CN103808745B - A kind of method realizing small angle X-ray diffraction function - Google Patents

Abstract

The invention discloses a kind of device and method realizing small angle X-ray diffraction function, a kind of device realizing small angle X-ray diffraction function of the present invention comprises X-ray source, X ray exit slit, sample stage, X ray reception slit, X-ray detector, turbine and worm jacking gear and step motor; Described X-ray source, sample stage, X-ray detector are arranged in same plane, X-ray source is provided with X ray exit slit, X-ray detector is provided with X ray and receives slit, the bottom surface of sample stage connects turbine and worm jacking gear, and turbine and worm jacking gear is driven by step motor.The present invention, by the common XRD diffractometer device of transformation, is equipped with the control method of sample stage that we propose, X source and detector, and cost that namely can be extremely low realizes the function of SAXRD on common XRD diffractometer.

Description

A kind of method realizing small angle X-ray diffraction function

Technical field

The present invention relates to the analysis and testing technology of material, particularly relate to a kind of device and method realizing small angle X-ray diffraction function.

Background technology

Small angle X-ray diffraction (SAXRD) is a kind of material analysis measuring technology, has important application at nano material, macromolecular material, biological macromolecule material and thin film materials art.Different from common X-ray diffraction technology (XRD), SAXRD to the matching requirements of instrument and the requirement of operative skill higher, and thus need stronger x-ray source because signal is more weak.Therefore, early stage SAXRD completes in Synchrotron Radiation.Along with the development of X-ray tube and weak X-ray detection technology, SAXRD experiment can be carried out in common laboratory at present.But the requirement of SAXRD to the matching requirements of instrument and operative skill is still very high.The price of separate unit SAXRD equipment is general all more than 1,000,000 yuan, and debugging is very difficult, and the operating personnel not through professional training are difficult to obtain perfect SAXRD spectrogram.

Summary of the invention

The present invention is directed to the deficiencies in the prior art, propose a kind of device and method realizing small angle X-ray diffraction function.

A kind of device realizing small angle X-ray diffraction function comprises X-ray source, X ray exit slit, sample stage, X ray reception slit, X-ray detector, turbine and worm jacking gear and step motor.Described X-ray source, sample stage, X-ray detector are arranged in same plane, X-ray source is provided with X ray exit slit, X-ray detector is provided with X ray and receives slit, the bottom surface of sample stage connects turbine and worm jacking gear, and turbine and worm jacking gear is driven by step motor.

The width of described X ray exit slit and sample stage center O angle, the X ray opened receive the width of slit and sample stage center O the angle of opening all be less than or equal to 0.01 degree;

The height of described sample stage is accurately adjustable, and step-length is less than or equal to 0.01mm.

A kind of method realizing small angle X-ray diffraction function: specifically comprise the following steps:

Step one: diffraction instrument is set and enters non-linkage pattern, i.e. incident angle α and emergence angle β Independent adjustable pattern;

Step 2: fall sample stage, makes the X ray sent from X ray exit slit unobstructedly can reach X ray and receives slit; Regulate incident angle α and emergence angle β, the signal of receiver is maximized, writes down maximal value M;

Step 3: Quality control platform lifting step motor, promotes sample stage gradually, make the signal of receiver be less than or equal to 0.5M;

Step 4: regulate incident angle α and emergence angle β, the signal of receiver is maximized; If the maximal value now recorded is less than or equal to 0.5M, then enter step 5; Otherwise, repeat step 4, until maximal value is less than or equal to 0.5M;

Step 5: setting into firing angle α is 0, setting out firing angle β is 0;

Step 6: arrange diffractometer and enter linkage pattern, i.e. α=beta model, sample stage arranges work and completes, and diffractometer can carry out little angle XRD to be tested.

Beneficial effect of the present invention: by transforming common XRD diffractometer device, is equipped with the control method of sample stage that we propose, X source and detector, and cost that namely can be extremely low realizes the function of SAXRD on common XRD diffractometer; The method that the present invention proposes has the advantages that device is simple, precision is high, simple to operate, and cost performance is high.

Accompanying drawing explanation

Fig. 1 is a kind of structural representation realizing the device of small angle X-ray diffraction function of the present invention;

Fig. 2 is from the SAXRD spectral line that thermal oxide silicon chip sample obtains in the embodiment of the present invention.

Embodiment

As shown in Figure 1, a kind of device realizing small angle X-ray diffraction function comprises X-ray source 1, X ray exit slit 2, sample stage 3, X ray reception slit 4, X-ray detector 5, turbine and worm jacking gear 6 and step motor 7.

Described X-ray source 1, sample stage 3, X-ray detector 5 are arranged in same plane, X-ray source 1 is provided with X ray exit slit 2, X-ray detector 5 is provided with X ray and receives slit 4, the bottom surface of sample stage 3 connects turbine and worm jacking gear 6, and turbine and worm jacking gear 6 is driven by step motor 7.

The width of described X ray exit slit 2 and sample stage center O angle, the X ray opened receive the width of slit 4 and sample stage center O the angle of opening all be less than or equal to 0.01 degree;

Described sample stage height degree of regulation numerical value and outgoing and receive the angle that slit width forms and be all less than or equal to 0.01 degree.

Embodiment

The different silica membrane of a slice thickness that utilized dry-oxygen oxidation technique at grown above silicon.Figure 2 shows the small angle X-ray diffraction curve that the apparatus and method that utilize this patent to propose are collected at common X-ray diffractometer.The oscillation of intensity because interference effect is formed can be observed significantly from figure.From formula the thickness of silicon dioxide layer in sample can be calculated and be respectively 3.5nm.Visible, the sample stage jacking gear that we propose and method can realize SAXRD function completely on common XRD spectrometer.

Claims (1)

1. realize a method for small angle X-ray diffraction function, the method by device comprise X-ray source, X ray exit slit, sample stage, X ray receive slit, X-ray detector, turbine and worm jacking gear and step motor;

It is characterized in that: described X-ray source, sample stage, X-ray detector are arranged in same plane, X-ray source is provided with X ray exit slit, X-ray detector is provided with X ray and receives slit, the bottom surface of sample stage connects turbine and worm jacking gear, and turbine and worm jacking gear is driven by step motor; The width of described X ray exit slit and sample stage center O the angle of opening be less than or equal to 0.01 degree; Described X ray receive the width of slit and sample stage center O the angle of opening be less than or equal to 0.01 degree; Described sample stage height is accurately adjustable, and step-length is less than 0.01mm; It is characterized in that, the method specifically comprises the following steps:

Step one: diffraction instrument is set and enters non-linkage pattern, i.e. incident angle α and emergence angle β Independent adjustable pattern;

Step 2: fall sample stage, makes the X ray sent from X ray exit slit unobstructedly can reach X ray and receives slit; Regulate incident angle α and emergence angle β, the signal of receiver is maximized, writes down maximal value M;

Step 3: Quality control platform lifting step motor, promotes sample stage gradually, make the signal of receiver be less than or equal to 0.5M;

Step 4: regulate incident angle α and emergence angle β, the signal of receiver is maximized; If the maximal value now recorded is less than or equal to 0.5M, then enter step 5; Otherwise, repeat step 4, until maximal value is less than or equal to 0.5M;

Step 5: setting into firing angle α is 0, setting out firing angle β is 0;

Step 6: arrange diffractometer and enter linkage pattern, i.e. α=beta model, sample stage arranges work and completes, and diffractometer can carry out little angle XRD to be tested.