JP2004193562A - Electric double layer capacitor - Google Patents
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- JP2004193562A JP2004193562A JP2003343835A JP2003343835A JP2004193562A JP 2004193562 A JP2004193562 A JP 2004193562A JP 2003343835 A JP2003343835 A JP 2003343835A JP 2003343835 A JP2003343835 A JP 2003343835A JP 2004193562 A JP2004193562 A JP 2004193562A
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Abstract
Description
本発明は電気二重層コンデンサに用いる集電箔に関する。 The present invention relates to a current collector foil used for an electric double layer capacitor.
従来、電気二重層コンデンサに相当する電気二重層キャパシタ、特にそれの集電箔（アルミニウム箔）のアルミニウム純度に注目した発明が知られている（例えば、特許文献１。）。
特許文献１の請求項１第４行〜第５行に「・・・前記アルミニウム箔の純度が、９９．９９％以上であり・・・」と記載され、同請求項２第１行〜第２行に「前記アルミニウム箔は、銅の含有量が１５０ｐｐｍ以下である・・・」と記載されている。 Claims 1 to 4 to 5 of Patent Document 1 state that "... the purity of the aluminum foil is 99.99% or more ...". The second line states that "the aluminum foil has a copper content of 150 ppm or less ...".
周知の通り、アルミニウムの製造では、ボーキサイトを出発原料とし、先ずアルミナを造り、このアルミナを電解炉により普通純度（アルミニウム純度９０．０〜９９．８５）のアルミニウム地金に精錬する。
されに必要なら三相電解法や偏析法により、普通純度地金を高純度（アルミニウム純度９９．９９％以上）に二次精錬する。
As is well known, in the production of aluminum, bauxite is used as a starting material, alumina is first produced, and this alumina is refined by an electrolytic furnace into aluminum ingot of normal purity (aluminum purity 90.0 to 99.85).
If necessary, the secondary metal is refined to a high purity (aluminum purity of 99.99% or more) by three-phase electrolysis or segregation.
特許文献１でのアルミニウム箔は９９．９９％であるから高純度アルミニウムである。純度を上げるには精錬を繰り返すため、高純度であればあるほど製造コストが嵩む。そのため、普通純度アルミニウムに比べ高純度アルミニウムは高価になる。
電気二重層コンデンサの主要部材であるアルミニウム箔が高価であれば、電気二重層コンデンサは必然的に高価になる。
Since the aluminum foil in Patent Document 1 has 99.99%, it is high-purity aluminum. Since refining is repeated to increase the purity, the higher the purity, the higher the production cost. Therefore, high-purity aluminum is more expensive than normal-purity aluminum.
If the aluminum foil, which is the main component of the electric double layer capacitor, is expensive, the electric double layer capacitor is necessarily expensive.
本発明は、電気二重層コンデンサにおいて、材料費を低減することができる技術を提供することを課題とする。 An object of the present invention is to provide a technique capable of reducing material costs in an electric double layer capacitor.
本発明者らは、電気二重層コンデンサの価格を下げるべく研究を進めるなかで、今まで常識とされてきた高純度アルミニウム箔を見直すことにした。多数の試作と評価を重ねた結果、Ｃｕなどアルミニウム以外の合金の含有量を管理することにより、普通純度のアルミニウム箔が使用可能であることを見出した。 The present inventors have decided to review high-purity aluminum foil, which has been regarded as common knowledge until now, while conducting research to reduce the price of the electric double layer capacitor. As a result of repeated trials and evaluations of a large number of prototypes, it was found that by controlling the content of alloys other than aluminum such as Cu, aluminum foil of normal purity can be used.
すなわち、請求項１は、一対の集電箔に各々活性炭を主体とした電極物質を貼り付けることで正極電極及び負極電極を造り、これらの正負極電極間にセパレータを介在させると共に電解液を介在させ、前記一対の集電箔を通じて充電及び放電を行うことのできる電気二重層コンデンサにおいて、
電極物質を貼り付ける段階での前記集電箔は、以下の条件を満足するものを用いたことを特徴とする電気二重層コンデンサ。
・集電箔は、Ｃｕ、Ｎｉ、Ｚｎ、Ｓｎ、Ｆｅの少なくとも１種を含み、アルミニウムが９９．８％以下の普通純度のアルミニウム箔を素材として、これにエッチング処理を施してあること。
・電極物質を貼り付ける直前に計測したＣｕ、Ｎｉ、Ｚｎ、Ｓｎの含有量が、いずれも１０ｐｐｍ以下であること。
・電極物質を貼り付ける直前に計測したＦｅの含有量が、３００ｐｐｍ以下であること。
That is, claim 1 forms a positive electrode and a negative electrode by attaching an electrode material mainly composed of activated carbon to a pair of current collecting foils, and a separator is interposed between the positive and negative electrodes and an electrolytic solution is interposed. In the electric double layer capacitor capable of performing charging and discharging through the pair of current collector foils,
An electric double layer capacitor, wherein the current collector foil used in the step of attaching an electrode material satisfies the following conditions.
-The current collector foil contains at least one of Cu, Ni, Zn, Sn, and Fe, and has been subjected to an etching treatment using a normal-purity aluminum foil containing 99.8% or less of aluminum.
-The content of Cu, Ni, Zn, and Sn measured immediately before the electrode material is attached is 10 ppm or less in all cases.
The Fe content measured immediately before the electrode material is attached is 300 ppm or less.
Ｃｕ、Ｎｉ、Ｚｎ、Ｓｎの含有量がいずれも１０ｐｐｍ以下であり、Ｆｅの含有量が３００ｐｐｍ以下であれば、９９．８％以下の普通純度のアルミニウム箔の使用が可能となる。 When the contents of Cu, Ni, Zn, and Sn are all 10 ppm or less and the content of Fe is 300 ppm or less, it is possible to use aluminum foil having a normal purity of 99.8% or less.
普通純度のアルミニウム箔が使用できれば、電気二重層コンデンサの材料費を下げることができる。あわせて、高純度化するために三相電解法では莫大な電気エネルギーを消費するが、請求項１によればそれが不要となり、貴重な地球エネルギー資源の節約を達成することができる。 If ordinary purity aluminum foil can be used, the material cost of the electric double layer capacitor can be reduced. At the same time, the three-phase electrolysis method consumes enormous amount of electric energy to achieve high purity. However, according to the first aspect, it is unnecessary, and valuable earth energy resources can be saved.
請求項１によれば、Ｃｕ、Ｎｉ、Ｚｎ、Ｓｎの含有量がいずれも１０ｐｐｍ以下であり、Ｆｅの含有量が３００ｐｐｍ以下であれば、９９．８％以下の普通純度のアルミニウム箔の使用が可能となる。 According to claim 1, if the content of Cu, Ni, Zn, and Sn is 10 ppm or less, and the content of Fe is 300 ppm or less, use of aluminum foil of normal purity of 99.8% or less can be used. It becomes possible.
普通純度のアルミニウム箔が使用できれば、電気二重層コンデンサの材料費を下げることができる。あわせて、高純度化するために三相電解法では莫大な電気エネルギーを消費するが、請求項１によればそれが不要となり、貴重な地球エネルギー資源の節約を達成することができる。 If ordinary purity aluminum foil can be used, the material cost of the electric double layer capacitor can be reduced. At the same time, the three-phase electrolysis method consumes enormous amount of electric energy to achieve high purity. However, according to the first aspect, it is unnecessary, and valuable earth energy resources can be saved.
発明を実施するための最良の形態を添付図に基づいて以下に説明する。
図１は本発明に係る電気二重層コンデンサの斜視図であり、電気二重層コンデンサ１０は、帯状の正極電極１１と帯状の負極電極１２とをセパレータ１３を介して積層し、密に巻き、容器１４に収納してなる円筒型電気二重層コンデンサである。
１５は封止板、１６は正極端子、１７は負極端子、１８は電解液を注入するための注液口である。
The best mode for carrying out the invention will be described below with reference to the accompanying drawings.
FIG. 1 is a perspective view of an electric double-layer capacitor according to the present invention. An electric double-
図２は電気二重層コンデンサの断面拡大図であり、正極電極１１は、アルミニウム箔などの集電箔２１と、この集電箔２１にシート状に貼り付けた活性炭素を主体とした電極物質２２とからなる。負極電極１２も、アルミニウム箔などの集電箔２１と、この集電箔２１にシート状に貼り付けた活性炭素を主体とした電極物質２２とからなる。なお、集電箔２１、２１の裏面にも電極物質２２、２２を貼り付けるが、説明を簡単にするために図示を省略した。
FIG. 2 is an enlarged cross-sectional view of the electric double layer capacitor. A
そして、電極物質２２、２２に適量の電解液を含浸させる。
正極端子１６と負極端子１７に直流を印加すると、電極物質２２、２２内部及び集電箔２１、２１の表面に正負イオンが吸着し、一方は正極、他方は負極を形成する。放電時においては、この吸着イオンが脱着することに伴う電子の移動により正・負極端子１６、１７を通じて電流を取出すことができる。
Then, the
When a direct current is applied to the
図３は本発明に係る電気二重層コンデンサの製造フロー、特に集電箔の製造を詳しく説明するフロー図である。ＳＴ××はステップ番号を示す。
ＳＴ０１：集電箔として、普通純度のアルミニウム箔を準備する。このアルミニウム箔の表面は実質的に平坦である。
FIG. 3 is a flowchart for explaining in detail the manufacturing flow of the electric double layer capacitor according to the present invention, particularly the manufacturing of the current collector foil. STxx indicates a step number.
ST01: A normal-purity aluminum foil is prepared as a current collector foil. The surface of the aluminum foil is substantially flat.
ＳＴ０２：前記アルミニウム箔を、塩酸を含むエッチング液中でエッチングを施す。このエッチングにより、箔の表面に微細な粗面が形成される。微細な粗面は後に貼り付ける電極物質を繋ぎ止めるくさびとなる。 ST02: The aluminum foil is etched in an etching solution containing hydrochloric acid. By this etching, a fine rough surface is formed on the surface of the foil. The fine rough surface serves as a wedge for retaining the electrode material to be applied later.
粗面の形成が終了したら、箔を中和処理し、所定の洗浄する。所定の洗浄とは残留塩素濃度が管理基準（１．０ｍｇ／ｍ２以下）を満足する程度に実施することを意味する。これにより、過剰な洗浄作業を行わぬ様にする。 After the formation of the rough surface is completed, the foil is subjected to a neutralization treatment and is subjected to predetermined cleaning. The predetermined cleaning means that the cleaning is performed to such an extent that the residual chlorine concentration satisfies the control standard (1.0 mg / m 2 or less). This prevents excessive cleaning work.
ＳＴ０３：箔の成分を分析する。具体的には箔から１ｇ分の箔を切り取り、この箔片をリン酸にて完全に溶解させ、この溶解液を誘導プラズマ発光分光分析装置（例えばセイコー電子工業性ＳＰＳ−４０００）により定量成分分析を行う。 ST03: Analyze the components of the foil. Specifically, a foil of 1 g is cut from the foil, the foil piece is completely dissolved with phosphoric acid, and the solution is analyzed by an inductive plasma emission spectrophotometer (for example, SPS-4000 manufactured by Seiko Denshi Kogyo) for quantitative component analysis. I do.
ＳＴ０４：Ｃｕ、Ｎｉ、Ｚｎ、Ｓｎの含有量がいずれも１０ｐｐｍ以下であるか否かを調べる。この根拠は後述する。ＹＥＳであれば次に進むが、ＮＯであれば、不合格品扱いとする。 ST04: It is checked whether or not the contents of Cu, Ni, Zn, and Sn are all 10 ppm or less. The basis for this will be described later. If YES, proceed to the next step, but if NO, treat it as a rejected product.
ＳＴ０５：Ｆｅの含有量が３００ｐｐｍ以下であるか否かを調べる。この根拠は後述する。ＹＥＳであれば次に進むが、ＮＯであれば、不合格品扱いとする。 ST05: Check whether the Fe content is 300 ppm or less. The basis for this will be described later. If YES, proceed to the next step, but if NO, treat it as a rejected product.
ＳＴ０６：以上の検査をクリアーした箔についてのみ、電極物質をシート状にして接着などにより貼り付ける。
ＳＴ０７：セパレータと共に捲回する。
ＳＴ０８：容器に収納する。
ＳＴ０９：封止板を取付ける。
ＳＴ１０：電解液を注入する。
以上で、図１に示す円筒型電気二重層コンデンサを得ることができる。
ST06: The electrode material is formed into a sheet and attached by bonding or the like only for the foil that has passed the above inspection.
ST07: Wound with the separator.
ST08: Store in container.
ST09: Attach the sealing plate.
ST10: Inject electrolyte.
Thus, the cylindrical electric double layer capacitor shown in FIG. 1 can be obtained.
なお、ＳＴ０４〜ＳＴ０５は、順序を入れ替えることは差し支えない。 Note that the order of ST04 to ST05 may be changed.
本発明に係る実施例を次に説明する。比較実験のために２０個のサンプルを造る。
１．サンプルの材料：
１−１．集電箔：
１−１−１．アルミニウム箔（原料箔）
９９．８％以下の普通純度のアルミニウム箔として、表１に示す成分の原料箔を準備した。
An embodiment according to the present invention will be described below. Make 20 samples for comparative experiments.
1. Sample material:
1-1. Current collector foil:
1-1-1. Aluminum foil (raw material foil)
Raw material foils having the components shown in Table 1 were prepared as aluminum foil having a normal purity of 99.8% or less.
すなわち原料箔は、数ｐｐｍ〜数十ｐｐｍのＣｕ、Ｎｉ、Ｚｎ又はＳｎを含み、３００〜５００ｐｐｍのＦｅを含み、アルミニウムの純度が９９．５〜９９．７％の箔である。 That is, the raw material foil is a foil containing several ppm to several tens ppm of Cu, Ni, Zn or Sn, containing 300 to 500 ppm of Fe, and having an aluminum purity of 99.5 to 99.7%.
１−１−１．実施例１〜１０及び比較例１〜１０に共通する前処理：
５０℃に加熱された５％塩酸に原料アルミニウム箔を、浸漬し、電解電流密度０．２５Ａ／ｃｍ２、電気量３５Ａ・ｍｉｎ／ｄｍ２とした５０Ｈｚ交流電流により表面をエッチングした。
エッチング槽から取出した箔を、５０℃に加温されたｐＨ１の酸性水溶液で１分間洗浄処理を行い、さらに１８０℃の温風で乾燥した。
1-1-1. Pretreatment common to Examples 1 to 10 and Comparative Examples 1 to 10:
The raw aluminum foil was immersed in 5% hydrochloric acid heated to 50 ° C., and the surface was etched with a 50 Hz alternating current having an electrolytic current density of 0.25 A / cm 2 and an electric quantity of 35 A · min / dm 2 .
The foil taken out of the etching tank was washed for 1 minute with an acidic aqueous solution of pH 1 heated to 50 ° C., and further dried with hot air at 180 ° C.
１−１−２．後処理及び測定：
実施例１〜１０並びに比較例１〜１０は、前記乾燥が終了した直後に、上述した要領で箔の成分を分析した。その結果を表２に示す。
1-1-2. Post-treatment and measurement:
In Examples 1 to 10 and Comparative Examples 1 to 10, immediately after the drying was completed, the components of the foil were analyzed in the manner described above. Table 2 shows the results.
表１に比較して、この表２では、Ｃｕ、Ｎｉ、Ｚｎ、Ｆｅの全てにおいて含有量が減少した。この理由は、箔の表面からエッチング液中に合金元素が溶解するときに、母材のアルミニウムに比較して、Ｃｕ、Ｎｉ、Ｚｎ、Ｆｅがより多く溶解し、結果として母材に対してＣｕ、Ｎｉ、Ｚｎ、Ｆｅが目減りしたと考えられる。 In Table 2, as compared with Table 1, the contents of Cu, Ni, Zn, and Fe all decreased. The reason is that when the alloy element is dissolved in the etching solution from the surface of the foil, Cu, Ni, Zn, and Fe are dissolved more than the aluminum of the base material, and as a result, Cu is dissolved in the base material. , Ni, Zn, and Fe are considered to have decreased.
１−２．電極物質：
活性炭９０重量部、黒鉛粉末５重量部及び四フッ化エチレン５重量部を混合し、混練し、成形し、圧延することで、厚さ１４５μｍ×幅１００ｍｍ×長さ１２００ｍｍのシート状電極物質を造る。
１−３．接着剤：
ＰＶＡ（ポリビニルアルコール）、黒鉛及び不定形炭素からなる導電性接着剤
1-2. Electrode material:
90 parts by weight of activated carbon, 5 parts by weight of graphite powder and 5 parts by weight of ethylene tetrafluoride are mixed, kneaded, molded, and rolled to produce a sheet-like electrode material having a thickness of 145 μm, a width of 100 mm, and a length of 1200 mm. .
1-3. adhesive:
Conductive adhesive composed of PVA (polyvinyl alcohol), graphite and amorphous carbon
１−４．セパレータ：
人造絹糸セパレータ。厚さ７５μｍ×幅１０５ｍｍの多孔性フィルム。
１−５．容器：
径が４０ｍｍで高さが１３０ｍｍの容器
１−６．電解液：
有機系電解液としてのＴＥＭＡ・ＢＦ４／ＰＣ。なお、ＴＥＭＡ・ＢＦ４はトリエチルメチルアンモニウムテトラフルオロボーレート、ＰＣはプロピレンカーボネートである。
1-4. Separator:
Artificial silk separator. A porous film having a thickness of 75 μm and a width of 105 mm.
1-5. container:
Container having a diameter of 40 mm and a height of 130 mm 1-6. Electrolyte:
TEMA.BF 4 / PC as an organic electrolyte. TEMA.BF 4 is triethylmethylammonium tetrafluoroborate, and PC is propylene carbonate.
２．サンプルの造り方：
上記集電箔の両面に、上記接着剤を用いて電極物質を貼り付ける。上記セパレータとともに捲回して、容器に収め、電解液を注入することで、円筒型電気二重層コンデンサを造る。比較実験に供するために２０種類のサンプルを造る。
2. How to make a sample:
An electrode material is attached to both sides of the current collector foil using the adhesive. It is wound together with the separator, placed in a container, and injected with an electrolytic solution to produce a cylindrical electric double layer capacitor. Twenty types of samples are prepared for comparison experiments.
３．追加測定
前記成分分析の他に、以下の測定を行う。
３−１．電圧維持率の測定：
図１の正負極端子１６、１７に２．５Ｖを印加して、６ｈｒの定圧充電を行う。６ｈｒ経過したら正負極端子１６、１７から給電ケーブルを外し、直ちに電圧Ｖ１を測定する。２５℃の雰囲気中で７２ｈｒ放置して自然放電をさせる。７２ｈｒ経過したら残存電圧Ｖ２を測定する。
そして、１００×（Ｖ１−Ｖ２）／Ｖ１の計算式により「電圧維持率」を求める。それを表３に示す。
3. Additional measurement In addition to the component analysis, the following measurement is performed.
3-1. Measurement of voltage maintenance rate:
A voltage of 2.5 V is applied to the positive and
Then, the “voltage maintenance ratio” is calculated by the formula of 100 × (V1−V2) / V1. It is shown in Table 3.
表３は、比較検討が容易になる様に、表２の右に電圧維持率の欄を加えた。
実施例１〜１０は、電圧維持率が全て９２％以上であり、結果は良好であった。これに対して、比較例１〜１０は電圧維持率が７０％又はそれ以下である。これは比較例１〜１０ではコンデンサの内部でショート現象が発生し、そのために蓄電エネルギーが消耗したと考えられる。
In Table 3, a column for the voltage maintenance ratio is added to the right of Table 2 to facilitate comparison.
In Examples 1 to 10, the voltage maintenance ratios were all 92% or more, and the results were good. In contrast, Comparative Examples 1 to 10 have a voltage maintenance ratio of 70% or less. This is presumably because in Comparative Examples 1 to 10, a short-circuit phenomenon occurred inside the capacitor, and thus the stored energy was consumed.
そこで、表３を詳細に検討すると、比較例１、２はＣｕが１５ｐｐｍ以上であり、実施例及び他の比較例が１０ｐｐｍ以下であることから、Ｃｕが過剰であり、これが電圧維持率を低下させた要因であると考えられる。 Therefore, when Table 3 is examined in detail, Cu is excessive in Comparative Examples 1 and 2 because Cu is 15 ppm or more, and Examples and other comparative examples are 10 ppm or less, which lowers the voltage maintenance ratio. It is considered to be the factor that caused the change.
同様に、比較例３、４はＮｉが１８ｐｐｍ以上であり、実施例３、４が１０ｐｐｍ以下であることから、Ｎｉが過剰であり、これが電圧維持率を低下させた要因であると考えられる。 Similarly, since Comparative Examples 3 and 4 contain 18 ppm or more of Ni and Examples 3 and 4 contain 10 ppm or less, it is considered that Ni is excessive, and this is a factor that lowers the voltage maintenance ratio.
比較例５、６はＺｎが１２ｐｐｍ以上であり、実施例及び他の比較例が１０ｐｐｍ以下であることから、Ｚｎが過剰であり、これが電圧維持率を低下させた要因であると考えられる。 In Comparative Examples 5 and 6, Zn was 12 ppm or more, and in Examples and other comparative examples were 10 ppm or less. Therefore, it is considered that Zn was excessive, and this was a factor that lowered the voltage maintenance ratio.
比較例７、８はＳｎが１６ｐｐｍ以上であり、実施例７、８が１０ｐｐｍ以下であることから、Ｓｎが過剰であり、これが電圧維持率を低下させた要因であると考えられる。 In Comparative Examples 7 and 8, Sn was 16 ppm or more, and Examples 7 and 8 were 10 ppm or less. Therefore, it is considered that Sn was excessive, and this was a factor that lowered the voltage maintenance ratio.
比較例９、１０はＦｅが３５０ｐｐｍ以上であり、実施例及び他の比較例が３００ｐｐｍ以下であることから、Ｆｅが過剰であり、これが電圧維持率を低下させた要因であると考えられる。 In Comparative Examples 9 and 10, Fe is 350 ppm or more, and Examples and other Comparative Examples are 300 ppm or less. Therefore, it is considered that Fe is excessive, and this is a factor that lowers the voltage maintenance ratio.
以上のことから、電極物質を貼り付ける直前に計測したＣｕ、Ｎｉ、Ｚｎ、Ｓｎの含有量が、いずれも１０ｐｐｍ以下であり、且つ電極物質を貼り付ける直前に計測したＦｅの含有量が、３００ｐｐｍ以下であれは、ショートの発生を抑えることができ、高い電圧維持率が得られると言える。 From the above, the contents of Cu, Ni, Zn, and Sn measured immediately before attaching the electrode material were all 10 ppm or less, and the Fe content measured immediately before attaching the electrode material was 300 ppm. Below, it can be said that the occurrence of short circuit can be suppressed and a high voltage maintenance ratio can be obtained.
尚、本発明は円筒型コンデンサの他、平板型コンデンサにも適用できるため、コンデンサの外観的形状は任意である。 In addition, since the present invention can be applied to a flat plate type capacitor in addition to a cylindrical type capacitor, the external shape of the capacitor is arbitrary.
本発明に係る電気二重層コンデンサは、車載バッテリに好適である。 The electric double layer capacitor according to the present invention is suitable for a vehicle-mounted battery.
１０…電気二重層コンデンサ、１１…正極電極、１２…負極電極、１３…セパレータ、２１…集電箔(箔)、２２…電極物質。
DESCRIPTION OF
Claims (1)
電極物質を貼り付ける段階での前記集電箔は、以下の条件を満足するものを用いたことを特徴とする電気二重層コンデンサ。
・集電箔は、Ｃｕ、Ｎｉ、Ｚｎ、Ｓｎ、Ｆｅの少なくとも１種を含み、アルミニウムが９９．８％以下の普通純度のアルミニウム箔を素材として、これにエッチング処理を施してあること。
・電極物質を貼り付ける直前に計測したＣｕ、Ｎｉ、Ｚｎ、Ｓｎの含有量が、いずれも１０ｐｐｍ以下であること。
・電極物質を貼り付ける直前に計測したＦｅの含有量が、３００ｐｐｍ以下であること。 A positive electrode and a negative electrode are produced by attaching an electrode material mainly composed of activated carbon to a pair of current collecting foils, and a separator is interposed between the positive and negative electrodes and an electrolytic solution is interposed therebetween. In electric double layer capacitors that can be charged and discharged through foil,
An electric double layer capacitor, wherein the current collector foil used in the step of attaching an electrode material satisfies the following conditions.
-The current collector foil contains at least one of Cu, Ni, Zn, Sn, and Fe, and has been subjected to an etching treatment using a normal-purity aluminum foil containing 99.8% or less of aluminum.
-The content of Cu, Ni, Zn, and Sn measured immediately before the electrode material is attached is 10 ppm or less in all cases.
The Fe content measured immediately before the electrode material is attached is 300 ppm or less.
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