JPH11166894A - Method for analyzing carbon material - Google Patents
Method for analyzing carbon materialInfo
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- JPH11166894A JPH11166894A JP35211297A JP35211297A JPH11166894A JP H11166894 A JPH11166894 A JP H11166894A JP 35211297 A JP35211297 A JP 35211297A JP 35211297 A JP35211297 A JP 35211297A JP H11166894 A JPH11166894 A JP H11166894A
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- waveform
- derived
- peak
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は炭素材料の解析方法
に係わり、特にアモルファス相と結晶相とが混在する炭
素材料について精度の高い構造解析や材料の差別化が行
える炭素材料の解析方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for analyzing a carbon material, and more particularly, to a method for analyzing a carbon material in which an amorphous phase and a crystalline phase are mixed, with which a highly accurate structural analysis and a material differentiation can be performed.
【０００２】[0002]
【従来の技術】従来、炭素材料の解析手法としてラマン
分光法を用いることは知られている。ー般に炭素材料を
ラマン分光法で解析する場合、そのスペクトルはＧ−ｂ
ａｎｄ、Ｄ−ｂａｎｄの２本のピークから構成されると
解釈されている。例えば、結晶相のみから構成される多
結晶グラファイトのラマンスペクトルは、１３５０ｃｍ
-1近傍のＤ−ｂａｎｄと１５９０ｃｍ-1近傍のＧ−ｂａ
ｎｄに由来する、互いに重なりのない独立した２本のピ
ークとして観察される。そのＧ−ｂａｎｄ、Ｄ−ｂａｎ
ｄのピーク強度比Ｉd ／Ｉg やＧ−ｂａｎｄ、Ｄ−ｂａ
ｎｄそれぞれの波形のピーク位置、波形幅等を用いて構
造解析する手法が古くから知られている。2. Description of the Related Art Hitherto, it has been known to use Raman spectroscopy as a technique for analyzing carbon materials. Generally, when a carbon material is analyzed by Raman spectroscopy, the spectrum is Gb
It is interpreted to be composed of two peaks, and and D-band. For example, the Raman spectrum of polycrystalline graphite composed only of the crystalline phase is 1350 cm
-1 near the D-band and the 1590 cm -1 vicinity of G-ba
nd is observed as two independent peaks that do not overlap with each other. G-band, D-ban
peak intensity ratio I d / I g , G-band, D-ba
A technique for performing a structural analysis using the peak position, the waveform width, and the like of each nd waveform has been known for a long time.
【０００３】他の例として、アモルファス相のみから構
成される、ダイアモンドライクカーボンに代表されるア
モルファスカーボンのラマンスペクトルは、Ｇ−ｂａｎ
ｄとＤ−ｂａｎｄの幅が広いために２本のピークが重複
したピークとして観察される。その２本のピークをガウ
ス関数を用いて波形近似後にピーク分離し、そのＧ−ｂ
ａｎｄ、Ｄ−ｂａｎｄのピーク強度比Ｉd ／Ｉg やＧ−
ｂａｎｄ、Ｄ−ｂａｎｄそれぞれの波形のピーク位置、
波形幅等を用いて構造解析が行われている。[0003] As another example, the Raman spectrum of amorphous carbon represented by diamond-like carbon composed of only an amorphous phase is represented by G-ban.
Since the width of d and D-band is wide, two peaks are observed as overlapping peaks. The two peaks are separated into peaks after waveform approximation using a Gaussian function, and the Gb
and D-band peak intensity ratios I d / I g and G-
band, peak position of each D-band waveform,
Structural analysis is performed using a waveform width or the like.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、Ｇ−ｂ
ａｎｄ、Ｄ−ｂａｎｄの２本のみのピークから構成され
るとは、単純に解釈出来ないラマンスペクトルを有する
炭素材料が存在する。この場合、精度の高い構造解析や
材料の差別化が困難な恐れがある。本発明はこのような
従来の課題に鑑みてなされたもので、アモルファス相と
結晶相とが混在する炭素材料について精度の高い構造解
析や材料の差別化が行える炭素材料の解析方法を提供す
ることを目的とする。However, Gb
A carbon material having a Raman spectrum that cannot be simply interpreted as being composed of only two peaks, and and D-band, exists. In this case, it may be difficult to perform highly accurate structural analysis and material differentiation. The present invention has been made in view of such conventional problems, and provides a method for analyzing a carbon material in which an amorphous phase and a crystalline phase are mixed, with which high-precision structural analysis and material differentiation can be performed. With the goal.
【０００５】[0005]
【課題を解決するための手段】このため本発明（請求項
１）は、炭素材料をラマン分光法を用いて解析する方法
であって、前記炭素材料のラマンスペクトルが、アモル
ファス相に由来するＧ−ｂａｎｄのピーク、結晶相に由
来するＧ−ｂａｎｄのピーク、アモルファス相に由来す
るＤ−ｂａｎｄのピーク及び結晶相に由来するＤ−ｂａ
ｎｄのピークから構成されると解し、前記各ピークをガ
ウス関数を用いて波形近似し、予め取得若しくは定義し
た各種炭素材料の前記各相に由来する前記各ｂａｎｄの
波形の形状、波形のピーク位置、波形ピーク値、波形幅
のいずれか少なくとも一つを含むパラメータを基に前記
炭素材料の性能判別を行うことを特徴とする。SUMMARY OF THE INVENTION Therefore, the present invention (claim 1) is a method for analyzing a carbon material by using Raman spectroscopy, wherein the Raman spectrum of the carbon material is derived from an amorphous phase. -Band peak, G-band peak derived from the crystalline phase, D-band peak derived from the amorphous phase, and D-ba derived from the crystalline phase
nd is understood to be composed of peaks, the respective peaks are approximated by using a Gaussian function, and the shapes of the respective bands derived from the respective phases of various carbon materials previously obtained or defined, the peaks of the waveforms The performance of the carbon material is determined based on a parameter including at least one of a position, a waveform peak value, and a waveform width.
【０００６】ラマン分光法を用いて炭素材料を解析す
る。炭素材料はアモルファス相と結晶相とが混在すると
想定して以下の解析を行う。ラマンスペクトルは、アモ
ルファス相に由来するＧ−ｂａｎｄのピーク、結晶相に
由来するＧ−ｂａｎｄのピーク、アモルファス相に由来
するＤ−ｂａｎｄのピーク、結晶相に由来するＤ−ｂａ
ｎｄの４本のピークから構成されると解釈する。そこ
で、まず炭素材料中のアモルファス相に由来するラマン
スペクトルのＧ−ｂａｎｄのピークに対し、ガウス関数
を用いて波形近似させる。同様に、炭素材料中の結晶相
に由来するラマンスペクトルのＧ−ｂａｎｄのピークを
ガウス関数を用いて波形近似させる。また、炭素材料中
のアモルファス相に由来するラマンスペクトルのＤ−ｂ
ａｎｄのピークに対しガウス関数を用いて波形近似させ
る。更に、炭素材料中の結晶相に由来するラマンスペク
トルのＤ−ｂａｎｄのピークをガウス関数を用いて波形
近似させる。The carbon material is analyzed using Raman spectroscopy. The following analysis is performed on the assumption that the amorphous phase and the crystalline phase are mixed in the carbon material. The Raman spectrum includes a G-band peak derived from an amorphous phase, a G-band peak derived from a crystalline phase, a D-band peak derived from an amorphous phase, and a D-ba derived from a crystalline phase.
nd is interpreted to be composed of four peaks. Therefore, first, the waveform of the G-band peak of the Raman spectrum derived from the amorphous phase in the carbon material is approximated using a Gaussian function. Similarly, the waveform of the G-band peak of the Raman spectrum derived from the crystal phase in the carbon material is approximated using a Gaussian function. Further, Db of Raman spectrum derived from the amorphous phase in the carbon material
The waveform of the and peak is approximated using a Gaussian function. Further, the waveform of the D-band peak of the Raman spectrum derived from the crystal phase in the carbon material is approximated using a Gaussian function.
【０００７】その後、予め取得若しくは定義した各種炭
素材料の各相に由来する各ｂａｎｄの波形の形状、波形
の面積、波形のピーク位置、波形ピーク値、波形幅のい
ずれか少なくとも一つを含むパラメータを基に炭素材料
の性能判別を行う。波形の形状等は、予め取得した各種
炭素材料のデータを用いてもよいし、また別途定義した
データを用いてもよい。波形幅は、例えば波形の最大値
より３ｄＢ減衰した点の波形の幅とする。このことによ
り、アモルファス相と結晶相とが混在する炭素材料につ
いて精度の高い構造解析や材料の差別化が行える。Thereafter, parameters including at least one of the waveform shape, waveform area, waveform peak position, waveform peak value, and waveform width of each band derived from each phase of various carbon materials obtained or defined in advance. The performance of the carbon material is determined based on For the shape of the waveform and the like, data of various carbon materials obtained in advance may be used, or data defined separately may be used. The waveform width is, for example, the width of the waveform at a point attenuated by 3 dB from the maximum value of the waveform. This enables highly accurate structural analysis and material differentiation of a carbon material in which an amorphous phase and a crystalline phase are mixed.
【０００８】また、本発明（請求項２）は、前記炭素材
料の性能判別は、結晶相に由来するＧ−ｂａｎｄの前記
ガウス関数のピーク値に対するアモルファス相に由来す
るＧ−ｂａｎｄの前記ガウス関数のピーク値を算出し、
その比を前記炭素材料のアモルファス度とすることを特
徴とする。結晶相に由来するＧ−ｂａｎｄに対し、波形
近似したガウス関数のピーク値に対する、アモルファス
相に由来するＧ−ｂａｎｄに対し、波形近似したガウス
関数のピーク値の比は、炭素材料のアモルファス度の指
標となることが実験により確かめられた。このため、こ
の比は、アモルファス相と結晶相とが混在する炭素材料
の性能判別に重要なパラメータといえる。Further, according to the present invention (claim 2), the performance of the carbon material is determined by comparing the Gaussian function of the G-band derived from the amorphous phase with respect to the peak value of the Gaussian function of the G-band derived from the crystalline phase. Calculate the peak value of
The ratio is defined as the degree of amorphousness of the carbon material. For the G-band derived from the crystalline phase, the ratio of the peak value of the Gaussian function whose waveform is approximated to the peak value of the Gaussian function whose waveform is approximated is the ratio of the peak value of the Gaussian function whose waveform is approximated to the amorphousness of the carbon material. It was confirmed by experiments that it could be an index. Therefore, this ratio is an important parameter for determining the performance of a carbon material in which an amorphous phase and a crystalline phase are mixed.
【０００９】[0009]
【発明の実施の形態】以下、本発明の実施形態について
説明する。炭素材料をラマン分光法を用いて解析する。
炭素材料は、アモルファス相と結晶相とが混在したもの
を対象とする。このときのラマンスペクトルは、アモル
ファス相に由来するＧ−ｂａｎｄのピーク、結晶相に由
来するＧ−ｂａｎｄのピーク、アモルファス相に由来す
るＤ−ｂａｎｄのピーク及び結晶相に由来するＤ−ｂａ
ｎｄのピークの合計４本のピークから構成されていると
解釈する。各ｂａｎｄのピーク位置は、予め想定してお
く。例えば、１６００ｃｍ-1近傍の２つのピークのうち
波形の比較的シャープな方が結晶相のＧ−ｂａｎｄ，波
形のブロードな方がアモルファス相のＧ−ｂａｎｄに由
来するものとし、１３５０ｃｍ-1近傍の２つのピークの
うち波形の比較的シャープな方が結晶相のＤ−ｂａｎ
ｄ，波形のブロードな方がアモルファス相のＤ−ｂａｎ
ｄに由来するものとする。Embodiments of the present invention will be described below. The carbon material is analyzed using Raman spectroscopy.
The target of the carbon material is a mixture of an amorphous phase and a crystalline phase. The Raman spectrum at this time includes a G-band peak derived from an amorphous phase, a G-band peak derived from a crystalline phase, a D-band peak derived from an amorphous phase, and a D-ba derived from a crystalline phase.
It is interpreted that the peak is composed of a total of four peaks of the nd peak. The peak position of each band is assumed in advance. For example, 1600 cm -1 relatively sharp towards the waveforms of the two peaks in the vicinity of and shall G-band of the crystal phase, is more broad waveform derived from G-band of the amorphous phase, 1350 cm -1 vicinity of The relatively sharp waveform of the two peaks is the D-ban of the crystal phase.
d, broader waveform is amorphous phase D-ban
d.
【００１０】これらの各ｂａｎｄに対して、ガウス関数
を用いてそれぞれカーブフィッティングさせる。このと
き、４本のガウス関数を合成した波形とラマンスペクト
ル間の誤差が極力小さくなるように各ガウス関数を調整
する。得られた各ガウス関数は分離して解析する。これ
らの各ガウス関数は炭素材料の特徴を顕著に表すものに
なっている。この特徴は、各ｂａｎｄの波形の形状、波
形の面積、波形のピーク位置、波形ピーク値、波形幅等
により判断出来る。結晶相のＧ−ｂａｎｄは波形のピー
ク位置が１６００〜１６２０ｃｍ-1、波形幅が３０〜５
０ｃｍ-1となり、アモルファス相のＧ−ｂａｎｄは波形
のピーク位置が１５３０〜１５９０ｃｍ-1、波形幅が８
０〜１２０ｃｍ-1となる。また、結晶相のＤ−ｂａｎｄ
は波形のピーク位置が１３４０〜１３６０ｃｍ-1、波形
幅が５０〜１００ｃｍ-1となり、アモルファス相のＤ−
ｂａｎｄは波形のピーク位置が１２３０〜１３７０ｃｍ
-1、波形幅が１７０〜２９０ｃｍ-1となる。また、これ
らの中で、結晶相に由来するＧ−ｂａｎｄのピーク値
（以下、Ｉg（ｇｒａｐｈｉｔｅ）と略す））に対する
アモルファス相に由来するＧ−ｂａｎｄのピーク値（以
下、Ｉg （ａ−ｃ）と略す））は、特にその炭素材料の
アモルファス度の指標と考えられ、炭素材料の性能判別
に重要なパラメータと考えられる。Each of these bands is curve-fitted using a Gaussian function. At this time, each Gaussian function is adjusted so that the error between the waveform obtained by combining the four Gaussian functions and the Raman spectrum is minimized. Each obtained Gaussian function is analyzed separately. Each of these Gaussian functions remarkably represents the characteristics of the carbon material. This feature can be determined by the shape of the waveform of each band, the area of the waveform, the peak position of the waveform, the waveform peak value, the waveform width, and the like. The G-band of the crystal phase has a waveform peak position of 1600 to 1620 cm -1 and a waveform width of 30 to 5
0 cm −1 , and the G-band of the amorphous phase has a waveform peak position of 1530 to 1590 cm −1 and a waveform width of 8
It becomes 0 to 120 cm -1 . Also, the D-band of the crystal phase
Indicates that the peak position of the waveform is 1340-1360 cm -1 , the waveform width is 50-100 cm -1 , and the amorphous phase D-
In the band, the peak position of the waveform is 1300 to 1370 cm.
-1 and a waveform width of 170 to 290 cm -1 . Further, among these, the peak value of the G-band derived from the crystalline phase (hereinafter, I g (graphite) and abbreviated) peak value of G-band derived from amorphous phase to) (hereinafter, I g (a- c)) is considered to be an index of the degree of amorphousness of the carbon material, and is an important parameter for determining the performance of the carbon material.
【００１１】[0011]
【実施例】以下、本発明の実施例、比較例を説明する。
図１は本発明の基本的な解析例として、市販の活性炭
（クラレ製ＢＰ−２０）のラマンスペクトルとそのカー
ブフィッティング解析結果を示している。波形１は実測
されたスペクトル、波形２はフィッティング曲線、波形
３はベースライン直線である。波形４〜波形７は４本の
ガウス関数として分離されたピークである。波形８は実
測スペクトルとフィッティグ曲線との差である。波形８
からもわかるように、全ての周波数において精度良くフ
ィッティティングされ、最小二乗法における誤差は１８
３．０であった。この解析結果から、この炭素材料はア
モルファス相と結晶相とが混在する炭素材料であり、波
形４〜波形７のピーク位置とピーク幅から、波形４はア
モルファス相由来のＤ−ｂａｎｄ、波形５は結晶相由来
のＤ−ｂａｎｄ、波形６はアモルファス相由来のＧ−ｂ
ａｎｄ、波形７は結晶相由来のＧ−ｂａｎｄと解釈され
る。この様にアモルファス相と結晶相とが混在する炭素
材料は、その他にクラレ製ＹＰ−１７、関西熱化学製Ｈ
５００、５０１、５０２、５０３、５５０、５５１、５
５２、三菱化学製Ｃ−３、Ｃ−４、Ｃ−５、Ｅ−１、鐘
紡製ＰＡＳなど多数が挙げられいずれも誤差が少なく解
析された。Examples Examples of the present invention and comparative examples will be described below.
FIG. 1 shows, as a basic analysis example of the present invention, a Raman spectrum of a commercially available activated carbon (BP-20 manufactured by Kuraray) and a curve fitting analysis result thereof. Waveform 1 is an actually measured spectrum, waveform 2 is a fitting curve, and waveform 3 is a baseline straight line. Waveforms 4 to 7 are peaks separated as four Gaussian functions. Waveform 8 is the difference between the measured spectrum and the fitting curve. Waveform 8
As can be seen from FIG. 11, fitting is performed accurately at all frequencies, and the error in the least square method is 18
3.0. From this analysis result, this carbon material is a carbon material in which an amorphous phase and a crystalline phase are mixed. From the peak positions and peak widths of waveforms 4 to 7, waveform 4 is D-band derived from the amorphous phase, and waveform 5 is D-band derived from the crystalline phase, waveform 6 is Gb derived from the amorphous phase
and, waveform 7 are interpreted as G-band derived from the crystalline phase. The carbon material in which the amorphous phase and the crystalline phase are mixed as described above is also available from Kuraray YP-17 and Kansai Thermochemical H
500, 501, 502, 503, 550, 551, 5
52, Mitsubishi Chemical C-3, C-4, C-5, E-1, Kanebo PAS, and many others, all of which were analyzed with little error.
【００１２】次に、比較例を用いて本発明の手法の有効
性について説明する。図２は、図１の実測スペクトル
を、従来の手法と同様に２本のＧ−ｂａｎｄ、Ｄ−ｂａ
ｎｄから構成されるとしてＧ−ｂａｎｄをガウス関数、
Ｄ−ｂａｎｄをローレンツ関数としてフィッティングを
行い、解析した結果である。最小二乗法における誤差は
３２８８．４と大きく、精度良く解析されなかった。Ｇ
−ｂａｎｄ、Ｄ−ｂａｎｄを他のモデル関数、例えば共
にガウス関数を用いて解析を行った場合の誤差は９７８
１．３６、共にローレンツ関数を用いた場合は４５１
２．３となり、フィッティング精度は改善されなかっ
た。Next, the effectiveness of the method of the present invention will be described using comparative examples. FIG. 2 shows the measured spectrum of FIG. 1 as two G-bands and D-ba
and G-band as a Gaussian function,
It is a result of performing fitting and analysis using D-band as a Lorentz function. The error in the least squares method was as large as 3288.4, and was not analyzed accurately. G
When the -band and D-band are analyzed using another model function, for example, a Gaussian function, the error is 978.
1.36, 451 when both use the Lorentz function
2.3, and the fitting accuracy was not improved.
【００１３】次に、活性炭の性能判別の一例を説明す
る。市販の各種活性炭について、アモルファス相由来の
Ｄ−ｂａｎｄ、結晶相由来のＤ−ｂａｎｄ、アモルファ
ス相由来のＧ−ｂａｎｄ、結晶相由来のＧ−ｂａｎｄの
各々について、そのピーク値をＩd （ａ−ｃ）、Ｉd
（ｇｒａｐｈｉｔｅ）、Ｉg （ａ−ｃ）、Ｉg （ｇｒａ
ｐｈｉｔｅ）とする。そして、結晶相におけるＤ−ｂａ
ｎｄ、Ｇ−ｂａｎｄのピーク値比Ｉd （ｇｒａｐｈｉｔ
ｅ）／Ｉg （ｇｒａｐｈｉｔｅ）、アモルファス相にお
けるＤ−ｂａｎｄ、Ｇ−ｂａｎｄのピーク値比Ｉd （ａ
−ｃ）／Ｉg （ａ−ｃ）、および結晶相由来のＧ−ｂａ
ｎｄピーク値に対するアモルファス相由来のＧ−ｂａｎ
ｄピーク値比Ｉg （ａ−ｃ）／Ｉg （ｇｒａｐｈｉｔ
ｅ）を求めた。Next, an example of determining the performance of activated carbon will be described. Regarding various types of commercially available activated carbon, the peak value of each of D-band derived from an amorphous phase, D-band derived from a crystalline phase, G-band derived from an amorphous phase, and G-band derived from a crystalline phase is represented by I d (a- c), I d
(Graphite), I g (a -c), I g (gra
phi). And D-ba in the crystal phase
nd, G-band peak value ratio I d (graphit
e) / I g (graphite), D-band and G-band peak value ratio I d (a
-C) / I g (ac), and G-ba derived from the crystalline phase
G-ban derived from amorphous phase for nd peak value
d Peak value ratio I g (ac) / I g (graphit
e) was determined.
【００１４】各活性炭を電気二重層キャパシタの分極性
電極として用いたときの、電極面積あたりの容量密度Ｃ
（μＦ／ｍ2 ）と容量変化率△ＰＡＳ（％）を調べた。
図３にＩg （ａ−ｃ）／Ｉg （ｇｒａｐｈｉｔｅ）に対
する電極面積あたりの容量密度Ｃ（μＦ／ｍ2 ）の関係
を示し、また、図４にＩg （ａ−ｃ）／Ｉg （ｇｒａｐ
ｈｉｔｅ）に対する容量変化率△ＰＡＳ（％）の関係を
示す。図３、図４に示すとおり、特にＩg （ａ−ｃ）／
Ｉg （ｇｒａｐｈｉｔｅ）とＣ，△ＰＡＳとの相関が良
いことが判明した。Ｉg （ａ−ｃ）／Ｉg （ｇｒａｐｈ
ｉｔｅ）はその活性炭のアモルファス度の指標と考えら
れ、活性炭の性能判別に重要なパラメータとなることが
わかった。なお、透過型電子顕微鏡による構造解析や、
電子エネルギー損失分光法による解析結果との整合性も
確認した。すなわち、Ｉg （ａ−ｃ）／Ｉg （ｇｒａｐ
ｈｉｔｅ）が大きくアモルファス度が高いほど、グラフ
ァイト構造の（００１）面の乱れが大きくなり、かつ電
子エネルギー損失スペクトルのπ* ピークが不明瞭にな
ってゆく。When each activated carbon is used as a polarizable electrode of an electric double layer capacitor, the capacitance density per electrode area C
(ΜF / m 2 ) and capacitance change rate ΔPAS (%) were examined.
Figure 3 shows the relationship between I g (a-c) / I g capacity per electrode area for (graphite) Density C (μF / m 2), also in FIG. 4 I g (a-c) / I g (Graph
3 shows the relationship between the capacity change rate ΔPAS (%) and the capacity change rate (%). As shown in FIGS. 3 and 4, in particular, I g (ac) /
It was found that the correlation between I g (graphite) and C, ΔPAS was good. I g (ac) / I g (graph
item) is considered to be an index of the amorphousness of the activated carbon, and was found to be an important parameter for determining the performance of the activated carbon. In addition, structural analysis using a transmission electron microscope,
Consistency with the analysis results by electron energy loss spectroscopy was also confirmed. That is, I g (ac) / I g (graph
(h) and the degree of amorphousness, the disorder of the (001) plane of the graphite structure increases, and the π * peak of the electron energy loss spectrum becomes less clear.
【００１５】[0015]
【発明の効果】以上説明したように本発明によれば、炭
素材料のラマンスペクトルを、アモルファス相又は結晶
相のＧ−ｂａｎｄ又はＤ−ｂａｎｄに則したガウス関数
を用いて波形近似し、この波形を基に炭素材料の性能判
別を行うこととしたので、アモルファス相と結晶相とが
混在する炭素材料について精度の高い構造解析や材料の
差別化が行える。特に、結晶相に由来するＧ−ｂａｎｄ
のガウス関数のピーク値に対するアモルファス相に由来
するＧ−ｂａｎｄのガウス関数のピーク値の比は、炭素
材料のアモルファス度の指標とすることが出来、炭素材
料の性能判別の重要なパラメータである。As described above, according to the present invention, the Raman spectrum of a carbon material is approximated by using a Gaussian function conforming to the G-band or D-band of an amorphous phase or a crystalline phase, and this waveform is approximated. Since the performance of the carbon material is determined based on the above, it is possible to perform highly accurate structural analysis and material differentiation of the carbon material in which the amorphous phase and the crystalline phase are mixed. In particular, G-band derived from the crystal phase
The ratio of the peak value of the G-band Gaussian function derived from the amorphous phase to the peak value of the Gaussian function can be used as an index of the degree of amorphousness of the carbon material, and is an important parameter for determining the performance of the carbon material.
【００１６】[0016]
【図１】 ラマンスペクトルとカーブフィッティング解
析結果を示す図FIG. 1 is a diagram showing Raman spectra and curve fitting analysis results.
【図２】 従来の手法と同様に２本のＧ−ｂａｎｄ、Ｄ
−ｂａｎｄのピークについて、Ｇ−ｂａｎｄをガウス関
数、Ｄ−ｂａｎｄをローレンツ関数としてフィッティン
グした結果を示す図FIG. 2 shows two G-bands and D in the same manner as in the conventional method.
The figure which shows the result of fitting about G-band as a Gaussian function and D-band as a Lorentz function about the peak of -band.
【図３】 Ｉg （ａ−ｃ）／Ｉg （ｇｒａｐｈｉｔｅ）
に対する電極面積あたりの容量密度Ｃ（μＦ／ｍ2 ）の
関係を示す図FIG. 3. I g (ac) / I g (graphite)
Showing the relationship between the capacitance density C (μF / m 2 ) per electrode area and
【図４】 Ｉg （ａ−ｃ）／Ｉg （ｇｒａｐｈｉｔｅ）
に対する容量変化率△ＰＡＳ（％）の関係を示す図FIG. 4 I g (ac) / I g (graphite)
Showing the relationship between the rate of change of capacity △ PAS (%) with respect to temperature
１ 実測されたスペクトル ２ フィッティング曲線 ３ ベースライン直線 ４ アモルファス相由来のＤ−ｂａｎｄ ５ 結晶相由来のＤ−ｂａｎｄ ６ アモルファス相由来のＧ−ｂａｎｄ ７ 結晶相由来のＧ−ｂａｎｄ ８ 実測スペクトルとフィッティグ曲線との差 1 Measured spectrum 2 Fitting curve 3 Baseline straight line 4 D-band derived from amorphous phase 5 D-band derived from crystalline phase 6 G-band derived from amorphous phase 7 G-band derived from crystalline phase 8 Actual measured spectrum and fitting curve Difference with
Claims (2)
る方法であって、前記炭素材料のラマンスペクトルが、
アモルファス相に由来するＧ−ｂａｎｄのピーク、結晶
相に由来するＧ−ｂａｎｄのピーク、アモルファス相に
由来するＤ−ｂａｎｄのピーク及び結晶相に由来するＤ
−ｂａｎｄのピークから構成されると解し、前記各ピー
クをガウス関数を用いて波形近似し、予め取得若しくは
定義した各種炭素材料の前記各相に由来する前記各ｂａ
ｎｄの波形の形状、波形のピーク位置、波形ピーク値、
波形幅のいずれか少なくとも一つを含むパラメータを基
に前記炭素材料の性能判別を行うことを特徴とする炭素
材料の解析方法。1. A method for analyzing a carbon material using Raman spectroscopy, wherein the Raman spectrum of the carbon material is:
G-band peak derived from the amorphous phase, G-band peak derived from the crystalline phase, D-band peak derived from the amorphous phase, and D derived from the crystalline phase
-Band is understood to be composed of peaks, and the respective peaks are approximated in waveform using a Gaussian function, and the respective ba derived from the respective phases of various carbon materials previously obtained or defined.
nd waveform shape, waveform peak position, waveform peak value,
A method for analyzing a carbon material, comprising determining the performance of the carbon material based on a parameter including at least one of the waveform widths.
来するＧ−ｂａｎｄの前記ガウス関数のピーク値に対す
るアモルファス相に由来するＧ−ｂａｎｄの前記ガウス
関数のピーク値を算出し、その比を前記炭素材料のアモ
ルファス度とすることを特徴とする請求項１記載の炭素
材料の解析方法。2. The performance discrimination of the carbon material is performed by calculating a peak value of the Gaussian function of G-band derived from the amorphous phase with respect to a peak value of the Gaussian function of G-band derived from the crystalline phase, and calculating a ratio thereof. 2. The method for analyzing a carbon material according to claim 1, wherein is set to the degree of amorphousness of the carbon material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35211297A JPH11166894A (en) | 1997-12-05 | 1997-12-05 | Method for analyzing carbon material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35211297A JPH11166894A (en) | 1997-12-05 | 1997-12-05 | Method for analyzing carbon material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH11166894A true JPH11166894A (en) | 1999-06-22 |
Family
ID=18421865
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP35211297A Pending JPH11166894A (en) | 1997-12-05 | 1997-12-05 | Method for analyzing carbon material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH11166894A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008116268A (en) * | 2006-11-02 | 2008-05-22 | Honda Motor Co Ltd | Device and method for estimating hardness of dlc film |
| JP2009113252A (en) * | 2007-11-02 | 2009-05-28 | Tokyo Metropolitan Industrial Technology Research Institute | Minute molding die material consisting of vitreous carbon material, method for manufacturing the same and minute molding die made with the same |
| JP2011204901A (en) * | 2010-03-25 | 2011-10-13 | Asahi Kasei Corp | Negative electrode material for nonaqueous lithium type energy storage element, and nonaqueous lithium type energy storage element using the same |
| JP2014038032A (en) * | 2012-08-16 | 2014-02-27 | National Institute Of Advanced Industrial & Technology | Microspectrographic simulation method |
| JP2015519579A (en) * | 2012-06-15 | 2015-07-09 | デ ビアーズ センテナリー アーゲー | Infrared analysis of diamond |
| KR20170047709A (en) * | 2015-10-23 | 2017-05-08 | 주식회사 엘지화학 | Evaluation method for electrical conductivity of conductive polymer composition comprising cnt |
| WO2020137849A1 (en) | 2018-12-28 | 2020-07-02 | 株式会社クラレ | Porous carbon material and production method therefor and use thereof |
-
1997
- 1997-12-05 JP JP35211297A patent/JPH11166894A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008116268A (en) * | 2006-11-02 | 2008-05-22 | Honda Motor Co Ltd | Device and method for estimating hardness of dlc film |
| JP2009113252A (en) * | 2007-11-02 | 2009-05-28 | Tokyo Metropolitan Industrial Technology Research Institute | Minute molding die material consisting of vitreous carbon material, method for manufacturing the same and minute molding die made with the same |
| JP2011204901A (en) * | 2010-03-25 | 2011-10-13 | Asahi Kasei Corp | Negative electrode material for nonaqueous lithium type energy storage element, and nonaqueous lithium type energy storage element using the same |
| JP2015519579A (en) * | 2012-06-15 | 2015-07-09 | デ ビアーズ センテナリー アーゲー | Infrared analysis of diamond |
| JP2014038032A (en) * | 2012-08-16 | 2014-02-27 | National Institute Of Advanced Industrial & Technology | Microspectrographic simulation method |
| KR20170047709A (en) * | 2015-10-23 | 2017-05-08 | 주식회사 엘지화학 | Evaluation method for electrical conductivity of conductive polymer composition comprising cnt |
| WO2020137849A1 (en) | 2018-12-28 | 2020-07-02 | 株式会社クラレ | Porous carbon material and production method therefor and use thereof |
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