EP0858596A1 - Procede de determination par fluorescence x de la composition d'une matiere, et dispositif permettant la mise en oeuvre d'un tel procede - Google Patents

Procede de determination par fluorescence x de la composition d'une matiere, et dispositif permettant la mise en oeuvre d'un tel procede

Info

Publication number
EP0858596A1
EP0858596A1 EP97921805A EP97921805A EP0858596A1 EP 0858596 A1 EP0858596 A1 EP 0858596A1 EP 97921805 A EP97921805 A EP 97921805A EP 97921805 A EP97921805 A EP 97921805A EP 0858596 A1 EP0858596 A1 EP 0858596A1
Authority
EP
European Patent Office
Prior art keywords
ray
axis
angle
spectrum
radiation
Prior art date
Legal status (The legal status 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 status listed.)
Withdrawn
Application number
EP97921805A
Other languages
German (de)
English (en)
Inventor
Volker RÖSSIGER
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Helmut Fischer GmbH and Co
Original Assignee
Helmut Fischer GmbH and Co
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
Application filed by Helmut Fischer GmbH and Co filed Critical Helmut Fischer GmbH and Co
Publication of EP0858596A1 publication Critical patent/EP0858596A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • G01N23/22—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 measuring secondary emission from the material
    • G01N23/223—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 measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/07—Investigating materials by wave or particle radiation secondary emission
    • G01N2223/076—X-ray fluorescence

Definitions

  • the invention relates to an X-ray fluorescence method for determining the composition of a material and a device for carrying out such a method according to the preamble of claim 1 and claim
  • X-ray fluorescence spectroscopy is a preferred method for the non-destructive determination of the composition of a material. This method can also be used in particular for the production control of workpieces placed in large series.
  • a typical example of this is the coating of workpieces with thin layers, e.g. the application of galvanic zinc layers on iron workpieces.
  • the results of coating processes of this type depend on the process parameters used for coating, and moreover, in the case of workpieces which have a complicated geometry, they are difficult to reproduce due to the workpiece geometry, so that the thickness and the composition of the deposited layer fluctuate within relatively wide limits .
  • cylindrical iron workpieces with a zinc layer thickness fluctuations of the zinc layer in the circumferential direction in the range of +/- 30% in the case of electroplating with normal care are not uncommon. Fluctuations in the range of +/- 15% can only be achieved with great effort.
  • the normal X-ray fluorescence measurement method can be used to determine the layer thickness and the composition.
  • primary X-ray radiation is directed onto a sample surface, the direction of irradiation not or only slightly deviating from the normal of the sample surface.
  • the X-ray fluorescence radiation excited in the surface and in the volume of the sample is observed under a detection direction that is only slightly tilted relative to the direction of irradiation for reasons of intensity.
  • the layer thickness and the composition of the layer can then be determined using mathematical models and / or calibrations from the intensities of the lines of the spectrum which are to be assigned to the atoms of the base material or the atoms of the layer material.
  • the layer material has an additive with atoms that correspond to or are similar to the atoms of the base material.
  • the service life of zinc coatings on iron base materials can be considerably improved by adding about 1% by weight of Fe or about 1% by weight of Co to the coating material.
  • the X-ray spectra of these atoms of the additive agree completely or largely with the X-ray spectra of the atoms of the base material, so that the number of foreign atoms, which is small because of the small layer thickness and the low concentration, is not taken from the atoms of the base when using the known X-ray fluorescence method ⁇ can distinguish material.
  • the present invention is therefore intended to develop an X-ray fluorescence method according to the preamble of claim 1 in such a way that the concentration of atoms, in particular a low concentration of foreign atoms, whose X-ray fluorescence spectra cannot or only slightly can be determined in a surface layer differs from those of the atoms of the base material.
  • the invention is intended to provide a device for carrying out such a method.
  • the invention proposes an X-ray fluorescence method with the features specified in claim 1 or a device for carrying it out with the features specified in claim 7.
  • the detection of the X-ray fluorescence radiation is carried out in a detection direction which strikes the workpiece surface.
  • X-rays which are generated in the volume of the base material, have to travel a long way through the base material and the layer on the way to the X-ray detector.
  • the X-ray fluorescence radiation of the base material is absorbed in the base material and in the layer.
  • the fluorescence radiation generated on the sample surface does not have to traverse any or only very little material, so that absorption does not take place or only to a very small extent.
  • the detection direction chosen according to the invention thus ensures that the fluorescence quanta measured by the detector originate from the sample surface or its immediate vicinity.
  • the method according to the invention can be carried out using known X-ray fluorescence measuring apparatus with only minor changes in apparatus.
  • a phantom part of inert or distinguishable material corresponding to the workpieces is provided with the coating.
  • additional workpiece base material is also dissolved in the chemical analysis; Due to the different chemical nature of the base, there are no coating ratios that correspond to the actual workpiece coating.
  • the method according to the invention can be carried out in the cycle time of the order of a few seconds, which is typical for X-ray fluorescence test methods, this method working non-destructively and also having the advantage that different areas of the surface of the real workpiece are measured separately can do what is excluded in chemical processes. Because of the simplicity, the reliability and the short time required, the method according to the invention is also suitable for a hundred percent inspection of workpieces, which is excluded in the known methods.
  • the short measuring cycle of the method according to the invention enables faulty workpieces to be rejected directly at the end of the production process and a quick action on process parameters of the coating method in order to counteract irregularities in the layer thickness and / or the composition of the layer material.
  • a grazing angle of reflection (angle between the direction of detection and the workpiece surface), as specified in claim 2, can be easily achieved with normal mechanical effort, and the contribution of the base material to the X-ray fluorescence spectrum is already negligible.
  • the X-ray fluorescence spectrum can be used for a plurality Measure different small drop angles and extrapolate the X-ray fluorescence spectrum for very small drop angles from the measured spectra. This procedure takes a little more time, but allows the method according to the invention to be used even under the difficult conditions described above.
  • the remaining portion of the base material spectrum for not very small angles of failure can also be determined in calibration measurements and mathematically for correcting the X-ray fluorescence spectrum of the coating deposited on the workpiece use as specified in claim 4.
  • the sensitivity of the method according to the invention can be increased according to claim 5 by letting the primary X-ray radiation graze the workpiece surface, either from the same half-space in which the X-ray detector is located or from the opposite half-space. If it is not possible to work with a very small angle of incidence for the primary X-ray radiation for apparatus or sample-related reasons, then the X-ray fluorescence spectrum can record for several not very small angles of incidence and, by extrapolation, back to the X-ray fluorescence spectrum for very small or vanishing ⁇ close the angle of incidence.
  • the method according to the invention which is outlined above together with its further developments, can be used not only in connection with surface layers separated from the base material by an inner interface.
  • This method can also be used to determine doped (e.g. diffusion-doped) edge areas of a macroscopically continuous base material.
  • a device according to claim 8 allows the sample to be tilted with respect to the detection direction.
  • a device in a device according to claim 9 there are two defined angles of reflection for the X-ray fluorescence radiation, which can be set simply and precisely, e.g. in order to be able to measure the composition of the layer material with grazing failure and the thickness of the deposited layer with a large angle of failure.
  • An embodiment of the sample table carrying, according to claim 11 is used on the one hand the further exclusion of Scattered radiation, on the other hand, ensures that an essentially sector-shaped flat tuft of the X-ray fluorescence radiation reaches the X-ray detector.
  • the development of the invention according to claim 11 ensures that the bottom surface of the depression is not an obstacle to X-ray fluorescence radiation, but on the other hand is closely adjacent to the fluorescence radiation bundle, so that primary X-ray radiation is well shielded from the observation beam path.
  • the x-ray fluorescence radiation which originates from the spot of the workpiece surface illuminated by the primary x-ray radiation and is emitted in the detection direction, can completely reach the x-ray detector, on the other hand, in turn, the best possible shielding against primary x-ray radiation is obtained.
  • the development of the invention according to claim 13 also serves to keep primary X-ray radiation away from the observation beam path.
  • the development of the invention according to claim 16 also serves to separate the excitation beam path and the observation beam path.
  • the development of the invention according to claim 17 enables the direction of failure to be set continuously.
  • One can do the X-ray fluorescence spectrum Easily measure for one or more small drop angles and one or more large drop angles without having to span the sample.
  • the angle of incidence of the excitation radiation can also be simply and continuously adjusted.
  • this setting of the angle of incidence can again be done by motor and thus under electrical control.
  • a device according to claim 21 can be operated easily with a constant angle of incidence of the x-ray radiation.
  • the angle of incidence and the angle of emergence can be adjusted in a predetermined manner in a coupled manner.
  • a device automatically discards workpieces that are determined to be faulty when measuring workpieces 100 percent.
  • FIG. 1 a schematic longitudinal section through a device for checking the composition of a layer material carried by a sample by X-ray fluorometry;
  • FIG. 2 shows a view of the front of a sample table of the device shown in FIG. 1;
  • Figure 3 is a plan view of the sample table of the device shown in Figure 1;
  • FIGS. 4 to 6 different X-ray fluorescence spectra of coated samples recorded under different conditions
  • FIG. 7 shows a longitudinal section through a modified device for analyzing the composition of a thin surface layer carried by a sample by X-ray fluorometry
  • FIG. 8 is a block diagram of an electronics unit, the mechanical with those shown in Figure 7
  • FIG. 9 a vertical longitudinal section through a modified sample table.
  • the X-ray fluorescence measuring apparatus shown in FIGS. 1 to 3 comprises a radiation source housing 10 and a detector housing 12, which are separated by vertical walls 14, 16, 18, a rear wall 19, a front wall not shown in the drawing and end plates 20, 22 are limited.
  • An X-ray tube 24 is arranged in the radiation source housing 10.
  • Two columns 26, 28 block an excitation beam 30 from the X-ray radiation emanating from the anode of the X-ray tube 24 and thus predefine an irradiation axis 31.
  • the excitation beam 30 passes through a window 32 which is provided in the upper end plate 22 and then enters a through hole 34 which is provided in a sample table 36.
  • the sample table 36 has an upper horizontal table surface 38 and an obliquely sloping table surface 40 on the left in FIG. 1.
  • the table surface 40 intersects the table surface 38 in a tilt axis 42 which is perpendicular to the plane of the drawing in FIG. 1 and which in turn is the beam axis 31 cuts at a right angle.
  • Switchable magnets 44, 46 serve to selectively fix a sample 48 made of iron to the table surface 38 and the table surface 40.
  • a depression 50 jumps back from the table surface 40, the bottom surface 52 of which forms a small angle with the table surface 40.
  • the bottom surface 52 intersects the table surface 38 at a point which is a small distance d (see FIG. 3) beyond the tilt axis 42 and the beam axis 31.
  • the sample 48 has a base material 54 made of iron or an iron alloy, on which a layer 56 is electrodeposited, the material of which comprises 99 percent by weight zinc and 1 percent by weight iron.
  • a fluorescent beam which leaves the layer at a small angle to the layer surface, that is to say grazing, is indicated at 58. Fluorescence radiation is emitted from the spot illuminated by the excitation beam 30 in the entire half space lying in front of the layer surface, but by providing an aperture, which will be dealt with later, only X-ray fluorescence beams that are grazing are used in the measurement in the device described here.
  • X-ray fluorescence radiation which is generated by the excitation beam 30 in the depth of the base material and runs essentially in the same direction as the fluorescence beam 58, has to traverse larger material stretches of the base material. These fluorescent rays are greatly weakened by absorption and therefore do not leave the sample surface.
  • a fluorescent radiation beam 64 and a detection axis 66 are predetermined by a gap 60, which is inserted into a window 62 of the end plate 22, and the illuminated spot on the sample surface.
  • the fluorescent radiation beam 64 falls on a proportional counter tube 68.
  • An operating unit 74 is connected to a central electrode 70 and an electrode 72 carried by the cylindrical housing. The latter generates the voltage required to operate the counter tube 68 and evaluates the current that flows in each case when an X-ray quantum strikes the counter tube.
  • the operating unit 74 also contains circuits which are known per se and which calculate the spectrum of the fluorescence radiation obtained from the received current pulses. This spectrum is output via a line 76 in the form of electrical signals which, for example in binary code, represent the intensity of the radiation obtained in successive equidistant energy intervals.
  • the gap 60 is arranged in such a way that the opening angle of the fluorescent radiation bundle is approximately 2 and the axis of the radiation bundle 66, viewed in three dimensions, has the shape of a sector-shaped flat wedge 66, viewed from above, an angle of approximately 2.5 with the Includes sample surface.
  • FIG. 4 shows schematically the spectrum of the fluorescence radiation which is obtained when grazing, that is, a very small angle of reflection of the fluorescence radiation.
  • the layer 56 is formed by a first metal M1, which is doped with a small amount of a second metal M2.
  • the metal M2 corresponds to the metal from which the base material 54 is made.
  • the part of the spectrum of FIG. 4 to be assigned to metal M2 is to be assigned to layer 56 and not to base material 54.
  • the concentration of the metal M2 in the layer 56 can thus be calculated directly from the ratio M2 / M1.
  • the base material can be provided with a layer 56 which contains only the metal M1. If the test conditions are otherwise the same, the spectrum shown schematically in FIG. 5 is obtained, in which the line to be assigned to the metal M2 is missing.
  • FIG. 6 shows an X-ray fluorescence spectrum which was obtained under a different irradiation geometry and a different observation geometry, as indicated schematically in the upper right corner.
  • the spectrum which is overall much more intense (compare qualitatively the units on the I axis), contains a very strong line to be assigned to the metal M2 and a weak line to be assigned to the metal Ml.
  • the thickness of the layer 56 can be determined from the ratio M1 / M2. Here one can neglect the vanishingly small proportions of line M2, which are due to metal atoms M2 in layer 56, since the concentration of metal M2 in layer 56 is very small according to the spectrum shown in FIG .
  • FIG. 7 shows a differently constructed X-ray fluorescence spectroscopy device, in which components which have already been explained in a functionally equivalent form with reference to FIGS. 1 to 3 again have the same reference numerals, even if these components differ in detail from those already described Differentiate components.
  • the radiation source housing 10 is attached to a device frame 78, which is only indicated schematically.
  • the device frame 78 also carries a bearing 80, in which a stub shaft 82 runs, which is supported by a bearing lever 84 is worn.
  • the detector housing 12 is arranged on the latter.
  • the sample table 36 carries a stub shaft 86, which runs in a bearing 88, which is arranged concentrically to the stub shaft 82 on the surface of the bearing lever 84 remote from the stub shaft 82.
  • the sample table 36 itself is dimensioned such that the surface of the sample 48 attached to it touches the coincident axes of rotation specified by the bearings 80 and 88.
  • a screw drive designated as a whole is provided.
  • This includes a stepper motor 92 with an associated rotary encoder 94.
  • the housing of the stepper motor 92 is connected in an articulated manner via a pivot pin 96 to a tab 98 carried by the radiation source housing 10.
  • the stepper motor 92 works on a threaded spindle 100 on which a threaded nut 102 runs.
  • the threaded nut 102 has bearing journals 104 on its side surfaces which engage in suitable bearing openings which are provided in tabs 106 which are carried by the detector housing 12.
  • a tab 108 is also provided on the detector housing 12, to which the housing of a further stepping motor 110 is pivotably attached by means of a pivot pin 112.
  • a rotary encoder 114 is assigned to the stepper motor 110.
  • the stepper motor 110 works on a threaded spindle 116, which cooperates with a threaded nut 118.
  • the latter carries trunnions 120 on its side surface, which run in bearing openings of tabs 122 which are arranged on the sample table 36.
  • the irradiation axis 31 runs at a very small angle of incidence with respect to the surface of the sample 48.
  • the angle between the detection axis 67 and the sample surface is also very small.
  • the fluorescent radiation is thus excited by grazing primary X-ray radiation, so that a stronger absorption of this radiation in the layer 56 is obtained.
  • the fluorescence radiation obtained in this way falls on the proportional counter tube 68.
  • the stepping motor 92 is controlled by a control of the device described in more detail below with reference to FIG. 8.
  • the stepper motor 110 can be controlled in a similar manner by this device in order to change the drop angle.
  • the encoders 94 and 114 are connected to the one inputs of controllers 124, 126, the outputs of which are connected to the control terminals of the stepper motors 92 and 110.
  • the second inputs of the controllers 124, 126 receive setpoint signals for the angles a, b from a freely programmable computer 128.
  • This data is loaded from the mass storage device 130 during measurement and is stored in a RAM area 132 of the device during the test of the sample. RAM of the computer 128 held.
  • correction functions u (i), v (i) and w (i) etc. which are used for different lines of metal Mu, Mv and Mw etc. appearing in the X-ray fluorescence spectrum. specify the correction factors with which one must multiply the intensities of the spectral lines for a given combination i of angle of incidence a (i) and angle of reflection b (i) in order to obtain the conditions at angle of reflection 0 (X-ray fluorescence originates exclusively from layer 56) .
  • the computer 128 receives the raw spectra provided by the operating unit 74 via line 76, corrects them in accordance with the correction functions u, v and w, calculates the concentration of the metals Mu, Mv, Mw etc. and checks whether these concentrations lie within predetermined tolerance limits.
  • the computer 128 determines the thickness of the layer 56 from the corresponding X-ray fluorescence spectrum.
  • the computer 128 also controls a stepper motor 140 with an associated rotary encoder 142 via a further controller 138 in order to successively transfer the surface area of the sample to be measured To lay the intersection between the beam axis and detector axis.
  • the values obtained for these different measurement positions are kept in the main memory of the computer, and can also be stored on the mass memory if required 130 are filed.
  • the computer 128 checks whether the composition and thickness of the layer lie within predetermined windows. This measurement result is displayed on a monitor 144 which, together with a keypad 146, also represents the operator interface of the computer 128.
  • the computer 128 actuates an ejection device 148, through which the workpiece 48 is fed into a reject Collection container is encountered.
  • results of the check in the form of a list or, if necessary, also printed out in the form of labels that can be attached to the tested workpieces or their packaging.
  • the computer 128 also transfers the type and the extent of the errors found to a process computer 152 which controls the manufacturing process of the workpieces, in the particular exemplary embodiment considered here a system for the galvanic application of the iron-doped zinc layer 56 to workpieces.
  • the process computer 152 actuates an electromagnetic metering valve 154, via which a metal salt storage container 156, in which the metal salt under consideration is present, for example, as a highly concentrated solution can be connected to a line 158 which leads into the electroplating bath.
  • the process computer 152 If the process computer 152 recognizes from the error data transmitted to it that the current strength during the electroplating is too high or too low, the process computer 152 controls a stepper motor 160 which works on the actuator of an adjustable resistor 162, which feeds into a feed line leading to the electrodes 164 is inserted.
  • the process computer 152 determines on the basis of the error data transmitted to it that the temperature of the electroplating bath is responsible for the errors which occur, it controls a stepper motor 166 which works on the actuator of an adjustable resistor 168, which is connected in series with a bath heating resistor 170 is switched.
  • the process computer 152 determines that the errors that have occurred are due to inhomogeneities in the electroplating bath, it controls an electric motor 172 that works on a stirrer 174.
  • the sample table is now designed as a one-piece bent sheet metal part and has a window 176 which is assigned to the sample support points of the table surfaces 40 and 38 and which replaces the depression 50.
  • a window 176 which is assigned to the sample support points of the table surfaces 40 and 38 and which replaces the depression 50.
  • an aperture 178 is arranged next to the window 32, which replaces the aperture 60.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

Pour qu'il soit possible de déterminer également la concentration d'atomes étrangers dont le spectre de fluorescence aux raxons X coïncide avec celui d'une matière de base (54), ou s'en rapproche, dans des échantillons (48) qui ont été pourvus d'un revêtement (56), il est proposé, selon l'invention, lors de la détermination de la concentration des atomes étrangers, d'analyser les rayons de fluorescence (58) qui partent, de façon rasante, de la surface de l'échantillon.
EP97921805A 1996-05-10 1997-04-27 Procede de determination par fluorescence x de la composition d'une matiere, et dispositif permettant la mise en oeuvre d'un tel procede Withdrawn EP0858596A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19618774 1996-05-10
DE1996118774 DE19618774A1 (de) 1996-05-10 1996-05-10 Röntgenfluoreszenz-Verfahren zum Bestimmen der Zusammensetzung eines Materiales sowie Vorrichtung zur Durchführung eines solchen Verfahrens
PCT/EP1997/002180 WO1997043626A1 (fr) 1996-05-10 1997-04-27 Procede de determination par fluorescence x de la composition d'une matiere, et dispositif permettant la mise en oeuvre d'un tel procede

Publications (1)

Publication Number Publication Date
EP0858596A1 true EP0858596A1 (fr) 1998-08-19

Family

ID=7793896

Family Applications (1)

Application Number Title Priority Date Filing Date
EP97921805A Withdrawn EP0858596A1 (fr) 1996-05-10 1997-04-27 Procede de determination par fluorescence x de la composition d'une matiere, et dispositif permettant la mise en oeuvre d'un tel procede

Country Status (3)

Country Link
EP (1) EP0858596A1 (fr)
DE (1) DE19618774A1 (fr)
WO (1) WO1997043626A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4262734B2 (ja) * 2005-09-14 2009-05-13 株式会社リガク 蛍光ｘ線分析装置および方法

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1986002164A1 (fr) * 1984-10-05 1986-04-10 Kawasaki Steel Corporation Procede permettant de determiner l'epaisseur et la composition d'un film en alliage
EP0372278A3 (fr) * 1988-12-02 1991-08-21 Gkss-Forschungszentrum Geesthacht Gmbh Procédé et appareil d'analyse d'échantillons par fluorescence aux rayons X
US5081658A (en) * 1989-03-30 1992-01-14 Nkk Corporation Method of measuring plating amount and plating film composition of plated steel plate and apparatus therefor
JP2853261B2 (ja) * 1989-05-16 1999-02-03 三菱マテリアル株式会社 金属分析方法および分析装置
EP0456897A1 (fr) * 1990-05-15 1991-11-21 Siemens Aktiengesellschaft Dispositif de mesure pour l'analyse par fluorescence de rayons X
JP3192846B2 (ja) * 1993-11-25 2001-07-30 株式会社東芝 汚染元素濃度分析方法および分析装置

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9743626A1 *

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Publication number Publication date
DE19618774A1 (de) 1997-11-13
WO1997043626A1 (fr) 1997-11-20

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