KR20140105810A - Container, vapor phase cracking method, vapor phase cracking device, analysis method, and analysis device - Google Patents

Container, vapor phase cracking method, vapor phase cracking device, analysis method, and analysis device Download PDF

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KR20140105810A
KR20140105810A KR1020147018491A KR20147018491A KR20140105810A KR 20140105810 A KR20140105810 A KR 20140105810A KR 1020147018491 A KR1020147018491 A KR 1020147018491A KR 20147018491 A KR20147018491 A KR 20147018491A KR 20140105810 A KR20140105810 A KR 20140105810A
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South Korea
Prior art keywords
compound sample
silicon carbide
sample
decomposition
container
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KR1020147018491A
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Korean (ko)
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료우 마치다
히데키 호시노
타카시 수에카네
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가부시키가이샤 스미카 분세키 센터
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Publication of KR20140105810A publication Critical patent/KR20140105810A/en

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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

Abstract

The container (10) has a closed space for containing a sample of a compound of carbon or a sample of silicon carbide and a decomposition liquid for decomposing the sample, and has an outer container (1) and an inner container , And an inner vessel (6) provided in the outer vessel (1) so as not to contact the decomposition liquid on its inner wall and housing the sample. Thus, the metal impurity derived from the decomposed liquid is prevented from being mixed into the decomposed sample.

Description

TECHNICAL FIELD [0001] The present invention relates to a container, a gas phase decomposition method, a gas phase decomposition device, an analysis method and an analyzing device,

The present invention relates to a container for decomposing a compound sample or a silicon carbide compound sample composed of carbon atoms, a gas phase decomposition method and a gas phase decomposition apparatus using the container, and a method and an analysis method of a compound sample or a silicon carbide compound sample composed of decomposed carbon atoms ≪ / RTI >

As a method for analyzing impurities contained in a silicon carbide compound, a chemical analysis method of a 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 and heated and pressurized to obtain a measurement specimen liquid by dissolving silicon carbide in a mixed acid solution. Then, the metal impurities contained in the measurement sample are detected.

Non-Patent Document 1: JIS R 1616-2007 "Pressurized Acid Digestion-ICP Emission Spectroscopy"

However, according to the method described in the non-patent document 1, since the silicon carbide compound sample and the mixed acid solution are in direct contact with each other, the metal contained in the mixed acid solution is mixed into the measurement sample solution and contamination of the measurement sample solution occurs. Further, the metal attached to the inner wall of the container containing the mixed acid solution or contained as an impurity is dissolved in the mixed acid solution by contacting with the mixed acid solution, and mixed into the sample solution.

In recent years, the application of a compound comprising a carbon atom or a silicon carbide compound as a semiconductor material has come into view, and a compound or a silicon carbide compound of a higher-purity carbon atom is required. Therefore, it is necessary to more accurately analyze the metal impurities contained in the compound made of carbon atoms or the silicon carbide compound, so that there is a problem of incorporation of a trace amount of metal at the time of analysis which has not been a problem in the past.

SUMMARY OF THE INVENTION The present invention has been made in view of the above problems and has as its object to provide a carbon compound It is an object of the present invention to provide a container for decomposing a sample or a silicon carbide compound sample, a gas phase decomposition method and a gas phase decomposition apparatus using the same, and a method for analyzing and analyzing a compound sample or a silicon carbide compound sample composed of decomposed carbon atoms .

In order to solve the above problems, a container according to the present invention is a container for decomposing a compound sample made of carbon atoms or a silicon carbide compound sample, and a decomposition liquid for decomposing a compound sample composed of the carbon atoms or a silicon carbide compound sample An outer container having an inner space having a closed space for accommodating the carbon atoms and having a pressure resistance against the pressure for decomposing the compound sample or the silicon carbide compound sample made of the carbon atoms; And an inner vessel which is formed of a material which is composed of a carbonaceous material and is made of a material which is composed of a carbonaceous material, Characterized in that the decomposition liquid is provided so as not to contact do.

The gas phase decomposition method according to the present invention is characterized in that a decomposition liquid for decomposing a compound sample made of carbon atoms or a silicon carbide compound sample is contained in the outer container of the aforementioned container and a compound sample or a silicon carbide compound sample made of carbon atoms is placed on the table And a step of pressurizing the compound sample or the silicon carbide compound sample containing carbon atoms by heating the inside of the outer container containing the decomposition solution and the compound sample or the silicon carbide compound sample containing the decomposition solution, And a decomposition step of decomposing by decomposition liquid gas.

A method of analyzing a compound sample or a silicon carbide compound sample made of a carbon atom according to the present invention is a method of detecting a metal impurity in a measurement sample obtained by decomposing a compound sample or a silicon carbide compound sample made of carbon atoms by the above- .

The gas phase decomposition apparatus of the carbon atomic compound sample or the silicon carbide compound sample according to the present invention is characterized by comprising the above-mentioned vessel and a heating means for heating the vessel.

The apparatus for analyzing a compound sample or a silicon carbide compound sample comprising a carbon atom according to the present invention is characterized in that a metal impurity in a sample to be measured obtained by gas phase decomposition of a sample of a compound made of carbon atoms or a sample of a silicon carbide compound in the above- And a detection means for detecting the position of the object.

A container for decomposing a compound sample or a silicon carbide compound sample made of a carbon atom according to the present invention has a closed space for accommodating a decomposition solution for decomposing a compound sample or a silicon carbide compound sample composed of the carbon atoms, An outer container which is pressure resistant to a pressure for decomposing the sample or the silicon carbide compound sample; and an outer container which is provided in the outer container and which is formed of a material which is content with respect to the decomposition liquid, Wherein the inner container is provided such that when the decomposition liquid is accommodated in the outer container, the decomposition liquid does not contact the inner wall of the inner container, a sample of the decomposed carbon atom or Silicon carbide compound It is possible to prevent metal impurities derived from the decomposed liquid from being mixed into the sample and to more accurately analyze the metal impurities in the compound sample or the silicon carbide compound sample made of carbon atoms.

1 is a cross-sectional view showing a container for decomposing a compound sample or a silicon carbide compound sample composed of carbon atoms according to an embodiment of the invention.

[Container (10)]

Hereinafter, one embodiment of the container according to the present invention will be described in detail with reference to Fig. 1 is a cross-sectional view showing a container for decomposing a compound sample or a silicon carbide compound sample made of carbon atoms according to an embodiment of the present invention.

Here, a compound sample composed of carbon atoms is a compound sample containing only carbon atoms. Examples of the compound sample made of carbon atoms include diamond, graphite, graphene, amorphous carbon, diamond like carbon, tetrahedral amorphous carbon, carbon nanotube , Carbon nanocoils, carbon fibers, carbon, and the like. The silicon carbide compound sample means a silicon carbide-based sample including SiC, SiOC, SiCN and the like. In the present embodiment, a form using a silicon carbide compound sample will be described as an example.

As shown in Fig. 1, the container 10 includes an outer container 1 and an inner container 6. As shown in Fig. The vessel 10 is used for decomposing the silicon carbide compound sample 7. In the present embodiment, the container 10 may further include a support portion 4 provided with a table (placement table) 5 on which the internal container 6 is placed.

(Outer container 1)

The outer vessel (1) has a closed space for accommodating therein a decomposition liquid (8) for decomposing the silicon carbide compound sample (7) and the silicon carbide compound sample (7). The outer container 1 is pressure resistant against the pressure applied to decompose the silicon carbide compound sample 7 contained therein. It is preferable that the outer container 1 is heat-resistant to the heat applied to decompose the silicon carbide compound sample 7 contained therein.

Here, the pressure resistance against the pressure applied to decompose the silicon carbide compound sample 7 means that it is difficult to expand or soften when pressure is applied to decompose the silicon carbide compound sample 7, And does not deform. The heat resistance against the heat applied to decompose the silicon carbide compound sample 7 means that it is difficult to dissolve or soften when heated to decompose the silicon carbide compound sample 7, .

<Inner cylinder (3)>

The outer vessel (1) has a double wall structure of the inner vessel (3) and the outer vessel (2) on the outer side thereof. The inner cylinder (3) is formed of a material which is in contact with the closed space and which is content with respect to the decomposition liquid (8). The inner cylinder 3 is formed of a material which is content with respect to the decomposition liquid 8 since it is in direct contact with the decomposition liquid 8 when the decomposition liquid 8 is accommodated in the closed space. It is more preferable that the content ingredient with respect to the decomposition liquid 8 means a material having little elution of the metal component with respect to the decomposition liquid 8 and is a material which does not elute the metal component with respect to the decomposition liquid 8. [

Examples of the material which is content with respect to the decomposition liquid 8 include fluorine resin, platinum or ceramics material. Examples of the fluororesin include PTFE = polytetrafluoroethylene (tetrafluoride), PFA = tetrafluoroethylene / perfluoroalkyl vinyl ether copolymer, PVDF = polyvinylidene fluoride (pentafluoride), PCTFE = And polychlorotrifluoroethylene (trifluoromethyl). Examples of the ceramics material include alumina, zirconia, calcia, magnesia, and yttria.

The shape of the inner cylinder 3 is not particularly limited and the inner cylinder 3 is not particularly limited and the inner cylinder 3 may have a closed space and the support portion 4 may be provided in the closed space to accommodate the silicon carbide compound sample 7 and the decomposition liquid 8 do. The inner cylinder 3 may be divided into two members such as a lower portion and a lid portion and the support portion 4 may be provided at the lower portion and the decomposition liquid 8 may be accommodated and the lid portion may be covered and closed as if covered from the upper portion. The thickness of the lower wall, the side wall, and the upper wall of the inner cylinder 3 is not particularly limited as long as it is a thickness that can prevent leakage of the decomposition liquid 8 contained therein and seal the inner space.

&Lt; External tub (2) &gt;

The outer cylinder (2) is located outside the inner cylinder (3) and is provided so as to surround the inner cylinder (3). The outer cylinder 2 is pressure resistant against the pressure for dissolving the silicon carbide compound sample 7. Therefore, even if the inner cylinder 3 is deformed due to the application of pressure by heating in order to decompose the silicon carbide compound sample 7 contained therein, the outer cylinder 2 is pressure resistant, Can be prevented. Further, it is preferable that the outer cylinder 2 is heat-resistant to the heat applied to dissolve the silicon carbide compound sample 7. Thus, deformation of the outer container 1 due to heat can be prevented.

The outer cylinder 2 is required to have pressure resistance and heat resistance against pressure and heat for dissolving the silicon carbide compound sample 7, and is formed of, for example, stainless steel. The outer cylinder 2 may be provided so as to enclose the inner cylinder 3 at least during pressurization and heating. That is, the outer cylinder 2 may be divided into two members, i.e., a lower portion and a lid portion, and the inner cylinder 3 may be accommodated in a lower portion thereof. The thickness of the lower wall, the side wall, and the upper wall of the outer cylinder 2 is not particularly limited as long as the desired pressure resistance and heat resistance can be obtained.

Since the inner cylinder 3 is in contact with the closed space in which the decomposition liquid 8 is accommodated and the outer cylinder 2 and the decomposition liquid 8 are not in contact with each other in the outer cylinder 1, It is possible to prevent contamination of the metal impurities resulting from the dissolution of the metal impurities into the decomposition liquid 8 and to suppress the dissolution of the metal into the decomposition liquid 8. [ On the other hand, the inner cylinder 3 may have a two-layer structure to more reliably prevent metal impurities derived from the outer cylinder 2 from leaching into the decomposition liquid 8.

(Inner container 6)

The inner vessel (6) is a columnar vessel formed of a material which is content with respect to the decomposition liquid (8) and is open at the top. The silicon carbide compound sample 7 is accommodated in the inner vessel 6 from the upper open portion. The inner vessel (6) is installed in the outer vessel (1) so that the decomposition liquid (8) does not contact the inner wall of the inner vessel (6). The inner vessel 6 is exposed to the decomposed liquid gas vaporized by the decomposition liquid 8 and therefore the inner vessel 6 is made of a material which does not dissolve the metal component to the decomposition liquid 8, As shown in Fig.

Examples of the material which is content with respect to the decomposition liquid 8 constituting the inner container 6 include fluororesin, platinum or ceramics. Examples of the fluororesin include PTFE = polytetrafluoroethylene (tetrafluoride), PFA = tetrafluoroethylene / perfluoroalkyl vinyl ether copolymer, PVDF = polyvinylidene fluoride (pentafluoride), PCTFE = And polychlorotrifluoroethylene (trifluoromethyl). Examples of the ceramics material include alumina, zirconia, calcia, magnesia, and yttria.

The inner vessel 6 is placed on the table 5 and placed on the lower side of the table 5 located above the liquid level of the decomposition liquid 8, The decomposition liquid container (not shown) containing the internal container 6 and the decomposition liquid may be placed adjacent to the table 5 and the internal container 6 may be placed on the table 5 (Not shown) containing the decomposition liquid may be placed on the upper side of the table. That is, the decomposition liquid 8 does not contact the inner wall of the inner vessel 6 and the silicon carbide compound sample 7 in the inner vessel 6 is exposed to the decomposed liquid gas vaporized by the decomposition liquid 8 . On the other hand, as the decomposition liquid container (not shown), it is possible to utilize the decomposition liquid which is formed of a material which is content with respect to the decomposition liquid and which contains the decomposition liquid from the open top.

A plurality of inner vessels 6 may be provided on the table 5, whereby it is possible to decompose a plurality of samples of silicon carbide compound 7 at the same time. The size of the inner container 6 is not particularly limited as long as the size of the contained silicon carbide compound sample 7 is sufficiently exposed to the decomposed liquid gas vaporized by the decomposition liquid 8.

(Supporting portion 4)

The support part (4) is installed in the outer container (1). The support portion 4 has a stand installed to protrude from the bottom surface of the inside of the outer container 1 and a table 5 provided on the top of the stand. The table 5 may be provided so as to be supported from below by support pins (not shown) projecting from at least two portions of the side wall of the outer container 1 (the side wall of the inner cylinder 3). In this case, the support portion 4 is constituted by the table 5 and the support pin.

The table 5 may be integrally formed with a stand or a support pin, and may be formed and assembled before use. The support portion 4 may be configured to change the height of the stand. It is preferable that the support portion 4 is formed of a soft material with respect to the decomposition liquid 8.

&Lt; Table (5) &gt;

On the table 5, the inner container 6 containing the silicon carbide compound sample 7 is placed. The diameter of the table 5 is the same as the inner diameter of the inner cylinder 3 and is set so as to be in contact with the side wall of the inner cylinder 3. [ The table 5 is a porous body provided with holes for allowing the decomposed liquid gas to pass therethrough. Therefore, the decomposition liquid 8, in which the holes provided in the table 5 are accommodated below, becomes the flow path of the decomposed liquid gas vaporized, and the decomposed liquid gas reaches the silicon carbide compound sample 7. On the other hand, the inner diameter of the table 5 may be made smaller than the inner diameter of the inner cylinder 3, and a gap may be formed between the table 5 and the inner cylinder of the inner cylinder 3. In this case, since the decomposed liquid gas flows from the clearance to reach the silicon carbide compound sample 7, it is not necessary to provide a hole in the table 5.

As described above, when the container 10 is used, the silicon carbide compound sample 7 is accommodated in the inner container 6 provided in the pressure-resistant outer container 1 accommodating the decomposition liquid 8, and the outer container 1 Is heated and pressurized, the silicon carbide compound sample 7 is vapor-phase decomposed by the decomposed liquid gas vaporized by the decomposition liquid 8. The metal impurities contained in the decomposition liquid 8 and the metal impurities attached to the inner wall of the outer container 1 (the inner wall of the inner cylinder 3) and the inner wall of the inner vessel 6 are contained in the silicon carbide compound sample 7 Can be decomposed and prevented from being incorporated into the obtained measurement specimen. As a result, if the silicon carbide compound sample 7 is decomposed using the vessel 10, a trace amount of metal contained in the silicon carbide compound sample 7 can be more accurately detected.

It is known that a compound sample composed of carbon atoms can be decomposed also under atmospheric pressure using a decomposition solution such as a mixture of sulfuric acid, nitric acid and perchloric acid (see, for example, Reference 1 (Wet Oxidative Decomposition: Graphite in Curcumin by Absorbance Spectrophotometry Determination of boron &quot;, Kazuo Watanabe et al., Analytical Chemistry, 44 (11), 939-942, 1995)). On the other hand, the silicon carbide compound sample (7) is not decomposed under atmospheric pressure even when using the same decomposition liquid. That is, when the container 10 is used, since the refractory silicon carbide compound sample 7 can be decomposed more than the compound sample made of carbon atoms, the ability to decompose a compound sample made of carbon atoms by using the container 10 Obvious.

On the other hand, the kind and amount of the decomposition liquid 8 for decomposing the silicon carbide compound sample 7 and the pressure and heat applied to the outer container 1 for decomposing the silicon carbide compound sample 7, Details of time and the like will be described later.

[Method of gas phase decomposition of a compound sample composed of carbon atoms or a sample of silicon carbide compound]

The gas phase decomposition method according to the present invention is a method for decomposing a compound sample or a silicon carbide compound sample composed of carbon atoms and a method for decomposing a compound sample or a silicon carbide compound sample made of carbon atoms into a decomposed solution gas in which a decomposition solution decomposing the sample is vaporized And a decomposition step of decomposing the decomposition product. According to the present invention, since a compound sample or a silicon carbide compound sample composed of carbon atoms is gas-phase decomposed, metal impurities contained in the decomposition solution can be prevented from being incorporated into a measurement sample obtained by decomposition of the sample.

The gas phase decomposition method according to the present invention is characterized in that before the decomposition step, a decomposition liquid for decomposing a compound sample or a silicon carbide compound sample made of carbon atoms is contained in the outer vessel (1) of the vessel (10) And a preparation step of placing a compound sample or a silicon carbide compound sample made of carbon atoms on a table (5), and in the decomposition step, it is preferable to pressurize and heat the inside of the outer container (1) containing the sample and the decomposition solution Do.

That is, the container 10 described above is one embodiment of the container used in the gas phase decomposition method according to the present invention. Therefore, the explanation of the container used in the gas phase decomposition method according to the present invention is based on the description of the container 10 described above. On the other hand, in the present embodiment, a case of using a silicon carbide compound sample will be described as an example.

(Preparation process)

In the preparation step, the decomposition liquid for decomposing the silicon carbide compound sample is first contained in the outer vessel 1 of the vessel 10, and the silicon carbide compound sample is contained in the inner vessel 6. The decomposition liquid is received so as not to contact the inner wall of the inner vessel (6). At this time, when the volume of the outer container 1 is assumed to be 100%, if the decomposed liquid is contained in an amount of 5 to 40% of the volume of the outer container 1, the silicon carbide compound sample can be efficiently decomposed Do.

The amount of the decomposition liquid contained in the outer container 1 may be an amount capable of sufficiently decomposing the silicon carbide compound sample. Therefore, for example, 2 to 20 ml of the decomposed solution may be contained per 1 g of the silicon carbide compound sample to be decomposed.

As the decomposition solution for decomposing the silicon carbide compound sample, 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 solution and perchloric acid can be used, It is a mixed acid solution of hydrofluoric acid and nitric acid.

The silicon carbide compound sample may be put on the table 5 in the inner container 6. The silicon carbide compound sample may be a bulk or a thin film. After the silicon carbide compound sample and the decomposed liquid are contained in the outer container 1, the outer container 1 is sealed.

(Decomposition step)

In the decomposition step, the inside of the sealed outer container (1) containing the silicon carbide compound sample and the decomposition liquid is heated and pressurized. Pressurization and heating in the outer container 1 can be appropriately performed by a conventionally known method.

The heating temperature of the outer container 1 may be any temperature that allows desired pressurization and vaporization of the decomposed liquid as described later, preferably 100 to 240 캜, more preferably 150 to 240 캜, and 180 Lt; 0 &gt; C to 240 &lt; 0 &gt; C. The heating time of the external container 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 1 by heating to the above-mentioned temperature is a pressure at which the silicon carbide compound sample can be decomposed by the vaporized decomposed liquid, preferably 1 to 15 MPa, more preferably 5 to 15 MPa And most preferably from 7 to 15 MPa.

When heating the outer container 1, it is preferable to heat the entire outer container 1. Particularly, when heat is applied to the upper part of the outer container 1, it is possible to prevent the droplets, which have flocculated on the upper wall (upper wall of the inner cylinder 3) in the outer vessel 1, from dropping onto the silicon carbide compound sample, .

As described above, the inside of the outer vessel 1 containing the silicon carbide compound sample and the decomposition liquid is heated and pressurized, whereby the silicon carbide compound sample is vapor-phase decomposed by the decomposed liquid gas vaporized. Therefore, the metal impurities contained in the decomposition liquid, the metal impurities adhered to the inner wall of the outer container 1 (the inner wall of the inner cylinder 3) and the inner wall of the inner vessel 6 are obtained by decomposing the silicon carbide compound sample And can be prevented from being mixed into the measurement sample. As a result, a trace amount of metal contained in the silicon carbide compound sample can be provided to the analysis for more accurate detection.

[Method for analyzing a compound sample or a silicon carbide compound sample made of carbon atoms]

A method of analyzing a compound sample or a silicon carbide compound sample made of a carbon atom according to the present invention is a method of detecting a metal impurity in a measurement sample obtained by decomposing a compound sample made of carbon atoms or a silicon carbide compound sample by the above- And a control unit.

Since the compound sample or the silicon carbide compound sample made of carbon atoms is vapor-phase decomposed by the decomposed liquid gas to sublimate, the metal impurities contained in the sample remain in the internal vessel 6 in which the sample is contained. In the present embodiment, the remaining metal impurities are detected as a measurement sample.

The metal impurities remaining in the inner container 6 may be recovered using the recovered liquid. As the recovered solution, conventionally known solutions can be used, and there is no particular limitation, and for example, nitric acid, or mixed acid of nitric acid and hydrochloric acid can be used. The recovered solution is dropped into the inner vessel 6 to dissolve the metal impurities attached to the inner wall of the inner vessel 6 and recover it. At this time, the metal impurities may be recovered by dropping the recovered solution in the inner vessel 6 and heating again. The recovered metal impurities may be returned to the solution by the recovered solution and provided for the measurement.

The recovered metal impurities are subjected to elemental analysis using a conventionally known measuring method as a measurement sample. Examples of a method for elemental analysis of a measurement sample include inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emission spectrometry (ICP-AES), and atomic absorption spectrometry (AAS).

Thus, by analyzing a measurement sample obtained by gas-phase decomposition of a compound sample made of carbon atoms or a silicon carbide compound sample, the metal impurity contained in the carbon sample or the silicon carbide sample can be more accurately detected.

[Gas phase decomposition apparatus of a compound sample made of carbon atoms or a silicon carbide compound sample]

The gas phase decomposition apparatus of the carbon atomic compound sample or the silicon carbide compound sample according to the present invention is characterized by comprising the above-mentioned vessel and a heating means for heating the vessel.

That is, 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 gas phase decomposition apparatus according to the present invention follows the description of the above-described gas phase decomposition method. On the other hand, a conventionally known heating apparatus can be used as the heating means.

[Analyzer of a compound sample made of carbon atoms or a sample of silicon carbide compound]

The apparatus for analyzing a compound sample or a silicon carbide compound sample comprising a carbon atom according to the present invention is characterized in that a metal impurity in a sample to be measured obtained by gas phase decomposition of a sample of a compound made of carbon atoms or a sample of a silicon carbide compound in the above- And a detection means for detecting the position of the object.

That is, the container 10 used in the above-described analysis method is an embodiment of the container used in the analyzing apparatus according to the present invention. Therefore, the description of the analyzing apparatus according to the present invention follows the description of the above-described analyzing method. On the other hand, a conventionally known detection device can be used as the detection means, and for example, ICP-MS manufactured by PerkinElmer can be used.

[Quality control method of a compound sample made of carbon atoms or a silicon carbide compound sample]

The method for controlling quality of a compound sample or a silicon carbide compound sample made of a carbon atom according to the present invention is a method for controlling quality of a compound sample or a silicon carbide compound sample by decomposing a compound sample made of carbon atoms or a silicon carbide compound sample by any one of the above- And an extraction step of extracting a compound sample or a silicon carbide compound sample composed of carbon atoms whose amount of metal impurities detected in the analysis step is equal to or less than a predetermined reference amount.

In the analysis step, the compound sample or the silicon carbide compound sample made of carbon atoms is decomposed by the gas phase decomposition method according to the present invention, and the remaining metal element is recovered as a metal impurity to be used as a measurement sample, Analysis is performed. Examples of a method for elemental analysis of a measurement sample include inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emission spectrometry (ICP-AES), and atomic absorption spectrometry (AAS).

Then, in the extraction step, a compound sample or a silicon carbide compound sample containing carbon atoms whose 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 composed of carbon atoms is selected based on the amount of metal impurities detected in the analysis process. On the other hand, in the extraction step, a compound sample or a silicon carbide compound sample composed of carbon atoms may be selected based on the kind of the metal impurity detected in the analysis step.

As described above, according to the quality control method of the present invention, metal impurities contained in a sample of a compound of carbon atoms or a sample of a silicon carbide compound can be accurately detected. Therefore, based on the detection result, a compound sample made of carbon atoms or a silicon carbide compound By selecting the sample, the quality of the compound sample or the silicon carbide compound sample made of 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 or a silicon carbide compound sample made of carbon atoms used for manufacturing a semiconductor, which requires more accurate quality control.

A container according to the present invention is a container for decomposing a compound sample made of carbon atoms or a silicon carbide compound sample and having a closed space for containing a decomposition liquid for decomposing a compound sample or a silicon carbide compound sample made of the above- An outer container which is pressure resistant to a pressure for decomposing a compound sample or a silicon carbide compound sample composed of the carbon atoms; and an outer container which is formed of a material which is content with respect to the decomposition liquid, And the inner container is provided so that the decomposition liquid does not contact the inner wall of the outer container when the decomposition liquid is accommodated in the outer container .

Further, in the container according to the present invention, the outer container may include an inner passage which is in contact with the closed space and is made of a material which is content with respect to the decomposition liquid, a compound sample located outside the inner cylinder, It is preferable that the double wall structure of the outer barrel is pressure resistant to the pressure for dissolving the compound sample.

In the container according to the present invention, it is preferable that the inner container is provided on a table located above the liquid level of the decomposition liquid when the decomposition liquid is contained in the outer container.

Further, it is preferable that the container according to the present invention further comprises a decomposition liquid container provided in the outer container, the decomposition liquid container being formed of a material which is content with respect to the decomposition liquid and from which the decomposition liquid is received.

The gas phase decomposition method according to the present invention is characterized in that a decomposition liquid for decomposing a compound sample made of carbon atoms or a silicon carbide compound sample is contained in the outer container of any one of the aforementioned containers and a sample of a compound made of carbon atoms A step of preparing a sample of a silicon carbide compound by heating the inner surface of the outer container containing the decomposition liquid and the compound sample or the silicon carbide compound sample containing the carbon atoms and the decomposition liquid to obtain a compound sample or a silicon carbide compound sample comprising the carbon atoms And a decomposition step of decomposing the decomposition liquid by the decomposed liquid gas vaporized.

Further, in the gas phase decomposition method according to the present invention, in the decomposition step, it is preferable to pressurize the outer container to 1 to 15 MPa by heating to 100 to 240 캜.

Further, in the gas phase decomposition method according to the present invention, the decomposition liquid is preferably 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 solution and perchloric acid.

A method of analyzing a compound sample or a silicon carbide compound sample made of a carbon atom according to the present invention is a method of analyzing a metal impurity in a measurement sample obtained by decomposing a compound sample made of carbon atoms or a silicon carbide compound sample by any one of the above- And a detecting step of detecting the detected signal.

The gas phase decomposition apparatus of the carbon atomic compound sample or the silicon carbide compound sample according to the present invention is characterized by comprising any one of the above-described vessels and a heating means for heating the vessel.

The apparatus for analyzing a compound sample or a silicon carbide compound sample made of carbon atoms according to the present invention is characterized in that the apparatus for analyzing a sample of a compound or a sample of a silicon carbide compound according to the present invention is characterized in that any one of the containers described above and the metal in the measurement specimen obtained by gas phase decomposition of the compound sample or the silicon carbide compound sample, And detecting means for detecting impurities.

The method for controlling quality of a compound sample or a silicon carbide compound sample made of a carbon atom according to the present invention is a method for controlling quality of a compound sample or a silicon carbide compound sample by decomposing a compound sample made of carbon atoms or a silicon carbide compound sample by any one of the above- And an extraction step of extracting a compound sample or a silicon carbide compound sample composed of carbon atoms whose amount of metal impurities detected in the analysis step is equal to or less than a predetermined reference amount.

[Example 1]

A blank test of gas phase decomposition using the vessel 10 was carried out. In the blank test, a treatment such as gas phase decomposition is performed using the container 10 without using a compound sample made of carbon atoms or a sample made of a silicon carbide compound, so that the metal impurities contained in the decomposed liquid and the metal impurities adhered to the inner wall of the outer container 1 The degree of incorporation of metal impurities into the measurement sample was examined.

A mixed solution of 40% hydrofluoric acid and 68% nitric acid (1: 1) was used as the decomposition solution. The inside of the inner vessel 6 was made empty and the decomposed liquid was exposed to the decomposed liquid gas vaporized. The inside of the outer vessel 1 was heated at 200 占 폚 for 5 hours to obtain a high-temperature pressurizing condition. SUS containers were used for the outer cylinder 2 and PTFE cylinders were used for the inner cylinder 3. Two internal containers 6 made of PTFE (VPD-1 and VPD-2) were placed on the table 5. The inner vessel 6 was taken out and nitric acid was dropped to collect metal impurities in the respective inner vessels 6 to prepare a measurement sample.

The measurement sample was measured by ICP-MS (manufactured by Perkin Elmer). As a result, the amount of metal impurities contained in the measurement sample was as shown in Table 1. On the other hand, the values shown in Table 1 were calculated by multiplying the concentration (ng / g) measured by ICP-MS by the liquid amount (g) adjusted by the liquid.

VPD-1 (ng) VPD-2 (ng) Na 0.01 0.03 Al 0.01 0.02 K 0.01 0.01 Ca 0.02 0.03 Cr 0.01 N.D. Fe 0.02 0.03 Ni N.D. N.D. Cu 0.01 N.D. Zu 0.01 0.01 CD N.D. N.D.

N.D .: Not detected

[Example 2]

The silicon carbide compound sample (SiC sample) was vapor-phase decomposed using the vessel 10. A mixed solution of 40% hydrofluoric acid and 68% nitric acid (1: 1) was used as the decomposition solution. A silicon carbide compound sample was placed in the inner vessel 6 to expose the decomposed liquid to the decomposed liquid gas vaporized. The inside of the outer vessel 1 was heated at 200 캜 for 5 hours to obtain a high-temperature pressurization condition. The silicon carbide compound sample in the inner vessel 6 was decomposed and sublimated.

[Example 3]

The container (10) was used to vapor-phase the certified reference material (CRM NMIJ 8001A) of silicon carbide. A mixed solution of 40% hydrogen fluoride and 68% nitric acid (1: 1) was used as the decomposition solution. And then heated at 230 DEG C for 96 hours to obtain a high-temperature pressurized condition. After the decomposition treatment, the inner vessel 6 was taken out and nitric acid was dropped to recover metal impurities in the inner vessel 6 to prepare a measurement sample.

The measurement sample was measured by ICP-MS (manufactured by Perkin Elmer). As a result, the measured values and authenticated values of the samples were as shown in Table 2. On the other hand, the values shown in Table 2 were calculated by multiplying the concentration (ng / g) measured by ICP-MS by the liquid amount (g) adjusted by the liquid and dividing by the amount of decomposed sample (g).

Measure
(/ / G) Authentication value
(/ / G) Recovery rate Al 79.3 83.2 95% Ti 5.92 6.37 93% Cr 1.86 1.98 94% Mn 0.51 0.53 97% Fe 49.1 46.7 105% Ni 1.43 1.52 94% Cu 0.42 0.47 90% Y 0.31 0.31 99%

It is to be understood that the present invention is not limited to the above-described embodiments, and that various changes can be made within the scope of the claims, and embodiments obtained by appropriately combining the technical means disclosed in the other embodiments with the technical scope .

[Industrial Availability]

The present invention can be used for analyzing metal impurities of a compound sample or a silicon carbide compound sample composed of carbon atoms used in various fields.

1 outer container
2 outer tub
3 inner tub
4 Support
5 Table (wit)
6 internal container

Claims (11)

As a container for decomposing a compound sample or a silicon carbide compound sample made of carbon atoms,
An outer container having a closed space for accommodating a decomposition liquid for decomposing a compound sample or a silicon carbide compound sample composed of the carbon atoms inside and having a pressure resistance against a pressure for decomposing a compound sample or a silicon carbide compound sample comprising the carbon atoms,
And an inner vessel which is provided in the outer vessel and is formed of a material which is content with respect to the decomposition liquid and from which the compound sample or the silicon carbide compound sample composed of the carbon atoms is received from the open top,
Wherein the inner container is provided so that when the decomposition liquid is received in the outer container, the decomposition liquid does not contact the inner wall of the inner container. The method according to claim 1,
Wherein the outer container comprises:
An internal passage formed in the enclosed space and made of a material which is content with respect to the decomposition liquid,
Wherein the inner cylinder is a double wall structure of an outer cylinder portion which is located outside the inner cylinder and is pressure resistant to a pressure for dissolving the compound sample or the silicon carbide compound sample made of the carbon atoms. 3. The method according to claim 1 or 2,
Wherein the inner container is provided on a table located above the liquid level of the decomposition liquid when the decomposition liquid is received in the outer container. 4. The method according to any one of claims 1 to 3,
Further comprising a decomposition liquid container provided in the outer container, the decomposition liquid container being formed of a material which is content with respect to the decomposition liquid and from which the decomposition liquid is received. A method for producing a carbon material, comprising the steps of accommodating, in an outer container of a container according to any one of claims 1 to 4, a decomposition liquid for decomposing a compound sample or a silicon carbide compound sample composed of carbon atoms in the outer container, A preparation step of containing a silicon compound sample,
The compound sample or the silicon carbide compound sample comprising the carbon atoms and the outer container containing the decomposition solution are heated to pressurize the sample of the compound or the sample of the silicon carbide compound by the decomposition liquid gas vaporized by the decomposition liquid And a decomposition step of decomposing the gas phase decomposition step. 6. The method of claim 5,
Wherein in the decomposition step, the inside of the outer container is pressurized to 1 to 15 MPa by heating to 100 to 240 캜. The method according to claim 5 or 6,
Wherein the decomposition liquid is 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 water and perchloric acid. A method for producing a carbon-carbon compound, which comprises a step of detecting a metal impurity in a measurement sample obtained by decomposing a compound sample or a silicon carbide compound sample composed of carbon atoms by the gas phase decomposition method according to any one of claims 5 to 7 A method for analyzing a compound sample or a silicon carbide compound sample comprising an atom. A container according to any one of claims 1 to 4,
And a heating means for heating the container. The gas phase decomposition apparatus of the carbon atom type compound sample or the silicon carbide compound sample. A container according to any one of claims 1 to 4,
And a detection means for detecting metal impurities in a measurement sample obtained by gas-phase decomposition of a compound sample or a silicon carbide compound sample made of carbon atoms in the container. 8. A gas phase decomposition method according to any one of claims 5 to 7, comprising the steps of: analyzing a metal impurity in a measurement specimen obtained by decomposing a compound sample or a silicon carbide compound sample made of carbon atoms;
Characterized by comprising an extraction step of extracting a compound sample or a silicon carbide compound sample composed of carbon atoms whose amount of metal impurities detected in the analysis step is equal to or less than a predetermined reference amount, How to manage.
KR1020147018491A 2011-12-06 2012-12-05 Container, vapor phase cracking method, vapor phase cracking device, analysis method, and analysis device KR20140105810A (en)

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