CN209513671U - The device of high-throughput powder diffraction for spread pen light beam - Google Patents

Abstract

The utility model provides a kind of device of high-throughput powder diffraction for spread pen light beam, belongs to x-ray powder diffraction techniques field.The device is the covering of the fan shape Soller Slit device that can distinguish sample different spatial diffraction, the multiple slypes being made up of multiple sheet metals among the device, the diffracted ray generated simultaneously in spread pen light beam irradiation section on sample is distinguished by sample position corresponding to each slype, realizes the effect for measuring multiple spot diffraction data on sample simultaneously using spread pen light beam.

Description

The device of high-throughput powder diffraction for spread pen light beam

Technical field

The utility model relates to x-ray powder diffraction techniques fields, particularly relate to a kind of high-throughput powder for spread pen light beam The device of last diffraction.

Background technique

X-ray Debye Scherrer method is to project a branch of thin quasi-parallel homogeneous X-ray on the sample of powder crystal, with photograph A kind of experimental method of the 2D detector such as egative film record diffracted ray intensity and angle position.Its main experimental provision is that powder shines Camera is called and does debye-Xie Le camera (abbreviation debye camera).The present apparatus is the quasi-parallel homogeneous X-ray to use spread pen shape A kind of device for doing powder diffraction experiment can achieve by using the present apparatus on synchrotron radiation light source while measure multiple (place) sample, is quickly obtained the effect of a large amount of diffraction datas.

Roentgen Laue has found the diffraction phenomena generated when X-ray passes through crystal within 1912, it was demonstrated that X-ray Fluctuation and crystal structure inside periodicity；The lattice that physics wife and children Prague of Britain in 1915 calculates NaCl is long, Dutch debye in 1916, thanking for Switzerland strangle utility model x-ray Debye Scherrer method.Hereafter, X-ray is widely used in crystal The fields such as structural analysis have promoted the hair of the spheres of learning and industrial circle such as physics, chemistry, the material science since 20th century Exhibition.

X-ray diffraction analysis need to be amorphous material, and according to the difference required sample morphology, it is big that experimental provision can be divided into two Class: single crystal diffractometer and polycrystalline diffractometer (also known as powder camera).The former is furnished with the complicated turntable of the homocentric circle of multiaxis, can meet list The diffraction conditions of various indexes in brilliant sample；Latter configuration is simple, since microparticle has the probability of various orientations, does not almost have to appoint What precise rotating platform sample can meet diffraction conditions.Since any material was all not easy to obtain the list of large scale at research initial stage Brilliant sample, so the structural analysis over-borrowing of material helps the method for powder diffraction.Although metal polycrystalline material is not powder, very More problems can be transferred through powder diffraction and be resolved.Other than structural analysis, macro-stress in material, after either processing Residual stress, powder diffraction studies also can be used in or the stress that load in situ generates.Powder diffraction techniques are from birth It rises, is always the conventional means of material characterization, and with the relevant technologies progress day such as equipment, method, data analysis and modeling Benefit is powerful, and application range is also being gradually expanded.

Earliest powder x-ray diffraction analysis method is Debye Scherrer method (Debye's method).In Debye's method, measured matter Powder is made into buttress shaft sample, is mounted on the axis of debye camera, in pen core X-ray beam vertical irradiation powder pillar.At this time There is numerous crystal grain while being irradiated by X-rays, the orientation of these crystal grain is different, always there are some diffraction surfaces of certain some particle Meet diffraction conditions and generate diffraction, therefore the diffraction for generating the identical diffraction surfaces of variable grain forms closing for a 2 θ apex angles Close circular cone.Distance values and the corresponding intensity that can be obtained by a series of diffraction surfaces of sample by powder photogrpah in this way are big It is small.Since photographic process is difficult to accurately measure the intensity of diffracted ray and resource that is linear and cannot effectively utilizing x-ray is quick Experiment, powder diffractometer method had gradually developed later.Diffractometer method in addition to can be improved light source utilization rate and angle measurement accuracy it Outside, photon counting detector technology is additionally used, diffraction image can with high s/n ratio be recorded.X-ray powder diffraction system is By x-ray generator, slit monochromatic system, sample stage and angular instrument, X-ray 2D strength measurement system and the big portion of data processing five It is grouped as.Used linear light source in order to efficiently utilize X-ray source, in powder diffractometer method, the slit of angle measurement also with linear light source It is parallel with sample/detector shaft；The X-ray diffraction face of sample is vertical with sample/detector shaft.Angular instrument is accurate Mechanical device cooperates the precise measurement angle of diffraction with slit system.Due to the direct phase of quality of the quality and diffraction spectra of x-ray source It closes, therefore the good incident beam of high-intensitive, low diverging, monochromaticjty is necessary to carrying out X-ray diffraction experiment.80 years 20th century X-ray light source has significant progress after occurring for Synchrotron Radiation, and synchrotron radiation light source has become current numerous subject bases The best light source of plinth research and high-tech development application study.

Utility model content

The X-ray powder diffraction experiment of synchrotron radiation light source still remains the initial design concept of debye-Xie Le camera, Use pen core homogeneous beam.Compared with the experimental provision of traditional experiment room, synchrotron radiation powder diffraction experiment undergoes over-angle point The improvement of the promotion of resolution, the evolution of detector etc., speed of detection higher than the high-resolution of traditional experiment is faster.But So far there has been no the breadth wise dimension for using incident light in relation to expanding, the technological progress in terms of diffraction experiment efficiency is improved.It is general same The light source of step radiation X-ray powder diffraction is all bending iron, and light beam is in flat spread pen type (laterally wide) after monochromatization.In order to pass The experiment model of the X-ray powder diffraction of system, generally be intended to slit light beam by spread pen type card at pen core type or on bunch Anchor ring mirror focus lamp spread pen type light beam is pooled into pen core type.This experiment model can slattern many incident light resources, Influence conventional efficient.The utility model is intended to actively use the light beam of spread pen type, and proposition is a set of can directly to use spread pen type light The powder diffraction experiment device of beam improves the efficiency of characterization sample.

The device is covering of the fan shape, and the made isolation of multiple equally spaced sheet metal is arranged in hollow fan-shaped frame Piece, forms multiple slypes, and slype is fan-shaped.

Specifically, the device includes outer framework, frame, sample stage, inner cylinder face window, spacer and outside cylinder face-port Mouthful, outer framework supports whole device, and frame supports slype, and multiple tracks spacer is arranged among frame, and frame is sector, frame Covering of the fan starting point is inner cylinder face window, and frame another side is external cylindrical surface window, the interior cylinder that inner cylinder face window is wrapped up Setting sample stage in vivo, whole device are a closed space.

Wherein, spacer quantity is greater than two panels, and the channel that every two spacer is formed corresponds to a sample or corresponds to A zonule on the sample.

The material that can penetrate x-ray is designed on inner cylinder face window and external cylindrical surface window.

Vacuum is formed with He gas displaced air or pumping in the device.

Spacer is made of thin steel strip.

Multiple slype cooperation 2D surface detectors can measure multiple spot diffraction fringe simultaneously.

The above-mentioned technical proposal of the utility model has the beneficial effect that:

Up to now powder diffractometer design is using pen core light beam and far from the long slit of sample and the semiconductor of 1D The mode that the imaging plate of probe or 2D combine collects diffraction data.Length of the utility model the 2D drum face at imaging plate Slit is changed to the covering of the fan Soller slit of the 3D close to sample, allow very little region generates on sample diffraction ring only some Detector can be reached along direction as defined in slit, the diffraction of adjacent sample area cannot reach, to guarantee that each zonule exists It is not interfere with each other in transverse direction.The complete utilization of synchrotron radiation light beam may be implemented in this way.The utility model uses a kind of Soller There are also the modes in conjunction with translation/rotation of sample to measure diffraction data with 2D probe by slit.Since diffraction ring may be non-circular Shape, the diffracted beam that slit penetrates cannot show complete diffraction ring, so the side of translation and rotation using a kind of sample Formula shows non-circular diffraction ring completely on 2D imaging plate, realizes the complete collection of information.

Detailed description of the invention

Fig. 1 is the apparatus structure schematic diagram of the high-throughput powder diffraction for spread pen light beam of the utility model.

Wherein: 1- synchrotron radiation light beam；2- sample stage；3- inner cylinder face window；4- spacer；5- external cylindrical surface window； 6- frame；7- outer framework.

Specific embodiment

In order to make the technical problems, technical solutions and advantages to be solved by the utility model clearer, below in conjunction with attached drawing And specific embodiment is described in detail.

The utility model provides a kind of device of high-throughput powder diffraction for spread pen light beam.

As shown in Figure 1, the device is covering of the fan shape, the metal foil of multiple equal intervals is set in hollow fan-shaped frame The made spacer of piece, forms multiple slypes.

Specifically, the device includes outer framework 7, frame 6, sample stage 2, inner cylinder face window 3, spacer 4 and outside cylinder Face-port mouth 5, outer framework 7 support whole device, and frame 6 supports slype, multiple tracks spacer 4, frame 6 is arranged among frame 6 For sector, 6 covering of the fan starting point of frame is inner cylinder face window 3, and 6 another side of frame is external cylindrical surface window 5, inner cylinder face window Sample stage 2 is set in 3 inner cylinders wrapped up, and whole device is a closed space.

The characteristics of device is distributed using bending iron synchrotron radiation horizontal direction, is directly used for powder diffraction for spread pen light beam Experiment.In order to distinguish the mutual laterally influence of diffraction ring generated everywhere using sample after spread pen light beam, the utility model is used A kind of soller-slit device being placed on sample downstream limits the trend from sample emergent light, makes spread pen light beam on sample Diffraction can only be walked along direction as defined in soller-slit, by sample plurality of positions generate diffraction light distinguish.This Although sample can only be collected into the sub-fraction of each zonule diffraction ring on a sample, multiple spot on sample can be measured simultaneously Data, improve conventional efficient, improve the utilization efficiency of synchrotron radiation light.

The soller-slit of large scale will generally cover hexagonal angle, and radius is greater than 300mm, according to the width of parallelism light beam The overall width for designing slit, it is also different according to the sum in the different channels of channel spacing.The partition in each channel is by thin steel strip structure At slit integrally has firm frame and supports installation section, can be used in existing synchrotron radiation powder diffraction device On.Thin steel strip when due to using in the device is parallel to gravity direction, there is no concern that large area separates the shape of thin steel strip Become.

In actual design, Soller slit is designed as a kind of shape of thick fan-shaped surface, supports with solid frame 6 Multiple tracks spacer 4 is arranged in the placement state of slit (i.e. slype) among it, and the covering of the fan starting point close to sample is in one Cylindrical surface window 3 has the material of permeable x-ray.Sample stage 2 is arranged inside inner cylinder.Covering of the fan end close to detector is One external cylindrical surface window 5, also there is the material of permeable x-ray.Soller slit entire in this way can be formed one it is closed Space can use He gas displaced air, reduce air absorption and background noise.The channel that every two spacer is formed corresponds to one A zonule on a sample or the sample, when synchrotron radiation light beam 1 is radiated on multiple samples, each sample cell Light beam on domain can all have respective diffraction.Because there is Soller slit spacer, the ring of each zonule of sample Shape diffraction light, which can be separated, to be come, and not lateral interference, can measure intensity/position of multiple groups diffraction light simultaneously each other, Obtain multiple groups diffraction data.Since the sub-fraction diffraction ring for the diffraction ring that very little region generates on sample can be along slit gauge Fixed direction reaches detector, cannot give expression to the comprehensive diffraction situation of entire sample plane.Rotation/translation can be passed through The method of sample shows the diffraction ring of entire sample plane complete area, gross information content can with pen core light beam by The result of spot scan is comparable.

The above is preferred embodiments of the present invention, it is noted that for the ordinary skill of the art For personnel, under the premise of not departing from principle described in the utility model, several improvements and modifications can also be made, these improvement It also should be regarded as the protection scope of the utility model with retouching.

Claims (6)

1. a kind of device of the high-throughput powder diffraction for spread pen light beam, it is characterised in that: the device is covering of the fan shape, in The made spacer of the sheet metal of the multiple equal intervals of setting, forms multiple slypes in empty fan-shaped frame；

Including outer framework (7), frame (6), sample stage (2), inner cylinder face window (3), spacer (4) and external cylindrical surface window (5), outer framework (7) supports whole device, and frame (6) supports slype, multiple tracks spacer (4) is arranged among frame (6), frame Frame (6) is sector, and frame (6) covering of the fan starting point is inner cylinder face window (3), and frame (6) another side is external cylindrical surface window (5), sample stage (2) are set in the inner cylinder that inner cylinder face window (3) is wrapped up, whole device is a closed space.

2. the device of the high-throughput powder diffraction according to claim 1 for spread pen light beam, it is characterised in that: it is described every It is greater than two panels from piece (4) quantity, the channel that every two spacer (4) is formed corresponds to one small on a sample or the sample Region.

3. the device of the high-throughput powder diffraction according to claim 1 for spread pen light beam, it is characterised in that: in described The material that can penetrate x-ray is designed on cylindrical surface window (3) and external cylindrical surface window (5).

4. the device of the high-throughput powder diffraction according to claim 1 for spread pen light beam, it is characterised in that: in device Vacuum is formed with He gas displaced air or pumping.

5. the device of the high-throughput powder diffraction according to claim 1 for spread pen light beam, it is characterised in that: described more A slype cooperation 2D surface detector can measure multiple spot diffraction fringe simultaneously.

6. the device of the high-throughput powder diffraction according to claim 1 for spread pen light beam, it is characterised in that: it is described every It is made from piece (4) of thin steel strip.