WO2013084948A1 - Contenant, procédé et dispositif de craquage en phase vapeur, et procédé et dispositif d'analyse - Google Patents

Contenant, procédé et dispositif de craquage en phase vapeur, et procédé et dispositif d'analyse Download PDF

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Publication number
WO2013084948A1
WO2013084948A1 PCT/JP2012/081533 JP2012081533W WO2013084948A1 WO 2013084948 A1 WO2013084948 A1 WO 2013084948A1 JP 2012081533 W JP2012081533 W JP 2012081533W WO 2013084948 A1 WO2013084948 A1 WO 2013084948A1
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compound sample
silicon carbide
decomposition
container
sample
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PCT/JP2012/081533
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English (en)
Japanese (ja)
Inventor
亮 町田
星野　英樹
高史 末包
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株式会社住化分析センター
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Priority to KR1020147018491A priority Critical patent/KR20140105810A/ko
Publication of WO2013084948A1 publication Critical patent/WO2013084948A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition

Definitions

  • the present invention relates to a container for decomposing a compound sample or silicon carbide compound sample comprising carbon atoms, a gas phase decomposition method and a gas phase decomposition apparatus using the vessel, and a compound sample or silicon carbide comprising decomposed carbon atoms.
  • the present invention relates to an analysis method and an analysis apparatus for compound samples.
  • Non-Patent Document 1 As a method for analyzing impurities contained in a silicon carbide compound, a chemical analysis method for silicon carbide fine powder described in Non-Patent Document 1 is known. According to the method described in Non-Patent Document 1, silicon carbide is immersed in a mixed acid solution in which a plurality of acids are mixed, heated and pressurized, and silicon carbide is dissolved in the mixed acid solution to obtain a measurement sample solution. And the metal impurity contained in this measurement sample is detected.
  • Non-Patent Document 1 since the silicon carbide compound sample and the mixed acid solution are in direct contact, the metal contained in the mixed acid solution is contained in the measurement sample solution, and contamination to the measurement sample solution is not caused. appear. Further, the metal adhering to the inner wall of the container containing the mixed acid solution or contained as an impurity dissolves into the mixed acid solution by coming into contact with the mixed acid solution and is contained in the measurement sample solution.
  • the present invention has been made in view of the above-mentioned problems, and its purpose is to prevent contamination of metal impurities derived from the decomposition solution, and more accurately in a compound sample or a silicon carbide compound sample composed of carbon atoms.
  • a container for decomposing a compound sample comprising silicon atoms or a silicon carbide compound sample capable of analyzing a metal impurity, a gas phase decomposition method and a gas phase decomposition apparatus using the container, and a decomposed carbon atom An analysis method and an analysis apparatus for a compound sample or a silicon carbide compound sample are provided.
  • a container according to the present invention is a container for decomposing a compound sample or silicon carbide compound sample comprising carbon atoms, and the compound sample or silicon carbide compound comprising carbon atoms therein.
  • An outer container portion having a sealed space for containing a decomposition solution for decomposing the sample, and having pressure resistance against pressure for decomposing the compound sample or silicon carbide compound sample composed of the carbon atom, and the outer container portion
  • An inner container that is formed of a material that is resistant to the decomposition solution and contains the compound sample or the silicon carbide compound sample composed of the carbon atom from the opened upper part. Is characterized in that when the decomposition solution is accommodated in the outer container part, the decomposition solution is not in contact with the inner wall.
  • a decomposition solution for decomposing a compound sample or a silicon carbide compound sample made of carbon atoms is accommodated in the outer container portion of any of the above-described containers, and carbon atoms are placed on the mounting table.
  • a preparatory step for placing the compound sample or silicon carbide compound sample comprising, and pressurizing by heating the inside of the outer container portion containing the compound sample or silicon carbide compound sample comprising the carbon atom and the decomposition solution A decomposition step of decomposing the compound sample composed of the carbon atom or the silicon carbide compound sample with a decomposition solution gas obtained by vaporizing the decomposition solution.
  • the method for analyzing a compound sample consisting of carbon atoms or a silicon carbide compound sample according to the present invention is a measurement obtained by decomposing a compound sample consisting of carbon atoms or a silicon carbide compound sample by any of the vapor phase decomposition methods described above. It includes a step of detecting metal impurities in the sample.
  • the vapor phase decomposition apparatus for a compound sample comprising silicon atoms or a silicon carbide compound sample according to the present invention is characterized by comprising any of the above-described containers and a heating means for heating the container.
  • the analyzer for analyzing a compound sample consisting of carbon atoms or a silicon carbide compound sample according to the present invention is obtained by vapor-phase decomposition of any of the above-described containers and a compound sample or silicon carbide compound sample consisting of carbon atoms in the container. And detecting means for detecting metal impurities in the measured sample.
  • a container for decomposing a compound sample comprising silicon atoms or a silicon carbide compound sample according to the present invention has a sealed space containing a decomposition solution for decomposing the compound sample comprising silicon atoms or the silicon carbide compound sample, An outer container portion that is pressure resistant to a pressure for decomposing a compound sample or silicon carbide compound sample composed of carbon atoms, and a material that is provided in the outer container portion and is resistant to the decomposition solution. And an inner container in which the compound sample composed of the carbon atoms or the silicon carbide compound sample is accommodated from the opened upper part, and the inner container is disposed when the decomposition solution is accommodated in the outer container part.
  • the decomposition solution does not come into contact with the inner wall, it is derived from the decomposition solution in the compound sample consisting of decomposed carbon atoms or the silicon carbide compound sample. Genus impurities prevents the contamination, it is more accurately can analyze metallic impurities of the compound samples or silicon carbide compound sample composed of carbon atoms.
  • FIG. 1 is a cross-sectional view showing a container for decomposing a compound sample or silicon carbide compound sample comprising carbon atoms according to an embodiment of the present invention.
  • the compound sample consisting of carbon atoms is a compound sample containing only carbon atoms.
  • Examples of compound samples comprising carbon atoms are intended to be diamond, graphite, graphene, amorphous carbon, diamond-like carbon, tetrahedral amorphous carbon, carbon nanotubes, carbon nanocoils, carbon fibers, carbon, etc.
  • the silicon carbide compound sample is intended to be a silicon carbide based sample containing SiC, SiOC, SiCN and the like. In the present embodiment, a mode using a silicon carbide compound sample will be described as an example.
  • the container 10 includes an outer container portion 1 and an inner container 6.
  • the container 10 is used for decomposing the silicon carbide compound sample 7.
  • the container 10 may further include a support portion 4 including a table (mounting table) 5 on which the inner container 6 is placed.
  • Outer container part 1 The outer container part 1 has a sealed space in which a silicon carbide compound sample 7 and a decomposition solution 8 for decomposing the silicon carbide compound sample 7 are accommodated. Outer container portion 1 is pressure resistant to the pressure applied to decompose silicon carbide compound sample 7 accommodated therein. Moreover, it is preferable that the outer container part 1 is heat resistant with respect to the heat
  • the pressure resistance against the pressure applied to decompose the silicon carbide compound sample 7 is difficult to expand or soften when pressure is applied to decompose the silicon carbide compound sample 7, It is intended to keep the shape constant and not deform.
  • heat resistance to heat applied to decompose the silicon carbide compound sample 7 means that when heated to decompose the silicon carbide compound sample 7, elution or softening is difficult and the shape is kept constant. It is intended not to deform.
  • the outer container part 1 has a double wall structure of an inner cylinder part 3 and an outer cylinder part 2 outside thereof.
  • the inner cylinder portion 3 faces the sealed space and is formed of a material that is resistant to the decomposition solution 8.
  • the inner cylinder portion 3 is formed of a material that is resistant to the decomposition solution 8 because the decomposition solution 8 is in direct contact with the decomposition solution 8 when the decomposition solution 8 is accommodated in the sealed space.
  • the material that is resistant to the decomposition solution 8 is intended to be a material that does not elute metal components from the decomposition solution 8, and is more preferably a material that does not elute metal components from the decomposition solution 8. preferable.
  • Examples of the material that is resistant to the decomposition solution 8 include a fluororesin, platinum, or a ceramic material.
  • PTFE polytetrafluoroethylene (tetrafluoride)
  • PFA tetrafluoroethylene / perfluoroalkyl vinyl ether copolymer
  • PVDF polyvinylidene fluoride (difluoride)
  • PCTFE polychlorotrifluoro Ethylene (trifluoride) etc.
  • the ceramic material include alumina, zirconia, calcia, magnesia, yttria and the like.
  • the shape of the inner cylinder part 3 is not particularly limited as long as the sealed space exists inside, the support part 4 is installed in the sealed space, and the silicon carbide compound sample 7 and the decomposition solution 8 can be accommodated.
  • the inner cylinder portion 3 is divided into two members, a lower portion and a lid portion. A support portion 4 is installed in the lower portion, the decomposition solution 8 is accommodated, and the lid portion is placed and sealed so as to close it from above. May be.
  • the thickness of the lower wall, the side wall, and the upper wall of the inner cylinder part 3 is not particularly limited as long as it is a thickness capable of preventing the stored decomposition solution 8 from flowing out and sealing the inner space.
  • the outer cylinder part 2 is located outside the inner cylinder part 3 and is provided so as to wrap around the inner cylinder part 3. And the outer cylinder part 2 is pressure-resistant with respect to the pressure for melt
  • FIG. Therefore, in order to decompose the silicon carbide compound sample 7 accommodated in the inside, even if pressure is applied by heating and the inner cylinder part 3 is deformed, the outer cylinder part 2 has pressure resistance. Deformation of the entire container unit 1 can be prevented. Moreover, it is preferable that the outer cylinder part 2 is heat resistant with respect to the heat applied in order to dissolve the silicon carbide compound sample 7. FIG. Thereby, the deformation
  • the outer cylinder portion 2 only needs to have pressure resistance and heat resistance against the pressure and heat for dissolving the silicon carbide compound sample 7, and is formed of, for example, stainless steel.
  • the outer cylinder part 2 should just be provided so that the inner cylinder part 3 may be wrapped at least at the time of pressurization and heating. That is, the outer cylinder part 2 is divided into two members, a lower part and a lid part. The inner cylinder part 3 is accommodated in the lower part, and the lid part is placed and sealed so as to close it from above. And may be subjected to heating.
  • the thickness of the lower wall, the side wall, and the upper wall of the outer cylinder part 2 is not particularly limited as long as desired pressure resistance and heat resistance can be obtained.
  • the inner cylinder part 3 faces the sealed space in which the decomposition liquid 8 is accommodated, and the outer cylinder part 2 and the decomposition liquid 8 are not in contact with each other. It is possible to prevent the derived metal impurities from being dissolved into the decomposition solution 8 and causing contamination, and to suppress the elution of the metal into the decomposition solution 8.
  • the inner cylinder part 3 may be further made into a two-layer structure to prevent the metal impurities derived from the outer cylinder part 2 from dissolving into the decomposition solution 8 more reliably.
  • the inner container 6 is formed of a material that is resistant to the decomposition solution 8 and is a columnar container having an open top.
  • the silicon carbide compound sample 7 is accommodated in the inner container 6 from the upper open part.
  • the inner container 6 is provided in the outer container part 1 so that the decomposition solution 8 does not contact the inner wall. Since the inner container 6 is exposed to the decomposition liquid gas in which the decomposition liquid 8 is vaporized, the inner container 6 is formed of a material that does not elute the metal component with respect to the decomposition liquid 8. Need to be.
  • Examples of the material that is resistant to the decomposition solution 8 constituting the inner container 6 include a fluororesin, platinum, or a ceramic material.
  • PTFE polytetrafluoroethylene (tetrafluoride)
  • PFA tetrafluoroethylene / perfluoroalkyl vinyl ether copolymer
  • PVDF polyvinylidene fluoride (difluoride)
  • PCTFE polychlorotrifluoro Ethylene (trifluoride) etc.
  • the ceramic material include alumina, zirconia, calcia, magnesia, yttria and the like.
  • the inner container 6 may be placed on the table 5, and the decomposition solution 8 may be stored below the table 5 positioned above the liquid surface of the decomposition solution 8.
  • the container 6 and a decomposition liquid container (not shown) containing the decomposition liquid may be placed adjacent to the table 5, and the inner container 6 is placed under the table 5.
  • a decomposition solution container (not shown) containing the decomposition solution may be placed on the upper side of the table. That is, the inner container 6 may be configured such that the decomposition liquid 8 does not contact the inner wall of the inner container 6 and the silicon carbide compound sample 7 in the inner container 6 is exposed to the decomposition liquid gas vaporized from the decomposition liquid 8.
  • a decomposition liquid container it is formed of a material that is resistant to the decomposition liquid, and a container in which the decomposition liquid is accommodated from an opened upper portion can be used.
  • a plurality of inner containers 6 may be placed on the table 5, whereby a plurality of silicon carbide compound samples 7 can be decomposed simultaneously.
  • the size of the inner container 6 is not particularly limited as long as the contained silicon carbide compound sample 7 is sufficiently exposed to the decomposition liquid gas from which the decomposition liquid 8 is vaporized.
  • the support part 4 is provided in the outer container part 1.
  • the support portion 4 includes a stand provided so as to protrude from the bottom surface inside the outer container portion 1 and a table 5 provided on the top of the stand.
  • the table 5 is provided so as to be supported from below by support pins (not shown) provided so as to protrude from at least two positions of the side wall of the outer container part 1 (side wall of the inner cylinder part 3). Also good.
  • the support part 4 is comprised by the table 5 and the support pin.
  • the table 5 may be formed integrally with a stand or a support pin, or may be formed separately and assembled before use.
  • the support unit 4 may be configured to be able to change the height of the stand.
  • the support portion 4 is preferably made of a material resistant to the decomposition solution 8.
  • the diameter of the table 5 is the same as the inner diameter of the inner cylinder part 3, and is provided so as to contact the side wall of the inner cylinder part 3.
  • the table 5 is a porous body provided with holes for allowing the cracked liquid gas to pass therethrough. Therefore, the hole provided in the table 5 becomes a flow path of the decomposition liquid gas in which the decomposition liquid 8 accommodated below is vaporized, and the decomposition liquid gas reaches the silicon carbide compound sample 7.
  • the inner diameter of the table 5 may be smaller than the inner diameter of the inner cylinder portion 3 so that a gap is formed between the table 5 and the inner wall of the inner cylinder portion 3. In this case, since the decomposition gas flows from the gap and reaches the silicon carbide compound sample 7, the table 5 does not have to be provided with holes.
  • the silicon carbide compound sample 7 is accommodated in the inner container 6 provided in the pressure-resistant outer container part 1 that accommodates the decomposition solution 8, and the inside of the outer container part 1 is heated.
  • the silicon carbide compound sample 7 is vapor-phase decomposed by the decomposition liquid gas obtained by vaporizing the decomposition liquid 8. Therefore, the metal impurities contained in the decomposition solution 8 and the metal impurities adhering to the inner wall of the outer container part 1 (inner wall of the inner cylinder part 3) and the inner wall of the inner container 6 are obtained by decomposing the silicon carbide compound sample 7. It can prevent mixing in the measured sample.
  • the silicon carbide compound sample 7 is decomposed using the container 10, it can be subjected to an analysis that more accurately detects a trace amount of metal contained in the silicon carbide compound sample 7.
  • a compound sample composed of carbon atoms can be decomposed even under atmospheric pressure using a decomposition solution such as a mixed acid of sulfuric acid, nitric acid and perchloric acid (for example, Reference 1 (“Wet oxidative decomposition: curcumin absorption Quantitative determination of boron in graphite by photometric method ", Kazuo Watanabe et al., Analytical Chemistry, 44 (11), 939-942, 1995)).
  • a decomposition solution such as a mixed acid of sulfuric acid, nitric acid and perchloric acid
  • the silicon carbide compound sample 7 which is harder to decompose than the compound sample made of carbon atoms can be decomposed. Therefore, it is clear that the compound sample made of carbon atoms can be decomposed using the container 10. is there.
  • the gas phase decomposition method is a method for decomposing a compound sample or silicon carbide compound sample comprising carbon atoms, wherein a decomposition solution for decomposing the sample or carbon carbide compound sample comprising carbon atoms is provided. It includes a decomposition step of decomposing by the vaporized decomposition gas. According to the present invention, since a compound sample comprising silicon atoms or a silicon carbide compound sample is vapor-phase decomposed, metal impurities contained in the decomposition solution are mixed into a measurement sample obtained by decomposing the sample. Can be prevented.
  • a decomposition solution for decomposing a compound sample composed of carbon atoms or a silicon carbide compound sample is accommodated in the outer container portion 1 of the container 10 described above before the decomposition step.
  • the container 10 described above is an embodiment of a container used in the vapor phase decomposition method according to the present invention. Therefore, the description of the container used in the vapor phase decomposition method according to the present invention conforms to the description of the container 10 described above. In the present embodiment, a case where a silicon carbide compound sample is used will be described as an example.
  • a decomposition solution for decomposing the silicon carbide compound sample is stored in the outer container portion 1 of the container 10, and the silicon carbide compound sample is stored in the inner container 6.
  • the decomposition liquid is accommodated so as not to touch the inner wall of the inner container 6.
  • the silicon carbide compound sample is efficiently decomposed if the decomposition solution is accommodated in an amount of 5 to 40% of the volume of the outer container portion 1. This is preferable.
  • the amount of the decomposition solution accommodated in the outer container portion 1 may be an amount capable of sufficiently decomposing the silicon carbide compound sample. Therefore, for example, 2 to 20 ml of decomposition solution may be accommodated per 1 g of the silicon carbide compound sample to be decomposed.
  • An acid solution containing at least one acid selected from the group consisting of hydrofluoric acid, nitric acid, hydrochloric acid, sulfuric acid, phosphoric acid, hydrogen peroxide, and perchloric acid is used as a decomposition solution for decomposing the silicon carbide compound sample.
  • it is a mixed acid solution of hydrofluoric acid and nitric acid.
  • the silicon carbide compound sample may be placed in the inner container 6 and placed on the table 5.
  • the silicon carbide compound sample may be a bulk or a thin film. After accommodating the silicon carbide compound sample and the decomposition solution in the outer container part 1, the outer container part 1 is sealed.
  • the silicon carbide compound sample and the decomposition solution are accommodated and pressurized by heating the inside of the sealed outer container part 1.
  • the pressurization and heating in the outer container part 1 can be suitably performed by a conventionally known method.
  • the heating temperature of the outer container part 1 may be any desired pressurization that will be described later and may be any temperature that vaporizes the decomposition solution, preferably 100 to 240 ° C, more preferably 150 to 240 ° C. Preferably, the temperature is from 180 to 240 ° C.
  • the heating time of the outer container part 1 is preferably 1 to 96 hours, more preferably 1 to 48 hours, and most preferably 5 to 48 hours per 1 g of the silicon carbide compound sample.
  • the pressure applied to the outer container part 1 by heating at the above-described temperature is a pressure at which the silicon carbide compound sample can be decomposed by the vaporized decomposition solution, preferably 1 to 15 MPa, and preferably 5 to 15 MPa. Is more preferable, and 7 to 15 MPa is most preferable.
  • the silicon carbide compound sample is decomposed in the gas phase by the decomposition solution gas from which the decomposition solution is vaporized. Therefore, metal impurities contained in the decomposition solution and metal impurities attached to the inner wall of the outer container part 1 (inner wall of the inner cylinder part 3) and the inner wall of the inner container 6 were obtained by decomposing the silicon carbide compound sample. Mixing in the measurement sample can be prevented. As a result, it can be subjected to an analysis that more accurately detects a trace amount of metal contained in a silicon carbide compound sample.
  • the method for analyzing a compound sample comprising silicon atoms or a silicon carbide compound sample is the method of analyzing a compound sample comprising silicon atoms or a silicon carbide compound sample obtained by decomposing the compound sample comprising silicon atoms or the silicon carbide compound sample.
  • the method includes a step of detecting a metal impurity.
  • the metal impurities contained in the sample are contained in the inner container 6 in which the sample is accommodated. Remains. In the present embodiment, the remaining metal impurities are used as detection targets using the measurement sample.
  • the metal impurities remaining in the inner container 6 may be recovered using a recovery liquid.
  • a conventionally known solution can be used as the recovery solution, and is not particularly limited.
  • nitric acid or a mixed acid of nitric acid and hydrochloric acid can be used.
  • the recovered liquid is dropped into the inner container 6 to dissolve and recover the metal impurities attached to the inner wall of the inner container 6.
  • the metal impurities may be recovered by dropping the recovered liquid into the inner container 6 and further heating.
  • the recovered metal impurities may be further adjusted with a recovery solution and used for measurement.
  • ICP-MS inductively coupled plasma mass spectrometry
  • ICP-AES inductively coupled plasma emission spectroscopy
  • AAS atomic absorption spectrometry
  • the metal impurities contained in the compound sample or silicon carbide compound sample consisting of carbon atoms are reduced. More accurate detection is possible.
  • a vapor phase decomposition apparatus for a compound sample comprising silicon atoms or a silicon carbide compound sample according to the present invention is characterized by comprising the container described above and a heating means for heating the container.
  • the container 10 used in the above-described gas phase decomposition method is an embodiment of the container used in the gas phase decomposition apparatus according to the present invention. Therefore, the description of the vapor phase decomposition apparatus according to the present invention is based on the above description of the vapor phase decomposition method. In addition, a conventionally well-known heating apparatus can be used as a heating means.
  • the analyzer for analyzing a compound sample or silicon carbide compound sample comprising carbon atoms comprises the above-described container and a measurement obtained by vapor phase decomposition of the compound sample or silicon carbide compound sample comprising carbon atoms in the container. And a detecting means for detecting metal impurities in the sample.
  • the container 10 used in the analysis method described above is an embodiment of a container used in the analyzer according to the present invention. Therefore, the description of the analysis apparatus according to the present invention conforms to the description of the analysis method described above.
  • the detection means a conventionally known detection device can be used, and an example is ICP-MS manufactured by PerkinElmer.
  • the quality control method for a compound sample or silicon carbide compound sample comprising carbon atoms according to the present invention was obtained by decomposing a compound sample or silicon carbide compound sample comprising carbon atoms by any one of the vapor phase decomposition methods described above.
  • the metal element remaining by decomposing the compound sample or silicon carbide compound sample composed of carbon atoms by the gas phase decomposition method according to the present invention is recovered as a metal impurity, and a conventionally known measurement method is used as a measurement sample.
  • Elemental analysis by Examples of the method for elemental analysis of the measurement sample include inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma emission spectroscopy (ICP-AES), and atomic absorption spectrometry (AAS).
  • a compound sample or a silicon carbide compound sample consisting of carbon atoms in which the amount of metal impurities detected in the analysis step is equal to or less than a predetermined reference amount is extracted. That is, a compound sample or a silicon carbide compound sample consisting of carbon atoms is selected based on the amount of metal impurities detected in the analysis step. In the extraction step, a compound sample or a silicon carbide compound sample made of carbon atoms may be selected based on the type of metal impurity detected in the analysis step.
  • the metal impurity contained in the compound sample or silicon carbide compound sample made of carbon atoms can be accurately detected.
  • the quality of the compound sample or silicon carbide compound sample comprising carbon atoms can be kept constant. Therefore, the quality control method according to the present invention is also suitable for quality control of a compound sample composed of carbon atoms or a silicon carbide compound sample used for semiconductor manufacturing, which requires more accurate quality control.
  • the container which concerns on this invention is a container for decomposing
  • the outer container portion faces the sealed space, and is located outside the inner tube portion and an inner tube portion formed of a material resistant to the decomposition solution. And it is preferable that it is a double wall structure with the outer cylinder part which is pressure-resistant with respect to the pressure for dissolving the compound sample or silicon carbide compound sample which consists of the said carbon atom.
  • the inner container may be provided on a mounting table located above the liquid level of the decomposition liquid when the decomposition liquid is accommodated in the outer container portion. preferable.
  • a container according to the present invention is a decomposition liquid container that is provided in the outer container part, is formed of a material that is resistant to the decomposition liquid, and contains the decomposition liquid from the opened upper part. Furthermore, it is preferable to provide.
  • a decomposition solution for decomposing a compound sample or a silicon carbide compound sample made of carbon atoms is accommodated in the outer container portion of any of the above-described containers, and carbon atoms are placed on the mounting table.
  • a preparatory step for placing the compound sample or silicon carbide compound sample comprising, and pressurizing by heating the inside of the outer container portion containing the compound sample or silicon carbide compound sample comprising the carbon atom and the decomposition solution A decomposition step of decomposing the compound sample composed of the carbon atom or the silicon carbide compound sample with a decomposition solution gas obtained by vaporizing the decomposition solution.
  • the decomposition step it is preferable to pressurize at 1 to 15 MPa by heating the inside of the outer container portion at 100 to 240 ° C.
  • the decomposition solution is at least one selected from the group consisting of hydrofluoric acid, nitric acid, hydrochloric acid, sulfuric acid, phosphoric acid, hydrogen peroxide solution, and perchloric acid.
  • An acid solution containing an acid is preferable.
  • the method for analyzing a compound sample consisting of carbon atoms or a silicon carbide compound sample according to the present invention is a measurement obtained by decomposing a compound sample consisting of carbon atoms or a silicon carbide compound sample by any of the vapor phase decomposition methods described above. It includes a step of detecting metal impurities in the sample.
  • the vapor phase decomposition apparatus for a compound sample comprising silicon atoms or a silicon carbide compound sample according to the present invention is characterized by comprising any of the above-described containers and a heating means for heating the container.
  • the analyzer for analyzing a compound sample consisting of carbon atoms or a silicon carbide compound sample according to the present invention is obtained by vapor-phase decomposition of any of the above-described containers and a compound sample or silicon carbide compound sample consisting of carbon atoms in the container. And detecting means for detecting metal impurities in the measured sample.
  • the quality control method for a compound sample or silicon carbide compound sample comprising carbon atoms according to the present invention was obtained by decomposing a compound sample or silicon carbide compound sample comprising carbon atoms by any one of the vapor phase decomposition methods described above.
  • a blank test of vapor phase decomposition using the container 10 was performed.
  • the metal impurities contained in the decomposition solution and the outer container part 1 The amount of metal impurities adhering to the inner wall mixed into the measurement sample was examined.
  • a decomposition solution As a decomposition solution, a mixed acid solution of 40% hydrofluoric acid and 68% nitric acid (1: 1) was used.
  • the inner container 6 was evacuated and exposed to the vaporized decomposition gas, and the inside of the outer container 1 was heated at 200 ° C. for 5 hours to obtain high-temperature pressurization conditions.
  • a SUS container was used as the outer cylinder part 2
  • a PTFE container was used as the inner cylinder part 3.
  • Two PTFE inner containers 6 (VPD-1 and VPD-2) were placed on the table 5. The inner container 6 was taken out and nitric acid was dropped to collect metal impurities in each inner container 6 to obtain a measurement sample.
  • the measurement sample was measured by ICP-MS (manufactured by PerkinElmer). As a result, the amount of metal impurities contained in the measurement sample was as shown in Table 1. The values shown in Table 1 were calculated by multiplying the concentration (ng / g) measured by ICP-MS and the liquid amount (g) adjusted with the liquid.
  • the silicon carbide compound sample (SiC sample) was vapor-phase decomposed using the container 10.
  • a mixed acid solution of 40% hydrofluoric acid and 68% nitric acid (1: 1) was used as the decomposition solution.
  • the silicon carbide compound sample is placed in the inner container 6 and exposed to the decomposed liquid gas in which the decomposed liquid is vaporized, and the inside of the outer container 1 is heated at 200 ° C. for 5 hours. did.
  • the silicon carbide compound sample in the inner container 6 was decomposed and sublimated.
  • a silicon carbide certified reference material (CRM NMIJ 8001A) was vapor-phase decomposed.
  • As the decomposition solution a mixed acid solution of 40% hydrogen fluoride and 68% nitric acid (1: 1) was used. High temperature pressurization conditions were obtained by heating at 230 ° C. for 96 hours. After the decomposition treatment, the inner container 6 was taken out and nitric acid was added dropwise to collect metal impurities in the inner container 6 to obtain a measurement sample.
  • the above measurement sample was measured by ICP-MS (manufactured by PerkinElmer). As a result, the measured values and certified values of the samples were as shown in Table 2. The values listed in Table 2 were calculated by multiplying the concentration (ng / g) measured by ICP-MS by the liquid amount (g) prepared by liquid adjustment and dividing by the decomposed sample amount (g). .
  • the present invention can be used for metal impurity analysis of compound samples composed of carbon atoms or silicon carbide compound samples used in various fields.

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Abstract

La présente invention concerne un contenant (10) qui comprend : une partie contenant externe (1) possédant un espace étanche à l'air qui renferme soit un échantillon de composé formé à partir d'atomes de carbone ou un échantillon de composé de carbure de silicium et un fluide de craquage qui craque l'échantillon, ledit contenant externe étant résilient à la pression pour craquer l'échantillon ; et un contenant interne (6) qui est disposé à l'intérieur de la partie contenant externe (1) de sorte que le fluide de craquage n'entre pas en contact avec la paroi interne associée, et qui renferme l'échantillon. Des impuretés métalliques issues du fluide de craquage ne peuvent ainsi pas se mélanger à un échantillon craqué.
PCT/JP2012/081533 2011-12-06 2012-12-05 Contenant, procédé et dispositif de craquage en phase vapeur, et procédé et dispositif d'analyse WO2013084948A1 (fr)

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JP2017146123A (ja) * 2016-02-15 2017-08-24 日鉄住金テクノロジー株式会社 ケイ素定量分析方法

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JP2017146123A (ja) * 2016-02-15 2017-08-24 日鉄住金テクノロジー株式会社 ケイ素定量分析方法

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