CN110850116B - Method for preparing three-dimensional atom probe sample in turnover mode - Google Patents
Method for preparing three-dimensional atom probe sample in turnover mode Download PDFInfo
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- CN110850116B CN110850116B CN201911087956.9A CN201911087956A CN110850116B CN 110850116 B CN110850116 B CN 110850116B CN 201911087956 A CN201911087956 A CN 201911087956A CN 110850116 B CN110850116 B CN 110850116B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/20—Sample handling devices or methods
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
Abstract
The invention belongs to the field of material preparation, and particularly relates to a method for preparing a three-dimensional atom probe sample in a turnover mode. The method comprises the following steps: marking a region of interest of a planar bulk sample; depositing a rectangular Pt layer on the upper surface of the planar bulk material in a direction perpendicular to the region of interest; extraction of a quadrangular-like bar sample: extracting by adopting an in-situ nanometer operating rod; flip-type quadrangular bar sample: transferring the quasi-quadrangular prism strip sample extracted in the step (3) to a rotating needle tip, overturning the needle tip by adopting an external rotating device, and then transferring the overturned quasi-quadrangular prism strip sample to an in-situ operation nano operating rod; forming a needle tip sample. According to the method, the quadrangular prism-like strip sample is turned for 180 degrees and then sharpened, the preparation of the needle point of the multilayer structure material and the material with the deep distance from the surface of the region of interest is realized, and the prepared needle point sample is beneficial to normal collection in three-dimensional atom probe equipment.
Description
Technical Field
The invention belongs to the field of micro-nano scale material sample preparation, and particularly relates to a turnover type method for preparing a three-dimensional atom probe sample.
Background
A three-dimensional atom probe is a measurement and analysis method with atomic-scale spatial resolution. Based on the principle of field evaporation, the three-dimensional atom probe applies a strong voltage pulse or a laser pulse on a sample to change surface atoms of the sample into ions one by one, then the ions are removed and collected, and finally a complete needle point sample is obtained through software reconstruction. The three-dimensional atom probe has a remarkable effect on element segregation, dislocation components, precipitated phase components, interface components and the like in the analysis material. The research on the distribution of trace elements in materials by using a three-dimensional atom probe technology is a novel method for representing metals and semiconductors in recent years.
In the current method for preparing three-dimensional atom probe samples, the focused ion beam system for preparing three-dimensional atom probe tips is a common fixed-point sample preparation method, and the sample is required to be a tip-shaped sample with the tip diameter of less than 100 nm. However, for the multi-layer structure material and the material with a deeper region of interest, the following problems can exist in the process of preparing and collecting the three-dimensional atom probe sample:
for a probe tip sample of a multi-layer structure material, due to different evaporation fields of different materials, when a three-dimensional atom probe collects multi-layer structure data, if the evaporation direction enters a low evaporation field region from a high evaporation field region, the probe tip is easy to break, so that the experiment fails. In order to improve the success rate of collecting the multilayer structure data, a material with a low evaporation field needs to be arranged at the upper end of the needle tip, and a material with a high evaporation field needs to be arranged at the lower end of the needle tip, so that the three-dimensional atom probe can smoothly collect the multilayer structure data when collecting the multilayer structure material.
For the material with the region of interest deeper from the surface of the sample, the traditional method for preparing the tip sample by using the focused ion beam is only suitable for preparing the sample with the region of interest on the surface or according to the position with the shallower surface, and the method can not prepare the sample with the region of interest deeper from the surface of the sample.
Disclosure of Invention
The invention aims to provide a method for preparing a three-dimensional atom probe sample in a turnover mode.
The technical solution for realizing the purpose of the invention is as follows:
a method for preparing a three-dimensional atom probe sample in a turnover mode, which adopts a focused ion beam system, comprises the following steps:
step 1: marking an interested area of the planar massive sample, wherein the interested area is 1-3 mu m away from the surface of the sample;
step 2: depositing a rectangular Pt layer on the upper surface of the planar bulk material in a direction vertical to the region of interest;
and step 3: extraction of a quadrangular-like bar sample: separating a quadrangular prism strip sample containing the region of interest from the matrix by adopting a focused ion beam, and extracting by adopting an in-situ nanometer control rod;
and 4, step 4: flip-type quadrangular bar sample: transferring the quasi-quadrangular prism strip sample extracted in the step (3) to a rotating needle tip, overturning the needle tip by adopting an external rotating device, and then transferring the overturned quasi-quadrangular prism strip sample to an in-situ operation nano operating rod;
and 5: forming a needle point sample;
step 5-1: transferring the overturned rectangular sample similar to the quadrangular prism to a silicon base;
step 5-2: and circularly cutting the focused ion beam to the interested area to obtain a sample suitable for the three-dimensional atom probe characterization requirement.
Further, in the step 2, the length of the rectangular Pt layer is 20-25 μm, and the width of the rectangular Pt layer is 2-3 μm, so that the region of interest is located under the rectangular Pt layer.
Further, the step 3 of extracting the quasi-quadrangular prism strip sample specifically comprises the following steps:
step 3-1: tilting the sample table to 54 degrees, and etching the left side, the upper side and the lower side of a Pt deposition area by using focused ion beams to form three vertical grooves so as to separate three side surfaces of the long-strip sample from the substrate;
step 3-2: tilting the sample table to 24 degrees, etching the left side, the upper side and the lower side of the strip sample in the step 3-1 by utilizing a focused ion beam, and ensuring that the bottom is completely separated from the substrate to form a cantilever beam type triangular prism-like strip sample;
step 3-3: keeping the inclination angle of the sample table unchanged at 24 degrees, etching the lower long side of the cantilever beam type triangular prism-like long strip sample by utilizing a focused ion beam, rotating the sample table by 180 degrees, and etching the rotated lower long side by adopting the same method to form a cantilever beam type quadrangular prism-like long strip sample;
step 3-4: the in-situ nanometer control rod enters the left side, and the in-situ nanometer control rod is welded with the left side surface of the cantilever beam type quadrangular-like strip sample by utilizing a focused ion beam;
step 3-5: and cutting off the connection part of the cantilever beam type quadrangular-like strip sample and the right side of the substrate by using a focused ion beam, and moving the in-situ nano control lever to extract the quadrangular-like strip sample.
Further, in the step 3-3, it is ensured that the region of interest still exists right below the cantilever-type quadrangular-like strip sample etched by using the focused ion beam.
Further, the step 4 of turning the quasi-quadrangular prism strip sample specifically comprises the following steps:
step 4-1: mounting the rotating needle tip on a rotating table, fixing the rotating table on a sample table, and etching a platform at the tip of the rotating needle tip by using an ion beam for placing a quadrangular prism-like strip sample;
step 4-2: transferring the quadrangular prism-like strip sample to a rotating needle point, and turning the rotating needle point for 180 degrees;
step 4-3: and welding the in-situ nanometer control rod and the left side surface of the quasi-quadrangular prism strip sample by using a focused ion beam, and transferring the quasi-quadrangular prism strip sample on the rotating needle point to the in-situ nanometer control rod again.
Compared with the prior art, the invention has the following remarkable advantages:
(1) according to the invention, the quadrangular prism-like strip sample is turned 180 degrees and then sharpened, so that the preparation of the needle point of the multilayer structure material and the material with a deeper distance from the interested area to the surface is realized, and the time for preparing the sample is saved.
(2) According to the invention, samples at different depth positions can be prepared according to experiment requirements, and irradiation damage of electron beams to the surface of the sample in the experiment process can be effectively avoided by turning 180 degrees, which is beneficial to accurately analyzing element information in the needle point sample.
(3) According to the invention, the material with a low evaporation field is placed at the top end of the needle tip in a turnover mode, so that the success rate of the experiment is greatly improved.
Drawings
FIG. 1 is a schematic view of a large sample block fixed on a loading stage.
FIG. 2 is an electron microscope image of a cantilever beam type triangular prism-like elongated sample.
FIG. 3 is a horizontal schematic view of a process for processing an Izod-like quadrangular bar sample.
FIG. 4 is an electron micrograph of a rectangular bar similar to a quadrangular prism.
Figure 5 is a schematic view of an apparatus for rotating a tip outside a focused ion beam instrument.
FIG. 6 is an electron microscope image of a sample similar to a quadrangular prism after the tip is turned.
FIG. 7 is an electron microscope image of a 2 μm deep finished needle tip.
Wherein, 1-bulk sample surface, 2-sample loading platform, 3-interested depth position, 4-rectangular region upper side, 5-rectangular region left side, 6-rectangular region lower side, 7-class triangular prism strip sample upper side angle, 8-class triangular prism strip sample lower side angle, 9-class quadrangular prism strip sample, 10-sample platform, and 11-needle tip rotation.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Examples
By utilizing the method for preparing the steel sample with the depth of 2 mu m in the irradiation layer, the preparation of the three-dimensional atom probe tip sample in the region of interest at a deeper position can be realized. The traditional focused ion beam preparation atom probe sample can only prepare a tip sample of a region of interest which is close to the surface. However, when a deeper region is prepared, the material is affected by the ion beam for a long time and damages are caused to the material. The method is different from the traditional preparation method of the focused ion beam, and adopts a method of turning 180 degrees to place a deeper region of interest at the top end of the quasi-quadrangular prism, thereby shortening the time of the focused ion beam for processing materials and reducing the damage to the materials.
The following description will be made of a specific example using a focused ion beam dual beam system, taking the three-dimensional atom probe tip sample processing of irradiated steel as an example.
Fixing the massive sample on the sample carrying table by conductive silver adhesive to ensure that the surface 1 of the massive sample is parallel to the plane of the sample carrying table 2, fixing the sample carrying table 2 on the sample table 10, putting the sample carrying table into a focused ion beam dual-beam system, and extracting vacuum.
The sample stage 10 is moved to the electron beam field of view, the sample stage 10 is tilted to 54 degrees, and the sample stage 10 is adjusted to a working distance of 5.1 μm. A rectangular area with the length of 25 μm and the width of 3 μm is selected on the surface of a large sample, and grooves are etched on the upper side 4, the left side 5 and the lower side 6 of the rectangular area by using a focused ion beam vertical to the surface of the sample.
The sample stage 10 is tilted to 24 degrees, and the upper side 4 of the rectangular area is etched by using ion beams; the sample stage is rotated 180 deg., and the underside 6 of the rectangular region is etched with a focused ion beam until the lower portion of the rectangular region is cut through, forming a cantilevered triangular prism-like elongated sample, as shown in fig. 2. By adopting the method shown in FIG. 3, etching the upper side angle 7 region of the triangular prism-like long sample below the center line of the cantilever beam type triangular prism in the ion beam field of view, rotating the sample table by 180 degrees, and etching the lower side angle 8 region of the triangular prism-like long sample by adopting the same steps to obtain the cantilever beam type quadrangular-like long sample 9, wherein the height of the quadrangular-like long sample shown in FIG. 3 is 3-4 μm, and the top angle of the quadrangular prism is smaller than 60 degrees, as shown in FIG. 4.
Calibrating the position of the quadrangular prism-like strip sample 9 under the electron beam and ion beam visual fields to be consistent under the two visual fields, then entering the in-situ nano-joystick, alternately switching the electron beam and ion beam visual fields, and observing the moving state of the in-situ nano-joystick, wherein the in-situ nano-joystick is always kept to be arranged at the left side of the quadrangular prism-like strip sample 9, and the tip of the in-situ nano-joystick is kept horizontal with the quadrangular prism-like strip sample 9. And (3) approaching the in-situ nano joystick to the quasi-quadrangular prism strip sample 9 until the in-situ nano joystick contacts the left side surface of the quasi-quadrangular prism strip sample 9, and then, the image of the ion beam field has contrast of light and shade.
The tip of the in-situ nano operating rod is tightly welded with the surface of the quasi-quadrangular long strip sample by a Pt deposition mode, the deposition area is 3 microns by 2 microns, the thickness is 0.5 microns, and the sufficient connection strength between the quasi-quadrangular long strip sample 9 and the in-situ nano operating rod is ensured.
The right side of the quadrangular prism-like strip sample 9 is cut off from the matrix by the ion beam, and slight jitter of the in-situ nano-joystick can be observed at the moment of disconnection.
Taking the sample platform out of the focused ion beam double-beam system, replacing the rotating needle tip 11, longitudinally and parallelly sticking the rotating needle tip 11 on the sample platform 10, and etching a platform at the top end of the needle tip by using an ion beam as shown in fig. 5 for placing a quadrangular prism-like strip sample 9.
And moving the in-situ nano operating rod to place the quadrangular prism-like strip sample 9 on the platform of the rotating needle point 11, and depositing Pt on two sides of the contacted edge of the quadrangular prism-like strip sample 9 and the rotating needle point 11 to ensure that the quadrangular prism-like sample 9 is tightly combined with the rotating needle point 11 and avoid the sample from falling off. Etching a quasi-quadrangular prism sample which is placed on the rotating needle point 11 by using an ion beam to separate the quasi-quadrangular prism sample from the in-situ nanometer operating rod; the tip was turned by 180 degrees manually outside the focused ion beam microscopy instrument so that the bottom edge of the quadrangular-like bar sample 9 was facing up, as shown in fig. 6.
Rotating the sample table 10 to 24 degrees, entering an in-situ nanometer operating rod, welding the in-situ nanometer operating rod with the left side surface of the quasi-quadrangular long strip sample 9, and etching the right end of the quasi-quadrangular long strip sample 9 by utilizing an ion beam to separate the quasi-quadrangular long strip sample from the rotating needle tip 11. And after taking out the rotating needle point 11, dropping the quadrangular prism-like strip sample 9 on a circular silicon base, welding two sides of the contact position of the quadrangular prism-like strip sample 9 and the silicon base by adopting a Pt deposition method, separating the left side of the quadrangular prism-like strip sample which is firmly adhered to the silicon base from one end of the quadrangular prism-like strip sample, observing that the quadrangular prism-like strip sample is disconnected, moving the nano control rod to the right, and ensuring that the nano control rod cannot touch the silicon base when the micro-tip silicon array is moved.
The above operation was repeated until a four-column-like strip sample was placed on the silicon base of the microtip silicon array in a cross section of 3 μm × 3 μm, and the nanojoystick was withdrawn.
And processing a small block of quadrangular prism-like sample by using a focused ion beam annular etching method until the top end of the needle tip is positioned at the interested depth position 3 to form a sharp point, wherein the diameter of the sharp point is less than 100nm, as shown in figure 7.
Claims (4)
1. The method for preparing the three-dimensional atom probe sample in a turnover mode is characterized in that a focused ion beam system is adopted, and the method comprises the following steps:
step 1: marking an interested area of the planar massive sample, wherein the interested area is 1-3 mu m away from the surface of the sample;
step 2: depositing a rectangular Pt layer on the upper surface of the planar bulk material in a direction perpendicular to the region of interest;
and step 3: extraction of a quadrangular-like bar sample: separating a quadrangular prism strip sample containing the region of interest from the matrix by adopting a focused ion beam, and extracting by adopting an in-situ nanometer control rod;
step 3, extracting a quadrangular prism-like strip sample specifically comprises the following steps:
step 3-1: tilting the sample table to 54 degrees, and etching the left side, the upper side and the lower side of a Pt deposition area by using focused ion beams to form three vertical grooves so as to separate three side surfaces of the long-strip sample from the substrate;
step 3-2: tilting the sample table to 24 degrees, etching the left side, the upper side and the lower side of the strip sample in the step 3-1 by utilizing a focused ion beam, and ensuring that the bottom is completely separated from the substrate to form a cantilever beam type triangular prism-like strip sample;
step 3-3: keeping the inclination angle of the sample table unchanged at 24 degrees, etching the lower long side of the cantilever beam type triangular prism-like long strip sample by utilizing a focused ion beam, rotating the sample table by 180 degrees, and etching the rotated lower long side by adopting the same method to form a cantilever beam type quadrangular prism-like long strip sample; the region of interest still exists at the right lower end of the cantilever-beam-type quadrangular-like strip sample in the step 3-3;
step 3-4: the in-situ nanometer control rod enters the left side, and the in-situ nanometer control rod is welded with the left side surface of the cantilever beam type quadrangular-like strip sample by utilizing a focused ion beam;
step 3-5: cutting off the connection part of the cantilever beam type quadrangular-like strip sample and the right side of the substrate by using a focused ion beam, and moving the in-situ nano control lever to extract the quadrangular-like strip sample;
and 4, step 4: flip-type quadrangular bar sample: transferring the quasi-quadrangular prism strip sample extracted in the step (3) to a rotating needle tip, overturning the needle tip by adopting an external rotating device, and then transferring the overturned quasi-quadrangular prism strip sample to an in-situ operation nano operating rod;
and 5: forming a needle point sample;
step 5-1: transferring the overturned rectangular sample similar to the quadrangular prism to a silicon base;
step 5-2: and circularly cutting the focused ion beam to the interested area to obtain a sample suitable for the three-dimensional atom probe characterization requirement.
2. The method of claim 1, wherein the rectangular Pt layer has a length of 20-25 μm and a width of 2-3 μm, and the region of interest is located directly below the rectangular Pt layer.
3. The method of claim 1, wherein the step 4 of flipping the sample of quadrangular prism-like bars comprises the steps of:
step 4-1: mounting the rotating needle tip on a rotating table, fixing the rotating table on a sample table, and etching a platform at the tip of the rotating needle tip by using an ion beam for placing a quadrangular prism-like strip sample;
step 4-2: transferring the quadrangular prism-like strip sample to a rotating needle point, and turning the rotating needle point for 180 degrees;
step 4-3: and welding the in-situ nanometer control rod and the left side surface of the quasi-quadrangular prism strip sample by using a focused ion beam, and transferring the quasi-quadrangular prism strip sample on the rotating needle point to the in-situ nanometer control rod again.
4. The method as claimed in claim 1, wherein in the step 5-2, the focused ion beam is used to circumscribe the region of interest to obtain a tip sample suitable for the three-dimensional atom probe characterization requirement, and the region of interest should be located at the tip of the tip by 10-100 nm.
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