Method for fractionation of carbon isotope

Abstract

The present invention relates to a carbon isotope separation apparatus using an electron beam heating method and a carbon isotope separation method using the same. Specifically, a carbon isotope separation apparatus according to one embodiment comprises: a high vacuum electron beam chamber; a magnetic metal cylinder provided within the high vacuum electron beam chamber and including a carbon mixture storage portion on its upper surface; and a water-cooled sample holder in contact with the lower surface of the magnetic metal cylinder, thereby enabling efficient separation and concentration of carbon isotopes.

Description

Technology Field

[0001] The present invention relates to a carbon isotope separation apparatus and a method for separating and concentrating carbon isotopes using the same. Background Technology

[0002] Isotope separation technology is a technique for separating a specific isotope from a mixture of isotopes composed of the same element with different atomic weights.

[0003] Meanwhile, carbon is carbon-12, which has a natural composition ratio of 98.89% ( 12 C) and 1.1% carbon-13 ( 13 C) There are two types of stable isotopes, and since each isotope is a highly useful material in various industrial fields, it is one of the most important targets for isotope separation and enrichment. However, current technologies used for carbon isotope separation have disadvantages, such as requiring expensive equipment and specialized skills, using materials harmful to the environment and human health, and having low separation efficiency. Prior art literature

[0004] Republic of Korea Published Patent Application No. 10-2020-0062947 A (June 4, 2020) The problem to be solved

[0005] One aspect of the present invention provides a separation apparatus capable of efficiently separating and concentrating carbon isotopes and a method for separating carbon isotopes using the same. means of solving the problem

[0006] One aspect of the present invention provides a carbon isotope separation apparatus comprising: a high vacuum electron beam chamber; a magnetic metal cylinder provided within the high vacuum electron beam chamber and having a carbon mixture storage portion on its upper surface; and a water-cooled sample holder in contact with the lower surface of the magnetic metal cylinder.

[0007] The magnetic metal mentioned above may be nickel or cobalt.

[0008] The above sample holder may be a graphite precipitation part.

[0009] The body of the above magnetic metal cylinder may be a diffusion path for carbon elements.

[0010] Another aspect of the present invention is a carbon isotope separation method using the carbon isotope separation device, wherein the carbon mixture storage portion of the magnetic metal cylinder 12 C and 13 A carbon isotope separation method is provided, comprising the steps of: introducing a carbon mixture containing C and eutecticizing it using an electron beam heating method; and precipitating graphite through the diffusion of carbon elements.

[0011] The magnetic metal cylinder may form a temperature gradient that decreases in the direction of the lower surface in the carbon mixture storage section.

[0012] The temperature of the carbon mixture storage portion above is 1300 ℃ to 1400 ℃, and the temperature of the bottom surface may be 600 ℃ to 900 ℃.

[0013] It may be possible to control the separated carbon isotopes by selecting the metal component of the above magnetic metal cylinder. Effects of the invention

[0014] According to the carbon isotope separation method of the present invention, carbon isotopes can be separated economically and in an environmentally friendly manner, and their relative abundance can be controlled.

[0015] Specifically, the carbon isotope separation method according to one embodiment is eco-friendly as it does not use materials harmful to the human body and the environment, and is also expected to be advantageous for application in actual industrial sites due to its simple process and high energy efficiency. Brief explanation of the drawing

[0016] FIG. 1 is a drawing of a magnetic metal cylinder according to one embodiment. Figure 2 is a photograph of the lower surface of a magnetic metal cylinder before and after carbon element diffusion according to one embodiment. FIG. 3 is a diagram of a magnetic metal cylinder according to one embodiment. Figures 4 to 6 are Raman spectra for the upper and lower surfaces of a magnetic metal cylinder after carbon element diffusion in Examples 1 to 3. Specific details for implementing the invention

[0017] Unless otherwise defined in this specification, all technical and scientific terms have the same meaning as generally understood by those skilled in the art to which the present invention pertains. The terms used in the description herein are merely for the purpose of effectively describing specific embodiments and are not intended to limit the present invention.

[0018] The singular form used in this specification is intended to include the plural form unless specifically indicated otherwise in the context.

[0019] Throughout this specification, the terms “comprising,” “having,” “containing,” or “having” any component mean that, unless specifically stated otherwise, other components are not excluded but may be included, and do not exclude elements, materials, or processes not additionally listed.

[0020] The numerical ranges used herein include lower and upper limits and all values ​​within the range, increments logically derived from the form and width of the defined range, all of which are limited, and all possible combinations of upper and lower limits of the numerical range defined in different forms. Unless otherwise specifically defined in this specification, values ​​outside the numerical range that may occur due to experimental error or rounding are also included in the defined numerical range.

[0021] Unless otherwise specifically defined in this specification, “about” may be considered to be a value within 30%, 25%, 20%, 15%, 10%, or 5% of the specified value.

[0022] The present disclosure will be described in detail below. However, this is merely illustrative and the present disclosure is not limited to the specific embodiments described illustratively.

[0023] One aspect of the present invention provides an apparatus capable of separating and concentrating carbon isotopes using electron beam heating, and a method for separating carbon isotopes using the same.

[0024] A carbon isotope separation device according to one embodiment may include: a high vacuum electron beam chamber; a magnetic metal cylinder (Fig. 1) provided within the high vacuum electron beam chamber and having a carbon mixture storage portion on its upper surface; and a water-cooled sample holder in contact with the lower surface of the magnetic metal cylinder.

[0025] The above magnetic metal may be used without limitation as long as it is a magnetic metal with high solubility in carbon, and may be nickel, cobalt, or iron as a non-limiting example.

[0026] The body of the magnetic metal cylinder may be a diffusion path for carbon elements, and the water-cooled sample holder may be a graphite precipitation part where the diffused carbon elements are cooled and precipitated.

[0027] Another aspect of the present invention provides a carbon isotope separation method using the carbon isotope separation apparatus described above.

[0028] A carbon isotope separation method according to one embodiment comprises a carbon mixture storage portion of the magnetic metal cylinder. 12 C and 13 It may include the step of introducing a carbon mixture containing C and eutecticizing the carbon mixture and the magnetic metal by an electron beam heating method; and the step of precipitating graphite through the diffusion of carbon elements.

[0029] A carbon isotope separation method according to one embodiment may further include a step of annealing a magnetic metal cylinder before introducing a carbon mixture, and may further facilitate the diffusion of carbon elements.

[0030] The above annealing can be performed, for example, for 40 to 60 hours at a temperature range of 1300 to 1400 ℃ under a hydrogen atmosphere.

[0031] According to a carbon isotope separation method according to one embodiment, a temperature gradient decreasing in the direction of the lower surface may be formed in the carbon mixture storage portion of the magnetic metal cylinder by the electron beam heating, and accordingly, carbon elements that diffuse and move may precipitate on the lower surface.

[0032] When performing the electron beam heating above, the temperature of the carbon mixture storage part may be 1,300 ℃ to 1,400 ℃, or 1,320 ℃ to 1,400 ℃, or 1,320 ℃ to 1,350 ℃, and the temperature of the lower surface (water-cooled sample holder, graphite precipitation part) may be 600 ℃ to 900 ℃ and may vary depending on the length of the magnetic metal cylinder.

[0033] The carbon isotope separation through the above-mentioned electric beam heating may be performed for 6 to 8 hours.

[0034] The metal component of the magnetic metal cylinder may be selected to control the separated carbon isotopes, and as an example, in a nickel-component magnetic metal cylinder, 12C diffuses more rapidly from the bottom surface 12 C can be concentrated and precipitated, and in magnetic metal cylinders containing cobalt, 13 C spreads more rapidly on the lower surface 13 C can be concentrated and precipitated.

[0035] The above-described embodiment will be explained in more detail below through examples. However, the following examples are for illustrative purposes only and do not limit the scope of the claims.

[0036] [Example 1]

[0037] A nickel metal bulk with a purity of 99.9 wt% (Shaanxi Super Metal Materials Co. Limited) was processed into the cylinder shape shown in Fig. 1, where the unit in Fig. 1 is mm. The magnetic metal cylinder made of the nickel was annealed at 1400°C for 60 hours in a hydrogen atmosphere.

[0038] since, 12 C carbon powder (Alfa Aesar) and 13 C carbon powder (Cambridge Isotope Laboratories Inc.) 12 C / 13 A carbon mixture source mixed at a weight ratio of C=1.4 was added to isopropanol and sonicated for 5 minutes (Qsonica sonicator at ~300 W power) to prepare a carbon mixture dispersion. The carbon mixture dispersion was then added to the carbon mixture reservoir of a magnetic metal cylinder using a micropipette, and the solvent was dried.

[0039] The above carbon mixture-magnetic metal cylinder system was installed inside a high vacuum electron beam chamber, and the lower surface of the magnetic metal cylinder was brought into contact with a water-cooled sample holder. The internal pressure of the high vacuum electron beam chamber was 10 -7 The temperature of the carbon mixture was heated to 1330°C using an electron beam method to eutectic the carbon mixture and the magnetic metal, thereby inducing the diffusion of carbon elements within the magnetic metal cylinder, and it was confirmed that graphite had precipitated on the lower surface of the magnetic metal cylinder after 6 hours (Fig. 2-(b)).

[0040] [Example 2]

[0041] The length of the magnetic metal cylinder is changed as shown in Fig. 3, and the isotope ratio of the carbon mixture ( 12 C / 13 Except for changing C) from a weight ratio of 1.4 to 1, the above embodiment was carried out in the same manner as 1.

[0042] [Example 3]

[0043] The above Example 1 was carried out in the same manner as above, except that 99.95 wt% pure cobalt metal bulk (Shaanxi Super Metal Materials Co. Limited) was used instead of nickel metal as the magnetic metal cylinder material.

[0044] Through the Raman spectrum results (Figs. 4 to 6) for the graphite precipitated in the carbon mixture storage unit (source side) and the water-cooled sample holder (bottom side) after the carbon element diffusion experiment in the above embodiment 13 Calculate C content (at%) Nano Lett. (2009, 9, 12, 4268-4272) and are listed in Table 1 below. Here, Raman spectra were obtained using a confocal Raman microscope (WITec) in mapping mode with a 532 nm laser source, x100 objective lens, ~1 mW laser output, 5 accumulations, and an acquisition time of 10 seconds, and the resulting spectra were plotted after analysis using Matlab software. The average position of the G peaks indicated in the figure was calculated using a Gaussian function.

[0045] Source side ( 13 C, at%) Bottom side ( 13 C, at%) Example 1 35.6 ±1.8 at % 31.1 ±1.0 at % Example 2 46.1 ±0.7 at % 41.3 ±1.1 at % Example 3 36.3 ±1.3 at % 41.5 ±1.8 at %

[0046] Referring to Table 1 above, in the case of Examples 1 and 2 using a magnetic metal cylinder made of nickel, the graphite precipitated in the water-cooled sample holder (bottom side) is concentrated relative to the graphite in the carbon mixture storage section (source side). 12 It can be seen that it has a C content. From this, the relatively light element12 It can be seen that C diffuses more rapidly through the nickel metal and can precipitate at a concentrated content on the bottom side.

[0047] On the other hand, in the case of Example 3 using a magnetic metal cylinder made of cobalt, concentrated at the bottom side 13 It was confirmed that it has a C content and shows results opposite to those of nickel.

[0048] In other words, carbon isotopes separated according to the type of magnetic metal can be selected, and through the repeated performance of this experiment, pure 13 C and 12 It is expected that C can be separated.

[0049] As described above, the present invention has been explained by limited embodiments, but this is provided only to aid in a more comprehensive understanding of the invention. The present invention is not limited to the above embodiments, and various modifications and variations are possible from this description by those skilled in the art.

[0050] Accordingly, the scope of the present invention is not limited to the described embodiments, and all things equivalent to or having equivalent variations to the claims set forth below, as well as the claims set forth below, shall be considered to fall within the scope of the concept of the present invention.

Claims

Claim 1 A carbon isotope separation apparatus comprising: a high vacuum electron beam chamber; a magnetic metal cylinder provided within the high vacuum electron beam chamber and having a carbon mixture storage portion on its upper surface; and a water-cooled sample holder in contact with the lower surface of the magnetic metal cylinder. Claim 2 A carbon isotope separation device according to claim 1, wherein the magnetic metal is nickel or cobalt. Claim 3 A carbon isotope separation device according to claim 1, wherein the sample holder is a graphite precipitation part. Claim 4 In claim 1, the body of the magnetic metal cylinder is a carbon isotope separation device that is a diffusion path for carbon elements. Claim 5 A carbon isotope separation method using a carbon isotope separation device according to any one of claims 1 to 4, wherein the carbon mixture storage portion of the magnetic metal cylinder 12 C and 13 A carbon isotope separation method comprising: a step of introducing a carbon mixture containing C and eutecticizing it using an electron beam heating method; and a step of precipitating graphite through the diffusion of carbon elements. Claim 6 A carbon isotope separation method according to claim 5, wherein the magnetic metal cylinder forms a temperature gradient that decreases in the direction of the lower surface in the carbon mixture storage section. Claim 7 A carbon isotope separation method according to claim 6, wherein the temperature of the carbon mixture storage portion is 1300 ℃ to 1400 ℃ and the temperature of the bottom surface is 600 ℃ to 900 ℃. Claim 8 A carbon isotope separation method according to claim 5, wherein the metal component of the magnetic metal cylinder is selected to control the separated carbon isotopes.

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