CN106959313A - A kind of method for quick of objects made from precious metals - Google Patents

A kind of method for quick of objects made from precious metals Download PDF

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Publication number
CN106959313A
CN106959313A CN201710374635.1A CN201710374635A CN106959313A CN 106959313 A CN106959313 A CN 106959313A CN 201710374635 A CN201710374635 A CN 201710374635A CN 106959313 A CN106959313 A CN 106959313A
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China
Prior art keywords
sample
sonigauge
quick
precious metals
objects made
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CN201710374635.1A
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Chinese (zh)
Inventor
杨佩
高亚伟
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Shenzhen Gold And Silver Jewelry Inspection Research Center Co Ltd
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Shenzhen Gold And Silver Jewelry Inspection Research Center Co Ltd
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Priority to CN201710374635.1A priority Critical patent/CN106959313A/en
Publication of CN106959313A publication Critical patent/CN106959313A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/22Investigating 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
    • G01N23/223Investigating 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01BMEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B17/00Measuring arrangements characterised by the use of infrasonic, sonic or ultrasonic vibrations
    • G01B17/02Measuring arrangements characterised by the use of infrasonic, sonic or ultrasonic vibrations for measuring thickness

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  • Physics & Mathematics (AREA)
  • General 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)
  • Immunology (AREA)
  • Pathology (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

The invention discloses a kind of method for quick of objects made from precious metals, the present invention is that a kind of method for quick of objects made from precious metals detects that the main component and component content on sample top layer tentatively judge whether sample is qualified using Xray fluorescence spectrometer, further sample is detected using sonigauge, the ultrasonic pulse sent by sonigauge reaches first material interface of sample and is reflected back the time that sonigauge is consumed, to calculate the thickness value d2 between sample test point and first material interface, the thickness value of the sample measured with slide measure is compared, if meeting | d2/d1 1 | * 100%≤5%, it can determine whether that sample is qualified.This method can lossless, quick, accurate, easily detect that whether sample is qualified, for large-scale inspection center in the case where inspection task is more, is greatly improved operating efficiency, reduces the cost.

Description

A kind of method for quick of objects made from precious metals
Technical field
The present invention relates to objects made from precious metals detection, more specifically a kind of method for quick of objects made from precious metals.
Background technology
At present, in noble metal detection field, Xray fluorescence spectrometer is a kind of for examining the normal of objects made from precious metals purity Detecting instrument is advised, the characteristics of with quick screening, but general Xray fluorescence spectrometer is for the detection office of objects made from precious metals Be limited to top layer (X-ray to gold only about 10 μm of investigation depth, to silver only about 50 μm of investigation depth), it is impossible to objects made from precious metals Inner case detected;There is a situation where that doping is faked inside noble metal, is only analyzed by X-ray fluorescence spectra on the market Objects made from precious metals surface, is easily judged by accident, detects inaccurate situation;Your also have using density synthesis that gold detected now Category, but there are problems that high cost, time-consuming, limitation, faked for passing through counterweight and the close metal of doping density Objects made from precious metals, then can not detect.
Therefore, it is necessary to design it is a kind of can it is lossless, quick, accurate, easily detect objects made from precious metals detection method.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of method for quick of objects made from precious metals.
To achieve the above object, the present invention uses following technical scheme:A kind of method for quick of objects made from precious metals, bag Include following steps:
S10, the condition of work for setting Xray fluorescence spectrometer, sample are placed in the detection of Xray fluorescence spectrometer On platform, the main component and component content on detection sample top layer;
The mark that S20, the sample data for measuring the multiple test points in sample top layer are averaged with sample Claim Value Data to be compared, if meeting standard value lower limit requirement, carry out next step detection, otherwise, stop detection, judge tested Failed sample;
S30, the thickness value d1 for measuring with gage two apparent surfaces at sample test point;
S40, the condition of work for setting sonigauge, the ultrasonic pulse sent by sonigauge reach quilt First material interface of test sample product is simultaneously reflected back the time that sonigauge is consumed, to calculate sample test point Thickness value d2 between surface and first material interface.
S50, d1 and d2 contrasted, if meeting | d2/d1-1 | * 100%≤5%, detected sample is qualified, otherwise, quilt Survey failed sample.
Its further technical scheme is:Also include the test that sample is cleaned with absolute ethyl alcohol before the step S10 Surface.
Its further technical scheme is:In the S10 steps, selection manganese element is differentiated at the peak of 5.89keV energy positions Rate is better than 170eV Xray fluorescence spectrometer.
Its further technical scheme is:In the step S20, the test point includes more than three test points, wherein, phase Air line distance between adjacent two test points is more than 10mm.
Its further technical scheme is:In the step S30, the gage is slide measure.
Its further technical scheme is:The minimum division value of the slide measure is 0.01mm~0.02mm.
Its further technical scheme is:In the step S40, sample test point and the amount of sonigauge detection The position for the sample test point that chi is surveyed is identical.
Its further technical scheme is:The step S40 specifically includes following sub-step:
S41:Range of choice/resolution ratio is 0.6-508mm/0.01mm, and error is ± 0.3%D+0.03mm, and the velocity of sound is 500-9999m/s sonigauge;
S42:Calibrate sonigauge;
S43:Couplant is coated on to the probe of sample test point and/or sonigauge;
S44:Probe is adjacent to and sample test point, regulation sonigauge running parameter, with what is stablized Thickness value d2.
Compared with the prior art, the invention has the advantages that:A kind of method for quick of objects made from precious metals of the present invention is adopted Detect sample surface main component and component content with Xray fluorescence spectrometer, can tentatively judge by sample whether It is qualified, sample inner case is further detected using sonigauge, the accuracy of detection is improved, separately Outside, combined by both Xray fluorescence spectrometer and sonigauge and sample is detected, test specimens will not be destroyed Product, realize Non-Destructive Testing, to the condition less-restrictive of sample, and step is easy, more can fast, easily detect, for big Type inspection center is greatly improved operating efficiency in the case where inspection task is more, reduces the cost.
Described above is only the general introduction of technical solution of the present invention, in order to better understand technical measure, and It can be practiced according to the content of specification, and in order to allow above and other objects of the present invention, feature and the advantage can be more Become apparent, below especially exemplified by preferred embodiment, and coordinate accompanying drawing, describe in detail as follows.
Brief description of the drawings
Fig. 1 is a kind of flow chart of the method for quick specific embodiment of objects made from precious metals of the invention;
Fig. 2 for a kind of objects made from precious metals of the invention method for quick specific embodiment in step S40 sub-step stream Cheng Tu;
Fig. 3 is the silver bullion main component of embodiment one and the data form of component content;
Fig. 4 is the vernier caliper measurement silver bullion thickness value d1 of embodiment one data form.
Embodiment
In order to more fully understand the technology contents of the present invention, technical scheme is entered with reference to specific embodiment One step introduction and explanation, but it is not limited to this.
As shown in Figure 1-2, a kind of method for quick of objects made from precious metals of the invention, comprises the following steps:
S10, the condition of work for setting Xray fluorescence spectrometer, sample are placed in the detection of Xray fluorescence spectrometer On platform, the main component and component content on detection sample top layer;
The mark that S20, the sample data for measuring the multiple test points in sample top layer are averaged with sample Claim Value Data to be compared, if meeting standard value lower limit requirement, carry out next step detection, otherwise, stop detection, judge tested Failed sample;
S30, the thickness value d1 for measuring with gage sample test point;
S40, the condition of work for setting sonigauge, the ultrasonic pulse sent by sonigauge reach quilt First material interface of test sample product is simultaneously reflected back the time that sonigauge is consumed, to calculate sample test point With the thickness value d2 between first material interface.
S50, d1 and d2 contrasted, if meeting | d2/d1-1 | * 100%≤5%, detected sample is qualified, otherwise, quilt Survey failed sample.
Further, the test surfaces that sample is cleaned with absolute ethyl alcohol are also included before step S10, go to degrease.
Further, in S10 steps, selection manganese element is better than 170eV X in the peak of 5.89keV energy positions, resolution ratio Ray fluorescence spectrometer.
Further, in step S20, test point includes more than three test points, wherein, between two neighboring test point Air line distance is more than 10mm.;The result that the aggregation of data analysis obtained from representative difference is drawn is more accurate.
Further, in step S30, gage is slide measure or micrometer;The minimum division value of slide measure is 0.01mm~0.02mm, preferably 0.01mm.
Further, in step S40, the detected sample that the sample test point that sonigauge is detected is surveyed with gage The position of product test point is identical.
Step S40 specifically includes following sub-step:
S41:Range of choice/resolution ratio is 0.6-508mm/0.01mm, and error is ± 0.3%D+0.03mm, and the velocity of sound is 500-9999m/s sonigauge;
S42:Calibrate sonigauge;
S43:Couplant is coated on to the probe of sample test point and/or sonigauge;
S44:Probe is adjacent to and sample test point, regulation sonigauge running parameter, with what is stablized Thickness value d2.
Specifically, the present embodiment one detects the specific side of pure silver 999 using a kind of method for quick of objects made from precious metals Method:
The first step:Silver bullion surface is cleaned with absolute ethyl alcohol, goes to degrease;
Second step:Select manganese element at the peak of 5.89keV energy positions, resolution ratio is better than 170eV X-ray fluorescence spectra Instrument, silver bullion is placed on the monitor station of Xray fluorescence spectrometer, closes detection hatchcover, the silver-colored series of tasks curve of selection;Choose 3 diverse locations are detected that obtained results averaged refer to the test data shown in Fig. 3, test result on silver bullion Silver content is 999.5 ‰, meets the scope of silver content nominal value in pure silver 999, Preliminary detection silver bullion is qualified;
3rd step:The slide measure that minimum division value is 0.02mm is selected, selects surface more smooth on silver bullion, it is relative Two surface flat shapes or coaxial test point, it is relative with vernier caliper measurement test point two with alcohol wipe test point surface and oil contaminant The distance on surface, i.e. thickness value d1;The test data shown in Fig. 4 is refer to, to same test point retest three times, is made even Average result is d1=2.62mm;
4th step:Range of choice/resolution ratio is 1.5-150mm/0.01mm, and error is ± 0.3%D+0.03mm, and the velocity of sound is 1000-9999m/s sonigauge, opens sonigauge, and the 4.00mm carried using sonigauge is stainless Steel disc carries out zero point correction, and coating couplant clicks on " calibration " button on steel disc, the steel disc for scribbling couplant is attached to by popping one's head in Surface, it is ensured that press close to, waits instrument to calibrate completion automatically;
5th step:Sonigauge is built-in with spread speed of the sound wave in the noble metal of gold, silver, platinum and the type of palladium 4, In this detection, " silver " type is selected, setting thickness value is 2.6mm, and couplant is coated in into silver bullion test point, probe is adjacent to Stable reading on sample surfaces, screen to be shown, reads thickness value d2=2.64mm;
6th step:D1=2.62mm, d2=2.64mm, meet | d2/d1-1 | * 100%≤5% explanation silver bullion surface with it is interior Portion is uniform, in the absence of defect and is mingled with, and judges that this silver bullion integrally meets the requirement of the quality of pure silver 999.
In other embodiments, selection manganese element is better than 170eV X-ray in the peak of 5.89keV energy positions, resolution ratio XRF, scope/resolution ratio is 0.6-508mm/0.01mm, and error is ± 0.3%D+0.03mm, and the velocity of sound is 500- 9999m/s sonigauge, minimum division value is detected for 0.02mm slide measure.
In other embodiments, the test table of sample is cleaned using the conventional organic solvent for going to degrease such as acetone Face.
Summary:A kind of method for quick of objects made from precious metals of the present invention employs Xray fluorescence spectrometer detection Sample surface main component and component content, whether by sample qualified, using sonigauge pair if can tentatively judge Sample inner case is further detected, improves the accuracy of detection, in addition, passing through Xray fluorescence spectrometer Combined with both sonigauges and sample is detected, test sample will not be destroyed, Non-Destructive Testing is realized, to being tested The condition less-restrictive of sample, step is easy, more can fast, easily detect, for large-scale inspection center inspection task compared with In the case of many, operating efficiency is greatly improved, is reduced the cost.
The above-mentioned technology contents that the present invention is only further illustrated with embodiment, in order to which reader is easier to understand, but not Represent embodiments of the present invention and be only limitted to this, any technology done according to the present invention extends or recreated, by the present invention's Protection.Protection scope of the present invention is defined by claims.

Claims (8)

1. a kind of method for quick of objects made from precious metals, it is characterised in that comprise the following steps:
S10, the condition of work for setting Xray fluorescence spectrometer, sample are placed in the monitor station of Xray fluorescence spectrometer On, the main component and component content on detection sample top layer;
The nominal value that S20, the sample data for measuring the multiple test points in sample top layer are averaged with sample Data are compared, if meeting standard value lower limit requirement, carry out next step detection, otherwise, are stopped detection, are judged sample It is unqualified;
S30, the thickness value d1 for measuring using gage the apparent surface of sample test point two;
S40, the condition of work for setting sonigauge, the ultrasonic pulse sent by sonigauge reach detected sample First material interface of product is simultaneously reflected back the time that sonigauge is consumed, to calculate sample test point and first Thickness value d2 between individual material interface.
S50, d1 and d2 contrasted, if meeting | d2/d1-1 | * 100%≤5%, detected sample is qualified, otherwise, detected sample Product are unqualified.
2. a kind of method for quick of objects made from precious metals according to claim 1, it is characterised in that the step S10 Also include the test surfaces that sample is cleaned with absolute ethyl alcohol before.
3. a kind of method for quick of objects made from precious metals according to claim 1, it is characterised in that the S10 steps In, selection manganese element is better than 170eV Xray fluorescence spectrometer in the peak of 5.89keV energy positions, resolution ratio.
4. a kind of method for quick of objects made from precious metals according to claim 1, it is characterised in that the step S20 In, the test point includes more than three test points, wherein, the air line distance between two neighboring test point is more than 10mm.
5. a kind of method for quick of objects made from precious metals according to claim 1, it is characterised in that the step S30 In, the gage is slide measure.
6. a kind of method for quick of objects made from precious metals according to claim 5, it is characterised in that the slide measure Minimum division value be 0.01mm~0.02mm.
7. a kind of method for quick of objects made from precious metals according to claim 1, it is characterised in that the step S40 In, the sample test point of sonigauge detection is identical with the position for the sample test point that gage is surveyed.
8. a kind of method for quick of objects made from precious metals according to claim 1, it is characterised in that the step S40 Specifically include following sub-step:
S41:Range of choice/resolution ratio is 0.6-508mm/0.01mm, and error is ± 0.3%D+0.03mm, and the velocity of sound is 500- 9999m/s sonigauge;
S42:Calibrate sonigauge;
S43:Couplant is coated on to the probe of sample test point and/or sonigauge;
S44:Probe is adjacent to and sample test point, regulation sonigauge running parameter, with the thickness stablized Value d2.
CN201710374635.1A 2017-05-24 2017-05-24 A kind of method for quick of objects made from precious metals Pending CN106959313A (en)

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US11614324B2 (en) 2019-10-24 2023-03-28 International Business Machines Corporation Non-destructive bond line thickness measurement of thermal interface material on silicon packages

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CN103412047A (en) * 2013-08-20 2013-11-27 陕西师范大学 Method for identifying true and false metal by ultrasonic non-destructive detection method
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11614324B2 (en) 2019-10-24 2023-03-28 International Business Machines Corporation Non-destructive bond line thickness measurement of thermal interface material on silicon packages

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Application publication date: 20170718