CN103868777 A CN 103868777A
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Abstract
The invention discloses a preparation method for a transmission electron microscope sample. The preparation method comprises the following steps: providing a device to be subjected to sample preparation and selecting a target region needing to be analyzed; preparing at least one section and enabling the section to be close to the target region; depositing protection layers on the corresponding positions of the target region; carrying out ion beam cutting on two surfaces deposited with the protection layers; when carrying out ion beam cutting along the direction perpendicular to any one surface of the two surfaces, stopping the cutting in the direction if finding that a hole is formed in the target region along the cutting direction; carrying out ion beam cutting along the direction perpendicular to the other surface and exposing the target region; and finishing the cutting of the device to be subjected to the sample preparation according to dimensional requirements to prepare a sample. According to the preparation method, the influences of curtain effect on the shape of the target region, caused by the hole, can be avoided effectively; defects are prevented from occurring and the reliability of sample analysis is improved.
Description
Technical field
The present invention relates to semiconductor devices analysis technical field, relate in particular to a kind of preparation method of sample for use in transmitted electron microscope.
Background technology
Transmission electron microscope (Transmission electron microscope, abbreviation TEM, be called for short transmission electron microscope) owing to thering is the resolution of superelevation and extremely strong analytic function, the topmost instrument that has at present become advanced technologies semiconductor crystal wafer factory and carry out structure and material analysis.
At present, main TEM sample preparation equipment has been integrated FIB(Focused ion beam, focused ion beam) and SEM(Scanning electron microscope, scanning electron microscope) two-beam ion beam system (DB-FIB), when ion beam cuts, can also use electron beam Synchronous, to guarantee the accurate of sample preparation position.
After semiconductor crystal wafer has been produced, because a variety of causes such as structure or technique can form some little holes (such as the hole between polysilicon side wall) at inside wafer.The ion beam of transmission electron microscope is in the time of the pertusate position of cutter, and the difference of cutting speed can cause the material below hole to cut sooner than other position, form " curtain(curtain) " effect.Below the observed object that wafer need to be analyzed is positioned at hole time, the observation quality of transmission electron microscope can be subject to the impact of curtain effect and reduce, and even cannot observe.
In Fig. 1, the top of sample inner analysis target location 11 has hole 12, in the time that ion beam cuts sample from top to bottom, due to the existence of hole 12, can be to the region 13 that exerts an influence below it, cause evaluating objects position 11 impaired, as the sample transmission electron microscope photo of Fig. 2.
Visible, how, in the process of preparing sample for use in transmitted electron microscope, the impact of avoiding inside wafer hole to produce evaluating objects region, is one of those skilled in the art's technical matters urgently to be resolved hurrily.
Summary of the invention
In order to solve the problem of above-mentioned prior art existence, the invention provides a kind of preparation method of sample for use in transmitted electron microscope, by changing cut direction, improve the impact of cutting process Hole on evaluating objects region.
The preparation method of sample for use in transmitted electron microscope provided by the invention comprises the following steps:
Step S01, provides and treats sample preparation device, the selected target area that needs analysis;
Step S02, prepares this at least one cross section for the treatment of sample preparation device and makes it near target area;
Step S03, to the adjacent device surface in Ji Yugai cross section, cross section near this target area, at the correspondence position deposition protective seam of target area;
Step S04, carries out ion beam cutting to two surfaces that deposit protective seam;
Step S05, while carrying out ion beam cutting along the perpendicular direction in arbitrary surface in two surfaces, if find, target area has hole along the top of cut direction, stops the cutting of this direction, carry out ion beam cutting along another perpendicular direction in surface, expose target area;
Step S06, completes the cutting for the treatment of sample preparation device dimensional requirement, makes sample.
Further, in step S03, at two perpendicular protective seams of device surface deposition of target area correspondence position, in step S04 and S05, cut direction is from the direction to device inside perpendicular to device surface.
Further, in step S05, once find in cutting process to expose the hole directly over target area, stop immediately the cutting of this direction, to avoid the impact of hole on target area.
Further, step S05 also comprises directly over target area, having hole if do not find in cutting process, continues to carry out this cutting action.
Further, in step S02, preparing cross section, to make the distance of itself and target area be 1-10 micron.
Further, the technique of preparing cross section in step S02 comprises sliver, cutting or grinding.
Further, step S03 to S06 completes by FIB equipment.
The present invention proposes a kind of preparation method of sample for use in transmitted electron microscope, by finding that in cutting process target area has hole above cut direction, stop immediately the cutting of this direction, carry out the cutting of other direction, can effectively avoid because of hole, target area pattern being produced the impact of curtain effect, prevent the generation of defect, improve the reliability of sample analysis.
Accompanying drawing explanation
For can clearer understanding objects, features and advantages of the present invention, below with reference to accompanying drawing, preferred embodiment of the present invention is described in detail, wherein:
Fig. 1 is the diagrammatic cross-section that prior art makes sample for use in transmitted electron microscope;
Fig. 2 is the TEM photo that prior art makes sample for use in transmitted electron microscope;
Fig. 3 is the schematic flow sheet that the present invention prepares sample for use in transmitted electron microscope;
Fig. 4 a-4f is the corresponding device architecture schematic diagram of the each step of preparation method's flow process of the present invention;
Fig. 5 is the TEM photo comparison diagram that the inventive method makes sample for use in transmitted electron microscope and prior art.
Embodiment
the first embodiment
Please refer to Fig. 3, Fig. 4 a-4f, in the present embodiment, the preparation method of sample for use in transmitted electron microscope comprises the following steps:
Step S01, provides and treats sample preparation device, the selected target area that needs analysis;
Step S02, prepares this cross section for the treatment of sample preparation device and makes it near target area, as shown in Fig. 4 a;
Step S03, to the adjacent device surface in Ji Yugai cross section, cross section near this target area, at the correspondence position deposition protective seam of target area; Wherein, this step comprises step S031, and device level is put into FIB equipment, at the protective seam that width is 120nm of device upper surface deposition of position, target area, as shown in Figure 4 b; Step S032, vertically puts into FIB equipment by device, at the protective seam that width is 120nm of device upper surface deposition of position, target area, forms mutually perpendicular L-type protective seam, as shown in Fig. 4 c;
Step S04, carries out ion beam cutting to two surfaces that deposit protective seam, and cut direction is from the direction to device inside perpendicular to device surface, two directions of arrow as shown in Fig. 4 d;
Step S05, cut gradually the device of attenuate protective seam both sides, when the region that cuts to protective seam and cover, while carrying out ion beam cutting along the A direction of arrow in Fig. 4 e, find that target area has hole (finding just to have exposed hole) directly over cut direction, stop immediately the cutting of this direction, then carry out ion beam cutting along the B direction of arrow, until expose target area to be analyzed;
Step S06, completes the cutting for the treatment of sample preparation device dimensional requirement, and making sample size is thickness 100nm, height 10 μ m, width 5 μ m.After 90 ° of this rotary samples, take the transmission electron microscope photo of routine observation direction, as shown in Fig. 4 f.
Can find out from Fig. 4 e and 4f, due to the change of ion beam cut direction, target area has effectively been avoided in the curtain effects region that hole produces.
In the present embodiment, directly over target area, there is hole if do not find in cutting process, continue to carry out the cutting action of this direction; In step S02, preparing cross section, to make the distance of itself and target area be 8 microns, so that the cutting of follow-up ion beam, this technique comprises the conventional meanses such as sliver, cutting or grinding; Step S03 to S06 completes by FIB equipment.
Please continue to refer to Fig. 5, in figure, the inventive method shown in a makes the TEM photo that sample is taken, b is that prior art makes the TEM photo that sample is taken, visible, the target area that the inventive method makes sample is not affected by hole, do not produce curtain effect in target area, good reference value can be provided, improved the reliability of product analysis.
Claims (7)
1. a preparation method for sample for use in transmitted electron microscope, is characterized in that, it comprises the following steps:
Step S01, provides and treats sample preparation device, the selected target area that needs analysis;
Step S02, prepares this at least one cross section for the treatment of sample preparation device and makes it near target area;
Step S03, to the adjacent device surface in Ji Yugai cross section, cross section near this target area, at the correspondence position deposition protective seam of target area;
Step S04, carries out ion beam cutting to two surfaces that deposit protective seam;
Step S05, while carrying out ion beam cutting along the perpendicular direction in arbitrary surface in two surfaces, if find, target area has hole along the top of cut direction, stops the cutting of this direction, carry out ion beam cutting along another perpendicular direction in surface, expose target area;
Step S06, completes the cutting for the treatment of sample preparation device dimensional requirement, makes sample.
2. the preparation method of sample for use in transmitted electron microscope according to claim 1; it is characterized in that: in step S03, at two perpendicular protective seams of device surface deposition of target area correspondence position, in step S04 and S05, cut direction is from the direction to device inside perpendicular to device surface.
3. the preparation method of sample for use in transmitted electron microscope according to claim 2, it is characterized in that: in step S05, once find in cutting process to expose the hole directly over target area, stop immediately the cutting of this direction, to avoid the impact of hole on target area.
4. the preparation method of sample for use in transmitted electron microscope according to claim 3, is characterized in that: step S05 also comprises, has hole if do not find in cutting process directly over target area, continues to carry out this cutting action.
5. according to the preparation method of the sample for use in transmitted electron microscope described in claim 1 to 4 any one, it is characterized in that: in step S02, preparing cross section, to make the distance of itself and target area be 1-10 micron.
6. the preparation method of sample for use in transmitted electron microscope according to claim 5, is characterized in that: the technique of preparing cross section in step S02 comprises sliver, cutting or grinding.
7. according to the preparation method of the sample for use in transmitted electron microscope described in claim 1 to 4 any one, it is characterized in that: step S03 to S06 completes by FIB equipment.
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| CN104697836A (en) * | 2015-03-30 | 2015-06-10 | 上海华力微电子有限公司 | TEM sample preparation method |
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| JPH03202746A (en) * | 1989-12-28 | 1991-09-04 | Nec Corp | Manufacture of sample for transmission electron microscope |
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| CN104155319A (en) * | 2014-07-25 | 2014-11-19 | 胜科纳米（苏州）有限公司 | Method utilizing FIB cutting to achieve stereoscopic observation of nanoscale sample |
| CN105510092A (en) * | 2014-09-22 | 2016-04-20 | 中芯国际集成电路制造(上海)有限公司 | TEM sample preparation method |
| CN105510092B (en) * | 2014-09-22 | 2019-11-01 | 中芯国际集成电路制造(上海)有限公司 | The preparation method of TEM sample |
| CN104697836A (en) * | 2015-03-30 | 2015-06-10 | 上海华力微电子有限公司 | TEM sample preparation method |
| CN105241718A (en) * | 2015-10-13 | 2016-01-13 | 武汉新芯集成电路制造有限公司 | Transmission electron microscope (TEM) sample preparation method |
| CN107976457A (en) * | 2017-11-18 | 2018-05-01 | 武汉钢铁有限公司 | Galvanized sheet overlay coating electron backscatter diffraction sample preparation methods |
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