WO2013018901A1 - Absorbant de rayonnement - Google Patents

Absorbant de rayonnement Download PDF

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Publication number
WO2013018901A1
WO2013018901A1 PCT/JP2012/069882 JP2012069882W WO2013018901A1 WO 2013018901 A1 WO2013018901 A1 WO 2013018901A1 JP 2012069882 W JP2012069882 W JP 2012069882W WO 2013018901 A1 WO2013018901 A1 WO 2013018901A1
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Prior art keywords
carbon nanotube
radiation
encapsulated
carbon nanotubes
peapod
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PCT/JP2012/069882
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English (en)
Japanese (ja)
Inventor
鶴岡　秀志
利彦 藤森
金子　克美
雅嗣 藤重
遠藤　守信
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国立大学法人信州大学
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Publication of WO2013018901A1 publication Critical patent/WO2013018901A1/fr

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    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F1/00—Shielding characterised by the composition of the materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/168—After-treatment
    • C01B32/178—Opening; Filling

Definitions

  • the present invention relates to a lightweight and easy-to-process radiation absorber that absorbs radiation emitted from radioactive materials leaked from a nuclear reactor, for example, with high efficiency.
  • a carbon nanotube (hereinafter referred to as CNT) is a hollow nano-sized diameter carbon fiber having a high aspect ratio obtained by winding a graphene sheet into a cylindrical shape.
  • peapods are those in which atoms, molecules, and particles are inserted into and encapsulated in the hollow part of CNTs. The synthesis of peapod was first reported in 1998, and several studies have been reported since then. However, since the physical properties are stable, there are still few reports on application methods (Non-patent Document 1). There are several patent applications regarding the application of peapods. The peapods that are used are peapods containing fullerenes or metal-encapsulated fullerenes (Patent Documents 1 to 6).
  • Non-Patent Document 2 describes the definition, measurement method, and numerical values for the mass absorption coefficient. According to this, the radiation absorption coefficient is determined by the atomic number of the substance, that is, the nuclide.
  • Non-Patent Documents 3 to 4 a patent application has been filed for electromagnetic wave absorption of CNTs in a broad sense including electromagnetic waves and light (Patent Document 10).
  • Patent Document 10 an electromagnetic wave absorbing material in which at least one selected from CNT and alkali metals, alkaline earth metals, rare earth metals and metals included in Group VIII of the periodic table is supported in a CNT tube.
  • Patent Document 11 an electromagnetic wave absorbing material in which at least one selected from CNT and alkali metals, alkaline earth metals, rare earth metals and metals included in Group VIII of the periodic table is supported in a CNT tube.
  • Patent Document 11 Patent Document 11
  • the electromagnetic wave is from the quasi-millimeter wave region to the millimeter wave region.
  • the present invention has been made to solve the above problems, and an object of the present invention is to provide a radiation absorbing material composed of peapods in which arbitrary atoms and molecules are encapsulated in CNTs or hollow portions of CNTs.
  • the radiation absorbing material according to the present invention is characterized in that particles comprising any one of atoms, molecules, compounds, or a combination thereof include particle-encapsulated carbon nanotubes encapsulated in the hollow of the carbon nanotubes.
  • particles comprising any one of atoms, molecules, compounds, or a combination thereof include particle-encapsulated carbon nanotubes encapsulated in the hollow of the carbon nanotubes.
  • atoms, molecules, and compounds encapsulated in the hollow of the carbon nanotube are collectively referred to as particles.
  • carbon nanotubes can contain various types of particles, various types of particle-containing carbon nanotubes can be created depending on the type of particles included. When enclosing the particles in the carbon nanotube, it is possible to enclose not only the same particles but also different kinds of particles.
  • the particle-containing carbon nanotubes can be used alone as a radiation absorbing material, but can be added to and mixed with other materials such as resin, metal, fiber, paint, and film to form a radiation absorbing material.
  • the particle-encapsulated carbon nanotubes are mixed with other materials, not only one type of particle-encapsulated carbon nanotubes but also a plurality of types of particle-encapsulated carbon nanotubes can be mixed and added to form a radiation absorbing material.
  • the radiation absorbing material according to the present invention includes lithium, beryllium, boron, sodium, magnesium, aluminum, silicon, phosphorus, sulfur, chlorine, potassium, calcium, scandium, titanium, vanadium, chromium, manganese, silver as the particles.
  • Cobalt nickel, copper, zinc, gallium, germanium, arsenic, selenium, bromine, rubidium, strontium, yttrium, zirconium, niobium, molybdenum, technetium, ruthenium, rhodium, palladium, silver, cadmium, indium, tin, antimony, tellurium , Iodine, cesium, barium, hafnium, tantalum, tungsten, rhenium, osmium, iridium, platinum, gold, mercury, thallium, lead, bismuth, polonium, astatine, radon, francium, la Um, lanthanum, cerium, praseodymium, eosin gym promethium, samarium, europium, gadolinium, terbium, dysprosium, one of uranium or may be configured to include any of the compounds.
  • the carbon nanotubes enclosing the particles single-walled, double-walled, or multi-walled carbon nanotubes of three or more layers can be used.
  • the radiation absorbing action by the particle-encapsulating carbon nanotube is due to the contribution of the radiation absorbing action of the particles encapsulated in the carbon nanotube in addition to the radiation absorbing action of the carbon nanotube itself. Therefore, a radiation absorbing material having an effective radiation absorbing action can be obtained by selecting the design of the carbon nanotubes and the type and concentration of the particles to be included.
  • the present invention is based on the finding that when carbon has a CNT structure, the mass absorption coefficient of CNT is clearly increased compared to the known mass absorption coefficient of carbon. Moreover, it is based on the knowledge that the mass absorption coefficient becomes equal to or larger than the value based on the conventional rule of addition of radiation absorption by using particle-encapsulated carbon nanotubes (peapods) encapsulating elements in CNTs.
  • the CNT used in the present invention may have an outermost diameter of 0.4 nm or more and 200 nm or less, but is particularly preferably 1 nm or more and 100 nm or less. In addition, the CNT used in the present invention can be used regardless of the type of single-walled CNT or two or more multilayered CNTs.
  • the particles encapsulated in the peapod used in the present invention may be either atoms or molecules, and may be compounds such as organic metals and organic substances.
  • the particles can be used in the form of a solid, liquid, or gas at normal temperature and pressure, and are preferably solid or liquid.
  • an element having high radiation absorbing ability into a CNT as a peapod, a material that is difficult to use as a radiation absorbing material is utilized without changing the surface physical properties of the material CNT.
  • elements such as iodine, which have high radiation absorption ability but are halogen, are not easily mixed with other materials, or elements that have not been used effectively so far because the solution or paste deteriorates the seal. It can be suitably used by encapsulating in CNTs in the form of molecules, atoms, or particles having less than 100 particles.
  • a known CNT application method can be used as it is.
  • the application range is paper, fiber, film, solid, resin, ceramic and metal, and there is no particular limitation as long as it is a material capable of coating and kneading CNT.
  • the peapod since the peapod is stable, the encapsulated particles are not easily discharged. Utilizing this property, it is possible to manufacture a material that blocks gamma rays with high efficiency by encapsulating elements such as lead and tungsten that are difficult to handle due to toxicity into peapods. is there. Further, the peapod can be safely and easily recovered by removing the surrounding material by burning it after use.
  • the radiation absorbing material of the present invention can be applied to various products as a lightweight and highly efficient radiation absorbing material.
  • FIG. 1 shows a transmission electron micrograph of multi-walled carbon nanotubes.
  • the multi-walled carbon nanotube in the illustrated example is a four-layer carbon nanotube.
  • known methods such as catalytic vapor phase epitaxy can be used.
  • a mixed gas of a hydrocarbon such as methane and a carrier gas such as hydrogen or argon is introduced into a heating atmosphere heated to a temperature at which carbon nanotubes are formed, in which a metal catalyst is present, Carbon nanotubes are grown from the surface of the metal catalyst in contact with the mixed gas.
  • FIG. 2 shows a transmission electron micrograph of a carbon nanotube (gadolinium peapod) containing gadolinium chloride.
  • the gadolinium peapod shown in FIG. 2 is obtained by incorporating gadolinium into a double-walled carbon nanotube. It can be seen that gadolinium is present at the center of the carbon nanotube.
  • FIG. 3 the schematic of the apparatus used for preparation of a peapod is shown.
  • a method of creating a peapod using this apparatus will be described.
  • 100 mg of carbon nanotubes are weighed with an electronic balance and put into the main tube 10 of the bifurcated glass tube shown in FIG.
  • 100 mg of gadolinium chloride (III) manufactured by Wako Pure Chemical Industries
  • iodine special grade reagent manufactured by Wako Pure Chemical Industries
  • the main pipe 10 is placed in the mantle heater 18 (FIG. 3B), the cock 14 is opened, and the degassing operation is performed by the vacuum pump 16 until the main pipe 10 and the branch pipe 12 are dried and evacuated.
  • the heating temperature of the mantle heater 18 is set to 150 ° C. to evaporate excess moisture.
  • the cock 14 is closed, and the neck portion 15 formed in the small diameter of the glass tube is melt-sealed with a burner.
  • the mantle heater 18 covering the main pipe 10 is removed, and the entire glass tube is placed in another mantle heater and left at 200 ° C. for 48 hours.
  • the glass tube is taken out from the mantle heater, left to cool, and the neck portion 15 is scratched with a file, cut by induction cutting, and the CNT is taken out from the main pipe 10.
  • a peapod containing gadolinium or iodine is obtained.
  • CNTs used for X-ray absorption measurements are single-walled carbon nanotubes (SWCNT), multi-walled carbon nanotubes manufactured by Mitsui & Co., Ltd. (trade name Mitsui MWNT-7), Bayer's multi-walled carbon nanotubes Baytubes (registered trademark), and JFE Engineering's multi-walled carbon nanotubes (JFE-CNT).
  • CNT carbon materials other than CNT
  • standard carbon materials HOPG: Highly Oriented Pylorized Carbon
  • fullerene fullerene
  • polyester fibers dyed with CNT C-Textile
  • the peapods used for the X-ray absorption measurement are gadolinium peapods and iodine peapods prepared by the method described above.
  • Double-walled carbon nanotubes manufactured by our laboratory were used for gadolinium peapods, and multi-walled carbon nanotubes (Mitsui MWNT-7) manufactured by Mitsui & Co., Ltd. were used for iodine peapods.
  • the CNT, carbon material, and peapod which are the above-mentioned measurement targets, are washed with ethanol (special grade reagent manufactured by Wako Pure Chemical Industries, Ltd.), and the vacuum specimen dryer RA-155S manufactured by Miyamoto Riken Kogyo Co., Ltd. is used. After drying and taking out, it is packed in a tablet-shaped preparation holder and tableted with a handy-type press. This is placed in front of the receiver of Rigaku RINT TTR II, X-ray equipment, and MoK ⁇ rays (50kV) are irradiated with X-rays monochromatized on the germanium crystal (1,1,1) plane (X-ray intensity I sample ). Similarly, the X-ray intensity was measured with no sample placed in front of the receiver (X-ray intensity I o ).
  • the X-ray mass absorption coefficient is calculated from the following equation (1).
  • ( ⁇ / ⁇ ) is the mass absorption coefficient
  • ⁇ is the linear absorption coefficient of the object to be measured
  • ⁇ is the density of the object to be measured
  • x is the thickness of the object to be measured.
  • FIG. 4 shows a sample of the four CNTs mentioned above (SWCNT, Mitsui MWNT-7, Baytubes (registered trademark), and JFE-CNT), a standard carbon material (HOPG), fullerene (C 60), shows the mass absorption coefficient measured for C-Textile.
  • Sample SWCNT is a single-walled carbon nanotube having a diameter of 1.2 to 1.4 nm
  • Mitsui MWNT-7 is a multi-walled carbon nanotube having a diameter of 60 to 70 nm
  • Baytubes (registered trademark) is a multi-walled carbon nanotube having a diameter of 20 to 30 nm. All of these CNT samples are hollow carbon nanotubes
  • JFE-CNT is a carbon nanotube filled with carbon (nanocarbon rod).
  • sample C-Textile is a woven fabric obtained by weaving polyester fibers in a dispersion liquid in which Baytubes (registered trademark) is dispersed to woven fibers dyed with CNTs. The X-ray absorption measurement of C-Textile was performed using a sample of a plurality of C-Textile cloths stacked.
  • Figure 4 shows three sample SWCNTs, Mitsui, which are hollow CNTs.
  • MWNT-7 and Baytubes registered trademark
  • the mass absorption coefficient for X-rays is clearly larger than that of standard carbon materials, JFE-CNT filled with carbon in the center, and fullerene (C 60 ). Show. That is, it can be seen that hollow CNTs are superior in X-ray absorption characteristics compared to CNTs filled with carbon in the center, and can absorb X-rays more efficiently than standard carbon materials and fullerenes.
  • X-ray absorption measurement result iodine-containing peapod
  • Measurements were performed at 50 kV, 4 mA, wavelength 0.6197 angstrom and 50 kV, 35 mA, wavelength 0.709 angstrom in Rigaku Ultima IV, X-ray apparatus.
  • the thickness of the sample (tablet) was 1.164 mm for the sample made of Mitsui & Co., Ltd. multi-walled carbon nanotube (Mitsui MWNT-7), and 1.561 mm for the sample in which iodine was encapsulated in this multi-walled carbon nanotube.
  • the results of measuring the X-ray mass absorption coefficient are as follows. A.
  • Wavelength 0.6197 Angstrom MWNT-7 0.404 Iodine-containing peapod: 0.496 cm 2 / g B.
  • Wavelength 0.709 Angstrom MWNT-7 0.539 Iodine-containing peapod: 0.716 cm 2 / g
  • X-ray absorption measurement result gadolinium inclusion peapod
  • Measurements were performed at 50 kV, 4 mA, wavelength 0.6197 angstrom and 50 kV, 35 mA, wavelength 0.709 angstrom in Rigaku Ultima IV, X-ray apparatus.
  • the thickness of the sample was 0.083 mm for the sample made of double-walled carbon nanotubes, and 0.109 mm for the peapod in which gadolinium was included in the double-walled carbon nanotubes.
  • the measured value (-ln (I sample / I o ) in equation (1)) is the measured sample thickness of 0.109 mm and the mass of gadolinium (I) chloride 2.424 g / ml And gadolinium trichloride (III) hexahydrate mass (2400 kg / m 3 (CAS No.13450-84-5))
  • the mass series coefficient was estimated by estimating the specific gravity of the encapsulated peapod.
  • the peapod in which gadolinium is encapsulated in a double-walled carbon nanotube has a greatly improved X-ray absorption efficiency compared to the double-walled carbon nanotube.
  • the peapot can effectively improve the X-ray absorption efficiency of the peapod as a whole by the X-ray absorption ability of the particles encapsulated in the carbon nanotubes.
  • X-ray (radiation) absorption capacity is higher for heavier elements than light elements, so it is considered effective to include elements with larger atomic numbers.
  • the absorption efficiency of X-rays (radiation) of a specific wavelength is particularly high depending on the element, it can be used for protection of radiation (radioactive material) of a specific wavelength.
  • a peapod can be produced by including any atom, molecule, or compound in CNT, and a combination of a plurality of types of atoms or compounds can also be included. It is also possible to produce a radiation absorbing material having an improved shielding function against specific radiation by combining a plurality of types of atoms and compounds.
  • Sulfur-containing peapod A single-walled carbon nanotube is placed in the main tube 10 of the bifurcated glass tube of the peapod creation apparatus shown in FIG. 3, sulfur is introduced into the branch tube 12, and after evacuation, the mantle heater 18 is heated to 773K and held for 48 hours. As a result, sulfur was introduced into the hollow of the carbon nanotube.
  • Sulfur has a one-dimensional structure with a length of several tens of nanometers or more. The long-dimensional one-dimensional structure of sulfur was confirmed by synchrotron X-ray diffraction and observed in a one-dimensional chain direction by a transmission electron microscope.
  • FIG. 5 shows the result of X-ray fluorescence analysis of a peapod in which gadolinium trichloride is encapsulated in a double-walled carbon nanotube.
  • the part enclosed by the square of the spectrum is the contribution part by gadolinium, and it was confirmed that Gd was included in the carbon nanotube.
  • the content of Gd is 3.1 wt%, and this content is an amount considered to substantially fill the hollow portion of the carbon nanotube.
  • FIG. 6 shows the result of X-ray fluorescence analysis of a peapod in which iodine is encapsulated in a double-walled carbon nanotube.
  • the part enclosed by the square of the spectrum is the part contributed by iodine.
  • the iodine content is 2.55 wt%, and in this case as well, iodine is considered to substantially fill the hollow portion of the carbon nanotube.
  • peapods have the property of retaining the encapsulated particles (atoms, compounds) inside the CNT without discharging them, so they contain halogens such as iodine, toxic elements such as lead and tungsten. Therefore, it can be provided as a radiation absorbing material that is safe and can be used for various purposes.

Abstract

L'invention concerne un absorbant de rayonnement caractérisé en ce qu'il comprend un nanotube de carbone contenant des particules encapsulées dans l'espace creux de celui-ci, lesdites particules comprenant un atome, une molécule, un composé ou une combinaison de ceux-ci et étant encapsulées dans l'espace creux du nanotube de carbone. Grâce à l'encapsulation d'un élément, d'une matière inorganique ou d'une matière organique ayant une capacité d'absorption de rayonnement élevée dans l'espace creux du nanotube de carbone, un absorbant de rayonnement, qui a une capacité d'absorption très efficace du rayonnement et qui maintient toutefois les propriétés de surface du nanotube de carbone, peut être obtenu. L'absorbant de rayonnement maintient les propriétés de surface du nanotube de carbone et, par conséquent, peut être ajouté à diverses matières ou mélangé à celles-ci avant l'utilisation.
PCT/JP2012/069882 2011-08-04 2012-08-03 Absorbant de rayonnement WO2013018901A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2015099123A (ja) * 2013-11-20 2015-05-28 国立大学法人信州大学 炭素粒子の空間分布同定方法
WO2017033482A1 (fr) * 2015-08-24 2017-03-02 古河電気工業株式会社 Agrégat de nanotubes de carbone, matériau composite à base de nanotubes de carbone et fil de nanotubes de carbone

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JPH06227806A (ja) * 1992-12-22 1994-08-16 Nec Corp 異物質内包カーボンナノチューブとその製造方法
JP2001205600A (ja) * 2000-01-27 2001-07-31 Canon Inc 微細構造体及びその製造方法
JP2003124011A (ja) * 2001-10-09 2003-04-25 Hitachi Ltd 電磁波吸収材及びそれを用いた製品
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WO2017033482A1 (fr) * 2015-08-24 2017-03-02 古河電気工業株式会社 Agrégat de nanotubes de carbone, matériau composite à base de nanotubes de carbone et fil de nanotubes de carbone
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JPWO2017033482A1 (ja) * 2015-08-24 2018-06-07 古河電気工業株式会社 カーボンナノチューブ集合体、カーボンナノチューブ複合材料及びカーボンナノチューブ線材
US10392253B2 (en) 2015-08-24 2019-08-27 Furukawa Electric Co., Ltd. Aggregate of carbon nanotubes, carbon nanotube composite material, and carbon nanotube wire

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