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CN100359316C - Preparation of two copper rings gripped transmission samples with ion beam - Google Patents

Preparation of two copper rings gripped transmission samples with ion beam Download PDF

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Publication number
CN100359316C
CN100359316C CNB2005100470864A CN200510047086A CN100359316C CN 100359316 C CN100359316 C CN 100359316C CN B2005100470864 A CNB2005100470864 A CN B2005100470864A CN 200510047086 A CN200510047086 A CN 200510047086A CN 100359316 C CN100359316 C CN 100359316C
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CN
China
Prior art keywords
sample
ion beam
preparation
ring
anchor clamps
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.)
Expired - Fee Related
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CNB2005100470864A
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Chinese (zh)
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CN1920519A (en
Inventor
谭军
张磊
温井龙
谢天生
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Institute of Metal Research of CAS
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Institute of Metal Research of CAS
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Priority to CNB2005100470864A priority Critical patent/CN100359316C/en
Publication of CN1920519A publication Critical patent/CN1920519A/en
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Publication of CN100359316C publication Critical patent/CN100359316C/en
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Abstract

The invention relates to a lens electric microscope sample preparation which uses focused ion beam and two copper rings to clamp, wherein one end of two copper rings for clamping sample is vertically fixed on the clamper, while another end is processed into one arc open at 145-160degrees; the preformed sample is parallel fixed on the arc open, to make the sample parallel with clamper fixing table; and it uses tow beams of focused ion beams to accurately position the thin sample, and vertically remove from two sides, until needed watch thickness of the electric microscope; then taking off two copper rings from the sample clamper, folding the low ring, and fixing processed electric microscope sample, to be watched. The invention uses two-ring groove method to replace sample indoor extraction and sample outdoor static adsorption, with simple method, high resolution, and better sample characteristic structure, without pollution and impact.

Description

A kind of preparation of transmission samples with the preparation of two copper rings with ion beam clamping
Technical field
The invention belongs to sample for use in transmitted electron microscope method for processing in the focused ion beam system, be specially and adopt the fixedly sample for use in transmitted electron microscope preparation method of double copper ring of separate type sample holder.
Background technology
At present, use in semiconductor factory at home and abroad and the research institution in the focused ion beam system processing sample for use in transmitted electron microscope method, generally adopt two kinds of methods of Electrostatic Absorption taking-up outside the sample chamber processes inner original position proposition method and sample chamber, but along with current science and technology development, crudy to transmission sample proposes more and more higher requirement, requires to prepare the sample that finishes simultaneously and avoids extraneous contamination and bump.Present like this two kinds of methods that generally adopt can not well satisfy the requirement of high-accuracy scientific research and semiconductor failure analysis, the sample chamber processes inner original position proposition method in shifting the sample process, to between sample and control needle point, deposit platinum or tungsten as connecting material, inevitable like this at sample surfaces deposition one layer of polymeric, and the collision of contact point and sample will appear in taking-up outside the sample chamber, cause other with external structure and defective, making subsequently, the electronic microscope photos result can not react the intrinsic structure.
Summary of the invention
The object of the present invention is to provide a kind of preparation of transmission samples with the preparation of two copper rings with ion beam clamping, the method that Electrostatic Absorption is taken out outside taking-up and the sample chamber in the employing dicyclo ditch channel process replacement sample chamber, simple, can prepare the sample that meets the high-resolution-ration transmission electric-lens demand, avoided polluting and collision the sample intrinsic structure of reaction needed analysis preferably.
Technical scheme of the present invention is:
A kind of preparation of transmission samples with the preparation of two copper rings with ion beam clamping, finish by following steps:
1) on the special-purpose double copper ring of transmission electron microscope ring to open one be the fan-shaped openings of 145~160 degree, and the thin district of need processing of sample is milled to 30~50 microns of thickness in advance, utilize conducting resinl that prefabricated sample both ends horizontal is fixed on fan-shaped opening both sides, keep processed sample parallel, need the position of preparation characterization to make progress with the anchor clamps fixed station;
2) be fixed with need the thin district of processing double copper ring down ring utilize fastening bolt to be vertically fixed on the anchor clamps fixed station, make simultaneously on the double copper ring that environmental protection is held in same plane under the ring and double copper ring;
3) adopt the two-beam focused ion beam that the thin district of required processed sample is accurately located, vertically peel off from both sides, the preparation groove keeps the intermediate features district simultaneously, reaches the transmission electron microscope observing needs until thickness.
The present invention has the pin that is connected with the focused ion beam system sample stage below the anchor clamps fixed station.
Described step 3) adds man-hour with focused ion beam, and the anchor clamps fixed station that verts makes sample both sides machined surface corresponding at a certain angle ion beam respectively, and by adjusting tilt angle, thickness is even up and down to make thin district.
During with one side, the thin district of focused ion beam processing, the anchor clamps fixed station that verts, making the plane at double copper ring place and the angle of surface level is 52.5~53.5 °; During with focused ion beam processing Bao Qu another side, the anchor clamps fixed station that verts, making the plane at double copper ring place and the angle of surface level is 50.5~51.5 °.
After the described step 3), take off double copper ring from the anchor clamps fixed station, folding double copper ring is ring down, and folding ring down and the fixing sample for use in transmitted electron microscope of completion of processing of last ring use in order to observing.
The invention has the beneficial effects as follows:
1, the present invention adopts the small sample of pre-grinding to be fixed on the copper ring, and easier imaging under electron beam reduces factor affecting such as sample and sample stage conducting and material self be non-conductive, creates conditions for preparing the high-resolution sample.
2, the present invention can reduce pollution that thin district caused and the interference to being processed in the process of taking out sample in the sample chamber.
3, process n.s. bump of the present invention can not produce other feature structures, has improved the accuracy of experimental result.
4, because double copper ring fixing, the present invention can effectively prevent processed sample shift and the transmission electron microscope observing process in come off.
Description of drawings
Fig. 1 is the fixing synoptic diagram of sample in the job operation of the present invention.
Fig. 2 is the side view of Fig. 1.
Fig. 3 is sample processing synoptic diagram in the job operation of the present invention.
Description of symbols among the figure:
1-1-sample encircles on 1-2-double copper ring, and 1-3-double copper ring is ring down, 1-4-fastening bolt, 1-5-anchor clamps binding, 1-6-anchor clamps fixed station, 1-7-thin district, 1-8-pin; 2-ion beam.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described further.
As Figure 1-3, the dicyclo ditch channel process of focused ion beam system sample for use in transmitted electron microscope processing of the present invention, specifically finish: at first on the special-purpose double copper ring of transmission electron microscope, process about 150 degree openings among the ring 1-2 by following procedure of processing, the planarization that will keep copper ring simultaneously, the required processed sample 1-1 that is milled to thickness 30-50 micron in advance is fixed to the both sides of encircling on the opening double copper ring, keep sample and double copper ring not to be distorted, make to process thin district 1-7 upwards with add the man-hour ion beam direction and 2 be consistent; Then the following ring 1-3 in the double copper ring is fixed between anchor clamps binding 1-5 and the anchor clamps fixed station 1-6, use fastening bolt 1-4 to fix, the separate type sample holder of forming by anchor clamps binding 1-5 and anchor clamps fixed station 1-6 keeps the stable of double copper ring, guarantee that sample is to anchor clamps fixed station 1-6 circuit turn-on, note simultaneously required processed sample 1-1 upper surface is tried one's best and anchor clamps fixed station 1-6 keeping parallelism, keep the electric conductivity between sample and the focused ion beam system sample stage simultaneously; Adopt focused ion beam system intermediate ion bundle 2 to peel off subsequently in the both sides, 1-7 position, thin district of required processed sample 1-1, reduce thin district 1-7 thickness gradually, in processing thin district 1-7 process, to successively change the inclination angle of anchor clamps fixed station, so that eliminate the thin district 1-7 phenomenon in uneven thickness up and down of processing, until reaching the required thickness of transmission electron microscope observing; From taking off ring 1-3 under the double copper ring between anchor clamps binding 1-5 and the anchor clamps fixed station 1-6, fold ring 1-3 down at last, overlapping with ring 1-2 on the double copper ring, fixing required processed sample 1-1 prepares against transmission electron microscope observing, utilizes fixedly completion of processing sample of complete copper ring down.
During with 1-7 one side, the thin district of focused ion beam processing, the anchor clamps fixed station that verts, making the plane at double copper ring place and the angle of surface level is 52.5~53.5 °; During with 1-7 another side, the thin district of focused ion beam processing, the anchor clamps fixed station that verts, making the plane at double copper ring place and the angle of surface level is 50.5~51.5 °.

Claims (5)

1. preparation of transmission samples with the preparation of two copper rings with ion beam clamping is characterized in that being finished by following steps:
1) on the special-purpose double copper ring of transmission electron microscope ring (1-2) to open one be the fan-shaped openings of 145~160 degree, and the thin district of need processing of sample (1-1) is milled to 30~50 microns of thickness in advance, utilize conducting resinl that prefabricated sample both ends horizontal is fixed on fan-shaped opening both sides, keep processed sample parallel, need the position of preparation characterization to make progress with the anchor clamps fixed station;
2) be fixed with need the thin district of processing (1-7) double copper ring down ring (1-3) utilize fastening bolt (1-4) to be vertically fixed on the anchor clamps fixed station (1-6), make simultaneously that ring (1-2) and double copper ring encircle (1-3) down on the double copper ring to remain on same plane;
3) adopt the two-beam focused ion beam that the thin district (1-7) of required processed sample (1-1) is accurately located, vertically peel off from both sides, the preparation groove keeps the intermediate features district simultaneously, reaches the transmission electron microscope observing needs until thickness.
2. according to the described preparation of transmission samples of claim 1, it is characterized in that: the pin (1-8) that is connected with the focused ion beam system sample stage is arranged in anchor clamps fixed station (1-6) below with the preparation of two copper rings with ion beam clamping.
3. according to the described preparation of transmission samples of claim 1 with the preparation of two copper rings with ion beam clamping, it is characterized in that: described step 3) adds man-hour with focused ion beam, the anchor clamps fixed station verts, make sample both sides machined surface corresponding at a certain angle ion beam respectively, by adjusting tilt angle, thickness is even up and down to make thin district (1-7).
4. according to the described preparation of transmission samples of claim 3 with the preparation of two copper rings with ion beam clamping, it is characterized in that: during with (1-7) side, the thin district of focused ion beam processing, the anchor clamps fixed station that verts, making the plane at double copper ring place and the angle of surface level is 52.5~53.5 °; During with (1-7) another side, the thin district of focused ion beam processing, the anchor clamps fixed station that verts, making the plane at double copper ring place and the angle of surface level is 50.5~51.5 °.
5. according to the described preparation of transmission samples of claim 1 with the preparation of two copper rings with ion beam clamping, it is characterized in that: after the described step 3), take off double copper ring from the anchor clamps fixed station, folding double copper ring is ring down, folding ring down and the fixing sample for use in transmitted electron microscope of completion of processing of last ring use in order to observing.
CNB2005100470864A 2005-08-24 2005-08-24 Preparation of two copper rings gripped transmission samples with ion beam Expired - Fee Related CN100359316C (en)

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CN100359316C true CN100359316C (en) 2008-01-02

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Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102466578B (en) * 2010-11-03 2013-12-04 中芯国际集成电路制造(上海)有限公司 Preparation method of transmission electron microscope (TEM) sample
CN102519771B (en) * 2011-12-30 2013-09-18 青岛大学 Method for preparing cross section transmission electron microscope sample
CN106525532B (en) * 2016-11-07 2019-09-20 上海达是能源技术有限公司 A kind of preparation method of transmission electron microscope sample
CN108089067A (en) * 2016-11-23 2018-05-29 中国科学院大连化学物理研究所 A kind of Electrostatic collection method for ionic migration spectrometer
CN107664593B (en) * 2017-08-03 2019-10-15 浙江大学 A method of preparing transmission electron microscope original position stretching sample
CN107703170B (en) * 2017-08-22 2020-05-12 青岛大学 Preparation method of electrostatic spinning fiber transmission electron microscope sample
CN109270100B (en) * 2018-11-30 2024-04-19 复旦大学 Transmission electron microscope in-situ electrical test chip for focused ion beam sample preparation process
CN111474197A (en) * 2020-04-16 2020-07-31 宸鸿科技(厦门)有限公司 Method for controlling contamination resulting from transmission electron microscope sample preparation

Citations (6)

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Publication number Priority date Publication date Assignee Title
CN1083591A (en) * 1992-09-03 1994-03-09 中国科学院金属研究所 The preparation method of metal powder film for transmission electron microscope
US5990478A (en) * 1997-07-10 1999-11-23 Taiwan Semiconductor Manufacturing Co. Ltd. Method for preparing thin specimens consisting of domains of different materials
JPH11329325A (en) * 1998-05-12 1999-11-30 Canon Inc Manufacture of mesh and thin piece of sample
US6683304B1 (en) * 2002-07-08 2004-01-27 Chartered Semiconductor Manufacturing Limited Method for a plan-view transmission electron microscopy sample preparation technique for via and contact characterization
CN1641067A (en) * 2004-01-09 2005-07-20 中国科学院金属研究所 Method for preparing film sample for transmission electron microscope
US6927174B2 (en) * 2003-08-12 2005-08-09 Texas Instruments Incorporated Site-specific method for large area uniform thickness plan view transmission electron microscopy sample preparation

Patent Citations (6)

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Publication number Priority date Publication date Assignee Title
CN1083591A (en) * 1992-09-03 1994-03-09 中国科学院金属研究所 The preparation method of metal powder film for transmission electron microscope
US5990478A (en) * 1997-07-10 1999-11-23 Taiwan Semiconductor Manufacturing Co. Ltd. Method for preparing thin specimens consisting of domains of different materials
JPH11329325A (en) * 1998-05-12 1999-11-30 Canon Inc Manufacture of mesh and thin piece of sample
US6683304B1 (en) * 2002-07-08 2004-01-27 Chartered Semiconductor Manufacturing Limited Method for a plan-view transmission electron microscopy sample preparation technique for via and contact characterization
US6927174B2 (en) * 2003-08-12 2005-08-09 Texas Instruments Incorporated Site-specific method for large area uniform thickness plan view transmission electron microscopy sample preparation
CN1641067A (en) * 2004-01-09 2005-07-20 中国科学院金属研究所 Method for preparing film sample for transmission electron microscope

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Title
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