CN104155158A - Method utilizing FIB cutting to achieve three-dimensional observation of nanoscale sample - Google Patents
Method utilizing FIB cutting to achieve three-dimensional observation of nanoscale sample Download PDFInfo
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- CN104155158A CN104155158A CN201410360305.3A CN201410360305A CN104155158A CN 104155158 A CN104155158 A CN 104155158A CN 201410360305 A CN201410360305 A CN 201410360305A CN 104155158 A CN104155158 A CN 104155158A
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Abstract
The invention discloses a method utilizing FIB cutting to achieve three-dimensional observation of a nanoscale sample. The method comprises the following steps: providing a sample to be observed; cutting the region of interest of the sample to be observed along a first direction to prepare a first TEM sheet sample, thus obtaining the first TEM sheet sample, and carrying out TEM observation from a second direction; cutting the first TEM sheet sample along the second direction to prepare second TEM sheet samples, thus obtaining the second TEM sheet samples, and carrying out TEM observation from the first direction; cutting the second TEM sheet samples along the first direction to prepare third TEM sheet samples, thus obtaining the third TEM sheet samples, and carrying out TEM observation from a third direction, wherein the first direction, the second direction and the third direction are vertical to each other. The method is low in cost, is simple and feasible, is convenient and has high reliability.
Description
Technical field
The present invention relates to but be not limited to semiconductor, hard disk, LED, LCD, alloy, biological field, particularly relating to the three-dimensional observation method that a kind of FIB of utilization in these fields cuts to realize nanometric sample.
Background technology
From 20 end of the centurys, focused ion beam (Focused ion beam, FIB) has been widely used in the preparation of transmission electron microscope (Transmission electron microscopy, TEM) sample.Traditional TEM sample preparation methods comprises hand lapping-pit-ion milling method, FIB H-bar sample preparation methods etc.In recent years, FIB removal (lift out) method has been proved to be in the accurate location for small region of interest ROI and has still reduced all have incomparable advantage aspect sample damage.
The method of utilizing FIB lift out to prepare sample is divided into again in-situ extraction (in-situ lift out) and dystopy is extracted (ex-situ lift out).The difference of these two kinds of methods is after sample attenuate, and ex-situ lift out method is taken out FIB vacuum chamber by sample, utilizes mechanical arm by TEM thin slice sample extraction and be placed on the TEM special purpose copper that carbon film supports online.And in-situ lift out method is to utilize mechanical arm sample directly to be extracted and pasted the TEM special purpose copper online (this kind of copper mesh do not have carbon film to support, and TEM thin slice sample directly sticks on the feet side of copper mesh) of in-situ lift out in FIB vacuum chamber.This species diversity has caused and has adopted sample that ex-situ lift out method prepares can not ether thin, can not carry out secondary attenuate or processing.
For various microns, the method that sub-micron and nano level region of interest ROI are carried out three-dimensional TEM imaging comprises the gradual cutting of FIB, the three-dimensional Tomography technology of TEM etc.Wherein the method for the gradual cutting of FIB is only applicable to micron-sized region of interest ROI, and will realize the three-dimensional observation of sub-micron and nano level region of interest ROI, and the best way is the three-dimensional Tomography technology of TEM at present.But the method for TEM Tomography needs expensive hardware plug and software kit, and needs experience and knowledgeable operator to learn complicated hardware and software operation, extremely labor intensive and financial resources, be difficult for universal.
Summary of the invention
The object of the invention is to, a kind of three-dimensional observation method that provides FIB of utilization to cut to realize nanometric sample, to realize convenient effective three-dimensional observation.
The FIB of utilization provided by the invention cuts to realize the three-dimensional observation method of nanometric sample, comprising:
Testing sample is provided, and described testing sample has defect;
The area-of-interest of described testing sample is carried out to a TEM thin slice sample preparation along first direction cutting, obtain a TEM thin slice sample, and carry out TEM observation from second direction;
A described TEM thin slice sample is carried out to the 2nd TEM thin slice sample preparation along second direction cutting, obtain the 2nd TEM thin slice sample, and carry out TEM observation from first direction;
Described the 2nd TEM thin slice sample is carried out to the 3rd TEM thin slice sample preparation along first direction cutting, obtain the 3rd TEM thin slice sample, and carry out TEM observation from third direction;
Described first direction, second direction and third direction are vertical between two.
Optionally, for the described FIB that utilizes, cut to realize the three-dimensional observation method of nanometric sample, utilize FIB cutting to carry out a TEM thin slice sample preparation, the thickness of a described TEM thin slice sample is more than or equal to the occupied maximum length of described defect.
Optionally, for the described three-dimensional observation method of utilizing FIB to cut to realize nanometric sample, the occupied large 50nm～100nm of maximum length of defect described in the Thickness Ratio of a described TEM thin slice sample.
Optionally, for the described FIB that utilizes, cut to realize the three-dimensional observation method of nanometric sample, a described TEM thin slice sample is prepared for being 0 ° or 90 ° with testing sample upper surface.
Optionally, for the described FIB that utilizes, cut to realize the three-dimensional observation method of nanometric sample, before cutting, first on testing sample surface, form the first protective seam.
Optionally, for the described three-dimensional observation method of utilizing FIB to cut to realize nanometric sample, utilize FIB cutting and the TEM observed result that carries out with reference to first direction carries out the 2nd TEM thin slice sample preparation.
Optionally; for the described FIB that utilizes, cut to realize the three-dimensional observation method of nanometric sample; before cutting; other the making marks of TEM observed result of first utilizing FIB electron beam to carry out at first direction; and forming the second protective seam at a TEM thin slice sample surfaces, the thickness of described the second protective seam is greater than the thickness of the first protective seam.
Optionally, for the described FIB that utilizes, cut to realize the three-dimensional observation method of nanometric sample, the thickness of described the second protective seam is 50nm～500nm.
Optionally, for the described three-dimensional observation method of utilizing FIB to cut to realize nanometric sample, utilize FIB cutting and the TEM observed result that carries out with reference to second direction carries out the 3rd TEM thin slice sample preparation.
Optionally; for the described FIB that utilizes, cut to realize the three-dimensional observation method of nanometric sample; before cutting; other the making marks of TEM observed result of first utilizing FIB electron beam to carry out in second direction; and forming the 3rd protective seam at the 2nd TEM thin slice sample surfaces, the thickness of described the 3rd protective seam is greater than the thickness of the second protective seam.
Optionally, for the described FIB that utilizes, cut to realize the three-dimensional observation method of nanometric sample, utilize FIB in-situ extraction method to carry out the 2nd TEM thin slice sample and the 3rd TEM thin slice sample preparation.
Compared with prior art, the FIB of utilization provided by the invention cuts to realize in the three-dimensional observation method of nanometric sample, through three times, along mutually perpendicular direction, cuts then observation respectively.Compared to existing technology, adopt this method can realize various microns, sub-micron and nano level area-of-interest are realized three-dimensional TEM imaging, so that omnibearing observation and analysis.Compared to the three-dimensional Tomography technology of existing TEM, the method needn't be installed expensive Tomography hardware plug and software kit, also needn't learn complicated hardware and software operation, simple, convenient and reliability is high.
Accompanying drawing explanation
Fig. 1 is that the embodiment of the present invention utilizes FIB to cut to realize the process flow diagram of the three-dimensional observation method of nanometric sample;
Fig. 2～Fig. 8 is that the embodiment of the present invention utilizes FIB to cut to realize the schematic diagram of testing sample in the three-dimensional observation procedure of nanometric sample.
Embodiment
The three-dimensional observation method of the FIB of utilization of the present invention being cut to realize nanometric sample below in conjunction with schematic diagram is described in more detail, the preferred embodiments of the present invention have wherein been represented, should be appreciated that those skilled in the art can revise the present invention described here, and still realize advantageous effects of the present invention.Therefore, following description is appreciated that extensively knowing for those skilled in the art, and not as limitation of the present invention.
For clear, whole features of practical embodiments are not described.They in the following description, are not described in detail known function and structure, because can make the present invention chaotic due to unnecessary details.Will be understood that in the exploitation of any practical embodiments, must make a large amount of implementation details to realize developer's specific objective, for example, according to the restriction of relevant system or relevant business, by an embodiment, change into another embodiment.In addition, will be understood that this development may be complicated and time-consuming, but be only routine work to those skilled in the art.
In the following passage, with reference to accompanying drawing, with way of example, the present invention is more specifically described.According to the following describes and claims, advantages and features of the invention will be clearer.It should be noted that, accompanying drawing all adopts very the form of simplifying and all uses non-ratio accurately, only in order to convenient, the object of the aid illustration embodiment of the present invention lucidly.
Central idea of the present invention is, provides a kind of FIB of utilization to cut to realize the three-dimensional observation method of nanometric sample, comprises the steps:
Step S101: testing sample is provided, and described testing sample has defect;
Step S102: the area-of-interest of described testing sample is carried out to a TEM thin slice sample preparation along first direction cutting, obtain a TEM thin slice sample, and carry out TEM observation from second direction;
Step S103: a described TEM thin slice sample is carried out to the 2nd TEM thin slice sample preparation along second direction cutting, obtain the 2nd TEM thin slice sample, and carry out TEM observation from first direction;
Step S104: described the 2nd TEM thin slice sample is carried out to the 3rd TEM thin slice sample preparation along first direction cutting, obtain the 3rd TEM thin slice sample, and carry out TEM observation from third direction;
Wherein, described first direction, second direction and third direction are vertical between two.
Based on this thought, the invention provides the following FIB that utilizes and cut to realize the three-dimensional observation method of nanometric sample, please refer to Fig. 1, and in conjunction with Fig. 2～Fig. 8, wherein, Fig. 1 is that the embodiment of the present invention utilizes FIB to cut to realize the process flow diagram of the three-dimensional observation method of nanometric sample; Fig. 2～Fig. 8 is that the embodiment of the present invention utilizes FIB to cut to realize the schematic diagram of testing sample in the three-dimensional observation procedure of nanometric sample.This method comprises:
Step S101, provides testing sample.Testing sample 10 as shown in Figure 2, this testing sample 10 can be the accurately microns of location of any needs, the product of sub-micron and nanoscale.For example, a certain hard disc structure has the defect (region at defect place is area-of-interest) that can observe with scanning electron microscope sem on surface, and this hard disc structure can be used as this testing sample.
Step S102, carries out a TEM thin slice sample preparation to the area-of-interest of described testing sample along first direction cutting, obtains a TEM thin slice sample, and carries out TEM observation from second direction.Preferably, in the present embodiment, first utilize FIB at testing sample plated surface one deck the first protective seam, preferred, the material of described the first protective seam can be metal, and for example Pt, can be also nonmetallic materials.Then at rejected region, fix a point to cut, as shown in Figure 3, utilize FIB cutting to carry out the preparation of a TEM thin slice sample 11, a described TEM thin slice sample 11 cuts preparation for being 0 ° or 90 ° with testing sample upper surface.In the present embodiment, employing is 0 ° cuts, on plane yoz, cut, and can be for example to cut at first direction (y direction), obtain a TEM thin slice sample 11,12 of the part testing samples of both sides are removed.Wherein, the scope of the defect that need to observe according to SEM, the thickness of definition the one TEM thin slice sample, the thickness of a described TEM thin slice sample 11 is more than or equal to the occupied maximum length of described defect, to be greater than 50nm～100nm, is advisable.For example this defect occupies the longest distance that approximately has 100nm, and the thickness of a described TEM thin slice sample can be 150nm～200nm, thereby this defect is surrounded completely.Certainly according to the size of different interest regions, this thickness can be adjusted in various degree, sums up, more than the thickness of a described TEM thin slice sample is preferably 100nm through inventor.After cutting completes, a TEM thin slice sample 11 is taken out to FIB vacuum chambers, utilize TEM to carry out imaging to a described TEM thin slice sample 11, i.e. observing along second direction (x direction) as shown in Figure 4.For example in the present embodiment, by TEM, observe and find that nano particle is present on the glass substrate of hard disk, be embedded in SUL layer.The sample preparation that now TEM can be next step to the accurate location of defect provides reference.
Step S103, carries out the 2nd TEM thin slice sample preparation to a described TEM thin slice sample along second direction cutting, obtains the 2nd TEM thin slice sample, and carries out TEM observation from first direction.Please refer to Fig. 5, a TEM thin slice sample is taken out to TEM vacuum chamber, reappose back the vacuum chamber of FIB.Defective locations with reference to the observation of TEM in step S102; utilize the ion beam of FIB to make marks on defect side; in order to guarantee that thin slice sample keeps enough physical strengths, a TEM thin slice sample two sides plate respectively than on the second thicker protective seam of sample preparation once.The thickness of described the second protective seam can be 50nm～500nm, and its material can be identical with the first protective seam.Then on plane xoz, cut, for example, in second direction (x direction) cutting, utilize FIB in-situ extraction method to prepare the 2nd TEM thin slice sample 12, the part of both sides the one 13, TEM thin slice sample is removed.After cutting completes, the 2nd TEM thin slice sample 12 is taken out to FIB vacuum chamber, utilize TEM to carry out imaging.As shown in Figure 6, along first direction (y direction), observe.TEM can present the y direction pattern of defect particles, and the sample preparation that now TEM can be next step to the accurate location of defect provides reference.
Step S104, carries out the 3rd TEM thin slice sample preparation to described the 2nd TEM thin slice sample along first direction cutting, obtains the 3rd TEM thin slice sample, and carries out TEM observation from third direction.Please refer to Fig. 7, the 2nd TEM thin slice sample is taken out to TEM vacuum chamber, reappose back the vacuum chamber of FIB.Defective locations with reference to the observation of TEM in step S103; utilize the ion beam of FIB to make marks on defect side; in order to guarantee that thin slice sample keeps enough physical strengths, the 2nd TEM thin slice sample two sides plate respectively than on the 3rd thicker protective seam of sample preparation once.The material of described the 3rd protective seam can be identical with the first protective seam.Then on plane xoy, cutting, for example, can be to cut at first direction (y direction), utilizes FIB in-situ extraction method to prepare the 3rd TEM thin slice sample 14, and the part of both sides the 2nd 15, TEM thin slice sample is removed.After cutting completes, the 3rd TEM thin slice sample 14 is taken out to FIB vacuum chamber, utilize TEM to carry out imaging.As shown in Figure 8, along third direction (z direction), observe.The nanometer defect that now TEM observes become a protected seam surrounding around three directions of x, y, z nanoscale features point as thin as a wafer all.
Thus, utilize the method that the present invention describes to realize the three-dimensional observation to nanoscale defect, in the above-described embodiments, finally obtained the feature of nanoscale defect.In the above-described embodiments, adopted the preparation of three samples, obvious, on the basis that those skilled in the art disclose at this embodiment of the present invention, can also carry out the preparation of three above samples, this belongs to protection content of the present invention.Compared to existing technology, method of the present invention is simple, convenient and reliability is high.
Through above-mentioned disclosure, when carrying out observing such as the cutting of chip, LED sample, LCD sample, metal sample and biological sample etc., technician is when can directly using method of the present invention, and therefore, the present invention does not give an example one by one at this.
Obviously, those skilled in the art can carry out various changes and modification and not depart from the spirit and scope of the present invention the present invention.Like this, if within of the present invention these are revised and modification belongs to the scope of the claims in the present invention and equivalent technologies thereof, the present invention is also intended to comprise these changes and modification interior.
Claims (11)
1. utilize FIB to cut to realize a three-dimensional observation method for nanometric sample, the method comprises:
Testing sample is provided, and described testing sample has defect;
The area-of-interest of described testing sample is carried out to a TEM thin slice sample preparation along first direction cutting, obtain a TEM thin slice sample, and carry out TEM observation from second direction;
A described TEM thin slice sample is carried out to the 2nd TEM thin slice sample preparation along second direction cutting, obtain the 2nd TEM thin slice sample, and carry out TEM observation from first direction;
Described the 2nd TEM thin slice sample is carried out to the 3rd TEM thin slice sample preparation along first direction cutting, obtain the 3rd TEM thin slice sample, and carry out TEM observation from third direction;
Described first direction, second direction and third direction are vertical between two.
2. the FIB of utilization as claimed in claim 1 cuts to realize the three-dimensional observation method of nanometric sample, it is characterized in that, utilize FIB cutting to carry out a TEM thin slice sample preparation, the thickness of a described TEM thin slice sample is more than or equal to the occupied maximum length of described defect.
3. the FIB of utilization as claimed in claim 2 cuts to realize the three-dimensional observation method of nanometric sample, it is characterized in that, the occupied large 50nm～100nm of maximum length of defect described in the Thickness Ratio of a described TEM thin slice sample.
4. the FIB of utilization as claimed in claim 2 cuts to realize the three-dimensional observation method of nanometric sample, it is characterized in that, a described TEM thin slice sample is prepared for being 0 ° or 90 ° with testing sample upper surface.
5. the FIB of utilization as claimed in claim 2 cuts to realize the three-dimensional observation method of nanometric sample, it is characterized in that, before cutting, first on testing sample surface, forms the first protective seam.
6. the FIB of utilization as claimed in claim 5 cuts to realize the three-dimensional observation method of nanometric sample, it is characterized in that, utilizes FIB cutting and the TEM observed result that carries out with reference to first direction carries out the 2nd TEM thin slice sample preparation.
7. the FIB of utilization as claimed in claim 6 cuts to realize the three-dimensional observation method of nanometric sample; it is characterized in that; before cutting; other the making marks of TEM observed result of first utilizing FIB electron beam to carry out at first direction; and forming the second protective seam at a TEM thin slice sample surfaces, the thickness of described the second protective seam is greater than the thickness of the first protective seam.
8. the FIB of utilization as claimed in claim 7 cuts to realize the three-dimensional observation method of nanometric sample, it is characterized in that, the thickness of described the second protective seam is 50nm～500nm.
9. the FIB of utilization as claimed in claim 8 cuts to realize the three-dimensional observation method of nanometric sample, it is characterized in that, utilizes FIB cutting and the TEM observed result that carries out with reference to second direction carries out the 3rd TEM thin slice sample preparation.
10. the FIB of utilization as claimed in claim 9 cuts to realize the three-dimensional observation method of nanometric sample; it is characterized in that; before cutting; other the making marks of TEM observed result of first utilizing FIB electron beam to carry out in second direction; and forming the 3rd protective seam at the 2nd TEM thin slice sample surfaces, the thickness of described the 3rd protective seam is greater than the thickness of the second protective seam.
11. FIB of utilization as claimed in claim 9 cut to realize the three-dimensional observation method of nanometric sample, it is characterized in that, utilize FIB in-situ extraction method to carry out the 2nd TEM thin slice sample and the 3rd TEM thin slice sample preparation.
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Application publication date: 20141119 |