JP7239564B2 - 硬質炭素材料の製造方法 - Google Patents
硬質炭素材料の製造方法 Download PDFInfo
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- JP7239564B2 JP7239564B2 JP2020512572A JP2020512572A JP7239564B2 JP 7239564 B2 JP7239564 B2 JP 7239564B2 JP 2020512572 A JP2020512572 A JP 2020512572A JP 2020512572 A JP2020512572 A JP 2020512572A JP 7239564 B2 JP7239564 B2 JP 7239564B2
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- solid
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Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/50—Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
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Description
・最も重要な違いは、本開示で説明する方法では、最初に室温でフルフリルアルコールを重合させて固体にする。これは、後続のすべての加熱工程で形成される材料の性質に影響を与えるため、重要である。他の特許に記載されている工程は、室温での浸漬は行わない。他の方法では、液体フルフリルアルコールを何らかの形で加熱するが、これは、重合中に発熱反応を起こし、大規模な工業環境では危険な場合がある。温和な室温工程では、熱暴走の危険性はない。
・本発明の手法は、真空蒸留工程を必要としない(米国特許第4,959,281号に記載ある)。本発明の手法は、H3PO4(有毒で危険な物質)を使用する米国特許第5,093,216号に記載されている方法とは異なり、弱い固体酸(有機酸)のみを使用している。本発明の手法は、初期のフルフリルアルコール前駆体を還流加熱する必要はない(米国特許第5,093,216号は、pHを維持するためのフルフリル樹脂水混合物の還流加熱を記載している)。本発明の手法では、固体が得られるまで、室温で長時間浸漬する(製造工程を単純に保つ)。
・本発明の手法では、黒鉛よりも大きなd002間隔を実現するためにリンを追加する必要はない(米国特許第5,093,216号および第4,959,281号にはリンの存在が必要)。本方法は、米国特許第5,716,732号に記載されているような、一定の低圧(約20 KPa)下での加熱を使用しない。
ケイ素含有硬質炭素:
Claims (19)
- フラン環含有化合物から非非晶質硬質炭素を生成する方法であって、
a.酸性触媒を、4個の炭素原子と1個の酸素原子を含む5員環を含むフラン環化合物を特徴とする液体フラン環含有化合物と混合して混合物を形成する工程と、
b.該混合物を室温で浸漬し、さらに該混合物を空気中で25℃から200℃の温度範囲で加熱して硬質高分子重合固体を形成する工程と、そして
c.不活性雰囲気下で該硬質高分子重合固体を200℃から800℃に加熱し、炭化させて、X線回折技術により測定される3.6オングストロームより大きいd002間隔を有することを特徴とする、非非晶質硬質炭素を得る工程と
を含む、方法。 - 前記フラン環含有化合物が、フルフリルアルコール、フルフルアルデヒド、5-ヒドロキシメチルフルフラール、5-メチルフルフラール、およびポリフルフリルアルコールの少なくとも1つである、請求項1に記載の方法。
- 前記酸性触媒がシュウ酸のpKa値以上のpKa値を有する有機酸の少なくともひとつであって、前記触媒は固体であるか、溶液を作るために脱イオン水に溶解される、請求項1に記載の方法。
- 前記非非晶質硬質炭素が、1gm/ccより大きい密度を有する、請求項1に記載の方法。
- 前記非非晶質硬質炭素が、532nmレーザー光源を使用して測定された場合、そのラマンスペクトルに1300/cmから1360/cmの「D」帯域ピークを有する、請求項1に記載の方法。
- 請求項1に記載の方法であって、さらに、
d.不活性雰囲気下で1000℃から1100℃で焼成する工程と
を含む方法。 - 前記非非晶質硬質炭素が、2から200m2/gmのBET比表面積を有する、請求項1に記載の方法。
- 前記非非晶質硬質炭素が、Liイオン電池、Naイオン電池、Naイオンキャパシタ、およびLiイオンキャパシタ用の電極を構築するために使用され、Liイオン電池、Naイオン電池、Naイオンキャパシタ、およびLiイオンキャパシタは、C/10から100Cのレートで充電および放電されることを特徴とする、請求項1に記載の方法。
- 前記フラン環含有化合物がアセチルフランであって、前記酸性触媒がジクロロジメチルシランおよびテトラクロロシランの少なくともひとつである、請求項1に記載の方法。
- 4個の炭素原子と1個の酸素原子を含む5員環を含むフラン環を特徴とするフラン環含有化合物から、X線回折法により測定して3.6オングストロームを超えるd002間隔を有することを特徴とするケイ素含有非非晶質硬質炭素を製造する方法であって、
a.フラン環含有化合物を不溶性ケイ素含有材料および酸性触媒と混合して混合物を形成する工程と、
b.該混合物を室温で浸漬し、該混合物を室温から200℃までさらに加熱して、高分子固体を形成する工程と、そして
c.不活性雰囲気下で該高分子固体を200℃から800℃で加熱して炭化させ、ケイ素含有硬質炭素材料を形成する工程と、
を含む方法。 - フラン環含有化合物が、フルフリルアルコール、フルフルアルデヒド、5-ヒドロキシメチルフルフラール、5-メチルフルフラール、2-アセチルフランおよびポリフルフリルアルコールの少なくともひとつである、請求項10に記載の方法。
- 酸性触媒がシュウ酸のpKa値より大きいpKa値を有する有機酸の少なくともひとつであって、触媒が固体であるか、溶液を作るために脱イオン水に溶解される、請求項10に記載の方法。
- 不溶性ケイ素化合物が、粒子サイズが-325メッシュ以下の金属ケイ素粉末および粒子サイズが-325メッシュ以下のアルミノケイ酸塩の少なくともひとつであって、アルミノケイ酸塩がハロイサイトである、請求項10に記載の方法。
- 前記ケイ素含有非非晶質硬質炭素が、エネルギー貯蔵デバイス用の電極を構築するために使用される、請求項10に記載の方法。
- 4個の炭素原子と1個の酸素原子を含む5員環を含むフラン環を特徴とするフラン環含有化合物からリチウム含有非非晶質硬質炭素を製造する方法であって、
a.フラン環含有化合物を不溶性リチウム化合物および酸性触媒と混合する工程と、
b.該混合物を室温で浸漬し、さらに200℃の温度まで加熱して高分子個体を形成する工程と、そして
c.該高分子個体を不活性雰囲気下で200℃から800℃の温度範囲で加熱し、炭化させて非非晶質のリチウム含有硬質炭素を形成する工程と、
を含む方法。 - フラン環含有化合物が、フルフリルアルコール、フルフルアルデヒド、5-ヒドロキシメチルフルフラール、5-メチルフルフラール、2-アセチルフランおよびポリフルフリルアルコールの少なくともひとつである、請求項15に記載の方法。
- 前記触媒が、シュウ酸のpKa値よりも大きいpKa値を有する有機酸のうちの少なくともひとつであり、直接または脱イオン水を含む溶液中にある、請求項15に記載の方法。
- 前記不溶性リチウム化合物がLi4Ti5O12である、請求項15に記載の方法。
- 前記リチウム含有非非晶質硬質炭素が、リチウムイオン電池およびリチウムイオンキャパシタ用の電極を構築するために使用される、請求項15に記載の方法。
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