CN108982475A - Prepare the method for direct-reading spark spectrum instrument sample, the method and direct-reading spark spectrum instrument of analyzing irregular metal material composition - Google Patents
Prepare the method for direct-reading spark spectrum instrument sample, the method and direct-reading spark spectrum instrument of analyzing irregular metal material composition Download PDFInfo
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- CN108982475A CN108982475A CN201810759330.7A CN201810759330A CN108982475A CN 108982475 A CN108982475 A CN 108982475A CN 201810759330 A CN201810759330 A CN 201810759330A CN 108982475 A CN108982475 A CN 108982475A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/67—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using electric arcs or discharges
Abstract
The invention discloses the methods of preparation direct-reading spark spectrum instrument sample, the method and direct-reading spark spectrum instrument of analyzing irregular metal material composition.Wherein, the method for preparing direct-reading spark spectrum instrument sample includes: 1) to cut to one end of metal sample to be measured, so as in one end Formation cross-section of the metal sample；(2) using powder is inlayed, hot pressing damascene process is carried out to metal sample obtained by step (1), form the package metal sample inlays sample block；(3) grinding and polishing processing is carried out to one end of metal sample obtained by step (2), to expose the section.Small sized metallic sample preparation can be simply and efficiently the sample for meeting direct-reading spark spectrum instrument analysis detection by the preparation method.
Description
Technical field
The present invention relates to Analysis of Metallic Materials fields, specifically, the present invention relates to preparation direct-reading spark spectrum instrument samples
Method, analyzing irregular shaped metal material composition method and direct-reading spark spectrum instrument.
Background technique
Spectroanalysis instrument uses the analysis principle of atomic emission spectroscopy, and the sample on spark table is passed through electric arc or spark
Discharge excitation generates atomic vapour, and the atom and ion in the steam generate emission spectrum after being excited.Emission spectrum passes through light
It leads fiber to enter in the light-splitting chamber of spectrometer, dispersion is at each spectral band.According to the wave-length coverage that each element emits, pass through
Photomultiplier tube can measure the best spectral line of every kind of element.Emission spectrum the intensity of spectral line of every kind of element is proportional in sample
The content of the element can measure its content by calibration curve pre-stored inside spectrometer, and by member each in sample to be tested
The composition of element shows have in elemental analysis of samples in metal material industry and widely answer directly with percent concentration
With.
But during using direct-reading spark spectrum instrument to sample analysis, instrument is to test specimen, especially sample
Product, the shape of thin sample, size and size have strict demand.The small sample for carrying out subsidiary analysis for borrowing fixture, more
The cuboid or oblate column that sample is made into specification are sought, convenient for finding center positioning, in favor of measurement analysis.Existing skill
In art, analysis for small sample generally requires and first polishes sample two sides, then the cylindrical body of rule or rectangular is made in sample
Body.If sample cannot be met the requirements, it is difficult to be analyzed.And in actual operation, often because sample volume is too small, can grasp
The property made is poor, cannot have progress two sides to polish, and sample is caused to be not used to spectrometer detection.
Thus, existing metallic element spectrum analysis means still have much room for improvement.
Summary of the invention
The present invention is directed to solve at least some of the technical problems in related technologies.For this purpose, of the invention
One purpose is the method for proposing the method for preparation direct-reading spark spectrum instrument sample, analyzing irregular shaped metal material composition
With direct-reading spark spectrum instrument.The method of the preparation direct-reading spark spectrum instrument sample can be simply and efficiently by small sized metallic sample system
Standby is the sample for meeting direct-reading spark spectrum instrument analysis detection.
In one aspect of the invention, the present invention proposes a kind of method for preparing direct-reading spark spectrum instrument sample,
It is characterized in that, comprising: (1) one end of metal sample to be measured is cut, cut to be formed in one end of the metal sample
Face；(2) using powder is inlayed, hot pressing damascene process is carried out to metal sample obtained by step (1), is formed and wraps up the metal sample
Inlay sample block；(3) grinding and polishing processing is carried out to one end of metal sample obtained by step (2), to expose the section.
The method of preparation direct-reading spark spectrum instrument sample according to an embodiment of the present invention, first to the to be measured of irregular shape
Metal sample is cut, and in one end Formation cross-section of metal sample, which is used as conducting surface directly and direct-reading in the detection
The contact of spark spectrum instrument spark table；And then inlay powder and hot pressing damascene process is carried out to the sample after cutting, make to inlay powder and is solidificated in
On sample, formed wrap up in the metal sample inlay sample block；Again to the progress grinding and polishing processing of sample block is inlayed, inlayed after guaranteeing grinding and polishing
Under the premise of the block-shaped rule of sample, the section cut on metal sample is exposed from inlaying in sample block, completes sample
Preparation.As a result, this method by small sample carry out hot pressing damascene process, make sample size become larger and shape become rule,
To meet requirement of the direct-reading spark spectrum analysis to sample.Meanwhile this method only need to cut metal sample to be measured to obtain one
As the conducting surface in detection, preparation section is more easy in a section, and further reduced detection and want to sample shape
It asks, extends the minimum dimension limit of sample analysis, substantially increase the application range of direct-reading spark spectrum instrument.
In addition, it is according to the above embodiment of the present invention preparation direct-reading spark spectrum instrument sample method can also have it is as follows
Additional technical characteristic:
In some embodiments of the invention, the section is the maximum area cut to the metal sample
Section.It can further improve the accuracy of testing result as a result,.
In some embodiments of the invention, the inscribed circle diameter in the section is not less than 12 millimeters.It as a result, can be further
Improve the accuracy of testing result.
In some embodiments of the invention, the area in the section is not less than 113 square millimeters.It as a result, can be further
Improve the accuracy of testing result.
In some embodiments of the invention, the sample block of inlaying is formed as cylindrical body, cuboid or square.As a result,
Sample block is inlayed by what the metal sample of irregular shape was prepared as regular shape, to meet direct-reading spark spectrum instrument to examination
The requirement of sample shape.
In some embodiments of the invention, the height for inlaying sample block is greater than at least 10 milli of metal sample thickness
Rice.It can further improve the accuracy of testing result as a result,.
In some embodiments of the invention, the powder of inlaying is bakelite powder.
In some embodiments of the invention, the hot pressing damascene process carries out under 130~165 degrees Celsius.
In some embodiments of the invention, the time that the hot pressing damascene process carries out is 8~10 minutes.
In some embodiments of the invention, the grinding and polishing processing is carried out using abrasive machine, the abrasive machine includes 30~
The grinding wheel of 80 mesh.It can further advantageously ensure that the surface roughness that sample block is inlayed after grinding and polishing is handled reaches test and wants as a result,
It asks.
In another aspect of this invention, the invention proposes a kind of methods of analyzing irregular shaped metal material composition.
According to an embodiment of the invention, this method comprises: preparing sample according to method described in above-described embodiment；Utilize direct-reading spark light
Spectrometer carries out chemical composition analysis to the sample, wherein the sample of the direct-reading spark spectrum instrument is connected using conductive material
Folder and spark table table top.
The method of analyzing irregular shaped metal material composition according to an embodiment of the present invention, side through the foregoing embodiment
Metal sample to be detected is prepared as sample by method, and carries out chemical composition analysis to the sample using direct-reading spark spectrum instrument.
Wherein, sample is fixed on direct-reading spark spectrum instrument spark table using specimen holder, the section that metal sample to be detected exposes
With spark table deck contact, specimen holder is fixed on nonconducting inlaid material part.In turn, conductive material connection direct-reading fire is utilized
The specimen holder and spark table table top of spectrometer are used up, that is, can guarantee the direct motion of detection, and testing result accuracy is high.
In addition, the method for analyzing irregular shaped metal material composition according to the above embodiment of the present invention can also have
Following additional technical characteristic:
In some embodiments of the invention, the conductive material passes through contact screw and the specimen holder and the spark
The connection of platform table top.The connection type of conductive material and specimen holder and spark table table top is simple and easy as a result, can further be conducive to
Guarantee the direct motion of detection.
In still another aspect of the invention, the invention proposes a kind of direct-reading spark spectrum instrument.According to an embodiment of the invention,
The direct-reading spark spectrum instrument includes: specimen holder；And spark table, it is formed and is electrically connected between the specimen holder and the spark table table top
It connects.The method that the direct-reading spark spectrum instrument is adapted for carrying out the analyzing irregular shaped metal material composition of above-described embodiment, this is straight
It reads spark spectrum instrument to be electrically connected by making to be formed between specimen holder and spark table table top, solves the edge being connected directly with specimen holder
Embedding material is non-conductive and causes to detect the problem of can not carrying out.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Detailed description of the invention
Above-mentioned and/or additional aspect of the invention and advantage will become from the description of the embodiment in conjunction with the following figures
Obviously and it is readily appreciated that, in which:
Fig. 1 is utilization direct-reading spark spectrum instrument analyzing irregular shaped metal material group according to an embodiment of the invention
At operation principle schematic diagram.
Description of symbols:
1- metal sample to be detected；2- inlaid material；3- electrode；4- specimen holder；5- conductive material；6- spark table.
Specific embodiment
The embodiment of the present invention is described below in detail, examples of the embodiments are shown in the accompanying drawings, wherein from beginning to end
Same or similar label indicates same or similar element or element with the same or similar functions.Below with reference to attached
The embodiment of figure description is exemplary, it is intended to is used to explain the present invention, and is not considered as limiting the invention.
In the description of the present invention, it is to be understood that, term " center ", " longitudinal direction ", " transverse direction ", " length ", " width ",
" thickness ", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outside", " up time
The orientation or positional relationship of the instructions such as needle ", " counterclockwise ", " axial direction ", " radial direction ", " circumferential direction " be orientation based on the figure or
Positional relationship is merely for convenience of description of the present invention and simplification of the description, rather than the device or element of indication or suggestion meaning must
There must be specific orientation, be constructed and operated in a specific orientation, therefore be not considered as limiting the invention.
In the present invention unless specifically defined or limited otherwise, the terms such as " installation ", " connected ", " connection ", " fixation "
It shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or is integral；It can be mechanical connection,
It is also possible to be electrically connected；It can be directly connected, can also can be inside two elements indirectly connected through an intermediary
The interaction relationship of connection or two elements, unless otherwise restricted clearly.For the ordinary skill in the art,
The specific meanings of the above terms in the present invention can be understood according to specific conditions.
In the present invention unless specifically defined or limited otherwise, fisrt feature in the second feature " on " or " down " can be with
It is that the first and second features directly contact or the first and second features pass through intermediary mediate contact.Moreover, fisrt feature exists
Second feature " on ", " top " and " above " but fisrt feature be directly above or diagonally above the second feature, or be merely representative of
First feature horizontal height is higher than second feature.Fisrt feature can be under the second feature " below ", " below " and " below "
One feature is directly under or diagonally below the second feature, or is merely representative of first feature horizontal height less than second feature.
Inventor has found in the research to metallic element spectrum analysis means, in utilization direct-reading spark spectrum instrument to sample
In analytic process, instrument has strict demand to the shape, size and size of test specimen, especially small sample, thin sample.For
Borrow the small sample that fixture carrys out subsidiary analysis, the cuboids or oblate column for requiring for sample to be made into specification, convenient for looking for more
It is positioned to center, in favor of measurement analysis.In the prior art, it for the analysis of small sample, generally requires sample two sides
It polishes, and controls its thickness within 2~100mm, or sample is made to the cylindrical body or cuboid of rule.If sample is not
It is able to satisfy requirement, then is difficult to be analyzed.It can be seen that being reduced when carrying out spectrum analysis to sample using spark spectrum instrument
Instrument limits lesser sample shape and extends the minimum dimension limit of sample, for expanding the application of direct-reading spark spectrum instrument
Range important in inhibiting.
In consideration of it, in one aspect of the invention, the present invention proposes a kind of direct-reading spark spectrum instrument sample for preparing
Method characterized by comprising (1) one end of metal sample to be measured is cut, so that one end in metal sample is formed
Section；(2) using powder is inlayed, hot pressing damascene process is carried out to metal sample obtained by step (1), forms the edge of package metal sample
Embedding sample block；(3) grinding and polishing processing is carried out to one end of metal sample obtained by step (2), to expose above-mentioned section.
The method of preparation direct-reading spark spectrum instrument sample according to an embodiment of the present invention, first to the to be measured of irregular shape
Metal sample is cut, and in one end Formation cross-section of metal sample, which is used as conducting surface directly and direct-reading in the detection
The contact of spark spectrum instrument spark table；And then inlay powder and hot pressing damascene process is carried out to the sample after cutting, make to inlay powder and is solidificated in
On sample, formed wrap up in metal sample inlay sample block；Again to the progress grinding and polishing processing of sample block is inlayed, sample block is inlayed after guaranteeing grinding and polishing
Under the premise of regular shape, the section cut on metal sample is exposed from inlaying in sample block, completes the system of sample
It is standby.As a result, this method by small sample carry out hot pressing damascene process, make sample size become larger and shape become rule, thus
Meet requirement of the direct-reading spark spectrum analysis to sample.Meanwhile this method need to only cut metal sample to be measured to obtain one section
As the conducting surface in detection, preparation section is more easy in face, and further reduced the requirement detected to sample shape, prolongs
The minimum dimension limit for having stretched sample analysis, substantially increases the application range of direct-reading spark spectrum instrument.
According to an embodiment of the invention, being to be cut to metal sample by cutting the section formed in metal sample one end
Cut available maximum area section.It can further improve the accuracy of testing result as a result,.Implementation according to the present invention
Example, can cut metal sample to be detected using tools such as wire cutting machine or saw blades according to the shape size situation of sample
It cuts.
According to an embodiment of the invention, the inscribed circle diameter in above-mentioned section is not less than 12 millimeters.It can further improve as a result,
The accuracy of testing result.
According to an embodiment of the invention, the area in above-mentioned section is not less than 113 square millimeters.It can further improve as a result,
The accuracy of testing result, and can guarantee that sample has enough thermal diffusivities in the detection process.
According to an embodiment of the invention, above-mentioned sample block of inlaying is formed as cylindrical body, cuboid or square.Pass through as a result,
Sample block is inlayed by what the metal sample of irregular shape was prepared as regular shape, to meet direct-reading spark spectrum instrument to sample shape
The requirement of shape.
According to an embodiment of the invention, the above-mentioned height for inlaying sample block is greater than at least 10 millimeters of metal sample thickness.As a result,
It can further improve the accuracy of testing result.It specifically, can be by controlling the edge inlaying the dosage of powder and being prepared
The height of embedding sample block.
According to an embodiment of the invention, the above-mentioned type for inlaying powder is not particularly restricted, as long as can effectively will be small
The sample preparation of size obtains inlaying sample block and having good insulating properties and thermosetting property for regular shape.In the present invention
Some embodiments in, inlaying powder can be used bakelite powder.
According to an embodiment of the invention, hot pressing damascene process can carry out under 130~165 degrees Celsius.It is according to the present invention
Embodiment, the time that hot pressing damascene process carries out are 8~10 minutes.It can further be conducive to inlay in hot pressing damascene process as a result,
The solidification of embedding powder, material property is stablized after guaranteeing solidification.In addition, in hot pressing damascene process, while applying the pressure of suitable size
Power is to guarantee to inlay sample block consolidation.
According to an embodiment of the invention, using abrasive machine to inlay sample block carry out grinding and polishing processing, abrasive machine include 30~
The grinding wheel of 80 mesh.It can further advantageously ensure that the surface roughness that sample block is inlayed after grinding and polishing is handled reaches test and wants as a result,
It asks.
In another aspect of this invention, the invention proposes a kind of methods of analyzing irregular shaped metal material composition.
According to an embodiment of the invention, this method comprises: the method according to above-described embodiment prepares sample；Utilize direct-reading spark spectrum instrument
Chemical composition analysis is carried out to sample, wherein utilize the specimen holder and spark table platform of conductive material connection direct-reading spark spectrum instrument
Face.
Specifically, the method for analyzing irregular shaped metal material composition according to an embodiment of the present invention, first by upper
Metal sample to be detected is prepared as sample by the method for stating embodiment, before detection, should ensure that sample surfaces are bright and clean.Further
Ground, with reference to Fig. 1, by the center alignment direct-reading spark spectrum instrument of sample conducting surface (i.e. sample, which exposes, inlays the section of sample block)
Sample is fixed on direct-reading spark spectrum instrument spark table 6 by electrode 3 using specimen holder 4, what metal sample 1 to be detected exposed
The deck contact in section and spark table 6, specimen holder 4 are fixed on nonconducting 2 part of inlaid material.In turn, conductive material 5 is utilized
The specimen holder 4 of direct-reading spark spectrum instrument and the table top of spark table 6 are connected, that is, can guarantee the direct motion of detection, and testing result is accurate
Degree is high.It should be noted that same described previously for feature and advantage described in the method for preparing direct-reading spark spectrum instrument sample
Suitable for the method for above-mentioned analyzing irregular shaped metal material composition, this is no longer going to repeat them.
According to an embodiment of the invention, conductive material can be connect by contact screw with specimen holder and spark table table top.By
This, the connection type of conductive material and specimen holder and spark table table top is simple and easy, can further advantageously ensure that the suitable of detection
Row.Copper conductor can be used in a specific example according to the present invention, conductive material.
In still another aspect of the invention, the invention proposes a kind of direct-reading spark spectrum instrument.According to an embodiment of the invention,
The direct-reading spark spectrum instrument includes: specimen holder and spark table.Wherein, it is formed and is electrically connected between specimen holder and the table top of spark table.
The method that the direct-reading spark spectrum instrument is adapted for carrying out the analyzing irregular shaped metal material composition of above-described embodiment, direct-reading fire
It uses up spectrometer to be electrically connected by making to be formed between specimen holder and the table top of spark table, solves and inlayed with what specimen holder was connected directly
Material is non-conductive and causes to detect the problem of can not carrying out.It should be noted that described previously for preparation direct-reading spark spectrum instrument examination
Feature and advantage described in the method for method and analyzing irregular shaped metal the material composition of sample are equally applicable to above-mentioned straight
Spark spectrum instrument is read, this is no longer going to repeat them.
Below with reference to specific embodiment, present invention is described, it should be noted that these embodiments are only to describe
Property, without limiting the invention in any way.
Embodiment
According to the following steps, the sample formed known to certain is analyzed using direct-reading spark spectrum instrument:
(1) one end of sample to be tested is cut, so as in one end Formation cross-section of sample；Guarantee the inscribed of the section
Circle is directly not less than 12 millimeters.
(2) using powder is inlayed, hot pressing damascene process is carried out to sample obtained by step (1), form package sample inlays sample
Block；It inlays the control of powder dosage and is greater than at least 10 millimeters of thickness of sample in the height for making gained inlay sample block；Hot pressing damascene process exists
Carried out under 130~165 degrees Celsius 8~10 minutes complete, and in hot pressing damascene process to provide impressed pressure to guarantee to inlay sample
Block consolidation.
(3) grinding and polishing processing is carried out to inlaying sample block using abrasive machine (grinding wheel be 30~80 mesh), exposed sample section, and
Gained sample is still regular shape after guaranteeing grinding and polishing.
(4) composition analysis is carried out to the sample prepared using direct-reading spark spectrum instrument, the results are shown in Table 1.
Table 1
| Chemical component (%) | C | Si | Mn | P | S | Ni | Cr |
| Theoretical value | 0.40 | 0.21 | 0.55 | 0.013 | 0.0015 | 0.06 | 0.015 |
| Actual measured value | 0.41 | 0.22 | 0.56 | 0.014 | 0.0017 | 0.07 | 0.017 |
The theoretical value and actual measured value of Partial Elements in sample to be tested are listed in table 1, the experimental results showed that, according to this
The method of invention analyzes sample, and actual measured results differ minimum, of the invention analysis side with known sample composition theoretical value
Method has good accuracy.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office
It can be combined in any suitable manner in one or more embodiment or examples.In addition, without conflicting with each other, the skill of this field
Art personnel can tie the feature of different embodiments or examples described in this specification and different embodiments or examples
It closes and combines.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, modifies, replacement and variant.
Claims (10)
1. a kind of method for preparing direct-reading spark spectrum instrument sample characterized by comprising
(1) one end of metal sample to be measured is cut, so as in one end Formation cross-section of the metal sample；
(2) using powder is inlayed, hot pressing damascene process is carried out to metal sample obtained by step (1), is formed and wraps up the metal sample
Inlay sample block；
(3) grinding and polishing processing is carried out to the sample block of inlaying, to expose the section.
2. the method according to claim 1, wherein the section is to be cut to obtain to the metal sample
Maximum area section.
3. the method according to claim 1, wherein the inscribed circle diameter in the section is not less than 12 millimeters；
Optionally, the area in the section is not less than 113 square millimeters.
4. the method according to claim 1, wherein the sample block of inlaying is formed as cylindrical body, cuboid or just
Cube；
Optionally, the height for inlaying sample block is greater than at least 10 millimeters of the metal sample thickness.
5. method according to any one of claims 1 to 4, which is characterized in that the powder of inlaying is bakelite powder.
6. according to the method described in claim 5, it is characterized in that, the hot pressing damascene process under 130~165 degrees Celsius into
Row, the time that the hot pressing damascene process carries out are 8~10 minutes.
7. according to the method described in claim 6, it is characterized in that, carrying out the grinding and polishing processing, the grinding wheel using abrasive machine
Machine includes the grinding wheel of 30~80 mesh.
8. a kind of method of analyzing irregular shaped metal material composition characterized by comprising
Sample is prepared according to the described in any item methods of claim 1~7；
Chemical composition analysis is carried out to the sample using direct-reading spark spectrum instrument, wherein connect using conductive material described straight
Read the specimen holder and spark table table top of spark spectrum instrument.
9. according to the method described in claim 8, it is characterized in that, the conductive material passes through contact screw and the specimen holder
It is connected with the spark table table top.
10. a kind of direct-reading spark spectrum instrument characterized by comprising
Specimen holder；With
Spark table is formed between the specimen holder and the spark table table top and is electrically connected.
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| CN111505472A (en) * | 2020-05-12 | 2020-08-07 | 全球能源互联网研究院有限公司 | Preparation method of thermoplastic insulation sample for electrical tree degradation experiment |
| CN114235784A (en) * | 2021-12-01 | 2022-03-25 | 中铁九桥工程有限公司 | Welding wire detection method for spark type spectrometer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111505472A (en) * | 2020-05-12 | 2020-08-07 | 全球能源互联网研究院有限公司 | Preparation method of thermoplastic insulation sample for electrical tree degradation experiment |
| CN111505472B (en) * | 2020-05-12 | 2022-06-10 | 全球能源互联网研究院有限公司 | Preparation method of thermoplastic insulation sample for electrical tree degradation experiment |
| CN114235784A (en) * | 2021-12-01 | 2022-03-25 | 中铁九桥工程有限公司 | Welding wire detection method for spark type spectrometer |
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Application publication date: 20181211 |