CN103076352B - Method for obtaining high-quality X-ray absorption spectrum of thin film sample - Google Patents
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- 238000000862 absorption spectrum Methods 0.000 title claims abstract description 43
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- 239000000758 substrate Substances 0.000 claims abstract description 28
- 230000008569 process Effects 0.000 claims abstract description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 3
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 3
- 239000001301 oxygen Substances 0.000 claims abstract description 3
- 239000000523 sample Substances 0.000 claims description 60
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 238000002056 X-ray absorption spectroscopy Methods 0.000 claims description 4
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- 201000004569 Blindness Diseases 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
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- NWAIGJYBQQYSPW-UHFFFAOYSA-N azanylidyneindigane Chemical compound [In]#N NWAIGJYBQQYSPW-UHFFFAOYSA-N 0.000 description 1
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a method for obtaining a high-quality X-ray absorption spectrum of a thin film sample. In a measuring process of the thin film sample, after diffraction spots are generated by exposing a single-crystal substrate of the thin film sample through a dry film, exposure points are shielded by a lead sheet to prevent diffraction signals caused by the substrate from entering a detector so as to obtain the high-quality X-ray absorption spectrum of the thin film sample. The dry film consists of carbon, nitrogen, oxygen and a trace element lithium, has an effective atomic number within 6-8 and the film thickness of about 100-200 microns, does not cause a serious background to the hard X-ray absorption spectrum, and particularly can be integrated with a light filter in the detector to filter out a scattering effect caused by incident light and a diffraction effect caused by the substrate of the thin film sample. Therefore, a simple and effective way for obtaining the high-quality X-ray absorption spectrum of the thin film sample is provided.
Description
Technical field
The present invention relates to a kind of method obtaining X ray absorption spectra, be specifically related to a kind of method obtaining high-quality X-ray absorption spectrum of thin film sample.
Background technology
In recent years, III-nitride semiconductor material (indium nitride, gallium nitride, aluminium nitride) as superior third generation semiconductor material, studied widely at numerous areas such as photoelectronic industry (comprising white-light illuminating), high-frequency high-speed device, high power device, Radar Technology, ultraviolet detector and obtained application.But III-nitride semiconductor material prepares mostly in foreign substrate.At present, in silicon base and Sapphire Substrate Epitaxial growth high-quality group III-nitride and the new round upsurge of adulterating and studying and becoming the research of whole group III-nitride overall application of being correlated with, also urgent electricity/optical property of wishing can to carry out being correlated with, the research work of doping impact/mechanism aspect, for further membraneous material growth and Physical Property Analysis provide experimental data.In addition, the integrated ferroelectric element based on ferroelectric thin film also has important application prospect, as ferro-electric field effect transistor, dynamic RAM and adjustable microwave element etc. in computerized information storage, data processing.Integrated ferroelectric electronic devices and components are in application research and development, as increasing integrated level, improving Performance And Reliability, also in the urgent need to understanding the several problem in science in preparation process and failure procedure, the most outstanding with film surface interface, size effect, ferroelectric fatigue.The progress of these problems significantly promotes being expected to produce the development of Integrated ferroelectrics.In addition, some transiting group metal elements mixes the dilute magnetic semiconductor of formation in semiconductive thin film because having ferromagnetism and semiconducting electrical conductivity matter concurrently, is the critical material of following spintronics.New approach is provided by for exploration solution dilute magnetic semiconductor material preparation and a modification difficult problem to the Local Structure research of film surface structure and doped chemical.
Synchrotron radiation applications absorption spectroscopy techniques has obtained many significant achievements in the local environment structure of research condensed state matter Atom.Based on X ray glancing incidence technology, people are by regulating the grazing angle of X ray can the penetration depth of control X-ray.By means of Grazing Incidence X-Ray absorption spectroscopy techniques, the occupy-place of specific atoms on the detectable film surface of people or interface, bond distance is provided, the Local atomic structure information such as coordination number, utilize the near side (ns) feature of absorption spectra can obtain and specific atoms symmetry, the information that electronic structure is relevant, this category information has important value to understanding the chemistry of film surface and physical process and even relevant practical application.
In order to detect Local Structure and the Electronic Structure Characteristics of film sample element-specific, the X ray absorption spectrum method under fluorescence mode is ideal method, and as shown in Figure 1, front ionization chamber and fluorescent probe constitute fluorescent X-ray absorption spectrum Setup Experiments.Front ionization chamber detection incident intensity I
0; Fluorescent probe receives the fluorescence that sample produces, fluorescence intensity I
fbe proportional to X ray absorption probability, carry out energy scan in specific energy range, and pointwise gathers I
0and I
f, the I obtained
fto I
0ratio and energy relationship curve.Here, the X ray that fluorescent probe receives both had comprised the fluorescent line corresponding with element of interest, comprised again the diffraction of single crystal substrates, and with elasticity and non-resilient (Compton) scattered x-ray etc.The wherein fluorescent line intensity I of element of interest
fas the signal intensity of X ray absorption spectrum, the diffraction of single crystal substrates and Elastic and Nonelastic Scattering then form back end signal.Under the fluorescence mode of high-quality, X ray absorption spectrum measuring technique requires to suppress back end signal section, improves the ratio of element fluorescence signal to be measured, thus improves signal to noise ratio (S/N ratio).
Those skilled in the art will know that, film sample is prepared in many cases and obtains in the single crystalline substrate such as silicon base, sapphire and quartz, what the X ray absorption spectra of experiment gained can be mixed with some causes diffracted signal because of single crystalline substrate, therefore, substrate contribution in X ray absorption spectrum is reduced to minimum, and the diffraction peak etc. weakened in X ray absorption spectrum, be problem demanding prompt solution in the high-quality X ray absorption spectra measuring technique of film sample.
Prior art discloses by fast rotational film sample, to reduce the technical scheme of the diffraction effect of its substrate, but the vibration of sample or wave, also can bring the error of X ray absorption spectrum.In addition, those skilled in the art also attempt selecting different incident angles, collect X ray absorption spectrum, but diffraction peak only change peak position sometimes, can't disappear.Also have with regard to the X ray absorption spectrum under splicing different incidence angles degree, deduct diffraction peak effect from experimental data, in this case, require each film sample uniform surface measured, back end is completely the same; The detector of energy resolution also can play fine effect in many cases, because diffraction peak and fluorescent peak energy have very large difference, detector only accepts the fluorescence that sample produces, but, when diffraction peak is enough strong time, energy-resolved detector temporary blindness can be caused, be unfavorable for that energy-resolved detector normally works.
Therefore, in the urgent need to proposing a kind of method of simple acquisition high-quality X-ray absorption spectrum of thin film sample.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of method obtaining high-quality X-ray absorption spectrum of thin film sample is provided.
For achieving the above object, the present invention adopts following technical scheme:
In the measuring process of film sample, after adopting diffraction spot caused by dry type exposure film sample substrate, cover diffraction spot by sheet lead, stop the diffracted signal caused by substrate to enter detector, thus obtain high-quality X-ray absorption spectrum of thin film sample.
More specifically, method of the present invention comprises the steps:
(1) what prepare X ray absorption spectroscopy sniffer adopts the front work of spectrum;
(2) spectrum is adopted to sample, quick collection experimental data, be confirmed whether to occur obvious diffraction peak, if having, perform step (3);
(3) before probe, the dry type film coincide with probe area size is placed, rapid data collection;
(4), after data acquisition terminates, take off dry type film, cover diffraction spot with sheet lead;
(5) before the dry type film after process being placed in probe again, rapid scanning again;
(6) observe absorption line and whether still occur diffraction peak, if having, when repeating salt free ligands peak superposition on step (4)-(5) to absorption line, then gather absorption spectra.
Wherein, above-mentioned method also comprises step (7) further: still occur diffraction peak if normally adopt in the absorption line of spectrum, by adopting in the interval energy range being arranged on diffraction peak appearance of spectrum, repeats step (4)-(6).
Method of the present invention, also comprises the adjustment to sample deflection angle in step (2).
The film sample X ray absorption spectra that method of the present invention is applicable in silicon substrate or Sapphire Substrate or other single crystalline substrate is measured.Wherein preferably described film sample is the film sample in silicon substrate or Sapphire Substrate, and the film thickness on substrate is from several nanometer to some tens of pm, and the energy range being detected element in film is at 5-20KeV.
Method of the present invention, described sheet lead thickness is 0.8-1.5mm, and preferably described sheet lead thickness is 1mm.The size of the large lab scale exposure station of sheet lead and determining, is specifically as the criterion can play bridging effect.
X-ray detection device of the present invention is preferably fluorescence mode X ray absorption spectroscopy sniffer.Described dry type film is the X-ray sensitive film of flushing-free, and described dry type film is the X-ray sensitive film of flushing-free, and this dry type film is by carbon, nitrogen, the elemental lithium of oxygen and trace is formed, and effective atomic number is between 6-8, and film stock thickness is about 100-200 micron.This film for the X-radiation-sensitive of energy range 4-20KeV, the actinometry film GAFCHROMIC EBT such as adopted in embodiments of the present invention, GAFCHROMICRTQA etc.Serious back end can not be brought to the measurement of hard X-x ray absorption spectrum x, particularly can also be integrated with the optical filter in sniffer.
In step as described in the present invention (3) and step (5), the optical filter accessible site in dry type film and sniffer uses.The diffraction effect that the scattering effect caused due to incident light with filtering and film sample substrate cause, thus, a kind of more simple and effective approach is provided, obtains the high-quality X-ray absorption spectra of film sample.
Below in conjunction with accompanying drawing, the present invention is further described in detail:
The method of acquisition high-quality X-ray absorption spectrum of thin film sample of the present invention, specifically comprises the steps:
1, under preparing fluorescence mode, adopting of X ray absorption spectra sniffer composes front work; Preliminary work described herein is understood, as device light path calibration etc. by those skilled in the art;
2, do not add any process, with routine operation quick collection experimental data, judge whether occur obvious diffraction peak in absorption line; If have, then perform step 3;
3, before scanning X-ray energy being moved on to limit, detector front end places a dry type film coincide with its probe area size, rapid data collection again;
4, after data acquisition terminates, take off dry type film, observe the diffraction spot (also exposure station can be claimed) on it, because the fluorescence signal detected is 4 π angular dispersed, so the exposure station of all essence all may produce harmful effect to experimental data, suitable size should be got in former capital, and thickness is that the lead of about 1mm covers diffraction spot;
5, before X-ray energy being moved on to element absorption limit to be measured, will cover before the dry type film processed is refitted in probe with lead, rapid scanning again;
6, observe absorption line and whether occur diffraction peak, if having, repeat step 4 to 6; If nothing, then gather absorption line.
In addition, if still there is diffraction peak in the absorption line of normal acquisition, by adopting in the interval energy range being arranged on diffraction peak appearance of spectrum, this diffraction peak of process can be blocked separately according to above disposal route, obtaining high-quality X-ray absorption spectrum of thin film sample.
Adopt technique scheme, the present invention is ingenious be make use of sheet lead and covers diffraction spot thus solve in existing film sample hard X ray absorption spectra because of diffraction peak problem that substrate diffraction effect causes.This technical scheme is simply controlled, but feasibility is high, compared with prior art, it significantly improves the precision of film sample hard X ray, further investigate film surface chemistry for those skilled in the art and physical process provides reliable foundation, be conducive to the development and application of promotion third generation semiconductor material.
Accompanying drawing explanation
Fig. 1 is the X ray absorption spectra sniffer structural representation of fluorescence mode;
Fig. 2 adopts the absorption line comparison diagram before and after the inventive method process;
Wherein, the 1, first slit; 2, front ionization chamber; 3, the second slit; 4, X ray absorption spectrum detector; 5, film sample; 6, dry type film; 7, optical filter; 8, the 3rd slit; 9, rear ionization chamber.
Embodiment
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
The present invention adopts X ray absorption spectra sniffer structure under fluorescence mode as shown in Figure 1, and monochromatic synchrotron radiation light horizontal direction size is limited in (<300um) very among a small circle by two horizontal narrow slits (first slit 1 and the second slit 3).Film sample 5 is placed on high precision deflection instrument, and can adjust sample in the position of vertical direction (precision 0.001mm) and adjust its deflection angle (precision 0.006deg), film sample 5 surface is to be slightly less than strict angle of total reflection θ
cangle θ
itowards the deflection of incident light bunch, the detection of some different depths can be obtained by changing film sample 5 deflection angle.Light beam line penetrates the degree of depth on film sample 5 surface when deflection angle is less than the angle of total reflection, is limited in several nm, and along with deflection angle theta
iincrease and deepen.Incident beam line strength I
0measured by front ionization chamber 2, penetrate light intensity and measured by rear ionization chamber 9.Fluorescence signal includes probe by the x-ray fluorescence detector 4(be vertically positioned at above film sample 5) gather.Because x-ray fluorescence detector 4 is positioned at directly over film sample 5, dry type film 6 and optical filter 7 between x-ray fluorescence detector 4 and film sample 5, the scattering effect that optical filter 7 causes due to incident light for filtering; Dry type film 6 is applied to the diffraction spot being recorded in and mixing in the hard X-radiation absorption spectrometry of film sample 5, then, covers exposure station by sheet lead, stops the diffracted signal caused by substrate to enter detector, thus obtains high-quality X-ray absorption spectrum of thin film sample.
Embodiment 1
Obtain the method for high-quality X-ray absorption spectrum of thin film sample described in the present embodiment, specifically comprise the steps:
1, under preparing fluorescence mode, adopting of X ray absorption spectra sniffer composes front work; Preliminary work described herein is understood, as device light path calibration etc. by those skilled in the art;
2, do not add any process, with routine operation quick collection experimental data, judge whether occur obvious diffraction peak in absorption line; If have, then perform step 3;
3, before scanning X-ray energy being moved on to limit, detector front end places a dry type film coincide with probe area size, rapid data collection again;
4, after data acquisition terminates, take off dry type film, observe diffraction spot on it, because the fluorescence signal detected is 4 π angular dispersed, so the exposure station of all essence all may produce harmful effect to experimental data, suitable size should be got in former capital, and thickness is that the lead of about 1mm covers obvious diffraction spot;
5, before X-ray energy being moved on to element absorption limit to be measured, before being refitted in detector probe with the dry type film of lead process, rapid scanning again;
6, observe absorption line and always whether occur diffraction peak, if having, repeat 4 to 6; If nothing, then gather absorption line.
In addition, if still there is diffraction peak in the absorption line of normal acquisition, by adopting in the interval energy range being arranged on diffraction peak appearance of spectrum, this diffraction peak of process can be blocked separately according to above disposal route, obtaining high-quality X-ray absorption spectrum of thin film sample.
In the present embodiment, described sample is the InGaN material that C surface sapphire substrate grows.Wherein InN molecular density is 6.81g/cm
3, GaN density is 6.15g/cm
3, sapphire (Al
2o
3) density is 3.98g/cm
3, InN and GaN ratio of component is 7:93, and during experiment, deflection angle is 0.15deg.
Adopt technique scheme, the present invention utilizes lead to cover exposure station to evade absorption spectra before and after diffraction peak more as shown in Figure 2, wherein labeling position is the position having obvious diffraction peak to occur.From two absorption lines relatively, this masking methods really effective and elimination easily diffraction peak, obtains the high-quality X ray absorption spectra of this film sample.
Although above with general explanation, embodiment and test, the present invention is described in detail, and on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (9)
1. one kind obtains the method for high-quality X-ray absorption spectrum of thin film sample, it is characterized in that: in the measuring process of film sample, after adopting diffraction spot caused by dry type exposure film sample substrate, diffraction spot is covered by sheet lead, stop the diffracted signal caused by substrate to enter detector, thus obtain high-quality X-ray absorption spectrum of thin film sample.
2. method according to claim 1, is characterized in that, described method comprises the steps:
(1) what prepare X ray absorption spectroscopy sniffer adopts the front work of spectrum;
(2) spectrum is adopted to sample, quick collection experimental data, be confirmed whether to occur obvious diffraction peak, if having, perform step (3);
(3) before probe, the dry type film coincide with probe area size is placed, rapid data collection;
(4), after data acquisition terminates, take off dry type film, cover diffraction spot with sheet lead;
(5) before the dry type film after process being placed in probe again, rapid scanning again;
(6) observe absorption line and whether still occur diffraction peak, if having, when repeating salt free ligands peak superposition on step (4)-(5) to absorption line, then gather absorption spectra.
3. method according to claim 2, it is characterized in that, described method also comprises step (7) further: still occur diffraction peak if normally adopt in the absorption line of spectrum, by adopting in the interval energy range being arranged on diffraction peak appearance of spectrum, repeat step (4)-(6).
4. method according to claim 2, is characterized in that, also comprises the adjustment to sample deflection angle in described step (2).
5. method according to claim 1, is characterized in that, described film sample is film sample in silicon substrate or Sapphire Substrate or other single crystalline substrate; The energy range being detected element in film is at 5-20KeV.
6. method according to claim 1, is characterized in that, described sheet lead thickness is 0.8-1.5mm.
7. method according to claim 6, is characterized in that, described sheet lead thickness is 1mm.
8. method according to claim 1, is characterized in that, described dry type film is the X-ray sensitive film of flushing-free, described dry type film by carbon, nitrogen, the elemental lithium of oxygen and trace is formed, effective atomic number is between 6-8, and film stock thickness is 100-200 micron.
9. method according to claim 2, is characterized in that, in described step (3) and step (5), and the integrated use of optical filter in dry type film and sniffer.
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| CN106841262A (en) * | 2017-02-28 | 2017-06-13 | 梧州市东麟宝石机械有限公司 | A kind of method that x-ray power dissipation fluorescent spectrometry characterizes jewel |
| CN107219241B (en) * | 2017-05-05 | 2020-10-16 | 中国科学院上海光学精密机械研究所 | Measuring device and measuring method for in-situ time-resolved X-ray absorption spectrum |
| CN107941836B (en) * | 2017-12-21 | 2024-04-09 | 长沙新材料产业研究院有限公司 | X-ray absorption spectrum measuring device and measuring method |
| CN113218975A (en) * | 2021-04-25 | 2021-08-06 | 中科合成油技术有限公司 | Surface X-ray absorption spectrum measuring device |
| CN113848221B (en) * | 2021-08-19 | 2023-02-17 | 中国科学院高能物理研究所 | In-situ X-ray absorption spectrum testing device and method |
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| CN103076352A (en) | 2013-05-01 |
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