CN111398326A - Method for tabletting samples for XRFS analysis of boric acid edged substrates - Google Patents
Method for tabletting samples for XRFS analysis of boric acid edged substrates Download PDFInfo
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- CN111398326A CN111398326A CN202010270037.1A CN202010270037A CN111398326A CN 111398326 A CN111398326 A CN 111398326A CN 202010270037 A CN202010270037 A CN 202010270037A CN 111398326 A CN111398326 A CN 111398326A
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- 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
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Abstract
The invention discloses a tabletting method of sample wafers for XRFS analysis of a boric acid edged substrate, which relates to the technical field of XRFS analysis tabletting and solves the problems of low speed and low sample wafer quality according to the existing tabletting method, and adopts the technical scheme that: a tabletting method of a sample wafer for XRFS analysis of a boric acid edged substrate comprises the steps of firstly, placing boric acid in a sample loading cavity of a tabletting machine by using a boric acid feeding spoon, then placing a feeding cylinder on the boric acid, and leveling and compacting a sample distribution area to obtain a substrate layer; secondly, adding a proper amount of sample into the feeding cylinder by using a sample spoon, and scraping the sample by using a scraper; thirdly, taking down the slicers, installing a pressing head of a tabletting machine, and pressing and molding; finally, demolding to obtain a sample wafer for XRFS analysis. According to the invention, the boric acid is added by the boric acid feeding spoon, the sample is added by the sample spoon, the feeding is rapid and accurate, the sample is stricken off by the strickler, the sample is uniform in material distribution thickness, the sample can be strickled off at one time, and the tabletting speed and the sample tablet quality are improved.
Description
Technical Field
The invention relates to the technical field of XRFS (X-ray diffraction FS) analysis tabletting, in particular to a tabletting method of a sample wafer for XRFS analysis of a boric acid substrate.
Background
Compared with the melt casting technology, the XRFS tabletting analysis technology has the characteristics of high tabletting speed, simple sample preparation, less pollution, low measurement lower limit and high analysis precision, and is very suitable for uniformity inspection. The conventional tabletting method includes a boric acid-rimmed substrate method, a plastic ring method, an iron ring method, an aluminum cup (iron cup) method, and the like. Among the more widely used sheeting methods are the boric acid edged substrate and the plastic ring method. Compared with the plastic ring method, the boric acid edged substrate has the advantages of less sample consumption, difficult pressure relief stripping and uniform sample wafer, but has the disadvantage of lower wafer making speed.
XRFS pellet analysis was used for homogeneity check. Since the ability to detect the nonuniformity of a sample by uniformity inspection depends on the accuracy of the analysis method, it is important for uniformity inspection to select a boric acid substrate edging method having a high density characteristic and to improve the inspection accuracy thereof. Factors affecting the accuracy of XRFS measurements include the measuring instrument and the prepared sample, and the flatness of the sample surface and the bulk density of the measured portion have a significant effect on the accuracy of the measurement.
Currently, the boric acid edged substrate sheeting method is: firstly, a certain amount of boric acid is taken and placed in a sample pressing cavity, then the boric acid substrate is leveled by an edge making auxiliary tool, namely an edge making device, samples are uniformly distributed in a leveling area, the boric acid is added outside the edge making device, then the edge making device is taken down, the pressure is applied, and finally the molding and the demolding are carried out. The tabletting method has the following defects: firstly, because boric acid has small specific gravity and larger particles than a sample, a powdery sample easily falls into pits formed by boric acid particles, and the boric acid on a substrate is turned up in the process of flattening the sample, so that the thickness of the sample is influenced, and the cloth thickness of the sample is uneven. Secondly, the tabletting method needs to add boric acid and a sample for multiple times, the material quality of the boric acid and the sample is difficult to accurately fix, and the obtained sample test pieces have different densities under the same pressure. Thirdly, the tabletting method needs multiple times of material distribution and sample leveling, has long operation time and influences the tabletting speed.
Disclosure of Invention
The invention provides a tabletting method of a sample wafer for XRFS analysis of a boric acid edged substrate, which solves the problems of low tabletting speed and low sample wafer quality according to the existing tabletting method.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method of tabletting coupons for XRFS analysis of boric acid edged substrates comprising the steps of:
s1, placing boric acid in a sample loading cavity of a tablet press by using a boric acid feeding spoon, then placing a feeding cylinder on the boric acid, and leveling and compacting a sample distribution area to obtain a substrate layer.
Specifically, the method comprises the following steps: in the step S1, the volume of the boric acid feeding spoon is 2.00-3.00 g of boric acid, and the volume precision is 0.05g of boric acid; the feeding cylinder is a cylinder, the inner diameter of the cylinder is 36.0-37.0 mm, the thickness of the cylinder wall of the cylinder is 0.5-1.0 mm, and the height of the cylinder is 25.0-30.0 mm.
Specifically, the method comprises the following steps: in step S1, the boric acid is industrial boric acid.
And S2, adding a proper amount of sample into the feeding cylinder by using the sample spoon.
Specifically, the method comprises the following steps: in step S2, the volume of the sample spoon is 2.00-3.00 g of sample, and the volume precision is 0.05g of sample.
Specifically, the method comprises the following steps: in step S2, the sample is a powder with a particle size of <0.1mm for chemical analysis.
And S3, leveling the sample through a leveling device.
Further, the method comprises the following steps: in step S3, the strickle comprises a cover plate, a connecting rod and a scraping rod, the cover plate is provided with a cross opening, the connecting rod and the scraping rod are perpendicular to each other, and the connecting rod penetrates through the cross opening and can slide along the cross opening; and (3) scraping the sample: put into the charging barrel with the scraper bar earlier, apron fell on the charging barrel top, and the scraper bar hangs in the charging barrel, moves the connecting rod along the cross opening again, and the sample is strickled off to the rotating connection pole simultaneously.
Specifically, the method comprises the following steps: in step S3, the connecting rod and the scraping rod are placed in a feeding cylinder, the distance between the bottom surface of the scraping rod and the top surface of the substrate layer is adjusted to be 1.0mm, and then the sample is scraped flat.
Furthermore, the connecting rod and the scraping rod are integrated into a whole and are L-shaped, the diameter of the connecting rod is smaller than the width of the cross opening, one end of the connecting rod, far away from the scraping rod, is connected with a limiting cap, the outer diameter of the limiting cap is larger than the width of the cross opening, and the diameter of the cover plate is larger than the inner diameter of the feeding cylinder.
And S4, taking down the strickle, installing a pressing head of a tabletting machine, and pressing and forming.
And S5, demolding to obtain an XRFS analysis sample.
Specifically, the method comprises the following steps: the material of the boric acid feeding spoon, the feeding cylinder, the sample spoon and the strickle is steel, plastic or aluminum alloy.
The invention has the beneficial effects that: the invention provides a tabletting method of a sample wafer for XRFS analysis, which has small sample density difference in an analysis area, uniform sample cloth thickness and high tabletting speed. According to the invention, the boric acid feeding spoon is used for adding boric acid, the sample spoon is used for adding a sample, the boric acid feeding spoon and the sample spoon are used as quantitative feeding tools, so that the rapidness and accuracy of each feeding can be ensured, the sample is strickled off by the strickle, and the sample is uniformly distributed; the one-time material distribution is realized, and the sample can be quickly scraped, so the sheet production efficiency is high. The XRFS sample distributing device has the characteristics of uniform density of XRFS analysis area samples, consistent sample distributing thickness and high flaking efficiency.
The strickle comprises a cover plate, a connecting rod and a scraping rod, the strickle is simple in structure and convenient to use, the scraping rod moves along a cross opening of the cover plate along with the connecting rod, a sample can be strickled quickly, and the uniformity of the thickness of the cloth is ensured.
Drawings
Fig. 1 is a schematic view of the construction of the screed according to the invention.
Fig. 2 is a plan view of the cover plate of fig. 1.
Reference numerals: the device comprises a cover plate 1, a connecting rod 2, a scraping rod 3 and a limiting cap 4.
Detailed Description
The invention is further illustrated by the following figures and examples.
The invention provides a tabletting method for a sample wafer for XRFS analysis of a boric acid edged substrate, which comprises the following steps:
s1, a spoon of boric acid is placed in a sample loading cavity of a tablet press by using a boric acid feeding spoon, then a feeding cylinder is placed on the boric acid, and a sample distribution area is leveled and compacted to obtain a substrate layer.
The boric acid feeding spoon comprises a hopper and a spoon handle, the volume of the hopper is fixed, for example, the volume of the boric acid feeding spoon is 2.00-3.00 g of boric acid, the volume precision is 0.05g of boric acid, and the mass error of the boric acid feeding spoon is within 0.05g of one-level-spoon boric acid each time. The charging barrel is a mould and mainly used for controlling the sample distribution area. The feeding cylinder is a cylinder, for example, the inner diameter of the cylinder is 36.0-37.0 mm, the thickness of the cylinder wall of the cylinder is 0.5-1.0 mm, and the height of the cylinder is 25.0-30.0 mm. In step S1, the boric acid is industrial boric acid. And S2, adding a proper amount of sample into the feeding cylinder by using the sample spoon. The proper amount of the sample is determined according to the tabletting requirement, and specifically is the amount of a flat spoon of the sample spoon. The sample is applied to the top surface of the substrate layer.
The sample spoon comprises a hopper and a spoon handle, wherein the volume of the hopper is fixed, for example, the volume of the sample spoon is 2.00-3.00 g of a sample, and the volume precision is 0.05g of the sample. The sample is a powder with a particle size of <0.1mm for chemical analysis.
And S3, leveling the sample through a leveling device.
The strickle is used for the appurtenance who strickles off sample in the charging cylinder. For example, as shown in fig. 1, the strickle comprises a cover plate 1, a connecting rod 2 and a scraping rod 3, and a cross-shaped opening is arranged on the cover plate 1, as shown in fig. 2. The operation mode of scraping the sample is as follows: put into the charging barrel with connecting rod 2 and scraping pole 3 earlier, apron 1 falls into the charging barrel top, scrapes material pole 3 and hangs in the charging barrel, moves connecting rod 2 along the cross opening again, and the sample is strickled off to rotating connecting rod 2 simultaneously.
Connecting rod 2 and scrape material pole 3 and be L shapes for an entirety, connecting rod 2 and scrape material pole 3 mutually perpendicular, connecting rod 2 and scrape material pole 3 can be buckled by the iron wire and form, the size of apron 1 is greater than the internal diameter of charging barrel, avoid apron 1 to fall into in the charging barrel, for example apron 1 is circular, for thickness 0.8 ~ 1.0 mm's steel sheet, the diameter of apron 1 is 2.0mm than the external diameter of charging barrel greatly, cross opening length 20.0mm, width 2.0mm, the diameter of connecting rod 2 is less than cross open-ended width, for example the diameter of connecting rod 2 is 2mm less than cross open-ended width, so that connecting rod 2 removes along the cross opening about the length of scraping material pole 3, need satisfy the condition, connecting rod 2 covers whole charging barrel when removing along the cross opening.
Because the vertical distance of 1 bottom surface of apron and scraping material pole 3 is for scraping the height difference between back sample top surface and the charging barrel top of strickleing off promptly, for the convenience of adjusting the relative position of apron 1 on connecting rod 2, the connecting rod 2 is kept away from the one end of scraping material pole 3, and limiting cap 4 is connected on the top of connecting rod 2 promptly, and the best threaded connection of limiting cap 4 is on the top of connecting rod 2, and limiting cap 4's external diameter is greater than cross open-ended width. Thus, the depth of the scraping rod 3 in the charging barrel can be adjusted by adjusting the limit cap 4.
When strickleing off the sample through strickleing off the ware, accessible stop cap 4 adjustment apron 1 relative position on connecting rod 2 makes the distance between the bottom surface of scraping material pole 3 and the substrate layer top surface be 1.0mm, strickles off the sample again. The strickle realizes the purpose of strickleing off the sample fast with even cloth thickness.
And S4, taking down the strickle, installing a pressing head of a tabletting machine, and pressing and forming.
And S5, demolding to obtain an XRFS analysis sample.
The materials of the boric acid feeding spoon, the feeding cylinder, the sample spoon and the strickle in the steps S1-S4 are steel, plastic or aluminum alloy.
Application example 1
The preparation method comprises the steps of firstly, placing a spoon of boric acid in a sample loading cavity of a tablet press by using a boric acid feeding spoon with the volume of a hopper being 3.00g of boric acid, placing a feeding cylinder on the boric acid, and leveling and compacting a cloth sample area to obtain a substrate layer. Secondly, adding a spoon of the vanadium slag sample with the volume of 2.50g by using a sample spoon of the hopper into the feeding cylinder; adjust above-mentioned strickle, make the strickle adorn back on the charging barrel, the distance between the bottom surface of scraping material pole 3 and the substrate layer top surface is 1.0mm, will strickle the ware again and adorn on the charging barrel, along cross opening moving connecting rod 2, rotating connecting rod 2 drives simultaneously and scrapes the rotation of material pole 3, scrapes off the sample. And thirdly, taking down the slicers, installing the pressing heads of the tabletting machines, and pressing and molding. Finally, the sample is demolded to obtain a sample for XRFS analysis, which is used for inspection on an X-ray fluorescence spectrometer.
Application example 2
The preparation method comprises the steps of firstly, placing a spoon of boric acid in a sample loading cavity of a tablet press by using a boric acid feeding spoon with the volume of a hopper of 3.00g, placing a feeding cylinder on the boric acid, and leveling and compacting a cloth sample area to obtain a substrate layer. Secondly, adding a spoon of the sample into a feeding cylinder by using a sample spoon with the hopper volume of 1.2g of the ferrovanadium sample; adjust above-mentioned strickle, make the strickle adorn back on the charging barrel, the distance between the bottom surface of scraping material pole 3 and the substrate layer top surface is 1.0mm, will strickle the ware again and adorn on the charging barrel, along cross opening moving connecting rod 2, rotating connecting rod 2 drives simultaneously and scrapes the rotation of material pole 3, scrapes off the sample. And thirdly, taking down the slicers, installing the pressing heads of the tabletting machines, and pressing and molding. Finally, the sample is demolded to obtain a sample for XRFS analysis, which is used for inspection on an X-ray fluorescence spectrometer.
Claims (9)
1. A method of tabletting a coupon for XRFS analysis of a boric acid edged substrate, characterized by: the method comprises the following steps:
s1, placing boric acid in a sample loading cavity of a tablet press by using a boric acid feeding spoon, then placing a feeding cylinder on the boric acid, and leveling and compacting a sample distribution area to obtain a substrate layer;
s2, adding a proper amount of sample into a feeding cylinder by using a sample spoon;
s3, leveling the sample through a leveling device;
s4, taking down the slicers, installing a pressing head of a tabletting machine, and pressing and forming;
and S5, demolding to obtain an XRFS analysis sample.
2. A method of tabletting coupons for XRFS analysis of boric acid rimmed substrates as claimed in claim 1 wherein: in the step S1, the volume of the boric acid feeding spoon is 2.00-3.00 g of boric acid, and the volume precision is 0.05g of boric acid; the feeding cylinder is a cylinder, the inner diameter of the cylinder is 36.0-37.0 mm, the thickness of the cylinder wall of the cylinder is 0.5-1.0 mm, and the height of the cylinder is 25.0-30.0 mm.
3. A method of tabletting coupons for XRFS analysis of boric acid rimmed substrates as claimed in claim 1 wherein: in step S1, the boric acid is industrial boric acid.
4. A method of tabletting coupons for XRFS analysis of boric acid rimmed substrates as claimed in claim 1 wherein: in step S2, the volume of the sample spoon is 2.00-3.00 g of sample, and the volume precision is 0.05g of sample.
5. A method of tabletting coupons for XRFS analysis of boric acid rimmed substrates as claimed in claim 1 wherein: in step S2, the sample is a powder with a particle size of <0.1mm for chemical analysis.
6. A method of tabletting coupons for XRFS analysis of boric acid edged substrates as claimed in any of claims 1 to 5, characterized in that: in the step S3, the strickle comprises a cover plate (1), a connecting rod (2) and a scraping rod (3), a cross opening is formed in the cover plate (1), the connecting rod (2) and the scraping rod (3) are perpendicular to each other, and the connecting rod (2) penetrates through the cross opening and can slide along the cross opening; and (3) scraping the sample: in putting into the charging barrel with connecting rod (2) and scraping pole (3), apron (1) fell on the charging barrel top, scrape pole (3) and hang in the charging barrel, along cross opening removal connecting rod (2) again, rotating connecting rod (2) simultaneously, strickle the sample.
7. The method of tabletting a coupon for XRFS analysis of a boric acid rimmed substrate of claim 6, wherein: in step S3, the connecting rod (2) and the scraping rod (3) are placed in a feeding cylinder, the distance between the bottom surface of the scraping rod (3) and the top surface of the substrate layer is adjusted to be 1mm, and then the sample is scraped flat.
8. The method of claim 6, wherein the tie bar (2) and the scraper bar (3) are integral and L-shaped, the tie bar (2) has a diameter less than the width of the cross opening, the end of the tie bar (2) remote from the scraper bar (3) is connected to a retaining cap (4), the outer diameter of the retaining cap (4) is greater than the width of the cross opening, and the diameter of the cover plate (1) is greater than the inner diameter of the feed cylinder.
9. The method of tabletting a coupon for XRFS analysis of a boric acid rimmed substrate of claim 6, wherein: the material of the boric acid feeding spoon, the feeding cylinder, the sample spoon and the strickle is steel, plastic or aluminum alloy.
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| CN202010270037.1A CN111398326B (en) | 2020-04-08 | 2020-04-08 | Method for tabletting samples for XRFS analysis of boric acid edged substrates |
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| CN202010270037.1A CN111398326B (en) | 2020-04-08 | 2020-04-08 | Method for tabletting samples for XRFS analysis of boric acid edged substrates |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113022000A (en) * | 2021-03-02 | 2021-06-25 | 中国科学院过程工程研究所 | Automatic mixing and tabletting device, tabletting method and application thereof |
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