CN113109415A - Multilayer film interface position characterization method suitable for secondary ion mass spectrometry - Google Patents
Multilayer film interface position characterization method suitable for secondary ion mass spectrometry Download PDFInfo
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- CN113109415A CN113109415A CN202110323804.5A CN202110323804A CN113109415A CN 113109415 A CN113109415 A CN 113109415A CN 202110323804 A CN202110323804 A CN 202110323804A CN 113109415 A CN113109415 A CN 113109415A
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- 238000001004 secondary ion mass spectrometry Methods 0.000 title claims abstract description 21
- 238000012512 characterization method Methods 0.000 title claims abstract description 14
- 150000002500 ions Chemical class 0.000 claims abstract description 89
- 238000012545 processing Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052593 corundum Inorganic materials 0.000 claims description 2
- 238000010884 ion-beam technique Methods 0.000 claims description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 2
- 239000010408 film Substances 0.000 abstract description 23
- 239000010409 thin film Substances 0.000 abstract description 23
- 239000000463 material Substances 0.000 abstract description 22
- 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
- 238000004458 analytical method Methods 0.000 description 10
- 239000000758 substrate Substances 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 5
- 239000011163 secondary particle Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 229910000789 Aluminium-silicon alloy Inorganic materials 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- 102100032047 Alsin Human genes 0.000 description 2
- 101710187109 Alsin Proteins 0.000 description 2
- 229910001417 caesium ion Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 150000005837 radical ions Chemical class 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910017113 AlSi2 Inorganic materials 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 class 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 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
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- 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
Images
Classifications
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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
Abstract
The invention discloses a multilayer film interface position characterization method suitable for secondary ion mass spectrometry, which is characterized in that atomic cluster type ions comprising characteristic elements in films on two sides of an interface are collected through a secondary ion mass spectrometer detector, signals of the atomic cluster type ions are analyzed, and the position of a sample interface is determined by utilizing the peak position of the atomic cluster type ions. The atomic cluster type ions can be tested together with or respectively tested by the element ions to be tested or the atomic cluster type ions to be tested, and interface positioning of the signals is realized after data processing and comparison. According to the invention, when the secondary ion mass spectrum is used for representing the thin film material, 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 test raw materials and the running cost of an instrument, so that the representation precision is improved, and the test efficiency is improved.
Description
Technical Field
The invention relates to the technical field of test analysis of thin film materials, in particular to a multilayer film interface position characterization method suitable for secondary ion mass spectrometry.
Background
The thin film material is increasingly widely applied in the aspects of information technology, life science, energy environment, military and national defense and the like due to excellent optical, mechanical, electromagnetic and other properties, and the growing trend of the thin film industry stimulates the vigorous development of the thin film technology and the thin film material. The interface is a very important part in the thin film material, and the interface may have a structure, electronics and mechanical properties completely different from those of the bulk material, and deeply influences the performance of the material. Therefore, with the rapid development of thin film materials, in the research of thin film materials, the characterization requirements on materials and material interfaces are higher and higher, and the secondary ion mass spectrometry as a very important analysis characterization instrument has great significance on the test analysis of the thin film materials.
The secondary ion mass spectrum is one of the most frontmost surface and near-surface material component characterization analysis tools, atoms, molecules and atomic groups on the surface of a sample are emitted by bombarding the surface of the sample by primary ions with certain energy, namely secondary particles, the secondary particles are mainly neutral, and a part of the secondary particles are charged, namely secondary ions, and the secondary ions are accelerated, separated and detected to obtain the secondary ion mass spectrum so as to realize the analysis of the surface components. The secondary ion mass spectrum can realize the analysis of micro doping in parts per million or even parts per million, is the most sensitive trace element analysis tool, and can also characterize the structure of the thin film material.
A very important function of the secondary ion mass spectrum is depth analysis spectrum, 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 positions of different thin films in the sample can be determined through the change of a base material signal of the sample, the position of 50% of the signal intensity change of the base material is generally taken as the interface position, but due to the base effect, in the characterization of thin film materials, the secondary ion yield difference of the same element is very large in the thin film layers with different components, so that the characterization difficulty is caused, particularly, in the position of a multilayer film interface, the change of the ion yield caused by materials on two sides of the multilayer film interface can be one or even several orders of magnitude, so that the obvious deviation of the data intensity is caused, the obvious deviation of the thin film interface position in the secondary ion mass spectrum data characterized by using the traditional method is caused, The difficulty of diffusion analysis and the difficulty of comparing test data with different programs.
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 atom cluster type ions comprising characteristic elements in films on two sides of a multilayer film interface, the atom cluster type ions are only capable of appearing at the multilayer film interface position, an atom cluster type ion signal is analyzed, and the peak position of the atom cluster type ion signal is used for determining the position of a sample interface, so that the problem that the multilayer film interface position is difficult to analyze in the secondary ion mass spectrometry is solved.
The purpose of the invention is realized as follows:
a multilayer film interface position characterization method suitable for secondary ion mass spectrometry is characterized in that: and collecting atomic cluster type ions comprising characteristic elements in films on two sides of the multilayer film interface by using a secondary ion mass spectrometer detector, analyzing signals of the atomic cluster type ions, and determining the interface position of the sample by using the peak position of the atomic cluster type ion signals.
Optionally, the atomic cluster type ions are composed of more than two elements, and at least one characteristic element is respectively arranged in the thin films on two sides of the interface of the multilayer film.
Optionally, the number of atoms of the characteristic element contained in the atomic cluster type ion is at least 1.
Optionally, the atomic cluster type ions contain atoms of non-characteristic elements, and the atoms of the non-characteristic elements are common element atoms on both sides of the multilayer film interface or atoms in the primary ion beam.
Optionally, the atom cluster type ions can be tested together with the element ions to be tested or the atom cluster type ions to be tested, so that the interface position in the element ions to be tested or the atom cluster type ion signals to be tested is determined through the peak position of the cluster type ion signals.
Optionally, the atom cluster type ions and the element ions to be detected or the atom cluster type ions to be detected are respectively tested, and the interface position in the element ions to be detected or the atom cluster type ion signals to be detected is determined after data processing and comparison.
Optionally, the atomic cluster type ions contain an element to be detected, so that direct analysis of the element to be detected is realized.
Optionally, the primary ion source can be Cs+Ion source, O2 +Ion source, Ga+Ion source, Ar+Ion source, C60+Ion sources or other ion sources that can be used for secondary ion mass spectrometry.
Optionally, the interface is AlN/Si interface, AlN/GaN interface, Ag/GaN interface, AlN/Al2O3An interface such as a semiconductor-semiconductor interface, a metal-metal interface, a metal-semiconductor interface, a metal-insulator interface, a semiconductor-insulator interface, but not limited to such an interface.
Compared with the prior art, the invention has the beneficial effects that: when the secondary ion mass spectrum is used for representing the thin film material, 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 test raw materials and the running cost of an instrument, so that the representation precision is improved, and the test efficiency is improved.
Drawings
FIG. 1 is a flow chart of the operation of an embodiment of the present invention;
FIG. 2 shows the use of AlSi in an embodiment of the present invention-Schematic diagram of determining interface position of Si substrate and AlN thin film by atomic cluster type ions, AlSi-Marking the peak position of the atomic cluster type ion signal as the interface position between the AlN thin film and the Si substrate;
FIG. 3 shows an embodiment of the present invention utilizing AlSiN+Atomic cluster type ion-determining Si substrateSchematic of the location of the interface with the AlN thin film, AlSiN+The peak position of the atomic cluster type ion signal is marked as the interface position between the AlN thin film and the Si substrate.
Detailed Description
The technical solution in the embodiment of the present invention is further described below with reference to the drawings in the embodiment of the present invention. In addition, the drawings of the present invention are not to scale, but are to be understood as being simplified and not to scale.
Example 1:
a multilayer film interface position characterization method suitable for secondary ion mass spectrometry is disclosed, as shown in FIG. 1, and comprises the following specific steps:
1) and analyzing an AlN film sample growing on the Si substrate by using a secondary ion mass spectrometer detector, wherein the elements to be detected are Si and Al during testing. When a sample is characterized by secondary ion mass spectrometry, Cs + ions with designed energy are utilized to bombard the surface of the sample, part of generated secondary particles are ionized to be 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 base material than on the Si base material, it can be seen from the data that Al-The signal is significantly reduced at a position close to Si, which is-The signal is significantly enhanced at a position close to Al. If the position of the interface is determined in SIMS data by the traditional method, the matrix effect of materials on two sides of the interface needs to be removed through very complicated data processing, and the matrix effect cannot be necessarily completed. The interface position cannot be determined directly through the existing data;
2) collecting Al-Ions and Si-Simultaneously with the ions, radical ions containing characteristic elements on both sides of the interface, such as AlSi, are detected-Or AlSi2 -；
3) Since Al and Si elements are present only at the interface position at the same time, AlSi is used-The signal of the radical type ion determines the interface position of the AlN thin film and the Si substrate, namely AlSi-The peak signal of the radical ion is labeled as AlN film andinterface position between Si substrates.
4) Combining the detected Al with the interface position determined in the previous step-Ions and Si-Ions, etc. capable of analyzing the condition of Si and Al or other elements such as Ga, In, C, H, O, etc. near the interface.
Example 2:
a multilayer film interface position characterization method suitable for secondary ion mass spectrometry is disclosed, as shown in FIG. 1, and comprises the following specific steps:
1) and analyzing an AlN film sample growing on the Si substrate by using a secondary ion mass spectrometer detector, wherein the elements to be detected are Si and Al during testing. When the secondary ion mass spectrum is used for characterizing a sample, the designed energy Cs is used+Bombarding the sample surface with ions, partially ionizing the generated secondary particles to obtain secondary ions, extracting cations from the secondary ions by designed bias voltage, separating and detecting, such as CsAl+Ions and Cs2Si+Ions, etc., as shown in fig. 3. Since the production of negative ions is more enhanced in the Si matrix material than in the Al matrix material, CsAl can be seen from the data+The signal is significantly enhanced at the site close to Si, while Cs2Si+The signal is significantly attenuated at positions close to Al. If the position of the interface is determined in SIMS data by the traditional method, the matrix effect of materials at two sides of the interface is removed by very complicated data processing, which cannot be finished necessarily, but the position of the interface cannot be determined directly by the existing data;
2) collection of CsAl+Ions and Cs2Si+Simultaneously with the ion, the radical type ion containing characteristic elements on both sides of the interface, such as AlNSi, is tested+；
3) Because Al, Si and N elements appear at the same time only at the interface position, AlNSi is utilized+Determining the interface position of the AlN thin film and the Si substrate by the signal of the radical type ions;
4) and analyzing the conditions of Si and Al or other doped or polluted elements, such as Mg, In, Fe and the like, near the interface by using the interface position determined In the last step.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present 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 solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. A multilayer film interface position characterization method suitable for secondary ion mass spectrometry is characterized by comprising the following steps: and collecting atomic cluster type ions comprising characteristic elements in films on two sides of the multilayer film interface by using a secondary ion mass spectrometer detector, analyzing signals of the atomic cluster type ions, and determining the interface position of the sample by using the peak position of the atomic cluster type ion signals.
2. The method of claim 1 for characterizing the location of an interface of a multilayer film suitable for secondary ion mass spectrometry, wherein: the atomic cluster type ions are composed of more than two elements, and at least one characteristic element is respectively arranged in the films on two sides of the interface of the multilayer film.
3. The method of claim 2 for characterizing the location of an interface of a multilayer film suitable for secondary ion mass spectrometry, wherein: the number of atoms of the characteristic element contained in the atomic cluster type ion is at least 1.
4. The method of claim 3 for characterizing the location of the interface of the multilayer film suitable for secondary ion mass spectrometry, wherein: the atomic cluster type ions contain atoms of a non-characteristic element.
5. The method of claim 4 for characterizing the location of the interface of a multilayer film suitable for secondary ion mass spectrometry, wherein: the atoms of the non-characteristic elements are common element atoms on two sides of the multilayer film interface or atoms in the primary ion beams.
6. The method of claim 5 for characterizing the location of an interface of a multilayer film suitable for secondary ion mass spectrometry, wherein: the atom cluster type ions can be tested together with element ions to be tested or atom cluster type ions to be tested, so that the interface position in the element ions to be tested or the atom cluster type ion signals to be tested is determined through the peak position of the cluster type ion signals.
7. The method of claim 5 for characterizing the location of an interface of a multilayer film suitable for secondary ion mass spectrometry, wherein: the atomic cluster type ions can be respectively tested with element ions to be tested or atomic cluster type ions to be tested, and interface positions in the element ions to be tested or the atomic cluster type ions to be tested are determined after data processing and comparison.
8. The method of claim 5 for characterizing the location of an interface of a multilayer film suitable for secondary ion mass spectrometry, wherein: the atomic cluster type ions contain elements to be detected, so that the elements to be detected can be directly analyzed.
9. The method of claim 1 for characterizing the location of an interface of a multilayer film suitable for secondary ion mass spectrometry, wherein: the interface is AlN/Si interface, AlN/GaN interface, Ag/GaN interface, AlN/Al2O3And (6) an interface.
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| CN116735643A (en) * | 2023-08-14 | 2023-09-12 | 季华实验室 | Method for measuring interface point of sample structure |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116735643A (en) * | 2023-08-14 | 2023-09-12 | 季华实验室 | Method for measuring interface point of sample structure |
| CN116735643B (en) * | 2023-08-14 | 2023-11-24 | 季华实验室 | Method for measuring interface cut-off point of sample structure |
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