CN220121775U - Multifunctional ion source device for nanoscale analysis of material surface - Google Patents
Multifunctional ion source device for nanoscale analysis of material surface Download PDFInfo
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- CN220121775U CN220121775U CN202223245803.2U CN202223245803U CN220121775U CN 220121775 U CN220121775 U CN 220121775U CN 202223245803 U CN202223245803 U CN 202223245803U CN 220121775 U CN220121775 U CN 220121775U
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- 238000004458 analytical method Methods 0.000 title claims abstract description 41
- 239000000463 material Substances 0.000 title claims abstract description 31
- 238000012360 testing method Methods 0.000 claims abstract description 29
- 238000001819 mass spectrum Methods 0.000 claims abstract description 10
- 229910001417 caesium ion Inorganic materials 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 5
- 239000004065 semiconductor Substances 0.000 abstract description 4
- 239000002114 nanocomposite Substances 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 description 62
- 238000010884 ion-beam technique Methods 0.000 description 34
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- 230000008901 benefit Effects 0.000 description 6
- 150000001450 anions Chemical class 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
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- 238000012827 research and development Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
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- 238000004544 sputter deposition Methods 0.000 description 4
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- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 238000001004 secondary ion mass spectrometry Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
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- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
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- 238000004969 ion scattering spectroscopy Methods 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
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- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The utility model belongs to the technical field of material surface detection, and discloses a multifunctional ion source device for nano-scale analysis of material surfaces, wherein a test bed is fixed in an ultrahigh vacuum cavity, and an ion source is fixed in the test bedThe device, mass spectrum analyzer and adjusting device, ion source generating device and mass spectrum analyzer pass through adjusting device to be fixed in the test bench upper end, and mass spectrum analyzer fixes directly over the test bench, is fixed with the sample in the middle of the test bench. The ion source generating device is provided with a penning gas ion source generator and Cs + The penning gas ion source generator is fixed on the right side of the sample, the structure is simple, the effect is obvious, and the depth profile analysis of the semiconductor ultra-shallow P-N junction and the nano composite multilayer structure film can be realized through the ion source generating device.
Description
Technical Field
The utility model belongs to the technical field of material surface detection, and particularly relates to a multifunctional ion source device for nano-scale analysis of a material surface.
Background
At present, the material surface detection means adopts low-energy ion beam analysis technology to perform nano-scale characterization analysis on the material surface, a main device is focused on a core device-ion source for generating ion beams in secondary ion mass spectrometry (secondary ion mass spectroscopy, SIMS), and a main stream metal steam ion source is a thermal evaporation type or sputtering type alkali metal ion source, such as Cs + An ion source. Most of the gas ion sources are penning ion sources, and can generate relatively stable inert gas Ar + ，Ne + Ion beam and reactive gas O 2 + Ion beam, and the like. Combining the two ion sources to extract Cs in the 10keV energy range + ，Ar + The plasma beam bombards the surface layer of the material to a depth of a few nanometers to hundreds of nanometers, and visual analysis is provided for the information such as elements, content, depth distribution and the like on the surface of the material.
However, due to failure of moore's law in the semiconductor industry, ultra-shallow layer injection or component analysis of the material surface faces great challenges, the existing single ion beam probe technology adopted for element screening and quantitative analysis of the material surface is immature, the detection range from the material surface to a certain depth is not wide under the condition of limited incident energy, and wide-range ion probe detection is difficult to realize.
Through the above analysis, the problems and defects existing in the prior art are as follows: the existing single-particle probe technology is immature in element screening and quantitative analysis on the surface of a material, has a narrow detection range from the surface of the material to a certain depth under the condition of limited incident energy, and is difficult to realize wide-range ion beam probe detection.
Disclosure of Invention
Aiming at the problems existing in the prior art, the utility model provides a multifunctional ion source device for nano-scale analysis of the surface of a material.
The utility model is realized in that a multifunctional ion source device for nanometer-scale analysis of the surface of a material is provided with: the test bed, the ion beam leading-out terminal, the mass/energy analysis spectrometer probe and the like are all positioned in a high vacuum cavity made of 304 stainless steel, the vacuum cavity is a three-way T-shaped structural cavity, the lowest end of the vacuum cavity is connected with an ultrahigh vacuum unit system, one end of the vacuum cavity is connected with a cabin door for placing a sample, and the other end of the vacuum cavity is connected with parts such as an external lead of the test bed capable of realizing front-back left-right two-dimensional movement. 5 windows are respectively arranged at different positions on the cylindrical cavity wall, and 4 windows are respectively used for fixing an ion beam extraction end and Cs of the penning gas ion generator + The device comprises an ion beam outlet end of an ion generator, an ion beam outlet end of a gas cluster ion source generator and a mass/energy analysis spectrometer probe, wherein quartz glass is installed at 1 window to be used as an observation window, a stainless steel baffle is added at one side of the quartz glass positioned in a vacuum cavity, and the baffle realizes the protection of the inner side of the quartz glass and the observation of the outer part through a plectrum outside the cavity. The test bed is fixed in the ultrahigh vacuum cavity, is a metal platform which can realize front-back and left-right movement through the control of the stepping motor, and the stepping motor electrical lead wire, the electrode and the sealing material which are connected from one section of the cavity are necessarily vacuum materials which can be suitable for high vacuum environment.
The three ion source devices are all independent devices, and the generated ion beams are respectively introduced into the 3 windows of the ultrahigh vacuum chamber through the suction electrode (accelerating electrode), and the ionized gas ion beams and Cs generated by the ion beam terminal + The ion beam and the gas cluster ion beam can independently perform irradiation tests on different positions of a sample placed on a metal platform of a test stand.
The three ion sources share one set of externally independent adjustable direct current high voltage power supply with the voltage adjusting range of 0-20 kV. The charged ion beam after the accelerating electric field enters the drift tube after passing through the distance of 10-20 mm, is focused by the electric quadrupole lens, is controlled by a graphite diaphragm with a central round hole of 1mm, the opening of the central hole is controlled by a poking piece outside the cavity, when the graphite diaphragm is not opened, a vacuum electric lead on the graphite diaphragm is connected with a beam integrator outside the cavity, the intensity of the ion beam striking the center of the graphite diaphragm can be monitored, the voltage of X, Y direction of the electric quadrupole lens power supply is regulated, the path envelope of the ion beam can be changed, when the beam intensity is large enough, the diaphragm hole is opened by an external poking piece, and the focused ion beam passes through the hole to bombard a sample on the metal platform. The three ion sources may share an external independent set of electro-quadrupole lens systems. When an ion beam generated by an ion source is used for analyzing a sample, the energy of the ion beam can be controlled by adjusting the voltage output by a direct-current high-voltage power supply, and the collimation and the flow intensity of the ion beam are controlled by an electric quadrupole lens system.
The probe of the mass/energy analysis spectrometer is connected through a No. 4 window of the ultrahigh vacuum cavity, and the position of the probe is fixed right above the test bed. The device may be used directly with the product Hiden EQS1000Mass Energy Analyser from Hiden Analytical, UK.
In combination with the technical scheme and the technical problems to be solved, the technical scheme to be protected has the following advantages and positive effects:
first, aiming at the technical problems in the prior art and the difficulty in solving the problems, the technical problems solved by the technical proposal of the utility model are analyzed in detail and deeply by tightly combining the technical proposal to be protected, the results and data in the research and development process, and the like, and some technical effects brought after the problems are solved have creative technical effects. The specific description is as follows:
the embodiment of the utility model is fixed in a T-shaped ultrahigh vacuum cavity by a test bed, the two ends of the cavity are respectively connected with an electric lead of a stepping motor and a cabin door for placing a sample, and 4 windows on the cavity wall are respectively fixed with an ion beam leading-out terminal generated by an ion sourceThe end, a mass/energy analysis spectrometer probe and 1 window are connected with quartz glass in a vacuum static seal mode to form a test observation window, the mass spectrometer is fixed right above a test bed, a cluster ion beam generator is positioned at the left end of the test bed, and a gas penning source generator and Cs + The ion source generator is positioned at the right end of the test section, and a sample is fixed in the middle of the test bed. The method can realize element screening and quantitative analysis of the outermost surface layer of the material, and can realize SIMS element tracing and imaging analysis of a high-sensitivity complex inorganic and organic (including biological sample) mixed system.
Secondly, the technical scheme is regarded as a whole or from the perspective of products, and the technical scheme to be protected has the following technical effects and advantages:
the embodiment of the utility model has compact structure and obvious effect, and can realize the depth profile analysis of the semiconductor ultra-shallow P-N junction and the nano composite multilayer structure film through the ion source generating device.
Thirdly, as inventive supplementary evidence of the claims of the present utility model, the following important aspects are also presented:
(1) The expected benefits and commercial values after the technical scheme of the utility model is converted are as follows:
at present, domestic SIMS devices generally depend on import, and most of related material surface scientific analysis and research are very unfavorable to advanced high-end manufacturing industries in the field of surface analysis scientific instruments in China by means of import devices. The utility model combines the respective structure and performance characteristics of the surface ionization ion source, the gas penning discharge ion source and the cluster ion source device, respectively integrates the ion beam extraction terminals thereof into an ultrahigh vacuum cavity with an adjustable metal sample stage fixed in the middle, and realizes the technologies of deep profile analysis, element distribution imaging and the like of the sample. Provides direct reference value for the commercialized research and development of the domestic material surface science analysis device.
(2) The technical scheme of the utility model fills the technical blank in the domestic and foreign industries:
the domestic SIMS device has some corresponding products in the aspects of surface ion sources and gas penning discharge sources, but has extremely low market share. The gas cluster ion source device is integrated on the two source devices to form the multifunctional ion source device, so that not only can new innovation points be brought to the research and development of the SIMS device, but also the functional research and development of the ion source generator on the ion accelerator device can be brought.
Drawings
FIG. 1 is a schematic diagram of a multifunctional ion source device for nanoscale analysis of a material surface according to an embodiment of the present utility model;
FIG. 2 is a schematic diagram of Ar of 2keV generated by a penning gas discharge source according to an embodiment of the present utility model + Ion scattering mass/energy spectrum of the intensity ion beam bombarding La crystal;
FIG. 3 is a schematic illustration of Ar-cluster ion beams and Cs of different energies provided by an embodiment of the present utility model + Ion beam bombardment of the PAA/PET schematic;
in the figure: 1. a sample; 2. an ultra-high vacuum chamber; 3. penning gas ion source generator; 4. cs (cells) + An ion source generator; 5. mass/energy analysis spectrometer; 6. a gas cluster ion source generator.
Detailed Description
The present utility model will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present utility model more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the utility model.
In order to fully understand how the utility model may be embodied by those skilled in the art, this section is an illustrative embodiment in which the claims are presented for purposes of illustration.
As shown in fig. 1, a multifunctional ion source device for nanoscale analysis of a material surface according to an embodiment of the present utility model includes: sample 1, ultra-high vacuum chamber 2, penning gas ion source generator 3, cs + An ion source generator 4, a mass/energy analysis spectrometer 5, a gas cluster ion source generator 6.
The test bed is fixed in the ultrahigh vacuum cavity 2, an ion source generating device, a mass spectrum analyzer and a regulating device are fixed in the test bed, the ion source generating device and the mass spectrum analyzer are fixed at the upper end of the test bed through the regulating device, the mass spectrum analyzer is fixed right above the test bed, and a sample 1 is fixed in the middle of the test bed.
The ion source generating device is provided with a penning gas ion source generator 3 and Cs + An ion source generator 4 and a gas cluster ion source generator 6, the gas cluster ion source generator 6 is fixed on the left side of the sample 1, and the penning gas ion source generator 3 is fixed on the right side of the sample 1.
The ultra-high vacuum chamber 2 is fixed in the ion source device.
Penning gas ion source generator 3 and Cs in ion source generating device + The rear ends of the ion source generator 4 and the gas cluster ion source generator 6 are connected with a suction power supply capable of adjusting direct current voltage.
The mass spectrometer is in particular a mass/energy analysis spectrometer 5.
The utility model, when in operation, has a vacuum degree of more than 10 -8 In the ultra-high vacuum chamber of Pa, cs is + The ion source, the penning gas ion source and the gas cluster ion source are arranged at fixed positions at proper angles, so that the aim of respectively leading out ion beams from the single ion source to bombard a sample for surface analysis can be fulfilled. The three ion sources can share one set of suction electrode power supply (0-20 kV) with adjustable direct-current voltage, can meet the characterization analysis of the depth of a sample surface from sub-nanometer to hundreds of nanometers, and the atomic yield generated by sputtering is detected by a mass/energy analysis spectrometer.
FIG. 2 is an Ar of 2keV + Ion bombardment of lanthanum (La) crystals forms low energy ion mass spectra. In FIG. 2, the ion kinetic energy is 50eV peak position, which is the case for sputtering 155 (LaO) + (superposition) 139 La + ) The intensity peak of the ion indicates that lanthanum oxide exists on the surface of La crystal; incident Ar + The ion kinetic energy is at about 770eV, corresponding to incident Ar + The ion beam bombards La sample and back scatters Ar which is received by mass spectrometer + Intensity peaks. FIG. 2 is a graph of almost all of the data analyzed while considering mass/energy resolutionThe ion signal peaks that occur are identified as such, 155 (LaO) + and 16 O + the peak indicates that La crystal has an oxide layer on the surface, and further, ar scattered not only at 770eV of the incident beam energy + Intensity peak, also at 385eV, appears weaker Ar 2+ Ion intensity peak.
As shown in FIG. 3, low energy Ar with different energies is used 2500 + Cluster ion beam and Cs + The ion beam is used for carrying out depth profile analysis on the surface of the PAA/PET composite film. Can accurately discriminate anions C generated by sputtering and coming from PAA layer 3 H 3 O 2 - (mass to charge ratio 71) and C 9 H 11 O 6 - (mass to charge ratio 215) and anions C from the PET layer 10 H 7 O 4 - Yield (mass to charge ratio 191). Whichever of the incident ion beams, the resulting PAA film thickness was about 50nm. With Ar of 5keV 2500 + The high mass anion yield ratio in the composite film uses low energy (0.25 keV and 1 keV) Cs when the cluster ion beam is incident + The yield of anions produced by ion sputtering is at least one order of magnitude higher. And in the depth range of tens of nanometers, the measurement of the mass-to-charge ratio anion yield is more accurate.
In order to prove the inventive and technical value of the technical solution of the present utility model, this section is an application example on specific products or related technologies of the claim technical solution.
The embodiment of the utility model is applied to the analysis and detection of the nanometer scale of the material surface. In particular to the shallow ion implantation and analysis of the ultra-shallow PN junction of a semiconductor, and has great potential advantages in the aspects of analysis of nano multi-layer films with modulation period ratio and biological material surface analysis.
The embodiment of the utility model has a great advantage in the research and development or use process, and has the following description in combination with data, charts and the like of the test process.
The above figures 2 and 3 are surface analyses of different samples with different ion sources, respectively.
In the description of the present utility model, unless otherwise indicated, the meaning of "a plurality" is two or more; the terms "upper," "lower," "left," "right," "inner," "outer," "front," "rear," "head," "tail," and the like are used as an orientation or positional relationship based on that shown in the drawings, merely to facilitate description of the utility model and to simplify the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the utility model. Furthermore, the terms "first," "second," "third," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
The foregoing is merely illustrative of specific embodiments of the present utility model, and the scope of the utility model is not limited thereto, but any modifications, equivalents, improvements and alternatives falling within the spirit and principles of the present utility model will be apparent to those skilled in the art within the scope of the present utility model.
Claims (6)
1. A multifunctional ion source device for nanoscale analysis of a surface of a material, the multifunctional ion source device for nanoscale analysis of a surface of a material comprising:
a test bed;
the test bed is fixed in the ultrahigh vacuum cavity, an ion source generating device, a mass spectrum analyzer and an adjusting device are fixed in the test bed, the ion source generating device and the mass spectrum analyzer are fixed at the upper end of the test bed through the adjusting device, the mass spectrum analyzer is fixed right above the test bed, and a sample is fixed in the middle of the test bed.
2. The multifunctional ion source device for nanometer-scale analysis of material surface according to claim 1, wherein the ion source generating device is provided with a penning gas ion source generator and Cs + Ion source generator and gas cluster ion source generator.
3. The multifunctional ion source device for nanoscale analysis of a surface of a material of claim 2, wherein the gas cluster ion source generator is affixed to the left side of the sample and the penning gas ion source generator is affixed to the right side of the sample.
4. The multifunctional ion source device for nanoscale analysis of a surface of a material of claim 1, wherein the ultra-high vacuum chamber is secured within the ion source device.
5. The multifunctional ion source device for nanoscale analysis of a material surface according to claim 1, wherein the penning gas ion source generator, cs, in the ion source generating device + The rear ends of the ion source generator and the gas cluster ion source generator are connected with a suction power supply capable of adjusting direct current voltage.
6. The multifunctional ion source device for nanoscale analysis of a surface of a material according to claim 1, wherein the mass spectrometer is in particular a mass/energy analysis spectrometer.
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