CN117007625A - Scanning electron microscope testing method for PN junction - Google Patents
Scanning electron microscope testing method for PN junction Download PDFInfo
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- CN117007625A CN117007625A CN202311267424.XA CN202311267424A CN117007625A CN 117007625 A CN117007625 A CN 117007625A CN 202311267424 A CN202311267424 A CN 202311267424A CN 117007625 A CN117007625 A CN 117007625A
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
The invention relates to the technical field of PN junction testing, in particular to a scanning electron microscope testing method of PN junctions, which comprises the steps of mechanically grinding a sample to be tested, grinding by an ion beam grinding instrument and plating a conductive film; the raw materials for preparing the sample to be tested comprise semiconductor materials; when a sample to be tested is tested by using a scanning electron microscope, the acceleration voltage is 3-15 kV; the working distance is 5-15 mm; the adopted condensing lens value is 600-900; the adopted beam current is 30-1000 pA. The method can clearly observe the appearance and junction depth of the PN junction without additionally purchasing other detectors, does not destroy sample components, is environment-friendly, and can save sample measuring time.
Description
Technical Field
The invention relates to the technical field of PN junction testing, in particular to a scanning electron microscope testing method of a PN junction.
Background
Different doping processes are used on two sides of one intrinsic semiconductor, so that a P-type semiconductor is formed on one side, an N-type semiconductor is formed on the other side, a special area called a PN junction is formed at the interface of the two parts, a doped area in the PN junction extends to a depth of 100-200 nm from the surface of the semiconductor, and the doped area is shallower in a modern device. PN junction has unidirectional conductivity, and is the basis of a plurality of semiconductor devices such as diodes, triodes, thyristors and the like, and is the basis of modern electronic technology.
When analyzing PN junction, it is important to observe the morphology and junction depth. The scanning electron microscope is important high-end equipment for microscopic morphology analysis in the scientific research field, is widely applied to various fields such as semiconductors, materials, biology and the like, and plays a vital role in quality monitoring and process diagnosis, device analysis, failure analysis and reliability research in the semiconductor industry. The principle is that the electron gun emits electron beams to focus and then makes raster scanning on the surface of the sample, the composition, the shape and the structure of the surface of the sample are observed and analyzed by detecting signals generated by the electrons acting on the sample, and the incident electrons act on the sample to excite various information, such as secondary electrons, back scattered electrons, absorbed electrons, auger electrons, cathode fluorescence, characteristic X rays and the like. By utilizing the difference generated by the scanning electron microscope electronic signals, different sample contrast, such as morphology contrast, component contrast, potential contrast, orientation contrast and the like, can be distinguished. In a scanning electron microscope, if the electric potentials of different micro areas of the observed surface are different, secondary electrons with lower energy can run from a place with low electric potential to a place with high adjacent electric potential, so that secondary electrons collected by a detector at the place with low original electric potential are reduced, secondary electron images showing contrast due to electric potential difference are obtained, and defects such as dislocation existing in PN junctions can be observed by utilizing the electric potential contrast. But at present, a scanning electron microscope is rarely used for analyzing PN junction depth directly. The method for analyzing the junction depth of the PN junction is commonly selected from a diffusion resistance test, a capacitance-voltage test method, a secondary ion mass spectrometry test, a chemical staining method, an EBIC (electron beam induced current) method and the like. However, the measuring equipment used in the diffusion resistance test, the capacitance voltage method test, the secondary ion mass spectrum test and the EBIC method is expensive, and the sample preparation requirement is generally high, for example, the EBIC method is a method for detecting a semiconductor device by providing a special EBIC detector on a scanning electron microscope. In contrast, the chemical dyeing method can be used for dyeing the polished sample to be detected and then placing the sample under an optical microscope to directly observe the dyed PN junction, and the principle is that the P area and the N area of the PN junction have different reaction rates with the dye, so that the P area and the N area have obviously different color shades, the limit of the PN junction is displayed, the cost is low and the operation is simple, but the method is used for carrying out chemical treatment on the sample to be detected by using a chemical reagent, the components of the sample to be detected are damaged, and the chemical has certain influence on the environment.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects that the method for observing the PN junction morphology and junction depth or the used equipment is expensive, has higher requirements on sample preparation or can damage the sample and pollute the environment in the prior art, thereby providing a scanning electron microscope test method for PN junctions.
Therefore, the invention provides the following technical scheme:
the invention provides a scanning electron microscope testing method of PN junction, the step of preparing sample to be tested includes mechanically grinding the sample to be tested to the position of PN junction, grinding the section to be smooth by ion beam grinding instrument, plating conductive film; the raw materials for preparing the sample to be tested comprise semiconductor materials; when a sample to be tested is tested by using a scanning electron microscope, the acceleration voltage is 3-15 kV; the working distance is 5-15 mm; the adopted condensing lens value is 600-900; the adopted beam current is 30-1000 pA.
Preferably, the acceleration voltage is 3-10 kV.
Preferably, the working distance is 8-12 mm.
Preferably, the adopted condensing lens value is 700-800.
Preferably, the beam current is 200-500 pA.
Optionally, the method for plating the conductive film includes an ion sputtering plating method, and the ion sputtering apparatus used in the ion sputtering plating method includes any one of a direct current sputtering apparatus, an intermediate frequency sputtering apparatus and a radio frequency sputtering apparatus.
Optionally, the target material used in the ion sputtering coating method includes at least one of a gold target, a silver target, a platinum target, a carbon target, a titanium target, a chromium target, a copper target, and a nickel target.
Optionally, the sputtering current is 5-30 mA.
Optionally, the sputtering time is 30-300 s.
Optionally, the ion beam mill comprises any one of a focused argon ion beam mill, a dual ion beam mill, and a tri-ion beam mill.
Optionally, the grinding voltage of the ion beam grinding instrument is 5-10 kV.
Optionally, the ion beam milling current is 0.1 to 1ma.
Optionally, the grinding time of the ion beam grinding instrument is 0.5-5 h.
Preferably, the ion sputtering apparatus used for the ion sputtering coating method includes a direct current sputtering apparatus.
Preferably, the target material used comprises at least one of a gold target and a platinum target.
Preferably, the sputtering current is 10-20 mA.
Preferably, the sputtering time is 60-180 s.
Preferably, the ion beam mill is a three ion beam mill.
Preferably, the grinding voltage of the ion beam grinding instrument is 8-10 kV.
Preferably, the grinding time of the ion beam grinding instrument is 2-5 hours.
Optionally, when mechanically grinding the sample to be measured, including primary grinding and secondary grinding, the grinding tool used comprises sand paper, grinding wheel, grinding head and the like, and can be selected according to actual needs.
Optionally, the number of grinding tools used for one-time grinding is 200-500 meshes.
Optionally, the number of grinding tools used for secondary grinding is 600-1000 meshes.
Preferably, the number of grinding tools used for one grinding is 200 mesh.
Preferably, the number of grinding tools used for the secondary grinding is 800 meshes.
Optionally, before mechanically grinding the sample to be tested, the method further comprises the step of embedding the semiconductor material with an embedding agent to obtain the sample to be tested.
Optionally, the embedding agent comprises at least one of epoxy embedding agent, OCT embedding agent, acrylic resin embedding agent and paraffin embedding agent.
Preferably, the embedding agent comprises at least one of an epoxy resin embedding agent and an acrylic resin embedding agent.
Optionally, a conductive adhesive is used to fix the sample to be tested to the sample stage of the scanning electron microscope before testing.
Optionally, the conductive adhesive includes any one of conductive carbon adhesive tape, conductive copper adhesive tape and silver paste conductive adhesive.
Preferably, the conductive adhesive is silver paste conductive adhesive.
The technical scheme of the invention has the following advantages:
the invention provides a scanning electron microscope testing method of PN junction, comprising the steps of mechanically grinding the sample to be tested to the position of PN junction, grinding the section to be smooth by an ion beam grinder, and plating conductive film; the raw materials for preparing the sample to be tested comprise semiconductor materials; when a sample to be tested is tested by using a scanning electron microscope, the acceleration voltage is 3-15 kV; the working distance is 5-15 mm; the adopted condensing lens value is 600-900; the adopted beam current is 30-1000 pA. The method can clearly observe the appearance and junction depth of the PN junction, does not need to purchase other detectors additionally, does not damage the components and internal structure of the sample, is environment-friendly, and can save the sample measuring time. When the sample to be measured is prepared, a mode of combining mechanical grinding and ion beam grinding is adopted, the sectional grinding reduces the use time, the section of the obtained sample is smooth and flat, mechanical stress is avoided, the components and the internal structure of the sample cannot be damaged, and the PN junction can be observed conveniently. And when the sample to be measured is prepared, the sample is not required to be dyed, the components of the sample are not damaged, the sample is convenient to recycle, and the environment is friendly. The acceleration voltage, working distance, condensing lens value and beam current range used for testing PN junction are definitely specified, the sample testing flow is simplified, and the sample testing time is saved. And the potential difference of the PN junction under the scanning electron microscope is utilized, the secondary electron image potential contrast is directly utilized to observe the PN junction in the sample under proper conditions, other detectors are not required to be additionally purchased, and the test cost is reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is an SEM image of the invention observed in example 1;
FIG. 2 is an SEM image of the invention of example 2;
FIG. 3 is an SEM image of the invention of example 3;
FIG. 4 is an SEM image of comparative example 1 of the present invention;
FIG. 5 is an SEM image of comparative example 2 of the present invention;
FIG. 6 is an SEM image of comparative example 3 of the present invention;
fig. 7 is an SEM image observed in comparative example 4 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made apparent and fully in view of the accompanying drawings, in which some, but not all embodiments of the invention are shown. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Experimental materials and equipment:
and (3) a chip: an experimental processor chip with the size of 1 cm multiplied by 1 cm and the manufacturing process of 22 nm;
epoxy resin: the low-viscosity epoxy king, shanghai Xiya detecting instrument limited company, is XCM4 resin and curing agent which are packaged;
and (3) target material: pt target, available from beijing midkine instruments inc, diameter 57mm;
conductive adhesive: nissan SPI8mm multiplied by 20mm double-sided carbon conductive tape;
ion beam mill: double ion beam mill, model AL-2000, beijing Ai Bozhi ion technology Co., ltd;
ion sputtering instrument: GVC-2000 magnetron ion sputtering instrument, beijing lattice micro-tech Co.
Example 1
The embodiment provides a scanning electron microscope testing method for PN junctions, which comprises the following specific steps:
(1) Preparing a sample to be tested: placing the chip on tinfoil, dripping epoxy resin on the chip by using a dropper until the chip is completely embedded, placing the tinfoil and the chip on a heat table, and preserving heat for 1h at 100 ℃;
taking down the embedded chip after complete solidification, firstly grinding the chip to be close to a target position by using 500-mesh sand paper, and then grinding and polishing the chip to the target position by using 800-mesh sand paper;
setting a grinding voltage of 8kV and a grinding current of 0.4mA by using an AL-2000 ion beam grinding instrument, placing a sample at a proper height, enabling an ion beam to act on the surface of a section of the sample, grinding for 2 hours, and grinding the surface to be flat;
and placing a Pt target by using a GVC-2000 magnetron ion sputtering instrument, setting sputtering current to be 10mA, and sputtering for 120s to finish coating to obtain a sample to be tested.
(2) Test using scanning electron microscopy: the sample to be measured prepared in the step (1) is fixed on a sample stage by using a double-sided carbon conductive adhesive tape, the sample is placed in a scanning electron microscope, the accelerating voltage is adjusted to be 5kV, the condensing lens value is set to be 720, the beam current value is 167 pA at the moment, the XY axis position is moved, the position of a PN junction is found, after the position of the PN junction is found, the focusing is adjusted to be clear, the contrast brightness is adjusted, the image shows different contrast of the PN junction, and the image is acquired to be as shown in the figure 1, and the working distance is 9.5mm at the moment.
Example 2
The comparative example provides a scanning electron microscope test method for PN junction, which is different from the example 1 only in that in the (2), the condensing lens value is adjusted to 900, the beam current value is 30 pA, and the acquisition of fig. 2 is adjusted.
Example 3
The comparative example provides a scanning electron microscope test method for a PN junction, which is different from the example 1 only in that (2) the acceleration voltage is adjusted to 15kV, the beam current value is 232 pA, and the acquisition of fig. 3 is adjusted.
Comparative example 1
The present embodiment provides a scanning electron microscope test method for a PN junction, which is different from embodiment 1 only in that (2) the acceleration voltage is adjusted to 1kV, the condenser value is set to 600, and the beam current value is 57 pA at this time, and fig. 4 is adjusted and collected.
Comparative example 2
The present embodiment provides a scanning electron microscope test method for a PN junction, which is different from embodiment 1 only in that (2) the accelerating voltage is adjusted to 20kV, the condensing lens value is set to 800, and the beam current value is 254 pA at this time, and fig. 5 is adjusted and collected.
Comparative example 3
The present embodiment provides a scanning electron microscope test method for a PN junction, which is different from embodiment 1 only in that (2) the accelerating voltage is adjusted to be 5kV, the condensing lens value is set to be 1300, and the beam current value is 4.1 pA at this time, and fig. 6 is adjusted and collected.
Comparative example 4
The comparative example provides a scanning electron microscope test method for a PN junction, which is different from the embodiment 1 only in that (2) the adjustment detector is a back scattering detector, and fig. 7 is adjusted and collected.
From fig. 1, a rectangular strip with higher brightness than other positions below the chip can be clearly observed, and the contrast, morphology and junction depth of the PN junction of the chip can be clearly observed. The potential contrast of the PN junction can also be observed in FIGS. 2 and 3, but the PN junction contrast is weaker than that of FIG. 1 because the selected parameters are not within the preferred ranges. Looking at fig. 2, it was found that the contrast of the PN junction was observed, but was not obvious as compared with fig. 1, because the condenser value was set too high, the beam spot was small, the beam current value was so small that enough signal electrons were not excited, and the potential difference was small in example 2. The contrast of the PN junction is also less obvious than that of fig. 1 when viewing fig. 3, mainly because the accelerating voltage is larger and the electron beam has a deeper depth of action in example 3, and the doped region of the PN junction is usually extended to a depth of 100-200 nm on the surface, which is usually characterized by using a low accelerating voltage within the range specified in the present invention.
In fig. 4 to 7, no PN junction contrast was observed. In fig. 4, in comparative example 1, the accelerating voltage is too small, and the surface morphology is mainly observed, and the implantation depth of the PN junction is not reached. In fig. 5, in comparative example 2, the acceleration voltage was too large, the depth of action of the electron beam was deep, and the observation depth was too deep. In fig. 6, in comparative example 3, the beam current was small, enough signal electrons were not excited, and the potential difference was small. In fig. 7, comparative example 4, a back scatter detector was used, which collected signals of mainly back scattered electrons, whereas potential contrast observation was mainly based on secondary electron signals, and thus a contrast image of PN junction could not be observed.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (10)
1. A scanning electron microscope testing method of PN junction is characterized in that the step of preparing a sample to be tested comprises the steps of mechanically grinding the sample to be tested, grinding by an ion beam grinding instrument and plating a conductive film;
the raw materials for preparing the sample to be tested comprise semiconductor materials;
when a sample to be tested is tested by using a scanning electron microscope, the acceleration voltage is 3-15 kV;
the working distance is 5-15 mm;
the adopted condensing lens value is 600-900;
the adopted beam current is 30-1000 pA.
2. The method for testing the PN junction of the scanning electron microscope according to claim 1, wherein the acceleration voltage is 3-10 kV;
and/or the working distance is 8-12 mm;
and/or the adopted condensing lens value is 700-800;
and/or the adopted beam current is 200-500 pA.
3. The method for scanning electron microscope testing of PN junction according to claim 1 or 2, wherein the method for plating conductive film comprises ion sputtering coating method, and the target material comprises at least one of gold target, silver target, platinum target, carbon target, titanium target, chromium target, copper target and nickel target;
the sputtering current is 5-30 mA;
sputtering time is 30-300 s;
and/or the ion beam mill comprises any one of a focusing argon ion beam mill, a double ion beam mill and a three ion beam mill;
and/or the grinding voltage of the ion beam grinding instrument is 5-10 kV;
and/or the grinding current of the ion beam grinding instrument is 0.1-1 mA;
and/or the grinding time of the ion beam grinding instrument is 0.5-5 h.
4. The method for scanning electron microscope testing of PN junction according to claim 3, wherein the target material comprises at least one of gold target and platinum target;
and/or sputtering current is 10-20 mA;
and/or sputtering time is 60-180 s;
and/or the ion beam mill is a tri-ion Shu Yanmo mill;
and/or the grinding voltage of the ion beam grinding instrument is 8-10 kV;
and/or the grinding time of the ion beam grinding instrument is 2-5 h.
5. The method for scanning electron microscope testing of PN junction according to claim 1 or 2, wherein the mechanical grinding of the sample to be tested comprises primary grinding and secondary grinding;
the number of grinding tools used for one-time grinding is 200-500 meshes;
the number of grinding tools used for secondary grinding is 600-1000 meshes.
6. The method for scanning electron microscope testing of PN junction according to claim 5, wherein the number of grinding tools used for one grinding is 200 mesh;
and/or, the number of grinding tools used for secondary grinding is 800 meshes.
7. The method for scanning electron microscope testing of PN junction according to claim 1 or 2, characterized by further comprising the step of embedding the semiconductor material with an embedding agent to obtain a sample to be tested before mechanically grinding the sample to be tested;
the embedding agent comprises at least one of an epoxy resin embedding agent, an OCT embedding agent, an acrylic resin embedding agent and a paraffin embedding agent.
8. The method according to claim 7, wherein the embedding medium comprises at least one of epoxy embedding medium and acrylic embedding medium.
9. The method for scanning electron microscope testing of PN junction according to claim 1 or 2, wherein the sample to be tested is fixed on the sample stage of the scanning electron microscope by using conductive adhesive before the test is performed;
the conductive adhesive comprises any one of conductive carbon adhesive tape, conductive copper adhesive tape and silver paste conductive adhesive.
10. The method for scanning electron microscope testing of PN junction according to claim 9, wherein the conductive adhesive is silver paste conductive adhesive.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311267424.XA CN117007625A (en) | 2023-09-28 | 2023-09-28 | Scanning electron microscope testing method for PN junction |
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