WO2016193687A1 - Dispositif d'analyse par rayons x - Google Patents

Dispositif d'analyse par rayons x Download PDF

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Publication number
WO2016193687A1
WO2016193687A1 PCT/GB2016/051559 GB2016051559W WO2016193687A1 WO 2016193687 A1 WO2016193687 A1 WO 2016193687A1 GB 2016051559 W GB2016051559 W GB 2016051559W WO 2016193687 A1 WO2016193687 A1 WO 2016193687A1
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WO
WIPO (PCT)
Prior art keywords
ray
characteristic
sample
line
detector
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PCT/GB2016/051559
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English (en)
Inventor
Graeme Mark HANSFORD
Original Assignee
University Of Leicester
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from GBGB1509329.7A external-priority patent/GB201509329D0/en
Priority claimed from GBGB1509314.9A external-priority patent/GB201509314D0/en
Priority claimed from GBGB1509396.6A external-priority patent/GB201509396D0/en
Application filed by University Of Leicester filed Critical University Of Leicester
Publication of WO2016193687A1 publication Critical patent/WO2016193687A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor

Definitions

  • the present invention relates to an X-Ray analysis device, in particular an X-Ray analysis device adapted to detect the presence of a crystalline material of interest in a sample, the crystalline material having a lattice structure comprising at least a first lattice spacing and a second lattice spacing.
  • crystalline materials including those materials classed as polycrystalline that is, comprising many crystallites, such as a sample of rock.
  • the lattice spacing d is the spacing between the planes in a crystal lattice, and can be calculated for each of the 14 Bravais lattice types based upon a combination of the lengths of each side of a unit cell making up the lattice (a, b and c). This set of d spacings is unique for each crystal structure, thus making X- Ray diffraction a useful tool in the identification of crystalline materials of interest.
  • One commonly used technique is to use a fixed X-Ray wavelength, for example a Ka X-Ray line, and, using a detector of appropriate sensitivity, scan through a range of ⁇ , such as in angle-dispersive X-Ray diffraction (ADXRD).
  • the commonly-used Bragg-Brentano diffractometer works on this principle.
  • An alternative implementation of the Bragg equation is to fix the scattering angle and scan the X-ray wavelength (equivalently, the X-ray energy).
  • This method can also be implemented without scanning the X-ray wavelength: a broadband X-ray source, such as an X-ray tube, can be used together with an energy-resolving detector.
  • a broadband X-ray source such as an X-ray tube
  • an energy-resolving detector In either case, this technique is known as energy-dispersive XRD (EDXRD).
  • EDXRD energy-dispersive XRD
  • the technique since the X-Ray source has a non-uniform spectral distribution, and diffraction and fluorescence peaks may overlap, making analysis relatively
  • the present invention aims to address this issue by providing an X-Ray analysis device adapted to detect the presence of a crystalline material of interest in a sample, the crystalline material having a lattice structure comprising at least a first lattice spacing and a second lattice spacing comprising: an X-Ray source arranged to emit a first characteristic X-Ray line and a second characteristic X-Ray line both incident on the sample; an X-Ray detector adapted to detect X-rays diffracted by the sample; wherein each of the first and second characteristic X-Ray lines is diffracted at a distinct diffraction angle determined by each of the first and second lattice spacings to produce four diffraction angles, and wherein two of the diffraction angles correspond to one another.
  • the two diffraction angles are coincident.
  • the first characteristic X-Ray line has a first emission energy and the second characteristic X-Ray emission line has a second emission energy, and wherein the ratio of the first lattice spacing to the second lattice spacing corresponds to the inverse ratio of the first emission energy to the second emission energy.
  • the X-Ray source may comprise a single element capable of emitting at least two characteristic X-Ray lines.
  • the X-Ray source may be a combination of at least two elements each capable of emitting at least one characteristic X-Ray line. In this latter situation, the X-Ray source is preferably an alloy of at least two elements each capable of emitting at least one characteristic X- Ray line.
  • the device further comprises a collimator arranged to collimate the first characteristic X-Ray line and the second characteristic X-ray line on exiting the at least one X-Ray source.
  • the device may also further comprise an image detector.
  • the image detector is a charge-coupled device.
  • the detector may be an energy-resolving detector.
  • the device may also further comprise a filter, the filter being arranged to filter the X- ray spectrum diffracted by the sample before entering the detector.
  • the device may further comprise a filter, the filter being arranged to filter the first and second characteristic X-ray lines emitted by the X-ray source.
  • the at least one X-Ray source is arranged in a back-reflection geometry with respect to the sample.
  • the crystalline material of interest has at least a third lattice spacing, and the X-ray source is arranged to emit at least a third characteristic X-Ray line, and wherein the third characteristic X-Ray line is diffracted at a further diffraction angle by the third lattice spacing, wherein the diffraction angle corresponds to those produced by the first and second characteristic X-Ray lines.
  • the crystalline material of interest may be a single crystalline phase or a combination of at least two crystalline phases.
  • the present invention also provides for the above device to be adapted to be housed within a handheld unit.
  • the present invention provides a method of X-Ray analysis of a sample to determine the presence of a crystalline material of interest, the crystalline material having a characteristic ratio of lattice spacings, comprising: selecting an X- Ray source having a first characteristic X-Ray line and a second characteristic X-Ray line; diffracting the first characteristic X-Ray line and the second characteristic X-Ray off the sample; detecting the X-Rays diffracted by the sample; wherein each of the first and second characteristic X-Ray lines is diffracted at a distinct diffraction angle determined by each of the first and second lattice spacings to produce four diffraction angles, and wherein two of the diffraction angles correspond to one another.
  • the X-Ray source comprises a single element capable of emitting at least two characteristic X-Ray lines.
  • the X-Ray source is a combination of at least two elements capable of emitting at least one characteristic X-Ray line.
  • the X-Ray source is preferably an alloy of at least two elements capable of emitting at least one characteristic X-Ray line.
  • the first characteristic X-Ray line has a first emission energy and the second characteristic X-Ray emission line has a second emission energy, and wherein the ratio of the first lattice spacing to the second lattice spacing corresponds to the inverse ratio of the first emission energy to the second emission energy.
  • Figure 1 is a schematic perspective view of a device in accordance with a first embodiment of the present invention adapted to detect the presence of a crystalline material of interest in a sample;
  • Figure 2 is a schematic cross-section view of a device in accordance with a second embodiment of the present invention adapted to detect the presence of a crystalline material of interest in a sample;
  • Figure 3 is a chart illustrating the emission energies of the L-series of characteristic X-Ray lines of an X-Ray source having a Pd (Palladium) anode;
  • Figure 5 is a chart illustrating the experimental confirmation of the correspondence between the X-Ray diffraction angles in quartz with a Pd X-Ray source
  • Figure 8 is a chart showing the simulation of the EDXRD spectrum of a sample of steel containing (by volume) 5% austenite, 60% martensite, 20% ferrite and 15 % cementite;
  • Figure 9 is a chart showing the enhanced detection of austenite in a steel sample using a source which emits In and Ti characteristic X-rays simultaneously.
  • the present invention takes the approach of maximising the X-Ray diffraction signal obtained at fixed 2 ⁇ by exploiting a coincidence of diffraction angles created by different X-Ray emission energies.
  • An X-ray analysis device can be adapted to detect the presence of a crystalline material of interest.
  • the crystalline material will have a lattice structure, which comprises at least a first lattice spacing and a second lattice spacing.
  • imagining the unit cell of a crystalline lattice being assigned a Cartesian co-ordinate system the distance between adjacent lattice planes in the x-direction gives rise to a first lattice spacing, and the distance between adjacent lattice planes in the y-direction gives rise to a second lattice spacing.
  • An X- Ray source can be arranged to emit a first characteristic X-Ray line and a second characteristic X-Ray line, both of which are incident on the sample.
  • An X-Ray detector adapted to detect X-Rays diffracted by the sample is used to detect any spectrum obtained.
  • Each of the first and second characteristic X-Ray lines is diffracted at a distinct diffraction angle determined by each of the first and second lattice spacings to produce four diffraction angles, and two of these diffraction angles correspond to each other.
  • This correspondence or in highly accurate cases, coincidence, can be used to enhance the signal detected when X-rays are diffracted from a material of interest.
  • the simultaneous observation of the two X-ray energies constitutes a signature of the material of interest and may be used to detect the presence of a crystalline material of interest in a sample.
  • E X-ray energy
  • h Planck's constant
  • c the speed of light
  • 6.19931 keV A is equal to 1 ⁇ 2 7c when E is expressed in units of keV
  • d is expressed in units of A.
  • the method described could be used to detect a class of minerals, such as micas or other subsets of clay minerals, rather than an individual crystalline phase, by selecting lattice spacings which are characteristic of that class.
  • the method could also be used to detect two distinct crystalline materials of interest simultaneously by selecting at least one lattice spacing from each material. Therefore the crystalline material of interest may be a single crystalline phase or a combination of at least two crystalline phases.
  • FIG. 1 is a schematic perspective view of a device in accordance with a first embodiment of the present invention adapted to detect the presence of a crystalline material of interest in a sample.
  • a sample stage 1 is provided with a sample holder 2 in which a sample 3 of a material of interest is placed.
  • a device 4 in accordance with a first embodiment of the present invention is positioned a distance L away from the sample stage 1 .
  • a back-reflection geometry is utilised.
  • the device 4 comprises an X-ray source 5 arranged to emit a first characteristic X-Ray line 6 and a second characteristic X-Ray line 7, both of which are incident on the sample 3 as indicated by arrow I.
  • An X-ray detector 8 adapted to detect the X-Rays emitted by the sample 3 is positioned out of the line of the incident X-Rays, and receives diffracted X-Rays as indicated by lines D.
  • the X-ray detector 8 is an energy dispersive X- Ray detector, such as a silicon drift detector, but may be an imaging device such as a charge coupled device (CCD).
  • a collimator 9 is positioned in front of the X-Ray source 5, and arranged to collimate the first characteristic X-Ray line and the second characteristic X-Ray line on exiting the X-Ray source 5, and a filter 10 is positioned between the sample 3 and the X-Ray detector 8.
  • the filter 10 is optional, and may be placed in a position 10a in the incident X-Ray beam I or in a position 10b in the diffracted X-Ray beam D adjacent the X-Ray detector 8, or in between as desired.
  • the filter 10 may therefore filter the characteristic X-Ray lines emitted by the X-Ray source 5 or diffracted by the sample 3 before entering the X-Ray detector 8.
  • the characteristic lines are part of a spectrum emitted by the X-Ray source 5.
  • FIG. 2 is a schematic cross-section view of a device in accordance with a second embodiment of the present invention adapted to detect the presence of a crystalline material of interest in a sample.
  • a housing 1 1 is provided to house an X-Ray source 12 arranged to emit a first characteristic X-Ray line and a second characteristic X- Ray line, and an X-Ray detector 13 adapted to detect X-Rays diffracted by a sample (not shown).
  • the housing 11 comprises a main body 14 housing the X-ray source 12 and the X-Ray detector 13, and a handle portion 15 adapted to be gripped easily by a user.
  • a screen 16 may be provided in the housing 1 1 to display information to a user, with a touchscreen being most preferable, such that a user may input commands to a processor controlling the X-Ray source 12 and the X-Ray detector 13. It may be desirable to include a collimator 17 positioned in front of the X-Ray source 12, and a filter 18, where the filter may be in the form of a fixed window 19 or an interchangeable filter arrangement.
  • quartz can present a hazard to miners when in the form of respirable silica, since this can cause silicosis. Quartz may also be present as an impurity in iron ore, where its hardness inhibits processing and thus increases the required energy, the detection of quartz in this situation could lead to an optimised processing method.
  • Figure 3 is a chart illustrating the emission energies of the L-series of characteristic X-Ray lines of an X-Ray source having a Pd (Palladium) anode.
  • the lines are essentially monochromatic although they sit on a continuum with an approximate comparable intensity when integrated across the entire energy range of the X-Ray source.
  • the X-Ray source is therefore a single element capable of emitting at least two characteristic X-Ray lines.
  • the ratio of the energies of these two characteristic X-Ray lines is 2.990 keV : 2.838 keV, or 1.0536.
  • Figure 4 was simulated using the ray tracing program, PoDFluX (see Hansford, Rev. Sci. Instrum., 80 (2009), 073903), and shows an energy-dispersed X- Ray diffraction (XRD) spectrum for quartz at 2 ⁇ with the L-series emission lines of Pd overlaid thereon.
  • the EDXRD spectrum of quartz is incident on the detector.
  • Figure 4 also illustrates the transmission of a 1 ⁇ thickness rhodium (Rh) foil on a 7 ⁇ thickness polyester support. Rhodium has an absorption edge at 3.013 keV, just above the Pd L- ⁇ characteristic X-Ray line at 2.990 keV.
  • Figure 5 is a chart illustrating the experimental confirmation of the correspondence between the X-Ray diffraction angles in quartz with a Pd X-Ray source.
  • the experimental set up forming the analysis device was as shown in Figure 1 , with a distance between the X-Ray source and the sample of 400 mm, a distance between the collimator (a 2 mm diameter aperture in a sheet of aluminium (Al)) and the sample of 200 mm and a distance between the sample and the detector of 70 mm.
  • a filter was also used, to suppress unwanted spectral features, comprising a 1 ⁇ thick rhodium coating on a 7 ⁇ thick polyester support.
  • the sample used was a pressed-powder pellet of quartz.
  • the X-Ray source was based on a copper (Cu)- anode with a thin plate of Pd mounted on the surface.
  • the electron incidence angle was 75° relative to the anode surface, and the X-Ray take off angle 15°.
  • the detector used was a charge-coupled device (CCD), a CCD-22 available from e2v technologies (UK) Ltd, 106 Waterhouse Lane, Chelmsford, Essex, M 1 2QU, operated in frame-transfer mode.
  • the CCD has an imaging area of 600 ⁇ 600 pixels with a 40 ⁇ pixel width, and when configured in a back reflection geometry covers a 2 ⁇ range of 148 - 168°.
  • Fig. 5 also shows the effect of introducing a rhodium filter between the X-ray source and sample, and illustrates the suppression of intensity in the spectrum at energies above the (200) - Pd-L peak at 2.990 keV.
  • the use of a high 2 ⁇ diffraction angle also reduces the sensitivity to sample morphology considerably. This allows unprepared or minimally prepared samples to be analysed.
  • the X-Ray diffraction peaks resulting from the correspondence between the (1 1 1 ) and (200) quartz diffraction peaks and the Pd-Lcn and Pd-L ⁇ are highlighted, again showing the success of the correspondence technique.
  • Fig. 6 demonstrate the feasibility of the phase-specific XRD method for unprepared samples exhibiting significant surface morphology.
  • data were acquired for the same sample at a reference position, rotated through 30° and moved 2 mm away from the source and detector.
  • the same on- and off-coincidence regions were selected for the three datasets and the extracted spectra are shown in Fig. 7.
  • the spectra have been offset on the vertical axis for greater clarity. There is very good correspondence between both the on- and off-coincidence spectra, demonstrating the tolerance of the method to changes in the sample position and orientation. It follows that the technique is tolerant to sample morphology on the same scale.
  • the ratio of the lattice spacings for any two given sets of lattice planes is not affected by variations in the unit cell size.
  • Austenite, or y-iron (Fe) has a small crystallographic unit cell and high symmetry, and therefore a sparse diffraction pattern. This makes it difficult to find a single element X-Ray source for which two angles of diffraction can be found to correspond.
  • d(220) 1.2880
  • a ⁇ 0.03°
  • a desirable possibility is to use an imaging detector that covers the full angular range, and that could therefore selectively detect and quantify austenite in steel over the full range of carbon content.
  • the selected lattice spacings are unlikely to cause any overlap or confusion with other possible phases that may be present in a steel sample, such as ferrite (cr-Fe), martensite (ferrite supersaturated with carbon) and cementite (Fe 3 C).
  • a combination of at least two elements, each of which is capable of emitting at least one characteristic X-Ray line, such as an alloy of indium (In) and titanium (Ti), say a 50/50 alloy, may be used to create the simultaneous emission of the two characteristic X-Ray lines of interest.
  • Figure 8 is a chart showing the simulation of the EDXRD spectrum of a sample of steel containing (by volume) 5% austenite, 60% martensite, 20% ferrite and 15-% cementite. The strong peaks at approximately 3.0keV and 4.3keV are due to martensite diffraction, with the other two peaks being as a result of the correspondence technique.
  • Identifying and quantifying the amount of retained austenite is a critical parameter in the manufacture of various products, where its presence may be seen as beneficial or harmful.
  • the amount of retained austenite indicates the success or failure of any heat treatment used to tailor mechanical properties of tools and dies, whereas in the preparation of bearings and gears the presence of austenite produces a mechanism by which the lifetime of such components may be extended by suppression of crack propagation.
  • Fig. 9 Experimental results demonstrating the enhanced detection of austenite in steel are shown in Fig. 9.
  • the sample is a high-Mn Twining-lnduced Plasticity (TWIP) steel with an estimated 40% austenite content with the balance made up with martensite and/or ferrite.
  • TWIP Twining-lnduced Plasticity
  • a Ti plate was coated with a thin layer of In using electro-deposition methods and mounted on the anode of the X-ray tube source.
  • Experiments were performed using the same laboratory set-up as for the detection of quartz using Pd. In this case, a 10 ⁇ thick Ti foil was mounted between the sample and the detector instead of the rhodium foil mounted between the source and sample.
  • Ti has an absorption edge at 4965 eV and the foil serves to suppress diffraction and fluorescence peaks at higher energies and also at lower energies, below approximately 2.5 keV for example.
  • the spectra shown in Fig. 9 are for on- and off-coincidence regions.
  • the main fluorescence and scattering peaks have been labelled, including the two coincidence diffraction peaks which are the strongest peaks in the on-coincidence spectrum.
  • the (200) peak is weaker than the (220) peak in the off-coincidence spectrum, illustrating how the two enhanced peaks can be equalised in intensity by optimising the thickness of the In layer on the InTi source.
  • the Ti- ⁇ peak is due to fluorescence from the Ti foil in front of the CCD, there is no Ti in the sample. There will also be a small contribution to the Ti- ⁇ peak in both spectra arising in the same way.
  • correspondence between the diffraction angles of two lattice planes at two particular characteristic X-Ray energies occurs.
  • the correspondence leads to an enhanced signal in the energy-dispersed X-Ray diffraction pattern obtained.
  • quartz and austenite are detected, many other applications are possible, such as the identification of shale in coal deposits by the detection of quartz within the shale, the detection of polymorphs and hydration states of crystalline materials in pharmaceutical manufacturing, quality control of alloys during manufacture where crystalline impurities and poor nucleation and growth of desired crystalline phases may be detected and the detection of deposited crystalline phases in the preparation of coatings.
  • a CCD camera was used as a detector to capture the X-Ray spectra.
  • an energy-dispersive detector such as a silicon drift detector, or a Si(Li) detector in place of or in addition to the CCD. This is particularly advantageous in a handheld device.
  • a filter comprising a thin foil of a material that suppresses X-Ray fluorescence peaks may be placed between the X-Ray source and the sample or between the sample and the X-Ray detector. In some circumstances positioning in front of the detector may be more suitable to achieve X-Ray fluorescence peak suppression.
  • At least a third diffraction angle correspondence may be used in the detection of a crystalline material of interest.
  • the X-Ray source is arranged to emit at least a third characteristic X-Ray line
  • the crystalline material of interest has at least a third lattice spacing.
  • the third characteristic X-Ray line is diffracted at a distinct diffraction angle determined by each lattice spacing.
  • the resulting X-Ray spectrum will have three peaks representing the three lattice spacings and the correspondence between the diffraction angles.

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Abstract

L'invention concerne un dispositif d'analyse par rayons X comprenant une source de rayons X et un détecteur de rayons X, et un procédé d'analyse. La source de rayons X est agencée pour émettre une première ligne de rayons X caractéristique et une seconde ligne de rayons X caractéristique toutes les deux incidentes sur l'échantillon. Le détecteur de rayons X est conçu pour détecter des rayons X diffractés par l'échantillon. Chacune des première et seconde lignes de rayons X caractéristique est diffracté avec un angle de diffraction distinct déterminé par chacun des premier et second espacements de réseau pour produire quatre angles de diffraction, et deux des angles de diffraction correspondent l'un avec l'autre.
PCT/GB2016/051559 2015-05-29 2016-05-27 Dispositif d'analyse par rayons x WO2016193687A1 (fr)

Applications Claiming Priority (6)

Application Number Priority Date Filing Date Title
GBGB1509329.7A GB201509329D0 (en) 2015-05-29 2015-05-29 X-ray analysis device
GB1509314.9 2015-05-29
GBGB1509314.9A GB201509314D0 (en) 2015-05-29 2015-05-29 X-ray analysis device
GB1509329.7 2015-05-29
GBGB1509396.6A GB201509396D0 (en) 2015-06-01 2015-06-01 X-ray analysis device
GB1509396.6 2015-06-01

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WO2016193687A1 true WO2016193687A1 (fr) 2016-12-08

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019099666A1 (fr) * 2017-11-16 2019-05-23 XRD by Design LLC Appareil compact et peu coûteux pour tester la production et la contrefaçon de produits pharmaceutiques et d'autres matériaux cristallins
CN112313505A (zh) * 2018-04-20 2021-02-02 奥图泰(芬兰)公司 X射线荧光分析仪和用于执行x射线荧光分析的方法

Citations (4)

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Publication number Priority date Publication date Assignee Title
US4128762A (en) * 1976-09-08 1978-12-05 Hitachi, Ltd. Apparatus for measuring mechanical stress using white X-rays
US6697453B1 (en) * 2002-02-08 2004-02-24 Metscan Technologies, Llc Portable X-ray diffractometer
WO2005031329A1 (fr) * 2003-08-04 2005-04-07 X-Ray Optical Systems, Inc. Systeme de diffraction des rayons x in-situ utilisant des sources et des detecteurs dans des positions angulaires fixes
US20130279653A1 (en) * 2012-04-19 2013-10-24 Graeme Mark Hansford Methods and apparatus for x-ray diffraction

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4128762A (en) * 1976-09-08 1978-12-05 Hitachi, Ltd. Apparatus for measuring mechanical stress using white X-rays
US6697453B1 (en) * 2002-02-08 2004-02-24 Metscan Technologies, Llc Portable X-ray diffractometer
WO2005031329A1 (fr) * 2003-08-04 2005-04-07 X-Ray Optical Systems, Inc. Systeme de diffraction des rayons x in-situ utilisant des sources et des detecteurs dans des positions angulaires fixes
US20130279653A1 (en) * 2012-04-19 2013-10-24 Graeme Mark Hansford Methods and apparatus for x-ray diffraction

Non-Patent Citations (1)

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Title
OOMAE H ET AL: "Studies of zinc-blende type MnAs thin films grown on InP(001) substrates by XRD", JOURNAL OF CRYSTAL GROWTH, vol. 378, 23 January 2013 (2013-01-23), pages 410 - 414, XP028680556, ISSN: 0022-0248, DOI: 10.1016/J.JCRYSGRO.2012.12.095 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019099666A1 (fr) * 2017-11-16 2019-05-23 XRD by Design LLC Appareil compact et peu coûteux pour tester la production et la contrefaçon de produits pharmaceutiques et d'autres matériaux cristallins
CN112313505A (zh) * 2018-04-20 2021-02-02 奥图泰(芬兰)公司 X射线荧光分析仪和用于执行x射线荧光分析的方法

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