CN104267055B - Synchrotron radiation energy stabilization device and method - Google Patents
Synchrotron radiation energy stabilization device and method Download PDFInfo
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- CN104267055B CN104267055B CN201410532846.XA CN201410532846A CN104267055B CN 104267055 B CN104267055 B CN 104267055B CN 201410532846 A CN201410532846 A CN 201410532846A CN 104267055 B CN104267055 B CN 104267055B
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- 238000000034 method Methods 0.000 title claims abstract description 15
- 230000005469 synchrotron radiation Effects 0.000 title claims abstract description 12
- 230000006641 stabilisation Effects 0.000 title claims abstract description 6
- 238000011105 stabilization Methods 0.000 title claims abstract description 6
- 239000013078 crystal Substances 0.000 claims abstract description 32
- 229910052751 metal Inorganic materials 0.000 claims description 70
- 239000002184 metal Substances 0.000 claims description 68
- 239000010408 film Substances 0.000 claims description 52
- 238000010521 absorption reaction Methods 0.000 claims description 24
- 230000000087 stabilizing effect Effects 0.000 claims description 16
- 239000010409 thin film Substances 0.000 claims description 15
- 230000001678 irradiating effect Effects 0.000 claims description 10
- 230000005855 radiation Effects 0.000 claims description 6
- 230000001360 synchronised effect Effects 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 229920001721 polyimide Polymers 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 238000013480 data collection Methods 0.000 abstract description 5
- 238000002474 experimental method Methods 0.000 abstract description 5
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 239000007850 fluorescent dye Substances 0.000 abstract 2
- 239000000523 sample Substances 0.000 abstract 1
- 230000002547 anomalous effect Effects 0.000 description 14
- 239000011669 selenium Substances 0.000 description 6
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910052711 selenium Inorganic materials 0.000 description 3
- 208000035389 Ring chromosome 6 syndrome Diseases 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 238000000790 scattering method Methods 0.000 description 2
- 238000012916 structural analysis Methods 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The present invention provides a kind of synchrotron radiation energy stabilization device and method.This synchrotron radiation energy stabilization device, including double-crystal monochromator, also include ionization chamber, metallic film, fluorescent probe, control module, described ionization chamber is positioned on the emitting light path of described double-crystal monochromator, described metallic film is positioned on the emitting light path of described ionization chamber, and described metallic film is obliquely installed relative to the emitting light path of described ionization chamber, the end of probe of described fluorescent probe is towards described metallic film, the fluorescence intensity produced for obtaining the light from described ionization chamber outgoing to be irradiated to described metallic film, described control module is for according to the control coefrficient corresponding to described fluorescence intensity and the relation between rotation threshold value, rotation to double-crystal monochromator is controlled.The program program achieves experiment limit, limit and carries out monitoring and the adjustment of energy, it is ensured that the stability of work, it is ensured that the correctness of data collection.
Description
Technical Field
The invention belongs to the technical field of protein crystal structure analysis, and particularly relates to a synchrotron radiation energy stabilizing device and method.
Background
One key issue in performing protein crystal structure analysis is the acquisition of phase. There are many methods for obtaining phase, and the most common method at present is anomalous scattering. When the energy of incident X-rays approaches the binding energy of an electron in an atom, a photoelectric effect is produced, and the scattering factor of the atom is greatly changed, which is called anomalous scattering. The anomalous scattering method allows the phase to be obtained quickly without actually replacing atoms in the crystal.
The phase problem is solved by the anomalous scattering method, which requires collecting anomalous scattering data separately at several wavelengths near the absorption edge of the atom where anomalous scattering occurs. Collecting data of only one wavelength is called single wavelength anomalous Scattering (SAD); collecting data at multiple wavelengths is called multi-wavelength anomalous scattering (MAD). The wavelength at which absorption is greatest at the absorption edge, the wavelength at the inflection point of the absorption edge, and the wavelength at the high energy end of the absorption edge are typically selected when collecting MAD data. Among them, data collection at the inflection point of the absorption edge is the most difficult. Because at the sharp inflection point of the absorption edge of the element, as shown in fig. 1, the Se element absorption edge and the Se element absorption edge inflection point are schematically shown, a slight energy jitter causes a drastic change of the atomic scattering factor, and in a severe case, the structural analysis fails.
The reasons for the energy change of the incident light are mainly as follows: 1. the angle change of incident light caused by the change of electron orbits; 2. the first crystal in the twin monochromator is deformed by heat.
Disclosure of Invention
The following presents a simplified summary of the invention in order to provide a basic understanding of some aspects of the invention. It should be understood that this summary is not an exhaustive overview of the invention. It is not intended to determine the key or critical elements of the present invention, nor is it intended to limit the scope of the present invention. Its sole purpose is to present some concepts in a simplified form as a prelude to the more detailed description that is discussed later.
The invention provides a synchronous radiation energy stabilizing device, which comprises a double-crystal monochromator, an ionization chamber, a metal film, a fluorescence detector and a control module, wherein the ionization chamber is arranged on the double-crystal monochromator;
the ionization chamber is positioned on an emergent light path of the double-crystal monochromator, the metal film is positioned on the emergent light path of the ionization chamber, and the metal film is obliquely arranged relative to the emergent light path of the ionization chamber;
the detection end of the fluorescence detector faces the metal film and is used for acquiring fluorescence generated when light emitted from the ionization chamber irradiates the metal film and calculating the intensity of the fluorescence;
wherein,I0is the standard incident light intensity of the ionization chamber, If0The standard fluorescence intensity generated when standard incident light irradiates on the film, I is the real-time incident light intensity of the ionization chamber, IfThe real-time fluorescence intensity generated by irradiating the real-time incident light on the metal film.
The invention also provides a synchronous radiation energy stabilizing method, which comprises the following steps:
obtaining the standard incident light intensity of the ionization chamber and the standard fluorescence intensity generated by the irradiation of the standard incident light on the thin film;
acquiring real-time incident light intensity of an ionization chamber and real-time fluorescence intensity generated by irradiating real-time incident light on a metal film;
wherein,I0is the standard incident light intensity of the ionization chamber, If0The standard fluorescence intensity generated when standard incident light irradiates on the film, I is the real-time incident light intensity of the ionization chamber, IfReal-time fluorescence intensity generated when real-time incident light irradiates on the metal film;
controlling the rotation of the bicrystal monochromator according to the relation between the control coefficient corresponding to the real-time intensity of the fluorescence generated by the film and the rotation threshold value, wherein the control coefficient is
The scheme provided by the invention has the advantages that: the energy at the inflection point of the multi-wavelength anomalous scattering absorption edge can be stabilized within the range of 0.2eV by changing the angle between the multi-wavelength anomalous scattering absorption edge and the incident light and changing the incident light energy; the energy can be monitored and adjusted while the experiment is carried out, and the correctness of data collection is ensured; simple and easy to implement, and low in implementation cost.
Drawings
The above and other objects, features and advantages of the present invention will be more readily understood by reference to the following description of the embodiments of the present invention taken in conjunction with the accompanying drawings. The components in the figures are meant to illustrate the principles of the present invention. In the drawings, the same or similar technical features or components will be denoted by the same or similar reference numerals.
FIG. 1 is a schematic diagram of the energy change at the inflection point of the absorption edge and the absorption edge of Se;
FIG. 2 is a schematic diagram of a synchrotron radiation energy stabilizing device provided by an embodiment of the present invention;
fig. 3 is a flowchart of a method for stabilizing energy of synchrotron radiation according to an embodiment of the present invention.
Description of reference numerals:
an ionization chamber-1; a metal thin film-2; a fluorescence detector-3;
a control module-4; a double crystal monochromator-5; storage ring-6;
a collimating mirror-7; a focusing mirror-8; a crystal-9 to be tested;
a detector-10.
Detailed Description
Embodiments of the present invention are described below with reference to the drawings. Elements and features depicted in one drawing or one embodiment of the invention may be combined with elements and features shown in one or more other drawings or embodiments. It should be noted that the figures and description omit representation and description of components and processes that are not relevant to the present invention and that are known to those of ordinary skill in the art for the sake of clarity.
Fig. 2 is a schematic diagram of a synchronous radiation energy stabilizing device according to an embodiment of the present invention.
The embodiment provides a synchronous radiation energy stabilizing device, which comprises a double-crystal monochromator 5, an ionization chamber 1, a metal film 2, a fluorescence detector 3 and a control module 4;
the ionization chamber 1 is positioned on an emergent light path of the double-crystal monochromator 5, the metal film 2 is positioned on the emergent light path of the ionization chamber 1, and the metal film 2 is obliquely arranged relative to the emergent light path of the ionization chamber 1;
the detection end of the fluorescence detector 3 faces the metal film 2 and is used for acquiring the fluorescence intensity generated when the light emitted from the ionization chamber 1 irradiates the metal film 2;
a control module 4 for controlling the rotation of the bicrystal monochromator 5 according to the relation between the control coefficient corresponding to the fluorescence intensity and the rotation threshold value, wherein the control coefficient is
Wherein,I0is the standard incident light intensity of the ionization chamber, If0The standard fluorescence intensity generated when standard incident light irradiates on the film, I is the real-time incident light intensity of the ionization chamber, IfThe real-time fluorescence intensity generated by irradiating the real-time incident light on the metal film.
The storage ring 6 emits a beam of light, the beam of light is incident on the double-crystal monochromator 5 after passing through the collimating lens 7, a focusing lens 8 is arranged on an emergent light path of the double-crystal monochromator 5, and the beam of light is incident on the collimating lens 7 through the double-crystal monochromator 5. A focusing mirror 8 is arranged on an emergent light path of the collimating mirror 7, and light beams are incident on the focusing mirror 8 through the collimating mirror 7. An ionization chamber 1 is arranged on an emergent light path of the focusing mirror 8, and light beams enter the ionization chamber 1 through the focusing mirror 8. A metal film 2 is arranged on an emergent light path of the ionization chamber 1, and light beams are emitted from the ionization chamber 1 and then incident on the metal film 2. A portion of the photons incident on the metal thin film 2 pass through the metal thin film 2, and a portion of the photons excite the metal thin film 2. The metal film 2 is obliquely arranged relative to the emergent light path of the ionization chamber 1, and can effectively absorb the light beam emitted from the ionization chamber 1.
The crystal 9 to be measured is arranged on an emergent light path of the metal film 2, light passing through the metal film 2 is incident on the crystal 9 to be measured, a detector 10 is arranged on the emergent light path of the crystal 9 to be measured, and the detector 10 collects MAD numerical values of the crystal 9 to be measured.
The detection end of the fluorescence detector 3 faces the metal film 2, the metal element on the metal film 2 is excited by photons, and the generated fluorescence intensity is captured by the fluorescence detector 3.
The control module 4 controls the rotation of the bicrystal monochromator 5 according to the relation between the control coefficient corresponding to the fluorescence intensity and the rotation threshold value, wherein the control coefficient is
Wherein,I0is the standard incident light intensity of the ionization chamber, If0The standard fluorescence intensity generated when standard incident light irradiates on the film, I is the real-time incident light intensity of the ionization chamber, IfThe real-time fluorescence intensity generated by irradiating the real-time incident light on the metal film.
The embodiment can effectively control the rotation of the double-crystal monochromator according to data, and can realize the stabilization of the energy at the inflection point of the multi-wavelength anomalous scattering absorption edge within the range of 0.2 eV;
the energy monitoring and adjusting can be realized while the experiment is carried out, and the correctness of data collection is ensured.
Further, based on the above embodiment, the metal film 2 is a polyimide film plated with a metal element on one side.
When a light beam is incident on the metal thin film 2, a part of photons can excite the metal element to generate fluorescence, and the generated fluorescence signal is collected by the fluorescence detector 3. A portion of the photons pass through the metal film 2.
Further, based on the above embodiment, the metal element is at least one of selenium, copper, gold, silver, and nickel.
And during detection, the corresponding metal film is put into the light path according to the selected element.
Further, the metal element is deposited on the polyimide film by ion sputtering.
Further, based on the above embodiment, an included angle between the metal element surface of the metal thin film and the emergent light path of the ionization chamber is 45 degrees.
This ensures that sufficient through light and sufficient fluorescence signal is fed back to the fluorescence detector 3.
Further, based on the above embodiment, the fluorescent detector 3 faces to form an angle of 45 degrees with the metal element surface of the metal film.
This ensures that the fluorescence detector 3 receives the maximum amount of fluorescence signal generated by the metal thin film.
Further, based on the above embodiment, the thickness of the element plated on the metal thin film 2 is preferably 60 to 120 nm.
This range of the thickness of the metal element ensures sufficiently strong through light and sufficiently strong fluorescence signal.
Further, the thickness of the element to be plated on the thin film is preferably 100 nm.
Fig. 3 is a flowchart of a method for stabilizing energy of synchrotron radiation according to an embodiment of the present invention.
As shown in fig. 3, another embodiment of the present invention discloses a method for stabilizing synchrotron radiation energy, which includes the following steps:
s1, obtaining the standard incident light intensity of the ionization chamber and the standard fluorescence intensity generated by the standard incident light irradiating the thin film;
s2, acquiring the real-time incident light intensity of the ionization chamber and the real-time fluorescence intensity generated by irradiating the real-time incident light on the metal film;
in the actual test process, the energy E at the inflection point of the absorption edge of a specific element in the crystal to be tested is selected0The metal film is selected accordingly according to the specific element. For example, but not limited to, if the selenium element in the crystal to be tested is selected for multi-wavelength anomalous scattering experiments, selenium with metal is used in collecting anomalous scattering data at the inflection point of the absorption edgeThe metal thin film of (2). Experiments indicate that under the condition that the bicrystal monochromator is in a standard stable working state, the energy E at the inflection point of the absorption edge of a specific element is acquired0The corresponding standard incident light intensity of the ionization chamber and the standard fluorescence intensity generated by the standard incident light irradiating the thin film are obtained according to the following relational expression0. The real-time absorption coefficient μ is also obtained from the following relational expression.
Wherein,I0is the standard incident light intensity of the ionization chamber, If0The standard fluorescence intensity generated when standard incident light irradiates on the film, I is the real-time incident light intensity of the ionization chamber, IfReal-time fluorescence intensity generated when real-time incident light irradiates on the metal film;
s3, controlling the rotation of the bicrystal monochromator according to the relation between the control coefficient corresponding to the real-time intensity of the fluorescence generated by the film and the rotation threshold value, wherein the control coefficient is
According to the embodiment, the rotation of the double-crystal monochromator can be controlled according to the relation between the corresponding control coefficient and the rotation threshold value of the real-time intensity of the fluorescence generated by the metal film, and further stable synchronous radiation energy can be obtained.
Further, controlling the rotation of the bicrystal monochromator according to the relationship between the control coefficient corresponding to the real-time intensity of the fluorescence generated by the metal film and the rotation threshold value, comprises:
if the control coefficient is larger than the rotation threshold, controlling the double-crystal monochromator to rotate by one step to cause the energy change of 0.2eV (namely, changing the incident light energy by changing the angle between the double-crystal monochromator and the incident light), and otherwise, controlling the double-crystal monochromator to keep still. Wherein the rotation threshold is used to characterize the minimum value of the bimorph monochromator that needs to be rotated, for example, but not limited to, the rotation threshold may be 0.1.
The embodiment can realize that the energy at the inflection point of the multi-wavelength anomalous scattering absorption edge is stabilized in the range of 0.2eV in a controllable range, and the MAD data is collected. The method avoids the severe change of the atomic scattering factor caused by the tiny energy jitter at the sharp inflection point of the absorption edge of the element, which leads to inaccurate data collection and even structural analysis failure.
The detector can be but not limited to a CCD detector, the relation between a control coefficient and a rotation threshold value can be judged after data acquisition every time, and rotation control is carried out on the double-crystal monochromator according to a judgment result.
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 (8)
1. A synchronous radiation energy stabilizing device comprises a double-crystal monochromator, an ionization chamber, a metal film, a fluorescence detector and a control module;
the ionization chamber is positioned on an emergent light path of the double-crystal monochromator, the metal film is positioned on the emergent light path of the ionization chamber, and the metal film is obliquely arranged relative to the emergent light path of the ionization chamber;
the detection end of the fluorescence detector faces the metal film and is used for acquiring the fluorescence intensity generated when the light emitted from the ionization chamber irradiates the metal film;
the control module is used for controlling the rotation of the bicrystal monochromator according to the relation between the control coefficient corresponding to the fluorescence intensity and the rotation threshold value, and the control coefficient is
Wherein,I0is the standard incident light intensity of the ionization chamber, If0Standard fluorescence intensity generated by irradiating standard incident light on the metal film, I real-time incident light intensity of the ionization chamber, IfReal-time fluorescence intensity generated when real-time incident light irradiates on the metal film; mu.s0Mu is the initial absorption coefficient and mu is the real-time absorption coefficient.
2. The synchrotron radiation energy stabilizing apparatus of claim 1, wherein said metal film is a polyimide film plated with a metal element on one side.
3. The synchrotron energy stabilizing apparatus of claim 2, wherein the metallic element is at least one of copper, gold, silver, and nickel.
4. The synchrotron energy stabilizing apparatus of claim 2, wherein the metal element surface of the metal film forms an angle of 45 degrees with the exit light path of the ionization chamber.
5. The synchrotron energy stabilizing apparatus of claim 2, wherein said fluorescence detector is oriented at an angle of 45 degrees with respect to a metal element surface of said metal film.
6. A synchrotron energy stabilizing apparatus as claimed in any one of claims 2 to 5, wherein said metal thin film is plated with metal elements having a thickness of 60 to 120 nm.
7. A synchrotron radiation energy stabilization method is characterized by comprising the following steps:
obtaining the standard incident light intensity of the ionization chamber and the standard fluorescence intensity generated by the irradiation of the standard incident light on the thin film;
acquiring real-time incident light intensity of an ionization chamber and real-time fluorescence intensity generated by irradiating real-time incident light on a metal film;
wherein,I0is the standard incident light intensity of the ionization chamber, If0Standard fluorescence intensity generated by irradiating standard incident light on the metal film, I real-time incident light intensity of the ionization chamber, IfReal-time fluorescence intensity generated when real-time incident light irradiates on the metal film;
controlling the rotation of the bicrystal monochromator according to the relation between the control coefficient corresponding to the real-time intensity of the fluorescence generated by the metal film and the rotation threshold value, wherein the control coefficient isμ0Mu is the initial absorption coefficient and mu is the real-time absorption coefficient.
8. The synchrotron radiation energy stabilization method of claim 7, wherein the controlling the rotation of the bimorph monochromator according to the relationship between the control coefficient corresponding to the real-time intensity of the fluorescence generated by the metal thin film and the rotation threshold comprises:
and if the control coefficient is larger than the rotation threshold, controlling the double-crystal monochromator to rotate by one step to cause energy change of 0.2eV, otherwise, controlling the double-crystal monochromator to keep still.
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| CN108707968A (en) * | 2018-04-10 | 2018-10-26 | 中国科学院高能物理研究所 | A kind of monochromating crystal and preparation method thereof of high throughput |
| CN109668917B (en) * | 2018-09-29 | 2020-06-19 | 中国科学院高能物理研究所 | Method for obtaining X-rays with different energy bandwidths by using monochromator |
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| CN1829910B (en) * | 2003-06-02 | 2012-05-23 | X射线光学系统公司 | Method and apparatus for implement XANES analysis |
| WO2011066447A1 (en) * | 2009-11-25 | 2011-06-03 | Columbia University | Confocal double crystal monochromator |
| GB201213789D0 (en) * | 2012-08-02 | 2012-09-12 | Commw Scient Ind Res Org | An X-ray fluorescence analyser |
| CN103175857B (en) * | 2013-03-14 | 2015-06-03 | 中国科学院高能物理研究所 | Device specially used for grazing incidence XAFS (X-ray Absorption Fine Structure) experiment and regulating method of device |
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