CN104267055B - Synchrotron radiation energy stabilization device and method - Google Patents

Synchrotron radiation energy stabilization device and method Download PDF

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Publication number
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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China
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metallic film
ionization chamber
real
time
double
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CN201410532846.XA
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Chinese (zh)
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CN104267055A (en
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常广才
王文佳
石泓
刘鹏
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中国科学院高能物理研究所
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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

Synchrotron radiation energy stabilization device and method
Technical field
The invention belongs to protein structures analytic technique field, particularly relate to a kind of synchrotron radiation energy Amount stabilising arrangement and method.
Background technology
During carrying out protein structures parsing, a key issue is the acquisition of phase place.Obtain The method taking phase place has a variety of, and presently the most conventional method is anomalous scattering method.As incident X Ray energy close to atom can produce during the binding energy of certain electronics photoelectric effect, at this moment the dissipating of atom Penetrating the factor and can produce great changes, this phenomenon is called anomalous scattering.Utilize the anomalous scattering method can be Phase place is obtained efficiently in the case of the most actually replacing crystal Atom.
Utilizing anomalous scattering method to solve phase problem, needing the Atomic Absorption limit there is anomalous scattering attached Closely collect anomalous scattering data respectively with several wavelength.The data only collecting a wavelength are referred to as Single wavelength Anomalous scattering (single wavelength anomalous diffraction, SAD);Collect multiple ripple Long data be referred to as multi-wavelength anomalous scattering (multi-wavelength anomalous diffraction, MAD).When collecting MAD data, it is typically chosen in ABSORPTION EDGE the wavelength absorbing maximum, ABSORPTION EDGE Wavelength at flex point, and the wavelength of ABSORPTION EDGE high-energy tail.Wherein, the data collection at ABSORPTION EDGE flex point Difficulty the most.Because at the ABSORPTION EDGE flex point that element is precipitous, Se element absorption limit as shown in Figure 1 And schematic diagram at ABSORPTION EDGE flex point, small energy shake will cause the violent change of atomic scattering factor Changing, serious situation eventually results in structure elucidation failure.
The reason causing incident illumination energy variation mainly has following 2 points: 1. electron orbit change causes Incident angle of light change;2. the first crystalline substance in double-crystal monochromator is by thermal deformation.
Summary of the invention
Brief overview about the present invention given below, in order to some side about the present invention is provided The basic comprehension in face.Should be appreciated that this general introduction is not that the exhaustive about the present invention is summarized.It It is not intended to determine the key of the present invention or pith, is not the model of the intended limitation present invention Enclose.Its purpose is only to provide some concept in simplified form, more detailed in this, as discuss after a while The thin preamble described.
The present invention provides a kind of synchrotron radiation energy stabilization device, including double-crystal monochromator, also includes electricity From room, metallic film, fluorescent probe, control module;
Described ionization chamber is positioned on the emitting light path of described double-crystal monochromator, and described metallic film is positioned at institute State on the emitting light path of ionization chamber, and described metallic film inclines relative to the emitting light path of described ionization chamber Tiltedly arrange;
The end of probe of described fluorescent probe is towards described metallic film, for obtaining from described ionization chamber The light of outgoing is irradiated on described metallic film the fluorescence of generation and calculates its intensity;
Wherein,I0For ionization chamber standard input light intensity, If0For standard input light Being irradiated on thin film the standard fluorescence intensity produced, I is the real-time incident intensity of ionization chamber, IfFor reality Time incident illumination be mapped on metallic film produce real-time fluorescence intensity.
The present invention also provides for a kind of synchrotron radiation energy stabilization method, comprises the following steps:
Obtain ionization chamber standard input light intensity, and standard input light is irradiated on thin film the standard of generation Fluorescence intensity;
Obtain the real-time incident intensity of ionization chamber, and incident illumination is mapped on metallic film generation in real time Real-time fluorescence intensity;
Wherein,I0For ionization chamber standard input light intensity, If0For standard input light Being irradiated on thin film the standard fluorescence intensity produced, I is the real-time incident intensity of ionization chamber, IfFor reality Time incident illumination be mapped on metallic film produce real-time fluorescence intensity;
According to described thin film produce fluorescence Real-time intensity corresponding to control coefrficient with rotate threshold value it Between relation, the rotation to double-crystal monochromator is controlled, and described control coefrficient is
The such scheme that the present invention provides, advantage is: can change with incident angle of light by changing it Become incident illumination energy, it is possible to achieve the energy stabilization at multi-wavelength anomalous scattering ABSORPTION EDGE flex point existed In the range of 0.2eV;Experiment limit, limit can be realized and carry out monitoring and the adjustment of energy, it is ensured that data are received The correctness of collection;Simple, implementation cost is low.
Accompanying drawing explanation
Below with reference to the accompanying drawings illustrate embodiments of the invention, the present invention can be more readily understood that Above and other objects, features and advantages.Parts in accompanying drawing are intended merely to illustrate that the present invention's is former Reason.In the accompanying drawings, same or similar technical characteristic or parts will use same or similar accompanying drawing Labelling represents.
Fig. 1 is energy variation schematic diagram at Se element absorption limit and ABSORPTION EDGE flex point;
The schematic diagram of the synchrotron radiation energy stabilization device that Fig. 2 provides for the embodiment of the present invention;
The flow chart of the synchrotron radiation energy stabilization method that Fig. 3 provides for the embodiment of the present invention.
Description of reference numerals:
Ionization chamber-1;Metallic film-2;Fluorescent probe-3;
Control module-4;Double-crystal monochromator-5;Storage rings-6;
Collimating mirror-7;Focus lamp-8;Crystal-9 to be measured;
Detector-10.
Detailed description of the invention
Embodiments of the invention are described with reference to the accompanying drawings.An accompanying drawing or a kind of real in the present invention Execute the element described in mode and feature can with in one or more other accompanying drawing or embodiment The element and the feature that illustrate combine.It should be noted that, for purposes of clarity, accompanying drawing and explanation save Omit unrelated to the invention, parts known to persons of ordinary skill in the art and the expression of process and retouched State.
The schematic diagram of the synchrotron radiation energy stabilization device that Fig. 2 provides for the embodiment of the present invention.
The present embodiment provides a kind of synchrotron radiation energy stabilization device, including double-crystal monochromator 5, also wraps Include ionization chamber 1, metallic film 2, fluorescent probe 3, control module 4;
Ionization chamber 1 is positioned on the emitting light path of double-crystal monochromator 5, and metallic film 2 is positioned at ionization chamber 1 Emitting light path on, and metallic film 2 is obliquely installed relative to the emitting light path of ionization chamber 1;
The end of probe of fluorescent probe 3 is towards metallic film 2, for obtaining from ionization chamber 1 outgoing Light is irradiated on metallic film 2 fluorescence intensity produced;
Control module 4, for according to the control coefrficient corresponding to fluorescence intensity and between rotation threshold value Relation, the rotation to double-crystal monochromator 5 is controlled, and control coefrficient is
Wherein,I0For ionization chamber standard input light intensity, If0For standard input light Being irradiated on thin film the standard fluorescence intensity produced, I is the real-time incident intensity of ionization chamber, IfFor reality Time incident illumination be mapped on metallic film produce real-time fluorescence intensity.
Storage rings 6 send light beam, and light beam incides on double-crystal monochromator 5 after collimating mirror 7, Being provided with focus lamp 8 on the emitting light path of double-crystal monochromator 5, light beam is incident via double-crystal monochromator 5 On collimating mirror 7.Being provided with focus lamp 8 on the emitting light path of collimating mirror 7, light beam is via collimating mirror 7 incide on focus lamp 8.Be provided with ionization chamber 1 on the emitting light path of focus lamp 8, light beam via Focus lamp 8 incides on ionization chamber 1.Metallic film 2 it is provided with on the emitting light path of ionization chamber 1, Light beam incides metallic film 2 after ionization chamber 1 outgoing.Incide on metallic film 2 wherein A part of photon can pass metallic film 2, and a part of photon can excite metallic film 2.Metallic film 2 are obliquely installed relative to the emitting light path of ionization chamber 1, can effectively absorb by ionization chamber 1 outgoing Light beam.
Crystal 9 to be measured is arranged on the emitting light path of metallic film 2, and the light through metallic film 2 enters It is mapped on crystal 9 to be measured, the emitting light path of crystal 9 to be measured is provided with detector 10, detector The 10 MAD numerical value collecting crystal 9 to be measured.
The end of probe of fluorescent probe 3 is towards metallic film 2, the metallic element quilt on metallic film 2 Photon excitation, the fluorescence intensity of generation is caught by fluorescent probe 3.
Control module 4 is according to according to the control coefrficient corresponding to fluorescence intensity and between rotation threshold value Relation, the rotation to double-crystal monochromator 5 is controlled, and control coefrficient is
Wherein,I0For ionization chamber standard input light intensity, If0For standard input light Being irradiated on thin film the standard fluorescence intensity produced, I is the real-time incident intensity of ionization chamber, IfFor reality Time incident illumination be mapped on metallic film produce real-time fluorescence intensity.
The present embodiment can effectively control the rotation of double-crystal monochromator according to data, it is possible to achieve by many ripples Energy stabilization at long anomalous scattering ABSORPTION EDGE flex point is in the range of 0.2eV;
Experiment limit, limit can be realized and carry out monitoring and the adjustment of energy, it is ensured that data collection correct Property.
Further, based on above-described embodiment, metallic film 2 is coated with the polyamides of metallic element for side Imines thin film.
When light beam incides on metallic film 2, a part of photon can excite metallic element to produce fluorescence, The fluorescence signal produced is collected by fluorescent probe 3.A part of photon passes metallic film 2.
Further, based on above-described embodiment, metallic element be in selenium, copper, gold, silver, nickel extremely Few one.
According to selected above-mentioned a kind of element during detection, corresponding metallic film is put in light path.
Further, above-mentioned metallic element is deposited with on Kapton by ion sputtering process.
Further, based on above-described embodiment, the metallic element face of metallic film and the outgoing of ionization chamber Light path angle is 45 degree.
So can ensure that enough straight-through light and enough fluorescence signals feed back to fluorescent probe 3.
Further, based on above-described embodiment, fluorescent probe 3 is towards the metal unit with metallic film The angle that vegetarian noodles is formed is 45 degree.
So can ensure that the fluorescence signal that fluorescent probe 3 the maximum amount of reception metallic film produces.
Further, based on above-described embodiment, metallic film 2 plated element thickness is preferably 60-120nm。
The thickness range of this metallic element can ensure that sufficiently strong straight-through light and produces sufficiently strong glimmering Optical signal.
Further, above-mentioned thin film plated element thickness is preferably 100nm.
The flow chart of the synchrotron radiation energy stabilization method that Fig. 3 provides for the embodiment of the present invention.
As it is shown on figure 3, further embodiment of this invention discloses a kind of synchrotron radiation energy stabilization method, Comprise the following steps:
S1, obtains ionization chamber standard input light intensity, and standard input light is irradiated on thin film generation Standard fluorescence intensity;
S2, obtains the real-time incident intensity of ionization chamber, and incident illumination is mapped on metallic film produce in real time Raw real-time fluorescence intensity;
In actual test process, energy at a certain element-specific ABSORPTION EDGE flex point in selected crystal to be measured Amount E0, select metallic film accordingly according to this element-specific.Such as but not limited to, if selected Collect the selenium element in crystal to be measured and carry out multi-wavelength anomalous scattering experiment, then collect ABSORPTION EDGE flex point The metallic film with metallic selenium is used during place's anomalous scattering data.Point out in experiment, namely twin crystal list In the case of color device is in standard stabiliser duty, obtain energy at element-specific ABSORPTION EDGE flex point E0Corresponding ionization chamber standard input light intensity, and standard input light is irradiated on thin film to produce Standard fluorescence intensity, and obtain initial absorptance μ according to relationship below0.It addition, go back root Real-time absorptance μ is obtained according to following relational expression.
Wherein,I0For ionization chamber standard input light intensity, If0For standard input light Being irradiated on thin film the standard fluorescence intensity produced, I is the real-time incident intensity of ionization chamber, IfFor reality Time incident illumination be mapped on metallic film produce real-time fluorescence intensity;
S3, produces the control coefrficient corresponding to the Real-time intensity of fluorescence and rotation threshold value according to described thin film Between relation, the rotation to double-crystal monochromator is controlled, and described control coefrficient is
The present embodiment can realize the Real-time intensity of the fluorescence according to metallic film generation to corresponding control Coefficient processed and the relation rotated between threshold value, the rotation to double-crystal monochromator is controlled, and then obtains Stable synchrotron radiation energy.
Further, the control coefrficient corresponding to Real-time intensity of fluorescence is produced according to described metallic film And the relation rotated between threshold value, the rotation to double-crystal monochromator is controlled, including:
If described control coefrficient more than described rotation threshold value, then controls described double-crystal monochromator and turns and move a step 0.2eV energy variation is caused (namely to change incidence by changing double-crystal monochromator and incident angle of light Light energy), otherwise control described double-crystal monochromator and remain stationary as.Wherein, rotate threshold value to be used for characterizing Double-crystal monochromator needs minima when rotating, and can be 0.1 such as but not limited to rotating threshold value.
The present embodiment can be implemented in controlled range, i.e. at multi-wavelength anomalous scattering ABSORPTION EDGE flex point Energy stabilization, in the range of 0.2eV, collects MAD data.Avoid because of the absorption precipitous at element At the flex point of limit, the acute variation of the atomic scattering factor that small energy shake causes, cause data to be received Collect the failure of inaccurate even structure elucidation.
Experiment time detector repeatedly go gather data, wherein, detector can be, but not limited to for Ccd detector, after each data acquisition, all can judge between control coefrficient and rotation threshold value Relation, and carry out double-crystal monochromator rotating control according to judged result, it is real that the program achieves limit Test limit and carry out monitoring and the adjustment of energy, it is ensured that the stability of work, it is ensured that data collection is just Really property.
Last it is noted that above example is only in order to illustrate technical scheme, rather than right It limits;Although the present invention being described in detail with reference to previous embodiment, this area common Skilled artisans appreciate that the technical scheme described in foregoing embodiments still can be repaiied by it Change, or wherein portion of techniques feature is carried out equivalent;And these amendments or replacement, not The essence making appropriate technical solution departs from the spirit and scope of various embodiments of the present invention technical scheme.

Claims (8)

1. a 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, and described metallic film is positioned at institute State on the emitting light path of ionization chamber, and described metallic film inclines relative to the emitting light path of described ionization chamber Tiltedly arrange;
The end of probe of described fluorescent probe is towards described metallic film, for obtaining from described ionization chamber The light of outgoing is irradiated on described metallic film the fluorescence intensity produced;
Described control module, for according to the control coefrficient corresponding to described fluorescence intensity and rotation threshold value Between relation, the rotation to double-crystal monochromator is controlled, and described control coefrficient is
Wherein,I0For ionization chamber standard input light intensity, If0For standard input light Being irradiated on metallic film the standard fluorescence intensity produced, I is the real-time incident intensity of ionization chamber, If The real-time fluorescence intensity produced it is mapped on metallic film for real-time incident illumination;μ0For initial absorption Coefficient, μ is real-time absorptance.
Synchrotron radiation energy stabilization device the most according to claim 1, it is characterised in that institute Stating metallic film is the Kapton that side is coated with metallic element.
Synchrotron radiation energy stabilization device the most according to claim 2, it is characterised in that institute Stating metallic element is at least one in copper, gold, silver and nickel.
Synchrotron radiation energy stabilization device the most according to claim 2, it is characterised in that institute The emitting light path angle in the metallic element face and described ionization chamber of stating metallic film is 45 degree.
Synchrotron radiation energy stabilization device the most according to claim 2, it is characterised in that institute Stating fluorescent probe towards the angle formed with the metallic element face of described metallic film is 45 degree.
6. according to the synchrotron radiation energy stabilization device described in any one of claim 2-5, its feature Being, the thickness of described metallic film institute plating element is 60-120nm.
7. a synchrotron radiation energy stabilization method, it is characterised in that comprise the following steps:
Obtain ionization chamber standard input light intensity, and standard input light is irradiated on thin film the standard of generation Fluorescence intensity;
Obtain the real-time incident intensity of ionization chamber, and incident illumination is mapped on metallic film generation in real time Real-time fluorescence intensity;
Wherein,I0For ionization chamber standard input light intensity, If0For standard input light Being irradiated on metallic film the standard fluorescence intensity produced, I is the real-time incident intensity of ionization chamber, If The real-time fluorescence intensity produced it is mapped on metallic film for real-time incident illumination;
The control coefrficient corresponding to the Real-time intensity of fluorescence and rotation threshold is produced according to described metallic film Relation between value, the rotation to double-crystal monochromator is controlled, and described control coefrficient is μ0For initial absorptance, μ is real-time absorptance.
Synchrotron radiation energy stabilization method the most according to claim 7, it is characterised in that institute State the control coefrficient corresponding to the Real-time intensity producing fluorescence according to described metallic film and rotation threshold value Between relation, the rotation to double-crystal monochromator is controlled, including:
If described control coefrficient more than described rotation threshold value, then controls described double-crystal monochromator and turns and move a step Cause 0.2eV energy variation, otherwise control described double-crystal monochromator and remain stationary as.
CN201410532846.XA 2014-10-10 2014-10-10 Synchrotron radiation energy stabilization device and method CN104267055B (en)

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