CN113109415B - Multilayer film interface position characterization method suitable for secondary ion mass spectrometry - Google Patents
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- 238000001004 secondary ion mass spectrometry Methods 0.000 title claims abstract description 19
- 238000012512 characterization method Methods 0.000 title claims abstract description 16
- 150000002500 ions Chemical class 0.000 claims abstract description 88
- 238000012545 processing Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 9
- 238000010884 ion-beam technique Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 20
- 238000012360 testing method Methods 0.000 abstract description 9
- 238000001819 mass spectrum Methods 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 39
- 238000004458 analytical method Methods 0.000 description 14
- 239000000758 substrate Substances 0.000 description 12
- 229910000789 Aluminium-silicon alloy Inorganic materials 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 6
- 239000011163 secondary particle Substances 0.000 description 5
- 229910001417 caesium ion Inorganic materials 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 102100032047 Alsin Human genes 0.000 description 2
- 101710187109 Alsin Proteins 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 150000001450 anions Chemical group 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001768 cations Chemical group 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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Abstract
The invention discloses a multilayer film interface position characterization method suitable for secondary ion mass spectrometry. The atomic cluster type ions can be tested together with element ions to be tested or the atomic cluster type ions to be tested or respectively tested, and interface positioning of the signals is realized after data processing and comparison. According to the invention, when the film material is characterized by utilizing the secondary ion mass spectrum, under the condition of not increasing the loss of the testing raw materials and the running cost of the instrument, the interface position of the multilayer film in the sample to be tested can be directly calibrated by using experimental data without data fitting, so that the characterization precision is improved, and the testing efficiency is improved.
Description
Technical Field
The invention relates to the technical field of test analysis of film materials, in particular to a multilayer film interface position characterization method suitable for secondary ion mass spectrometry.
Background
The film material is increasingly widely applied in the aspects of information technology, life science, energy environment, military national defense and the like due to the excellent optical, mechanical, electromagnetic and other performances, and the film industry is increasingly growing and stimulated to the vigorous development of the film technology and the film material. The interface is a very important part of the film material, and the interface may have completely different structure, electronics and mechanical properties from the bulk material, and deeply influences the performance of the material. Therefore, with the rapid development of thin film materials, in the research of the thin film materials, the requirements on the characterization of the materials and the material interfaces are also higher and higher, and the secondary ion mass spectrum is taken as a very important analysis characterization instrument to have great significance on the test analysis of the thin film materials.
The secondary ion mass spectrum is one of the most front surface and near surface material composition characterization analysis tools, primary ions with certain energy bombard the surface of a sample to cause the emission of atoms, molecules and atomic groups on the surface of the sample, namely secondary particles, wherein the secondary particles are mainly neutral, and part of the secondary particles are charged, namely secondary ions, and the secondary ion mass spectrum is obtained through the acceleration, mass separation and detection of the secondary ions, so that the analysis of the surface composition is realized. The secondary ion mass spectrum can realize the analysis of micro doping of parts per million or even parts per million, is the most sensitive trace element analysis tool, and can also characterize the structure of the film material.
One very important function of secondary ion mass spectrometry is depth analysis spectrum, so that the condition that the concentration of an element to be detected changes along with the depth of a sample can be obtained, meanwhile, the interface position of different films in the sample can be determined through the change of a signal of a substrate material of the sample, generally, 50% of the change of the signal intensity of the substrate material is used as the position of the interface, but due to the substrate effect, in the characterization of the film material, the secondary ion yield difference of the same element is very large in film layers with different components, so that the characterization difficulty is caused, particularly in the position of a multi-layer film interface, the change of the ion yield caused by materials at two sides of the multi-layer film interface can be one or even several orders of magnitude, thus causing obvious deviation of data intensity, causing obvious deviation of the position of the film interface in the secondary ion mass spectrometry data characterized by a traditional method, causing difficulty in element distribution and diffusion analysis near the interface and difficulty in comparison analysis of different program test data.
Disclosure of Invention
The invention aims to provide a multilayer film interface position characterization method suitable for secondary ion mass spectrometry, which is characterized in that a secondary ion mass spectrometer detector is used for collecting atomic cluster type ions comprising characteristic elements in films on two sides of a multilayer film interface, the atomic cluster type ion signal is analyzed by utilizing the characteristic that the atomic cluster type ions can only appear at the position of the multilayer film interface, and the position of a sample interface is determined by utilizing the peak position of the atomic cluster type ion signal, so that the problem that the multilayer film interface position analysis is difficult in the secondary ion mass spectrometry is solved.
The purpose of the invention is realized in the following way:
a multilayer film interface position characterization method suitable for secondary ion mass spectrometry is characterized by comprising the following steps: and collecting atom cluster type ions comprising characteristic elements in films at two sides of the interface of the multilayer film by using a secondary ion mass spectrometer detector, analyzing signals of the atom cluster type ions, and determining the interface position of the sample by using the peak position of the signals of the atom cluster type ions.
Optionally, the atomic cluster ion is composed of more than two elements, and at least one characteristic element is respectively arranged in the films at two sides of the interface of the multilayer film.
Optionally, the number of atoms of the characteristic element contained in the cluster ion is at least 1.
Optionally, the atom cluster ion contains atoms of non-characteristic elements, and the atoms of the non-characteristic elements are common element atoms at two sides of the interface of the multilayer film or atoms in the primary ion beam.
Optionally, the atom cluster type ion can be tested together with the element ion to be tested or the atom cluster type ion to be tested, so that the determination of the interface position in the element ion to be tested or the atom cluster type ion signal to be tested is realized through the peak position of the cluster type ion signal.
Optionally, the atom cluster type ions can be tested with the element ions to be tested or the atom cluster type ions to be tested respectively, and the interface positions in the element ions to be tested or the atom cluster type ion signals to be tested are determined after data processing and comparison.
Optionally, the atom cluster type ions contain elements to be detected, so that the direct analysis of the elements to be detected is realized.
Alternatively, the primary ion source can be a Cs + ion source, an O 2 + ion source, a Ga + ion source, an Ar + ion source, a C60 + ion source, or other ion source that can be used in secondary ion mass spectrometry.
Optionally, the interface is a semiconductor-semiconductor interface, such as an AlN/Si interface, an AlN/GaN interface, an Ag/GaN interface, an AlN/Al 2O3 interface, a metal-metal interface, a metal-semiconductor interface, a metal-insulator interface, or a semiconductor-insulator interface, but is not limited to such an interface.
Compared with the prior art, the invention has the beneficial effects that: when the film material is characterized by utilizing the secondary ion mass spectrum, the interface position of the multilayer film in the sample to be tested can be directly calibrated by using experimental data without data fitting under the condition of not increasing the loss of the testing raw materials and the running cost of the instrument, so that the characterization precision is improved and the testing efficiency is improved.
Drawings
FIG. 1 is a flow chart illustrating the operation of an embodiment of the present invention;
FIG. 2 is a schematic diagram of determining the interface position between a Si substrate and an AlN film by using AlSi - atomic cluster type ions in the embodiment of the invention, and the peak position of the AlSi - atomic cluster type ion signal is marked as the interface position between the AlN film and the Si substrate;
FIG. 3 is a schematic diagram of determining the interface position between a Si substrate and an AlN film using AlSiN + atomic cluster ions in an embodiment of the invention, the peak position of the AlSiN + atomic cluster ion signal being marked as the interface position between the AlN film and the Si substrate.
Detailed Description
The technical solutions in the embodiments of the present invention are further described below with reference to the accompanying drawings in the embodiments of the present invention. In addition, the drawings of the present invention are all to a very simplified, non-precise scale, and are only used to facilitate a convenient and clear description of the present invention.
Example 1:
A multilayer film interface position characterization method suitable for secondary ion mass spectrometry analysis is shown in fig. 1, and comprises the following specific steps:
1) And analyzing an AlN film sample grown on the Si substrate by using a secondary ion mass spectrometer detector, wherein elements to be tested are Si and Al during the test. When the secondary ion mass spectrum is used for characterizing the sample, cs+ ions with designed energy are utilized to bombard the surface of the sample, partial ionization exists in generated secondary particles, the generated secondary ions are secondary ions, anions in the secondary ions are extracted through designed bias voltage, and separation and detection are carried out, such as Al - ions and Si - ions, as shown in fig. 2. Since the generation of negative ions is more enhanced on the Al matrix material than on the Si matrix material, it can be seen from the data that the Al - signal is significantly reduced near Si, while the Si - signal is significantly enhanced near Al. If the location of the interface is determined in SIMS data using conventional methods, the matrix effects of the materials on both sides of the interface need to be removed by a very complex data processing, and are not necessarily accomplished. The interface position can not be determined directly through the existing data;
2) While collecting Al - ions and Si - ions, detecting atomic group ions containing characteristic elements on two sides of an interface, such as AlSi - or AlSi 2 -;
3) Since the two elements of Al and Si only appear at the interface position, the signal of AlSi - atomic group type ions is used for determining the interface position of the AlN film and the Si substrate, namely the peak signal of AlSi - atomic group type ions is marked as the interface position between the AlN film and the Si substrate.
4) By using the interface position determined in the previous step and combining detected Al - ions, si - ions and the like, si and Al or other element conditions near the interface, such as Ga, in, C, H, O and the like, can be analyzed.
Example 2:
A multilayer film interface position characterization method suitable for secondary ion mass spectrometry analysis is shown in fig. 1, and comprises the following specific steps:
1) And analyzing an AlN film sample grown on the Si substrate by using a secondary ion mass spectrometer detector, wherein elements to be tested are Si and Al during the test. When the secondary ion mass spectrum is used for characterizing the sample, cs + ions with designed energy are utilized to bombard the surface of the sample, partial ionization exists in generated secondary particles, the generated secondary ions are secondary ions, cations in the secondary ions are extracted through designed bias voltage, and separation and detection are carried out, such as CsAl + ions, cs 2Si+ ions and the like, as shown in fig. 3. Since the generation of negative ions is more enhanced in the Si matrix material than in the Al matrix material, it can be seen from the data that CsAl + signal is significantly enhanced near Si, while Cs 2Si+ signal is significantly attenuated near Al. If the position of the interface is determined in SIMS data by a traditional method, the matrix effect of materials at two sides of the interface needs to be removed by complex data processing, and the method is not necessarily completed, but the position of the interface cannot be determined directly by the existing data;
2) Collecting CsAl + ions and Cs 2Si+ ions, and simultaneously testing atomic group type ions containing characteristic elements on two sides of an interface, such as AlNSi +;
3) Because three elements of Al, si and N only appear at the interface position at the same time, determining the interface position of the AlN film and the Si substrate by utilizing the signal of AlNSi + atomic group ions;
4) Si and Al near the interface, or other doping or contamination elements such as Mg, in, fe, etc. are analyzed by using the interface position determined In the previous step.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (7)
1. A multilayer film interface position characterization method suitable for secondary ion mass spectrometry is characterized in that: collecting atom cluster type ions comprising characteristic elements in films at two sides of a multi-layer film interface by using a secondary ion mass spectrometer detector, analyzing signals of the atom cluster type ions, and determining the interface position of a sample by using the peak position of the signal of the atom cluster type ions; the atomic cluster type ions consist of more than two elements, and at least one characteristic element is respectively arranged in the films at the two sides of the interface of the multilayer film; the number of atoms of the characteristic element contained in the atomic cluster type ion is at least 1.
2. The method for characterizing the interface position of a multilayer film suitable for secondary ion mass spectrometry according to claim 1, wherein: the atom cluster ion contains atoms of non-characteristic elements.
3. The method for characterizing the interface position of a multilayer film suitable for secondary ion mass spectrometry according to claim 2, wherein: the atoms of the non-characteristic elements are common element atoms on two sides of the interface of the multilayer film or atoms in the primary ion beam.
4. The method for characterizing the interface position of a multilayer film suitable for secondary ion mass spectrometry according to claim 3, wherein: the atomic cluster type ions can be tested together with the element ions to be tested or the atomic cluster type ions to be tested, so that the determination of the interface positions in the element ions to be tested or the atomic cluster type ion signals to be tested is realized through the peak positions of the cluster type ion signals.
5. The method for characterizing the interface position of a multilayer film suitable for secondary ion mass spectrometry according to claim 3, wherein: the atomic cluster type ions can be respectively tested with the element ions to be tested or the atomic cluster type ions to be tested, and the interface positions in the element ions to be tested or the atomic cluster type ion signals to be tested are determined after data processing and comparison.
6. The method for characterizing the interface position of a multilayer film suitable for secondary ion mass spectrometry according to claim 3, wherein: the atomic group type ion contains the element to be detected, so that the element to be detected is directly analyzed.
7. The method for characterizing the interface position of a multilayer film suitable for secondary ion mass spectrometry according to claim 1, wherein: the interface is AlN/Si interface, alN/GaN interface, ag/GaN interface and AlN/Al 2O3 interface.
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| CN101330055A (en) * | 2007-06-20 | 2008-12-24 | 株式会社东芝 | Method of manufacturing semiconductor device and semiconductor device |
| CN101425544A (en) * | 2007-11-01 | 2009-05-06 | 株式会社半导体能源研究所 | Thin film transistor, and display device having the thin film transistor |
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| JP3318186B2 (en) * | 1995-05-19 | 2002-08-26 | 科学技術振興事業団 | Gas cluster forming method and thin film forming method |
| JP2956627B2 (en) * | 1996-12-16 | 1999-10-04 | 日本電気株式会社 | Impurity concentration analysis method |
| JP2001091482A (en) * | 1999-09-27 | 2001-04-06 | Nec Corp | Contained element analyzing method |
| JP4291496B2 (en) * | 2000-04-28 | 2009-07-08 | 新日本製鐵株式会社 | High accuracy secondary ion mass spectrometry |
| JP2004079912A (en) * | 2002-08-21 | 2004-03-11 | Sharp Corp | Semiconductor substrate reforming method and semiconductor device using the same |
| KR101202073B1 (en) * | 2007-03-23 | 2012-11-15 | 아사히 가세이 일렉트로닉스 가부시끼가이샤 | Compound semiconductor laminate, process for producing the compound semiconductor laminate, and semiconductor device |
| MX2011009486A (en) * | 2011-09-09 | 2013-03-15 | Ct Investig Y Estudios Del Ipn | Combined method of secondary ion mass spectroscopy and energy dispersive x-ray for quantitative chemical analysis of various solid materials and thin films. |
| CN102842492A (en) * | 2012-07-24 | 2012-12-26 | 南昌大学 | Crystal silicon laser-assisted aluminum-boron co-doping and electrode preparation method |
| JP6278591B2 (en) * | 2012-11-13 | 2018-02-14 | 株式会社Sumco | Manufacturing method of semiconductor epitaxial wafer, semiconductor epitaxial wafer, and manufacturing method of solid-state imaging device |
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| CN109632925B (en) * | 2018-12-20 | 2020-07-31 | 北京科技大学 | SIMS (simple in-situ chemical vapor deposition) optimization detection method for concentration and distribution of trace impurity elements in AlN (aluminum nitride) |
| CN109755148B (en) * | 2018-12-20 | 2020-04-10 | 北京科技大学 | SIMS (separation-independent modeling system) optimization detection method for concentration and distribution of trace impurities in InP and GaN |
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| CN101330055A (en) * | 2007-06-20 | 2008-12-24 | 株式会社东芝 | Method of manufacturing semiconductor device and semiconductor device |
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