Graphite device capable of manufacturing regular molten glass sheets

Abstract

The invention provides a graphite device capable of manufacturing a regular molten glass sheet, which comprises a graphite crucible and a graphite cover plug, and the graphite crucible and the graphite cover plug are combined for use when the regular molten glass sheet is manufactured. Molten glass sheets which are different in thickness and diameter and meet the measurement requirements of different analytical instruments can be manufactured by changing the specification and size of the graphite device, and a plurality of samples can be molten at the same time by combining an induction furnace manufactured in the patent of the invention CN115978995A, so that the working efficiency is greatly improved.

Description

Technical Field

[0001] The invention relates to the field of instrument analysis, in particular to a graphite device capable of manufacturing a molten glass sheet meeting the requirements of solid sample analysis. Background Art

[0002] Common large-scale analytical instruments, wavelength dispersive X-ray fluorescence spectrometer (XRF) and laser ablation ICP-MS mass spectrometer, have the function of directly analyzing molten glass flake solid samples. Molten glass flakes are usually obtained by melting samples at high temperatures using borate flux. The molten glass flakes referred to in the present invention are molten glass flakes used in XRF and laser ablation ICP-MS technologies, rather than conventional glass products.

[0003] In XRF analysis, samples are melted in platinum + gold crucibles. Large sampling volumes are often taken and more flux is used to obtain more molten materials. The molten objects are quickly poured onto platinum + gold molds of fixed sizes at high temperatures to produce regular molten glass sheets. Release agents and the like need to be introduced during the production process. It can be seen that the production of molten glass sheets in XRF instrument analysis wastes precious samples and fluxes, and because the overall amount of flux is large, more impurities will be introduced. In addition, the existing high-temperature furnaces for making molten glass sheets that meet XRF analysis generally have only six crucibles, and can melt up to six samples at the same time, which is not efficient. To complete the simultaneous melting of more samples, high-temperature furnaces are difficult to meet actual needs. In the high-temperature furnaces currently used for XRF analysis, it is clear that the method of using platinum + gold vessels to make molten glass sheets still has obvious shortcomings.

[0004] In laser ablation ICP-MS mass spectrometer analysis, the most researched method is to use graphite crucibles to make molten glass sheets. Generally, the sampling volume is small, the amount of flux used is not much, the sample dilution multiple is small, and the impurities introduced are few. When a completely flat-bottomed graphite crucible is used for melting, it is easy to shrink to obtain a molten glass body with poor regularity, multiple pieces, and more bubbles; when a graphite crucible with a certain curvature around the bottom of the crucible is used, the melt is mostly concentrated in the center of the crucible, and it is easy to shrink into a molten glass body (molten bead) of different sizes, nearly spherical, and containing more bubbles. It can be seen that by changing the shape of the bottom of the graphite crucible, molten glass bodies of different sizes, poor regularity, and containing bubbles can be obtained, but in order to make it better meet the requirements of the machine measurement, it must also be subjected to multiple grinding and polishing and other processing steps, and when measuring, it is also necessary to avoid the bubbles. Summary of the invention

[0005] The object of the present invention is to provide a graphite device capable of producing regular molten glass sheets, so as to solve the problems existing in the above-mentioned prior art.

[0006] The device of the present invention can produce molten glass sheets of different thicknesses and diameters that meet the measurement requirements of different analytical instruments by changing the specifications and dimensions of the graphite device. In addition, the induction furnace produced by the invention patent CN115978995A can be used in combination to melt multiple samples at the same time, greatly improving work efficiency.

[0007] To achieve the above object, the present invention provides the following solutions:

[0008] A graphite device capable of making a regular molten glass sheet comprises a graphite crucible 1 and a graphite plug 2. The graphite crucible 1 and the graphite plug 2 are used in combination when making the regular molten glass sheet.

[0009] Furthermore, the inner diameter D of the graphite crucible 1 is selected in the range of 5 mm to 40 mm, preferably 10 mm to 30 mm, and regular molten glass sheets of different sizes can be obtained by changing the size of the inner diameter D.

[0010] Furthermore, the bottom of the graphite crucible 1 has a curvature, and the curvature R of the bottom of the graphite crucible 1 is selected in the range of 1 mm to 5 mm, preferably 1.5 mm to 3.5 mm. The thickness of the regular molten glass sheet can be adjusted by changing the curvature R of the bottom.

[0011] Furthermore, the middle of the bottom of the graphite crucible 1 is a plane portion, and the diameter d of the plane portion is determined according to the curvature R of the bottom and the inner diameter D. By changing the diameter d, the diameter of the regular molten glass sheet can also be changed.

[0012] Furthermore, the inner height H of the graphite crucible 1 is selected in the range of 7 mm to 50 mm, preferably 9 to 30 mm, and the inner height H needs to satisfy the requirement that after the sample and the flux are contained, the total volume of the materials does not exceed two-thirds of the inner volume of the crucible.

[0013] Furthermore, the wall thickness L of the graphite crucible 1 is selected in the range of 0.5 mm to 2 mm. Different wall thicknesses L are selected for graphite crucibles 1 of different sizes. The wall thickness L of the graphite crucible is closely related to the safety of the graphite crucible in use.

[0014] Furthermore, the cylindrical diameter r of the graphite plug 2 varies with the inner diameter D of the graphite crucible 1, and the size of the graphite plug 2 is such that it can fit exactly into the graphite crucible 1, and the selection range of the gap between the graphite crucible 1 and the graphite plug 2 after combination is Dr=0.1mm~1mm.

[0015] Furthermore, the cylindrical height h of the graphite plug 2 varies according to the inner height H of the graphite crucible 1 and satisfies the condition: Hh=R.

[0016] Furthermore, the graphite plug 2 includes a brim portion 3, and the width B and thickness b of the brim portion are both in the range of 0.5 mm to 2 mm. By designing a graphite plug with a brim structure, it is beneficial to keep the graphite plug balanced during the falling process, and it is convenient to take the graphite plug out of the graphite crucible, and the maximum falling distance can also be controlled.

[0017] In some preferred embodiments, the graphite plug 2 may also be an "inverted T" structure or a structure in which a portion of the upper middle portion of a cylinder is hollowed out.

[0018] When the device of the present invention is used, a graphite crucible containing a sample and a flux that are evenly stirred is covered with a graphite plug and moved into a graphite matrix of a high-temperature induction furnace. As the heating temperature of the induction furnace increases, the sample and the flux form a melt, which freely falls through the graphite plug. When it falls to the upper part of the arc R, the graphite plug no longer descends due to size control, thereby avoiding complete compaction of the melt and leaving a certain amount of free shrinkage space for the melt.

[0019] The special structure designed by the present invention is that the middle of the bottom of the graphite crucible is a plane with a certain curvature around it. The middle plane can control the diameter and lower surface of the molten glass sheet, and the curvature can control the thickness of the molten glass sheet. The upper surface of the molten glass sheet can be controlled by the free fall motion of the graphite plug. Only when the bottom of the graphite crucible has a curvature, the molten body can freely shrink and break away from the bottom of the graphite crucible due to the surface tension of the graphite in the graphite crucible, and obtain a molten glass sheet that is easy to take out; when the bottom of the graphite crucible is completely flat around it, it is difficult for the molten body to find a free shrinkage space between the bottom of the graphite crucible and the graphite plug, and the molten glass sheet will not be separated from the bottom of the graphite crucible to obtain a complete molten glass sheet. When there is no graphite plug, a plurality of incompletely regular molten glass bodies will be obtained, and they will contain a large number of bubbles.

[0020] The beneficial effects of the present invention are:

[0021] The present invention adopts a graphite device with a special structure, loads samples and flux, and moves them into the induction furnace made by the invention patent CN115978995A for high-temperature melting. By changing the specifications and dimensions of the graphite device, molten glass sheets of different thicknesses and diameters that meet the measurement requirements of different analytical instruments can be produced. Since a graphite plug is placed inside the graphite crucible, the molten glass sheet obtained no longer contains bubbles through the free fall motion of the graphite plug, and the upper and lower surfaces of the molten glass sheet are basically flat. When the induction furnace made by the invention patent CN115978995A is used in combination with the special graphite device of the present invention, multiple samples can be melted at the same time to obtain a molten glass sheet with excellent regularity and no longer containing bubbles. As a result, the obtained molten glass sheet is very easy to use for machine measurement.

[0022] The outstanding feature of the present invention is that the graphite crucible is processed into a bottom with a certain curvature around it and a flat surface in the middle. This bottom structure makes it easy for the melt to shrink and separate from the bottom of the crucible; when a graphite cover plug is placed inside the graphite crucible, the melt is pressed due to the gravity of the cover plug, so that bubbles generated in the melt are easily removed, and a molten glass sheet with both upper and lower surfaces being flat and free of bubbles is obtained; the thickness of the molten glass sheet can be controlled by adjusting the curvature of the graphite crucible; and molten glass sheets with different diameters can be produced by changing the inner diameter of the graphite crucible and controlling the curvature. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 It is a schematic diagram of the overall structure of the graphite device of the present invention, and at this time the graphite crucible and the graphite cover plug are in a separated state.

[0024] Figure 2 It is a schematic diagram of the finished products made by the embodiments and comparative examples of the present invention. DETAILED DESCRIPTION

[0025] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0026] In addition, in order to better illustrate the present invention, some specific details are given in the specific embodiments below. It should be understood by those skilled in the art that the present invention can also be implemented without certain specific details. In some embodiments, raw materials, elements, methods, means, etc. well known to those skilled in the art are not described in detail, so as to highlight the main purpose of the present invention.

[0027] Unless explicitly stated otherwise, throughout the specification and claims, the term “comprise” or variations such as “include” or “comprising”, etc., will be understood to include the stated elements or components but not to exclude other elements or components.

[0028] The core solution of the present invention is to provide a graphite device capable of producing regular molten glass sheets. The graphite device is composed of a graphite crucible 1 and a graphite plug 2, which are used in combination. After the sample and flux are placed in the graphite crucible 1, the graphite plug 2 is placed in the graphite crucible 1. When heated and melted in an induction furnace, the graphite plug 2 is allowed to fall freely in the graphite crucible 1.

[0029] Shape and size of graphite crucible 1:

[0030] The inner diameter of the graphite crucible 1 is D (mm), and the selection range of the inner diameter D is 5 mm to 40 mm, preferably 10 mm to 30 mm. The size change of the inner diameter D can obtain molten glass sheets with different diameters.

[0031] The curvature R (mm) of the bottom of the graphite crucible 1 is selected in the range of 1 mm to 5 mm, preferably 1.5 mm to 3.5 mm. By changing the curvature R, the thickness of the molten glass sheet can be controlled.

[0032] The diameter of the plane portion in the middle of the bottom of the graphite crucible 1 is d (mm), and the diameter d is determined by the curvature R and the inner diameter D of the graphite crucible 1. The change of the diameter d can also control the diameter of the molten glass sheet.

[0033] The inner height of the graphite crucible 1 is H (mm), and the selection range of the inner height H is 7 mm to 50 mm, preferably 9 to 30 mm. The inner height H needs to meet the requirement that after the sample and the flux are loaded, the total volume of the material should not exceed two-thirds of the inner volume of the graphite crucible.

[0034] The wall thickness L (mm) of the graphite crucible 1 is selected in the range of 0.5 mm to 2 mm. Different wall thicknesses are selected for graphite crucibles of different sizes to ensure the safe use of the graphite crucible.

[0035] Shape and size of graphite plug 2:

[0036] The diameter of the cylindrical part of the graphite plug 2 is r (mm), and r changes with the inner diameter D of the graphite crucible 1. When the graphite plug 2 is placed in the graphite crucible 1, the gap around the graphite crucible 1 and the graphite plug 2 is approximately Dr = 0.1 mm to 1 mm;

[0037] The height of the cylindrical part of the graphite plug 2 is h (mm), and h varies with the inner height H of the graphite crucible 1, satisfying the condition, Hh = R;

[0038] The width of the brim portion 3 of the graphite plug 2 is B (mm) and the thickness is b (mm), and the selection range is 0.5 mm to 2 mm.

[0039] Embodiment 1, a graphite device and a method of using the same.

[0040] The dimensions of the graphite crucible are: outer diameter 14mm, inner height H10mm, inner diameter D10mm, curvature R1.5mm, and wall thickness 2mm.

[0041] The dimensions of the graphite plug are: cylinder diameter r9.9mm, cylinder height h8.5mm.

[0042] Weigh 50 mg of domestic standard GSR-1 sample and 100 mg of lithium metaborate flux into a graphite crucible, stir evenly with a thin glass rod, then transfer to an induction furnace made with invention patent application number CN115978995A, heat to 1000℃ and keep warm for ten minutes, and take out the melt after cooling. The melt is approximately a round cake with a diameter of about 8.5 mm and a thickness of about 1 mm. Figure 2 .

[0043] Embodiment 2, a graphite device and a method of using the same.

[0044] The dimensions of the graphite crucible are: outer diameter 14mm, inner height H10mm, inner diameter D10mm, curvature R1.5mm, and wall thickness 2mm.

[0045] The dimensions of the graphite plug are: cylinder diameter r9.9mm, cylinder height h8.5mm.

[0046] Weigh 50 mg of domestic standard GSR-3 sample and 100 mg of lithium metaborate flux into a graphite crucible, stir evenly with a thin glass rod, then transfer to an induction furnace made with invention patent application number CN115978995A, heat to 1000℃ and keep warm for ten minutes, and take out the melt after cooling. The melt is approximately a round cake with a diameter of about 8 mm and a thickness of about 1 mm. Figure 2 .

[0047] Embodiment 3, a graphite device and a method of using the same.

[0048] The dimensions of the graphite crucible are: outer diameter 14mm, inner height H10mm, inner diameter D10mm, curvature R1.5mm, and wall thickness 2mm.

[0049] The dimensions of the graphite plug are: cylinder diameter r9.9mm, cylinder height h8.5mm.

[0050] Weigh 50 mg of the international standard GSP-2 sample and 100 mg of lithium metaborate flux into a graphite crucible, stir evenly with a thin glass rod, then transfer to an induction furnace made with invention patent application number CN115978995A, heat to 1000°C and keep warm for ten minutes, and take out the melt after cooling. The melt is approximately a round cake with a diameter of about 8.5 mm and a thickness of about 1 mm. Figure 2 .

[0051] In order to further verify the special performance and effect of the present invention, the following comparative examples of molten glass sheets are prepared using some parameters or methods not in the present invention, so as to allow those skilled in the art to better understand the superiority of the present invention.

[0052] Comparative Example 1

[0053] The dimensions of the graphite crucible are: outer diameter 14mm, inner height H10mm, inner diameter D10mm, curvature R1.5mm, wall thickness 2mm, and no graphite cover.

[0054] Weigh 50 mg of domestic standard GSR-1 sample and 100 mg of lithium metaborate flux into a graphite crucible, stir evenly with a thin glass rod, then transfer to an induction furnace made with invention patent application number CN115978995A, heat to 1000℃ and keep warm for ten minutes, and take out the melt after cooling. The melt is similar to a solid ball with a diameter of about 4.8 mm. Figure 2 .

[0055] Comparative Example 2

[0056] The dimensions of the graphite crucible are: outer diameter 14mm, inner height H10mm, inner diameter D10mm, curvature R1.5mm, wall thickness 2mm, and no graphite cover.

[0057] Weigh 50 mg of domestic standard GSR-3 sample and 100 mg of lithium metaborate flux into a graphite crucible, stir evenly with a thin glass rod, then transfer to an induction furnace made with invention patent application number CN115978995A, heat to 1000℃ and keep warm for ten minutes, and take out the melt after cooling. The melt is similar to a solid ball with a diameter of about 4.5 mm. Figure 2 .

[0058] Comparative Example 3

[0059] The dimensions of the graphite crucible are: outer diameter 14mm, inner height H10mm, inner diameter D10mm, curvature R1.5mm, wall thickness 2mm, and no graphite cover.

[0060] Weigh 50 mg of the international standard GSP-2 sample and 100 mg of lithium metaborate flux into a graphite crucible, stir evenly with a thin glass rod, then transfer to an induction furnace made with invention patent application number CN115978995A, heat to 1000°C and keep warm for ten minutes, and take out the melt after cooling. The melt is similar to a solid ball with a diameter of about 4.8 mm. Figure 2 .

[0061] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the embodiments of the present invention.

[0062] Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments, or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A graphite device capable of producing regular molten glass sheets, characterized in that: It comprises a graphite crucible (1) and a graphite plug (2). The graphite crucible (1) and the graphite plug (2) are used in combination when making the regular molten glass sheet.

2. A graphite device capable of producing regular molten glass sheets according to claim 1, characterized in that: The inner diameter D of the graphite crucible (1) is selected in the range of 5 mm to 40 mm, preferably 10 mm to 30 mm, and regular molten glass sheets of different sizes can be obtained by changing the size of the inner diameter D.

3. A graphite device capable of producing regular molten glass sheets according to claim 1, characterized in that: The bottom of the graphite crucible (1) has a curvature, and the curvature R of the bottom of the graphite crucible (1) is selected in the range of 1 mm to 5 mm, preferably 1.5 mm to 3.5 mm. The thickness of the regular molten glass sheet is adjusted by changing the curvature R of the bottom.

4. A graphite device capable of producing regular molten glass sheets according to claim 1, characterized in that: The middle of the bottom of the graphite crucible (1) is a plane part, and the diameter d of the plane part is determined according to the curvature R of the bottom and the inner diameter D. By changing the diameter d, the diameter of the regular molten glass sheet can also be changed.

5. A graphite device capable of producing regular molten glass sheets according to claim 1, characterized in that: The inner height H of the graphite crucible (1) is selected in the range of 7 mm to 50 mm, preferably 9 to 30 mm. The inner height H is required to ensure that after the sample and the flux are contained, the total volume of the materials does not exceed two thirds of the inner volume of the crucible.

6. A graphite device capable of producing regular molten glass sheets according to claim 1, characterized in that: The wall thickness L of the graphite crucible (1) is selected in the range of 0.5 mm to 2 mm.

7. A graphite device capable of producing regular molten glass sheets according to claim 1, characterized in that: The cylindrical diameter r of the graphite plug (2) varies with the inner diameter D of the graphite crucible (1), the size of the graphite plug (2) is sufficient to be placed in the graphite crucible (1), and the selection range of the gap after the graphite crucible (1) and the graphite plug (2) are combined is Dr = 0.1 mm to 1 mm.

8. The graphite device capable of producing regular molten glass sheets according to claim 1, characterized in that: The cylindrical height h of the graphite cover plug (2) varies with the inner height H of the graphite crucible (1) and satisfies the condition: Hh=R.

9. A graphite device capable of producing regular molten glass sheets according to claim 1, characterized in that: The graphite plug (2) comprises a brim portion (3), and the width B and thickness b of the brim portion are selected in the range of 0.5 mm to 2 mm.

10. A graphite device capable of producing regular molten glass sheets according to claim 7, characterized in that: The graphite plug (2) may also be an "inverted T" shaped structure or a structure in which a portion of the upper middle portion of a cylinder is hollowed out, and the "T" shaped structure of claim 7 is preferred, as it is more convenient to process.

Images