CN105259194A - Measuring method for modulation period and uniformity of multiple layers of films - Google Patents
Measuring method for modulation period and uniformity of multiple layers of films Download PDFInfo
- Publication number
- CN105259194A CN105259194A CN201510793444.XA CN201510793444A CN105259194A CN 105259194 A CN105259194 A CN 105259194A CN 201510793444 A CN201510793444 A CN 201510793444A CN 105259194 A CN105259194 A CN 105259194A
- Authority
- CN
- China
- Prior art keywords
- modulation period
- multilayer film
- homogeneity
- measuring
- measuring method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention provides a measuring method for the modulation period and uniformity of multiple layers of films. The method includes the steps that lithium fluoride powder is compacted to form a cylindrical target block, the surface is processed to be in a concave cone shape, and then a lithium fluoride target block is obtained; the lithium fluoride target block is installed at the target head position of an ion source of an accelerator, a negative lithium ion beam is led out, nitrogen is charged, and after the lithium ion beam is collided and stripped by stripping gas in an accelerator tube, a bivalent Li2+ positive ion beam is obtained; the multiple layers of films to be measured are placed on a sample table in a Rutherford back scattering measuring target chamber, a beam integrator is used for measuring the Li2+ beam, an RBS is formed, and then the modulation period and uniformity information of the multiple layers of films is obtained. According to the method, the RBS is used for measuring the modulation period, element distribution and uniformity of the films, measuring precision is high, and sample damage is avoided. The nondestructive detection method for the multiple layers of films method is high in precision and quality.
Description
Technical field
The present invention relates to a kind of method measuring multilayer film modulation period and homogeneity thereof.Belong to surface of the work measured thin film analysis technical field.
Background technology
Measured thin film technology is significant in commercial Application.General measure comprises thin film composition analysis, element depth distribution, and thicknesses of layers Non-Destructive Testing, the measurement such as film hardness and film adhesion.The measurement of rete can reflect the quality of film quality, detects film quality, improves film-forming process tool and has very great help.
Conventional Correlative measurement method all has certain relativity and not enough increasing is thick: (1) elemental composition is measured: conventional method is very low to the sensitivity of light element, is difficult to measure the composition containing light element film; (2) measurement (EDS, XPS, SIMS) of element depth distribution all needs sputtering, serious to specimen breakdown; Or carry out the observation of rete cross-sectional scans by scanning tunnel microscope, also directly can destroy sample; (3) the direct observation of xsect is generally made in thickness measure of scanning tunneling microscope, or adopt step instrument to measure rete, two kinds of methods all need to carry out destructiveness damage to sample, also gross thickness can only be measured simultaneously, modulation period can not be measured, i.e. the thickness of each cycle individual layer.
The measurement in coating modulation cycle generally needs the high-resolution lens scan of carrying out xsect, because modulation period is very thin, scope may only have several nanometer, general scanning tunnel microscope can not be observed, and can only adopt the high-resolution lens scan that enlargement factor is higher, but first this kind of method is destroyed to sample, secondly sample preparation needs to make through the complicated means of the thinning grade of polishing, need to consume the plenty of time, commercial Application is had little significance, can only laboratory study be applied to.
The present invention adopts ion backsatering energy spectrum analysis method to measure elemental composition and the modulation period of rete, to sample without any damage, can directly detect the sample putting sample chamber into, the elemental composition comprising light element can be detected, the clear and intuitive homogeneity seeing rete film forming, calculate the thickness of rete modulation period accurately, method is ripe relative to conventional method effectively.
Before the present invention, a kind of apparatus for measuring thickness of thin film has been prepared in CN201310717708.4 application, the invention provides the reflected incident light of a kind of monochromatic ultraviolet light source through light billows to the surfaces externally and internally of film to be measured, calculate the method for film thickness according to the reflected light of the surfaces externally and internally through film to be measured.This patent of invention is simple to operate, can measure thicknesses of layers, but has certain requirement to thin film to be measured, requires the necessary printing opacity of film to be measured, greatly limit the kind of film.The modulation period of rete can not be measured simultaneously, more can not observe the homogeneity of rete.
Summary of the invention
The object of the present invention is to provide a kind of method measuring multilayer film modulation period and homogeneity thereof, with Rutherford backscattering (RutherfordBackscatteringSpectrometry, be called for short RBS) ion beam analysis technology, when not damaging sample, ion beam analysis is carried out to sample, obtains modulation period and the homogeneity information of rete.
A measuring method for multilayer film modulation period and homogeneity thereof, comprises the steps:
(1) by purity be 99.9% lithium fluoride powder compacting become cylindrical target block, and its surface working is become concave cone shape, that is, lithium fluoride target block;
(2) lithium fluoride target block is mounted to the ionogenic target head place (see 4 places in explanation accompanying drawing 2) of accelerator, draw negative lithium ion line, in accelerator tube, be filled with nitrogen further, make Lithium ion beam in accelerator tube with the accelerating potential of 1.0-2.0MeV under after strip gas collision is peeled off, obtain the Li of divalence
2+positive ion beam;
(3) be placed on by multilayer film to be measured at (see 4 places in explanation accompanying drawing 4) on sample stage in Rutherford backscattering measurement target chamber, the scattering angle regulating Au Si surface barrier detector is 100-200
o, the vacuum tightness measuring target chamber is 0.6 × 10
-3-1.0 × 10
-3pa, measures Li with line integraph
2+the line of bundle, read the tale of RBS spectrum with line integraph, multichannel analyzer is connected to computing machine, and the backward scattering ion that detector receives inputs computing machine after multichannel analyzer analysis simultaneously, forms RBS spectrum;
(4) RBS of computer acquisition spectrum is imported in SIMNRA software, corresponding experiment parameter is set, draws modulation period and the homogeneity information of multilayer film.
The diameter of described cylindrical target block is 7mm, is highly 15mm.
The ionization electric current in described step (2) intermediate ion source is 23A, and target voltage is 5-6kV, and probe voltage is 20kV.
In described step (2), the accelerating potential at accelerating tube place is adjusted to 1.52MV, and the nitrogen pressure be filled with in accelerating tube is 5 × 10
-3-7 × 10
-3pa.
The scattering angle of described Au Si surface barrier detector is 170
o, the vacuum tightness measuring target chamber is 0.8 × 10
-3pa.
Described multilayer film comprise MoN/CrN multilayer film.
The present invention, for achieving the above object, has used a kind of accelerator installation, and it is primarily of ion gun, accelerating tube, detector, sample chamber and vacuum system composition.Ion gun, accelerating tube, detector are connected successively with measurement target chamber, make device inside keep high vacuum state by vacuum system.Ion gun produce ion beam, the ion beam obtained through accelerating tube accelerate after with sample generation scattering, detector receive scattered information, formed scattering spectra.By the analysis to scattering spectra, obtain modulation period and the homogeneity information of rete.Schematic diagram is as Fig. 1.
Ion gun of the present invention as shown in Figure 2, is made up of caesium stove, ionization device, lithium target, a few part of extraction electrode.Ionogenic principle of work: the liquid metal caesium in caesium stove evaporates under heat effect, the caesium steam produced arrives the surface of ionization device, the surface of ionization device is spill, the armouring tantalum wire simultaneously heated by big current is coiled into, the gas molecule of cold caesium runs into the tantalum wire of heat and ionizes, the cesium ion produced accelerates to move towards target under negative target voltage effect, lithium atom in target is sputtered out, the lithium atom sputtered has captured the electronics of caesium film at target material surface, become the negative ion of a band negative charge, anion beam accelerates toward extraction electrode motion under an extraction electrode negative voltage effect higher than target current potential, ion beam is drawn by extraction electrode the most at last.
Under suitable vacuum condition, produce Lithium ion beam, after accelerator accelerates with cesium ion sputtering lithium target, with sample generation scattering, analyze coating structure according to the scattering spectra obtained, the uniform distribution of coating can be obtained clearly, and the modulation period of some multilayer films.This method RBS measures modulation period and the homogeneity of film, and its measuring accuracy is high, and does not damage sample, is the novel detection film process of a kind of high precision, high-quality.
The present invention is using lithium lithium fluoride as sputtering target, and sputter face is concave cone face, and sputtering voltage Vsp is 5-6kV; The ion beam that sputtering produces is drawn by extraction electrode fairlead, probe voltage V
eXbe generally 20kV.The Cluster Beam corresponding to lithium ion of drawing as shown in Figure 3, wherein Vsp=5.6kV, V
eX=20.0kV.
Detector of the present invention is: gold silicon surface barrier solid probe.
The structural drawing of measurement target chamber of the present invention as shown in Figure 4.
The invention has the beneficial effects as follows and provide a kind of method measuring multilayer film modulation period and homogeneity thereof, its advantage is; (1) not lesioned sample structure; (2) be not limited to sample size, sample is without the need to special process; (3) modulation period of multilayer film can be measured; (4) can be visual and clear see membrane uniformity information; (5) measurement for multilayer film is very accurate.
Accompanying drawing explanation
Fig. 1 is apparatus of the present invention schematic diagram.In figure, target chamber is measured in (1) caesium stove, (2) ion gun, (3) accelerating tube, (4) Signal reception and treating apparatus, (5).
Fig. 2 is ionogenic structural drawing of the present invention.(6) caesium stove, (7) ionization device, (8) cooling medium, (9) lithium target, (10) cathode insulation in figure.
Fig. 3 is the Cluster Beam that the lithium ion of this device sputtering generation is corresponding.
The structural drawing of the measurement target chamber of Fig. 4 designed by the present invention.(11) external shielding layer, (12) view window, (13) internal shield, (14) sample stage, (15) detector, (16) connecting line in figure.
Fig. 5 is the Li of this device 1.52MeV
2+the RBS of MoN/CrN multilayer film measured by ion beam under rotating speed is 3rpm measures spectrum and simulated spectrum.
Fig. 6 is the cross-sectional image of the multilayer film recorded with high-resolution-ration transmission electric-lens.
Embodiment
The present invention is further illustrated below in conjunction with example.
Embodiment 1:
Negative lithium ion line can be drawn from the ion source of 2 × 1.7MV tandem accelerator, target voltage is set to 5-6keV, probe voltage is set to 20keV, stable and when increasing to maximal value until beam intensity, line size is ~ 1.5 μ A, and now flowed to by negative ion in rear measurement target chamber and guide, in guiding way, line can through multiplication of voltage accelerating tube, be filled with nitrogen gas in accelerating tube, air pressure is about 6 × 10
-3pa, the collision of the outer-shell electron of negative lithium ion can peel off by these nitrogen molecules, makes negative Lithium ion beam stream translation become the positive lithium ion line of band two positive charges, i.e. Li
2+line, the high voltage in accelerating tube is by Li
2+shu Yinzhi RBS measures in target chamber, and line size is generally 1 ~ 4nA, and the RBS for rear target chamber sample measures.When classical RBS measures, it is 170 that detector is placed in scattering angle usually
oposition.
The signal of the backward scattering ion received is sent into prime amplifier by ion beam detector, and signal after treatment inputs computing machine after multichannel analyzer analytic record, forms RBS spectrum.Need counting when adopting spectrum, count more in theory, data statistically better, measuring error is less, but composite measurement efficiency and accuracy are considered, common total count value is 3-5 μ C, directly can be read by line integraph.The RBS recorded composes available SIMNRA software and simulates, and draws thickness information and the constituent content information of sample, as illustrated as shown in accompanying drawing 5.The thickness of the MoN layer that the analog result in this figure provides is about 40nm, and the thickness of CrN layer is about 30nm, matches with the HRTEM image illustrated in accompanying drawing 6.RBS measures the size not being limited to sample, and sample does not need other processing procedures as loaded down with trivial details in XPS, SEM, HRTEM etc. yet, can not destroy sample, is a kind of nondestructive analysis means.Sample also can continue on for the test of other characterization methods after carrying out RBS measurement, improve the utilization factor of sample, to some be difficult to preparation or sample with high costs seem particularly important.After RBS measurement spectrum being simulated with SIMNRA software, modulation period and the composition information of sample can be obtained simultaneously.
Embodiment 2:
When ectonexine radome in this explanation accompanying drawing 4 is not installed, the line that in measurement target chamber, line integraph records has the contribution from secondary electron, can be bigger than normal than the line of reality so measure line, and detector also can be mingled with secondary electron when receiving backward scattering ion, these secondary electrons also have unfavorable contribution for sample RBS spectrum, and the constituent content value that simulation can be made to obtain is higher than actual value.Experiment proves, after the secondary electron radome in accompanying drawing 4, the sample message that the RBS spectrum recorded draws after SIMNRA simulation is more accurate.
Claims (6)
1. a measuring method for multilayer film modulation period and homogeneity thereof, is characterized in that, comprises the steps:
(1) by purity be 99.9% lithium fluoride powder compacting become cylindrical target block, and its surface working is become concave cone shape, that is, lithium fluoride target block;
(2) lithium fluoride target block is mounted to the ionogenic target head place of accelerator, draw negative lithium ion line, in accelerator tube, be filled with nitrogen further, make Lithium ion beam in accelerator tube with the accelerating potential of 1.0-2.0MeV under after strip gas collision is peeled off, obtain the Li of divalence
2+positive ion beam;
(3) be placed on by multilayer film to be measured on sample stage in Rutherford backscattering measurement target chamber, the scattering angle regulating Au Si surface barrier detector is 100-200
o, the vacuum tightness measuring target chamber is 0.6 × 10
-3-1.0 × 10
-3pa, measures Li with line integraph
2+the line of bundle, read the tale of RBS spectrum with line integraph, multichannel analyzer is connected to computing machine, and the backward scattering ion that detector receives inputs computing machine after multichannel analyzer analysis simultaneously, forms RBS spectrum;
(4) RBS of computer acquisition spectrum is imported in SIMNRA software, corresponding experiment parameter is set, draws modulation period and the homogeneity information of multilayer film.
2. the measuring method of multilayer film modulation period according to claim 1 and homogeneity thereof, is characterized in that, the diameter of cylindrical target block is 7mm, is highly 15mm.
3. the measuring method of multilayer film modulation period according to claim 1 and homogeneity thereof, is characterized in that, the ionization electric current in step (2) intermediate ion source is 23A, and target voltage is 5-6kV, and probe voltage is 20kV.
4. the measuring method of multilayer film modulation period according to claim 1 and homogeneity thereof, is characterized in that, in step (2), the accelerating potential at accelerating tube place is adjusted to 1.52MV, and the nitrogen pressure be filled with in accelerating tube is 5 × 10
-3-7 × 10
-3pa.
5. the measuring method of multilayer film modulation period according to claim 1 and homogeneity thereof, is characterized in that, the scattering angle of Au Si surface barrier detector is 170
o, the vacuum tightness measuring target chamber is 0.8 × 10
-3pa.
6. the measuring method of multilayer film modulation period according to claim 1 and homogeneity thereof, is characterized in that, described multilayer film comprise MoN/CrN multilayer film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510793444.XA CN105259194A (en) | 2015-11-18 | 2015-11-18 | Measuring method for modulation period and uniformity of multiple layers of films |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510793444.XA CN105259194A (en) | 2015-11-18 | 2015-11-18 | Measuring method for modulation period and uniformity of multiple layers of films |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105259194A true CN105259194A (en) | 2016-01-20 |
Family
ID=55098964
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510793444.XA Pending CN105259194A (en) | 2015-11-18 | 2015-11-18 | Measuring method for modulation period and uniformity of multiple layers of films |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105259194A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106645991A (en) * | 2016-12-13 | 2017-05-10 | 上海卫星工程研究所 | Electron radiation test device and method of space-borne ultra-light alloy material |
| CN109343102A (en) * | 2018-09-11 | 2019-02-15 | 东莞中子科学中心 | A kind of white light neutron source charged particle detection spectrometer vacuum target chamber |
| CN110441476A (en) * | 2019-07-19 | 2019-11-12 | 合肥国轩高科动力能源有限公司 | Method for rapidly evaluating coating uniformity |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08178874A (en) * | 1994-12-27 | 1996-07-12 | Hitachi Ltd | Surface-analyzing apparatus |
| US20050067567A1 (en) * | 2003-09-26 | 2005-03-31 | Kabushiki Kaisha Kobe Seiko Sho(Kobe Steel, Ltd.) | Sample analyzer |
| CN103119197A (en) * | 2010-08-31 | 2013-05-22 | 株式会社岛津制作所 | Amorphous silicon nitride film and method for producing same |
-
2015
- 2015-11-18 CN CN201510793444.XA patent/CN105259194A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08178874A (en) * | 1994-12-27 | 1996-07-12 | Hitachi Ltd | Surface-analyzing apparatus |
| US20050067567A1 (en) * | 2003-09-26 | 2005-03-31 | Kabushiki Kaisha Kobe Seiko Sho(Kobe Steel, Ltd.) | Sample analyzer |
| CN103119197A (en) * | 2010-08-31 | 2013-05-22 | 株式会社岛津制作所 | Amorphous silicon nitride film and method for producing same |
Non-Patent Citations (5)
| Title |
|---|
| X. M. WANG ET AL.: "Small cluster ions from source of negative ions by cesium sputtering", 《NUCLEAR INSTRUMENTS AND METHODS IN PHYSICS RESEARCH B》 * |
| 刘博志: "铬基金属与氮化物纳米多层薄膜调制结构研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 尚世铉: "《近代物理实验技术》", 30 June 1993, 高等教育出版社 * |
| 李青年: "《薄膜制品设计生产加工新工艺与应用新技术实务全书》", 30 April 2004, 银声音像出版社 * |
| 陆家和 等: "《现代分析技术》", 30 September 1995, 清华大学出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106645991A (en) * | 2016-12-13 | 2017-05-10 | 上海卫星工程研究所 | Electron radiation test device and method of space-borne ultra-light alloy material |
| CN106645991B (en) * | 2016-12-13 | 2019-02-15 | 上海卫星工程研究所 | A kind of the electron radiation experimental rig and method of spaceborne ultra-light alloy material |
| CN109343102A (en) * | 2018-09-11 | 2019-02-15 | 东莞中子科学中心 | A kind of white light neutron source charged particle detection spectrometer vacuum target chamber |
| CN109343102B (en) * | 2018-09-11 | 2020-09-29 | 东莞中子科学中心 | Vacuum target chamber of white-light neutron source charged particle detection spectrometer |
| CN110441476A (en) * | 2019-07-19 | 2019-11-12 | 合肥国轩高科动力能源有限公司 | Method for rapidly evaluating coating uniformity |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103226057B (en) | Multifunctional high-efficiency laser damage test device and method in vacuum environment | |
| US9312111B2 (en) | Apparatus and method for sub-micrometer elemental image analysis by mass spectrometry | |
| US4864131A (en) | Positron microscopy | |
| CN105259194A (en) | Measuring method for modulation period and uniformity of multiple layers of films | |
| CN107078011A (en) | Charged particle beam apparatus and information processor | |
| CN105301088A (en) | Accelerator mass spectrometer with simultaneous isotope measurement function | |
| Calligaro et al. | Ion beam analysis with external beams: Recent set-up improvements | |
| CN104965217B (en) | A kind of measuring device and method of pulsed ionizing beam cross-sectional image | |
| Yamada et al. | MeV-energy probe SIMS imaging of major components in animal cells etched using large gas cluster ions | |
| CN109632925B (en) | SIMS (simple in-situ chemical vapor deposition) optimization detection method for concentration and distribution of trace impurity elements in AlN (aluminum nitride) | |
| Sharp et al. | Uranium ion yields from monodisperse uranium oxide particles | |
| Eller et al. | SIMS instrumentation and methodology for mapping of co-localized molecules | |
| Allison et al. | The scintillation response from nai (tl) crystals under bombardment with positive ions of energies 60-600 kev | |
| WO2016154958A1 (en) | Accelerator mass spectrometry device for simultaneously measuring isotopes | |
| Li et al. | Charge integration in external PIXE–PIGE for the analysis of aerosol samples | |
| US5063293A (en) | Positron microscopy | |
| CN103954680B (en) | Identification device that a kind of optical thin film laser is injured and recognition methods | |
| Ismail et al. | Comprehensive method to analyze thick insulating samples using PIXE technique | |
| CN111060545B (en) | Method for detecting coating integrity of active substance of lithium ion battery | |
| Xu et al. | Beam charge integration in external beam PIXE–PIGE analysis utilizing proton backscattering with an extraction window | |
| Ridley | A large aperture detector for slow positive ions | |
| Harton et al. | Mass fractionation of carbon and hydrogen secondary ions upon Cs+ and O2+ bombardment of organic materials | |
| Burducea et al. | Applications at the 3 MV TandetronTM from IFIN-HH | |
| Hua et al. | Tpx3Cam applications: 3D momentum reconstruction based on analytic time-walk correction and noise reduction | |
| CN101650441A (en) | Method for detecting electron emission of plasma |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160120 |