CN100592065C - Method for implementing backscattering characterization of example interface processed by ion beam - Google Patents
Method for implementing backscattering characterization of example interface processed by ion beam Download PDFInfo
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- CN100592065C CN100592065C CN200610134135A CN200610134135A CN100592065C CN 100592065 C CN100592065 C CN 100592065C CN 200610134135 A CN200610134135 A CN 200610134135A CN 200610134135 A CN200610134135 A CN 200610134135A CN 100592065 C CN100592065 C CN 100592065C
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Abstract
The invention relates to a backscattering characterization method via ion beam machining samples, belonging to the backscattering imaging method utilizing characterization interface systematically made by double beam fragmentation focus ion beam, adopting bi-inclinable filling sampling table to fix characterization samples so as to conduct ion beam preparation characterization interface and enablebackscattering imaging. The sample is fixed in the focus ion beam system and the part which requires preparation characterization is arranged on the lateral side; the samples is calibrated and identified using secondary electron imagingand the upper surface of the sample is focused; the ion beam is turned on to conduct double beam alignment treatment, the ion beam processing position and the electron beam observation position are kept consistent; big beam flux of ion beam is used to preprocess the characterization interface and small beam flux is used to fine process the required characterization interface of the prepared sample; an auxiliary inclinable filling table is rotated to enable the ion beam processing interface to be vertical to incident electron beams and the backscattering detector is started to enable interface characterization of the back scattered electrons. The invention can prepare backscattering characterization samples which can meet the requirement of scanning electron microscope.
Description
Technical field
The invention belongs to the preparation and the imaging technique at sample characterization interface, be specially a kind of method that realizes backscattering characterization with the I.B.M. example interface, thereby it is a method of utilizing the example interface processed realization of two-beam focused ion beam system back scattering imaging, adopts the fixing sample that characterizes of two sample stage of verting to carry out ion beam preparation characterization interface and realize back scattering imaging.
Background technology
Scanning electron microscope (SEM) generally adopts the secondary electron imaging to carry out the material surface microstructure and characterizes, because secondary electron energy low (being lower than 50 electron-volts) has only apart from sample surfaces very near
The top layer secondary electron could the effusion sample surfaces, and detected, amplification and imaging.Be used to detect the detector of secondary electron, the secondary electron that the sample surfaces all directions can be sent all collects, so the secondary electron image of scanning electron microscope has very strong stereoscopic sensation, directly reflects surface appearance feature.And the contained sample message of backscattered electron is made of average element, morphology, crystallization and magnetic property etc., while backscattered electron energy height, sample is charged and damage ratio is less, can obtain the experiment information of 1 μ m, and electron backscattered in recent years technology is widely used in the materials microstructure analysis.At present in scanning electron microscope back scattering imaging sample preparation methods, generally adopt at first mechanical buffing to carry out the method for chemical polishing subsequently, along with science and technology development, specimen method is proposed more and more higher requirement, especially in the backward scattering specimen preparation of a lot of easily oxidations, corrosion and low-durometer material, be difficult to prepare the sample that meets sign, can't realize the back scattering diffraction style.In addition, as sample being placed on the uniclinal turntable that is used to process wafer, may make sample in transfer process, cause damage.
Summary of the invention
The object of the present invention is to provide a kind of method that realizes backscattering characterization with the I.B.M. example interface, two swivel angle plate methods replace being used to process the uniclinal turntable of wafer and utilize focused ion beam processing backscattered electron sign interface in the employing sample chamber, simple, can prepare the backscattering characterization sample that meets the scanning electron microscope demand, avoided the influence of oxidation, corrosion and surface scratch, better reflection needs the sample surfaces feature of analysis.
Technical scheme of the present invention is:
Backward scattering example interface I.B.M. of the present invention and characterizing method adopt focused ion beam system to carry out ion beam preparation characterization interface in conjunction with two sample stage of verting with the fixing sample that characterizes, and then realize back scattering imaging, are mainly finished by following steps:
1, in focused ion beam system, will need the sample that characterizes to adopt carbonaceous conductive glue to be fixed in the sample holder, with the holder of fastening bolt fixed sample on the secondary swivel angle plate of focused ion beam system, prevent to become flexible, keep the satisfactory electrical conductivity between secondary swivel angle plate of focused ion beam system and the sample, need the position of preparation characterization to place to the side;
2, utilize the secondary electron imaging that height of specimen is calibrated identification, the operating distance between sample and the secondary electron detector is adjusted into 4.9～5.1mm, focus on the sample upper surface;
3, vert focused ion beam system master swivel angle plate to spending from the horizontal by 50～54, open ion beam simultaneously, carry out two-beam centering and handle, ion beam pole shoe and sample are 16.3～16.7mm to middle distance, keep the unification of I.B.M. position and secondary electron observation position;
4, adopt the big line of ion beam (＞3nA) preprocessing characterizes the interface, (finishing of 50PA～100PA) the preparation sample that finishes need characterize the interface, and it is bright and clean that factory interface is minute surface, no line pectination vestige to adopt little line, reach the sign requirement, clear Kikuchi lines style in back scattering diffraction, occurs;
5, rotary-focusing ion beam system master swivel angle plate 50～54 degree are got back to the original equilibrium position, need this moment the backscattering characterization interface parallel with electron beam;
6, secondary swivel angle plate 90 degree of rotary-focusing ion beam system, realization I.B.M. interface is vertical with incident beam, enables the backward scattering detector and realizes that the backscattered electron interface characterizes.
Described two sample stage of verting is for turning to the secondary swivel angle plate of identical focused ion beam system by transmission shaft installation and focused ion beam system master swivel angle plate on focused ion beam system master swivel angle plate, the secondary swivel angle plate of focused ion beam system verts by the gear driven transmission shaft.
In the described step 4), big line scope is 3-20nA.
In the described step 1), sample adopts carbonaceous conductive glue to be fixed in the sample holder, uses the holder of fastening bolt fixed sample on the secondary swivel angle plate of focused ion beam system.
In the described step 1), the sample holder is fixed by the pin one end plug-in mounting that is connected with the secondary swivel angle plate of focused ion beam system, fixes with fastening bolt with the pin other end that the secondary swivel angle plate of focused ion beam system is connected.
The present invention adopts the two-beam focused ion beam system, and " two-beam " is meant electron beam+ion beam; In the two-beam focused ion beam system, the effect of ion beam is a processed sample, realizes the bright and clean planarization at the interface of sample characterization gradually; The effect of electron beam is secondary electron imaging and back scattering imaging, keeps vertical with the sample factory interface, selects the backward scattering detector that the sample factory interface is characterized.The ion beam pole shoe is the assembly bottom at electron beam system, can apply electric field, realizes that electronics enters detector.
The invention has the beneficial effects as follows:
1, the present invention utilizes focused ion beam system to carry out the processing of backward scattering example interface in conjunction with two swivel angle plates and characterizes, adopt focused ion beam system processing backscattered electron to characterize the interface, easier imaging under the backscattered electron bundle, the influence and the interference of factors such as the burn into oxidation of minimizing sample and surface scratch are for realizing that high resolution analysis characterizes sample and creates conditions.
2, the present invention can realize that need characterize the position to sample carries out pinpoint, location processing, breaks through the sign that two-dimentional yardstick development realizes micro interface under the material surface.
3, process of the present invention can not produce other feature structures in the unstressed residual and temperature effect of example interface, has improved the accuracy of experimental result.
4, the present invention increases the secondary swivel angle plate of focused ion beam system on original main uniclinal turntable basis, owing to use two swivel angle plates, prevent that effectively sample from causing damage in transfer process, can in two-beam focused ion beam system sample chamber, realize interface processing and sign.
Description of drawings
Fig. 1 is the fixing synoptic diagram of sample in the job operation of the present invention.
Fig. 2 is job operation of the present invention median surface processing synoptic diagram.
Fig. 3 characterizes synoptic diagram for job operation of the present invention median surface.
Description of symbols among the figure:
1-1-side hanging backward scattering detector fixed support, 1-2-side hanging backward scattering detector, 1-3-sample factory interface, 1-4-pin, 1-5-fastening bolt, the 1-6-driving gear set of verting, 1-7-rotary drive motor, 1-8-main swivel angle plate, 1-9-electron beam patterning system, 1-10-ion beam light path system, 1-11-sample holder, 1-12-secondary swivel angle plate, 1-13-sample.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described further.
As Figure 1-3, device of the present invention comprises side hanging backward scattering detector fixed support 1-1, side hanging backward scattering detector 1-2, sample factory interface 1-3, the pin 1-4, the fastening bolt 1-5 that are connected with the secondary swivel angle plate of focused ion beam system, the driving gear set of verting 1-6, rotary drive motor 1-7, focused ion beam system master swivel angle plate 1-8, the 1-9 of electron beam patterning system, ion beam light path system 1-10, sample holder 1-11, focused ion beam system pair swivel angle plate 1-12; Wherein, side hanging backward scattering detector fixed support 1-1, side hanging backward scattering detector 1-2, the 1-9 of electron beam patterning system, ion beam light path system 1-10 are the parts in the existing two-beam focused ion beam system; Different with existing apparatus is, the present invention has adopted two sample stage of verting in the two-beam focused ion beam system, on focused ion beam system master swivel angle plate 1-8, turn to the secondary swivel angle plate 1-12 of identical focused ion beam system with focused ion beam system master swivel angle plate 1-8 by the transmission shaft installation, the secondary swivel angle plate 1-12 of focused ion beam system drives transmission shaft by the driving gear set 1-6 that verts that rotary drive motor 1-7 drives, and secondary swivel angle plate 1-12 is verted.Sample 1-13 is fixed on the sample holder 1-11 by carbonaceous conductive glue, and sample holder 1-11 is inserted on the secondary swivel angle plate 1-12 by pin 1-4, and pin 1-4 fixes by fastening bolt 1-5.
Thereby the two-beam focused ion beam system that utilizes of the present invention is specifically finished by following procedure of processing in conjunction with the two example interface processed realization of swivel angle plate back scattering imaging methods:
At first needs being carried out backscattered electron sign sample 1-13 utilizes the carbonaceous conductive double faced adhesive tape to be fixed on the sample holder 1-11, need the sample factory interface 1-3 that characterizes to be in the side, by pin 1-4 and the fastening bolt 1-5 that is connected with the secondary swivel angle plate of focused ion beam system sample holder 1-11 is fixed on the secondary swivel angle plate 1-12 of focused ion beam system, keeps the satisfactory electrical conductivity (Fig. 1) between the secondary swivel angle plate 1-12 of sample holder 1-11 and focused ion beam system; By the 1-9 of electron beam patterning system height of specimen is discerned, rising focused ion beam system master swivel angle plate 1-8 makes it highly be 5mm; Be rotated counterclockwise main swivel angle plate 1-8 to spending with horizontal direction angle 52, open ion beam light path system 1-10, carry out the centering of 1-9 of electron beam patterning system and ion beam light path system 1-10, keeping the ion beam pole shoe of sample and ion beam light path system 1-10 is 16.5mm (Fig. 2) to middle distance; Adopt the big line of ion beam light path system 1-10 (＞3nA) carry out the preparatory processing of the sample factory interface 1-3 of backscattering characterization, (50～100PA) interface finishing realize the desired planarization of sample factory interface 1-3 of sample characterization gradually to adopt the little line of focused ion beam system 1-10 subsequently; Rotary-focusing ion beam system master swivel angle plate 1-8 is to the original equilibrium position, driving the driving gear set 1-6 that verts by control rotary drive motor 1-7 subsequently revolves the axle of the secondary swivel angle plate 1-12 of focused ion beam system on focused ion beam system master swivel angle plate 1-8 to turn 90 degrees, make electron beam and sample factory interface 1-3 maintenance vertical (Fig. 3); Select backward scattering detector 1-2 that sample factory interface 1-3 is characterized.
Result: adopt the present invention can prepare the sign sample that meets experiment condition, avoid and overcome the influence of oxidation in traditional specimen preparation process, corrosion and surface scratch, realize pinpoint, location back scattering diffraction style analysis, imaging under the backscattered electron bundle, make electronic microscope photos bearing reaction intrinsic structure subsequently, for realizing that high resolution analysis characterizes sample and creates conditions.
Claims (3)
1. method that realizes backscattering characterization with the I.B.M. example interface, it is characterized in that adopting focused ion beam system to carry out ion beam preparation characterization interface with the fixing sample that characterizes in conjunction with two sample stage of verting, and then the realization back scattering imaging, finish by following steps:
1) in focused ion beam system, the sample that needs are characterized is fixed in the sample holder, and the sample holder is installed on the secondary swivel angle plate of focused ion beam system, needs the position of preparation characterization to place to the side;
2) utilize the secondary electron imaging that height of specimen is calibrated identification, the operating distance between sample and the secondary electron detector is adjusted into 4.9～5.1mm, focus on the sample upper surface;
3) vert focused ion beam system master swivel angle plate to from the horizontal by 50～54 degree, open ion beam simultaneously, carry out two-beam centering and handle, ion beam pole shoe and sample are 16.3～16.7mm to middle distance;
4) adopting ion beam is the big line preprocessing sign interface of 3-20nA, and the tuftlet stream finishing of employing 50PA～100PA prepares the sample that finishes and need characterize the interface;
5) rotary-focusing ion beam system master swivel angle plate 50～54 degree are got back to the original equilibrium position, need this moment the backscattering characterization interface parallel with electron beam;
6) secondary swivel angle plate 90 degree of rotary-focusing ion beam system, realization I.B.M. interface is vertical with incident beam, enables the backward scattering detector and realizes that the backscattered electron interface characterizes;
Described two sample stage of verting is for turning to the secondary swivel angle plate of identical focused ion beam system by transmission shaft installation and focused ion beam system master swivel angle plate on focused ion beam system master swivel angle plate, the secondary swivel angle plate of focused ion beam system verts by the gear driven transmission shaft;
Described focused ion beam system is the two-beam focused ion beam system, and the two-beam focused ion beam system provides ion beam and electron beam respectively.
2. the method that realizes backscattering characterization with the I.B.M. example interface according to claim 1, it is characterized in that: in the described step 1), sample adopts carbonaceous conductive glue to be fixed in the sample holder, uses the holder of fastening bolt fixed sample on the secondary swivel angle plate of focused ion beam system.
3. the method that realizes backscattering characterization with the I.B.M. example interface according to claim 1, it is characterized in that: in the described step 1), the sample holder is fixed by the pin one end plug-in mounting that is connected with the secondary swivel angle plate of focused ion beam system, fixes with fastening bolt with the pin other end that the secondary swivel angle plate of focused ion beam system is connected.
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| CN101780630B (en) * | 2009-01-16 | 2012-11-21 | 财团法人工业技术研究院 | Article processing method for focused ion beam system and carrier applied to same |
| CN101988909B (en) * | 2009-08-06 | 2012-03-07 | 中芯国际集成电路制造(上海)有限公司 | Failure analysis method of low k dielectric material |
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| CN102495237B (en) * | 2011-12-14 | 2013-10-30 | 中国科学院苏州纳米技术与纳米仿生研究所 | In-situ processing test device for material interface |
| NL2009696C2 (en) * | 2012-10-25 | 2014-04-29 | Univ Delft Tech | Apparatus and method for inspecting a surface of a sample. |
| CN104122282B (en) * | 2013-04-24 | 2017-01-18 | 泰科英赛科技有限公司 | Circuit tracing using a focused ion beam |
| CN104183453B (en) * | 2014-07-17 | 2016-08-24 | 胜科纳米（苏州）有限公司 | Sample stage and microscopic system |
| CN105067647A (en) * | 2015-07-28 | 2015-11-18 | 江苏省沙钢钢铁研究院有限公司 | Characterization method for spatial form and distribution of compound inclusions in steel |
| CN106449340B (en) * | 2016-08-26 | 2018-06-15 | 深圳市华星光电技术有限公司 | A kind of sample plummer and double-beam system electron microscope |
| CN109632415B (en) * | 2018-12-17 | 2021-04-13 | 攀枝花学院 | Method for improving electrical conductivity of irregular sample |
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| CN111289546B (en) * | 2020-04-02 | 2021-04-13 | 贵研检测科技（云南）有限公司 | Preparation and characterization method of precious metal superfine wire EBSD test sample |
| CN112577982A (en) * | 2020-12-09 | 2021-03-30 | 广州添利电子科技有限公司 | Quality analysis method for PCB surface treatment metal thin layer |
| CN113433149B (en) * | 2021-05-26 | 2022-10-11 | 中国科学院金属研究所 | Method for realizing cross-scale continuous automatic characterization analysis and test of EBSD (electronic brake force sensor) system |
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| EP1204133A2 (en) * | 2000-11-02 | 2002-05-08 | Hitachi, Ltd. | Method and apparatus for processing a micro sample |
| 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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| EP1204133A2 (en) * | 2000-11-02 | 2002-05-08 | Hitachi, Ltd. | Method and apparatus for processing a micro sample |
| 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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