TWI542537B - Porous carbon and a method for producing the same - Google Patents
Porous carbon and a method for producing the same Download PDFInfo
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- TWI542537B TWI542537B TW101108126A TW101108126A TWI542537B TW I542537 B TWI542537 B TW I542537B TW 101108126 A TW101108126 A TW 101108126A TW 101108126 A TW101108126 A TW 101108126A TW I542537 B TWI542537 B TW I542537B
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- Prior art keywords
- carbon
- porous carbon
- present
- mesopores
- carbonaceous wall
- Prior art date
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 219
- 229910052799 carbon Inorganic materials 0.000 title claims description 190
- 238000004519 manufacturing process Methods 0.000 title description 9
- 239000011148 porous material Substances 0.000 claims description 38
- 230000002093 peripheral effect Effects 0.000 claims description 7
- 238000002441 X-ray diffraction Methods 0.000 claims description 6
- 238000001228 spectrum Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 description 37
- 239000007789 gas Substances 0.000 description 28
- 239000002245 particle Substances 0.000 description 25
- 238000001179 sorption measurement Methods 0.000 description 23
- 239000011347 resin Substances 0.000 description 19
- 229920005989 resin Polymers 0.000 description 19
- 239000003575 carbonaceous material Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 13
- 238000002474 experimental method Methods 0.000 description 12
- 238000000034 method Methods 0.000 description 12
- 230000001590 oxidative effect Effects 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- 239000002253 acid Substances 0.000 description 9
- 239000012298 atmosphere Substances 0.000 description 9
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 9
- 239000012530 fluid Substances 0.000 description 7
- 239000010410 layer Substances 0.000 description 7
- 239000000395 magnesium oxide Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 239000003463 adsorbent Substances 0.000 description 5
- 239000003990 capacitor Substances 0.000 description 5
- 239000007772 electrode material Substances 0.000 description 5
- 125000001153 fluoro group Chemical group F* 0.000 description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 5
- 239000007773 negative electrode material Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
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- 229910003481 amorphous carbon Inorganic materials 0.000 description 4
- -1 and the like Substances 0.000 description 4
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- 229910052731 fluorine Chemical group 0.000 description 4
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- 229920000642 polymer Polymers 0.000 description 4
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
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- LONILYZRIIFLSK-UHFFFAOYSA-N 2,3,6-trifluoro-5-(1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-henicosafluorodecoxy)aniline Chemical compound NC1=C(C(=CC(=C1F)OC(C(C(C(C(C(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)F)F LONILYZRIIFLSK-UHFFFAOYSA-N 0.000 description 1
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- JPOVYMXWPJDYEK-UHFFFAOYSA-N 2-(1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-henicosafluorodecoxy)-5-methoxybenzene-1,4-diamine Chemical compound NC1=C(C=C(C(=C1)OC(C(C(C(C(C(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)N)OC JPOVYMXWPJDYEK-UHFFFAOYSA-N 0.000 description 1
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- Nanotechnology (AREA)
Description
本發明係關於多孔質碳及其製造方法,尤其,本發明係關於具備介孔(mesoporous)之多孔質碳及其製造方法。
多孔質碳之製造方法習知為以木材紙漿、鋸木屑、椰殼、棉籽殼、稻殼等之纖維素質,或栗、稗、玉蜀黍等澱粉質,木質素(lignin)等之植物性原料,煤炭或焦炭、石油瀝青等之礦物性原料,以及酚樹脂或聚丙烯腈等合成樹脂等作為原料,使該等在非氧化性環境下加熱並碳化之方法,另外,以藥劑處理該等碳化物(活性碳)而賦活化之方法亦充分悉知。
又最近,使用氫氧化鉀作為賦活用之藥劑,且使其與有機質樹脂混合,在非氧化性環境下加熱,確認可獲得高達3000m2/g之比表面積之活性碳,而受到矚目(參照下述專利文獻1)。
不過,該方法對於有機質樹脂需要4倍以上之賦活劑,因此雖然嘗試鉀之回收再利用但回收率低且成本高,而且,鹼金屬在賦活用之加熱步驟中會揮發而污染乃至損傷加熱爐,且在作為各種工業材料使用時成為引起浸蝕之原因,再者以鹼金屬化合物處理之活性碳可燃性高且容易引火等,於工業規模之實用化仍留有諸多問題。
考慮該等,而提案有包含使有機質樹脂與由鹼土類金
屬之氧化物、氫氧化物、碳酸鹽、有機酸鹽所組成群組選出之鹼土類金屬化合物之至少一種混合,且在非氧化性環境加熱燒成之步驟的活性碳之製造方法(參照下述專利文獻2)。
[先前技術文獻]
專利文獻
專利文獻1:特開平9-86914號公報
專利文獻2:特開2006-062954號公報
如上述之多孔質碳雖可藉各種方法製造,但為改良特性,已嘗試該多孔質碳之進一步加熱處理。然而,加熱處理如上述之多孔質碳時,而有不僅無法提高結晶性(無法石墨化),且比表面積亦變小,就連所期待之特性改良,亦有使本來特性更差之課題。
本發明之特徵為具備有介孔(mesoporous)與構成該介孔之外圍輪廓之碳質壁,且上述碳質壁存在有形成層狀構造之部分。
碳質壁中形成層狀構造之部分可謂結晶質發達。該層狀構造通常係藉由在某溫度以上加熱處理碳材而生成。然而,由於碳材在加熱處理中會引起收縮,故使碳材中之孔
崩潰,使比表面積變小,而難以獲得為結晶質且比表面積亦高之多孔質碳。本發明之多孔質碳由於具有介孔與構成該介孔之外圍輪廓之碳質壁,故認為可耐受加熱處理中之收縮,而可在該碳質壁中形成層狀構造。亦即,本發明之多孔質碳由於存在介孔,故可抑制比表面積變小。如此,由於比表面積在某程度大小之狀態下結晶質部分發達,故本發明之多孔質碳可使用於各種領域(例如,氣體吸附材料、非水電解質電池之負極材料、電容之電極材料等)中。
又,並不需要使碳質壁之全部部分成為層狀構造,亦可一部份存在非晶質部分。又,本發明之多孔質碳中,介孔為必須但微孔則非必要。因此,微孔可存在亦可不存在。
此處,本說明書中,將細孔徑未達2nm者稱為微孔,將細孔徑2~50nm者稱為介孔。
上述碳質壁宜作成三次元網目構造。
若碳質壁作成三次元網目構造,則在多孔質碳之用途需要彈性之情況下,本發明之多孔質碳亦適用。且,使用本發明之多孔質碳作為氣體吸附劑時,由於不會阻礙氣體之流動,故可提高氣體吸附能力,再者,使用本發明之多孔質碳作為非水電解質電池之負極材料或電容之電極材料時,鋰離子等可順利移動。
比表面積宜為200m2/g以上。
比表面積未達200m2/g時,會有難以形成三次元網目
構造之問題,且會有氣孔之形成量不足,使氣體吸附能下降之問題。另一方面,比表面積宜為1500m2/g以下。比表面積超過1500m2/g時,會有無法保持碳質壁形狀之情況,且有無法充分形成介孔之可能性。
上述介孔為開氣孔,宜成為氣孔部分連續之構成。
若為上述構成,則在使用本發明之多孔質碳作為氣體吸附劑時,由於氣體之流動順利,故氣體之捕捉更容易。另外,使用作為非水電解質電池之負極材料或電容之電極材料時,鋰離子等順利移動。
上述介孔之容量宜為0.2ml/g以上。
介孔之容量未達0.2ml/g時,難以確保比表面積,且,原因為於相對壓力較高時會有氣體吸附能下降之可能性。
容積密度宜為0.1g/cc以上且1.0g/cc以下。
容積密度未達0.1g/cc時,難以確保比表面積,會有無法保持碳質壁形狀之情況,另一方面,容積密度(Bulk density)超過1.0g/cc以下時,會有難以形成三次元網目構造之問題,會有介孔之形成不充分,使氣體吸附能下降之情況。
形成上述層狀構造之部分之厚度宜為1nm以上且100nm以下。
鄰接層之層間距離為0.33nm左右,形成多數層時,形成層狀構造之部分之厚度變大,另一方面形成少數層時,形成層狀構造之部分之厚度變小。此處,製作多孔質碳
時,減少鑄型粒子之量時,碳質壁之厚度變大,由於形成多數層,因此形成層狀構造之厚度變大,另一方面,增加鑄型粒子之量時,碳質壁之厚度變小,僅能形成少數層,故形成層狀構造之部分之厚度變小。層狀構造之厚度未達1nm時,會有結晶質部分之發達不充份之可能性。另一方面,超過100nm時,有必要進行延長加熱處理之時間、提高加熱溫度等之處理,故製造上困難,有使本發明之多孔質碳之其他特性下降之可能性。
本發明之特徵為具備介孔與構成該介孔外圍輪廓之碳質壁,其對於CuKα線(波長1.541埃)之X射線繞射光譜中,在布拉格(Bragg)角度2θ之26.45°具有峰。
X射線繞射光譜中,若布拉格角度2θ之26.45°具有峰,則可謂碳質壁經石墨化。且,由於存在介孔,故可抑制比表面積變小。據此,比表面積在某程度大小之狀態下可石墨化,故可用於各種領域(例如,氣體吸附材料、非電解質電池之負極材料、電容之電極材料等)中。
又,碳質壁並不需要全部部分均石墨化,於一部分亦可存在未石墨化之非晶質部分。且,介孔為必須但微孔則為非必要。因此,微孔可存在亦可不存在。
基於與上述理由相同之理由,碳質壁宜作成三次元網目構造,比表面積宜為200m2/g以上1500m2/g以下。另外,介孔為開氣孔,較佳為成為氣孔部分連續的構成,介孔之容量宜為0.2ml/g以上。另外,容積密度宜為0.1g/cc以上1.0g/cc以下,碳質壁宜存在作成層狀構造之部分。
本發明之特徵為具備介孔及構成該介孔外圍輪廓之碳質壁,且比電阻為1.0×102Ω.cm以下。
若為上述構成,則由於存在介孔,故可抑制比表面積變小,而且,比電阻小至1.0×102Ω.cm以下。據此,若比表面積於某種程度大小之狀態可降低比電阻,則本發明之多孔質碳可使用於各種領域中。
又,上述碳質壁至少部分具有層狀構造,且較好成為結晶質。碳質壁並不須全部部分均成為結晶質,亦可於一部分存在非晶質部分。且,本發明之多孔質碳中,介孔為必須但微孔並非必須。因此,微孔可存在亦可不存在。
基於與上述理由相同之理由,碳質壁宜作成三次元網目構造,比表面積宜為200m2/g以上1500m2/g以下。且,介孔宜為開氣孔,且成為氣孔部分連續的構成,介孔之容量宜為0.2ml/g以上。再者,容積密度宜為0.1g/cc以上1.0g/cc以下,碳質壁宜存在作成層狀構造之部分。
又,本發明之特徵為在非氧化環境或減壓環境下,使具有介孔之碳質燒成體在非晶質碳結晶化之溫度以上進行熱處理。
具有介孔之碳質燒成體宜藉如下製造:使含有有機質樹脂之流動性材料、與由鹼土類金屬之氧化物、氫氧化物、碳酸鹽、有機酸鹽所成群組選出之鹼土類金屬化合物之至少一種所成之鑄型粒子混合,製作混合物之步驟;在非氧化性環境中加熱燒成上述混合物,製作燒成物之步驟;去除上述燒成物中之上述鑄型粒子之步驟。
依據該製造方法,於熱處理具有介孔之碳質燒成體時,不會導致比表面積降低,可製造具有結晶質之多孔質碳。比表面積之降低推測係肇因於熱處理中之碳收縮所致者,但推測熱處理前之碳燒成體具有介孔,故可耐受碳之收縮而抑制比表面積降低者。
又,以該方法製作時,由於在非晶質之碳結晶化之溫度以上進行熱處理,故本發明之多孔質碳在高溫環境下使用時(例如,在高溫環境下使用作為吸附構件時),若該溫度為未達非晶質之碳結晶化溫度之溫度,則可防止多孔質碳變質。所謂該結晶化之溫度以上較好為800℃以上,更好為2000℃以上。尤其,考量在2000℃以上使用多孔質碳之情況少,因此,可在各種用途中使用本發明之多孔質碳。
此處,藉由改變鑄型粒子之直徑或有機質樹脂之種類,可調整細孔之直徑、多孔質碳之細孔分佈以及碳質壁之厚度。因此,藉由適當選擇鑄型粒子之直徑與有機質樹脂之種類,亦可製備具有更均一細孔徑、具有更大細孔容量之多孔質碳。另外,由於碳源係使用含有有機質樹脂之流動性材料,而且,不經過賦活處理步驟而可製備多孔質碳,故所得多孔質碳成為純度極高者。
又,使用鹼土類金屬化合物作為鑄型粒子,由於鹼土類金屬化合物可利用弱酸或熱水去除(亦即,不使用強酸即可去除鑄型粒子),故去除鑄型粒子之步驟中,可抑制多孔質碳本身之性質變化。又,使用弱酸時,有加速去除
速度之優點,但另一方面,使用熱水時,具有可防止酸殘留而成為雜質缺陷之優點。且,去除鑄型粒子之步驟中,溶出之氧化物溶液可再度作為原料使用,可降低多孔質碳之製造成本。
上述流動性材料之碳收率宜為40%以上且85%以下,上述鑄型粒子之粒徑宜為大致相同粒徑。
若如上述之鑄型粒子之直徑約為相同之直徑,則由於鑄型粒子均勻地分散在基質(燒成物中),故鑄型粒子間之間隔偏差較小。因此,成為碳質壁之厚度趨近均一之三次元網目構造。但,流動性材料之碳收率過小或過大時(具體而言,流動性材料之碳收率未達40%,超過85%時),成為無法保持三次元網目構造之碳粉末,但如上述,若碳收率限定在40%以上85%以下,則去除鑄型粒子後,可獲得鑄型粒子存在之部位具有成為連續孔之三次元網目構造之多孔質碳。且,若鑄型粒子之直徑為幾乎相同之直徑,則由於形成相同尺寸之連續孔,故可製作海綿狀且略籠狀之多孔質碳。
此處,作為上述流動性材料,宜使用在200℃以下之溫度產生流動性者,具體而言,例示為單位構造中含有至少一個以上之氮或氟原子之由聚醯亞胺、酚樹脂及瀝青所組成群組選出之至少一種。
但,流動性材料並不限於在200℃以下之溫度產生流動性者,即使是在200℃以下之溫度未產生流動性,而可溶於水或有機溶劑中之高分子材料亦可使用於本發明中。
去除上述鑄型粒子之步驟中,去除後之鑄型粒子之殘留率宜限制為0.5%以下。
原因為去除後之鑄型粒子之殘留率超過0.5%時,介孔內殘留之鑄型粒子變多,而廣泛產生無法發揮作為細孔之角色之部位。
依據本發明,可發揮即使具有層狀構造之碳仍可提供比表面積極高之多孔質碳之優異效果。
以下,說明本發明之實施形態。
本發明之多孔質碳係使有機質樹脂與氧化物(鑄型粒子)在溶液或粉末狀態下經濕式或乾式混合,且使混合物在非氧化環境或減壓環境,在例如500℃以上之溫度碳化後,經洗淨處理而去除氧化物,製作非晶質之多孔質碳(碳燒成體)。隨後,使該非經質之多孔質碳在非氧化環境或減壓環境下,在非晶質之多孔質碳結晶化溫度以上(例如,2000℃)下熱處理而獲得。
前述非晶質多孔質碳具有大小約略相同之多數個介孔,該介孔間形成之碳質壁中之面向介孔之位置較好成為如形成微孔之構造。該非晶質之多孔質碳之熱處理中,維持了存在多數介孔之狀態,而且,碳部分(碳質壁)之至少一部分形成層狀構造。因此,藉由該熱處理,獲得結晶性發
達之多孔質碳。
至於上述有機質樹脂,較好使用單位構造中含有至少一個以上之氮或氟原子之聚醯亞胺或碳收率為40重量%以上85重量%以下之樹脂,例如酚樹脂或瀝青。
此處,上述單位構造中含有至少一個以上之氮或氟原子之聚醯亞胺可藉由酸成分與二胺成分之聚縮合獲得。但,該情況下,酸成分及二胺成分之任一者或二者須含有一個以上之氮原子或氟原子。
具體而言,可藉由使聚醯亞胺之前驅物的聚醯胺酸成膜,藉加熱去除溶劑獲得聚醯胺酸膜。接著,在200℃以上使所得聚醯胺酸膜熱醯亞胺化,而製造聚醯亞胺。
至於前述二胺可例示為2,2-雙(4-胺基苯基)六氟丙烷[2,2-Bis(4-aminophenyl)hexafluoropropane]、2,2-雙(三氟甲基)聯苯胺[2,2’-Bis(trifluoromethyl)benzidine]、4,4’-二胺基八氟聯苯,或3,3’-二氟-4,4’-二胺基二苯基甲烷、3,3’-二氟-4,4’-二胺基二苯基醚、3,3’-二(三氟甲基)-4,4’-二胺基二苯基醚、3,3’-二氟-4,4’-二胺基二苯基丙烷、3,3’-二氟-4,4’-二胺基二苯基六氟丙烷、3,3’-二氟-4,4’-二胺基二苯甲酮、3,3’,5,5’-四氟-4,4’-二胺基二苯基甲烷、3,3’,5,5’-四(三氟甲基)-4,4’-二胺基二苯基甲烷、3,3’,5,5’-四氟-4,4’-二胺基二苯基丙烷、3,3’,5,5’-四(三氟甲基)-4,4’-二胺基二苯基丙烷、3,3’,5,5’-四氟-4,4’-二胺基二苯基六氟丙烷、1,3-二胺基-5-(全氟壬氧基)苯、1,3-二胺基-4-甲基-5-(全氟壬氧基)苯、1,3-二胺基-4-甲氧基-
5-(全氟壬氧基)苯、1,3-二胺基-2,4,6-三氟-5-(全氟壬氧基)苯、1,3-二胺基-4-氯-5-(全氟壬氧基)苯、1,3-二胺基-4-溴-5-(全氟壬氧基)苯、1,2-二胺基-4-(全氟壬氧基)苯、1,2-二胺基-4-甲基-5-(全氟壬氧基)苯、1,2-二胺基-4-甲氧基-5-(全氟壬氧基)苯、1,2-二胺基-3,4,6-三氟-5-(全氟壬氧基)苯、1,2-二胺基-4-氯-5-(全氟壬氧基)苯、1,2-二胺基-4-溴-5-(全氟壬氧基)苯、1,4-二胺基-3-(全氟壬氧基)苯、1,4-二胺基-2-甲基-5-(全氟壬氧基)苯、1,4-二胺基-2-甲氧基-5-(全氟壬氧基)苯、1,4-二胺基-2,3,6-三氟-5-(全氟壬氧基)苯、1,4-二胺基-2-氯-5-(全氟壬氧基)苯、1,4-二胺基-2-溴-5-(全氟壬氧基)苯、1,3-二胺基-5-(全氟己烯氧基)苯、1,3-二胺基-4-甲基-5-(全氟己烯氧基)苯、1,3-二胺基-4-甲氧基-5-(全氟己烯氧基)苯、1,3-二胺基-2,4,6-三氟-5-(全氟己烯氧基)苯、1,3-二胺基-4-氯-5-(全氟己烯氧基)苯、1,3-二胺基-4-溴-5-(全氟己烯氧基)苯、1,2-二胺基-4-(全氟己烯氧基)苯、1,2-二胺基-4-甲基-5-(全氟己烯氧基)苯、1,2-二胺基-4-甲氧基-5-(全氟己烯氧基)苯、1,2-二胺基-3,4,6-三氟-5-(全氟己烯氧基)苯、1,2-二胺基-4-氯-5-(全氟己烯氧基)苯、1,2-二胺基-4-溴-5-(全氟己烯氧基)苯、1,4-二胺基-3-(全氟己烯氧基)苯、1,4-二胺基-2-甲基-5-(全氟己烯氧基)苯、1,4-二胺基-2-甲氧基-5-(全氟己烯氧基)苯、1,4-二胺基-2,3,6-三氟-5-(全氟己烯氧基)苯、1,4-二胺基-2-氯-5-(全氟己烯氧基)苯、1,4-二胺基-2-溴-5-(全氟己烯氧基)苯或不含氟原子之對-苯二胺(PPD)、二氧基二
苯胺等芳香族二胺。且,上述二胺成分亦可組合兩種以上之上述各芳香族二胺而使用。
另一方面,作為酸成分列舉為含氟原子之4,4-六氟亞異丙基二鄰苯二甲酸酐(6FDA)、及不含氟原子之3,4,3’,4’-聯苯四羧酸二酐(BPDA)、聯苯二酸二酐(PMDA)等。
且,作為聚醯亞胺前驅物之溶劑使用之有機溶劑列舉為N-甲基-2-吡咯烷酮、二甲基甲醯胺等。
醯亞胺化之方法係如習知方法[參照例如,高分子學會編「新高分子實驗學」共立出版,1996年3月28日,第3卷高分子之合成.反應(2)158頁]所示,依循加熱或化學醯亞胺化之方法,但本發明並不限於該醯亞胺之方法。
另外,聚醯亞胺以外之樹脂可使用石油系焦炭瀝青、丙烯酸樹脂等具有40%以上之碳收率者。
另一方面,作為上述氧化物使用之原料除鹼土類金屬氧化物(氧化鎂、氧化鈣等)以外,亦可使用在利用熱處理之熱分解過程中,變化成氧化鎂之狀態之金屬有機酸(檸檬酸鎂、草酸鎂、檸檬酸鈣、草酸鈣等)。
又,去除氧化物之洗淨液係使用鹽酸、硫酸、硝酸、檸檬酸、乙酸、甲酸等一般無機酸,且較好以2mol/l以下之稀酸使用。又,亦可使用80℃以上之熱水。
另外,前述混合物之碳化較好在非氧化環境或減壓環境下,在500℃以上1500℃以下之溫度碳化。其原因為高碳收率之樹脂由於為高分子,故在未達500℃會有因碳化
不足使細孔發達不充份之情況,另一方面在1500℃以上由於收縮大,氧化物經燒結而粗大化,故無法減小細孔尺寸而使比表面積變小。所謂非氧化性環境為氬氣環境或氮氣環境等,所謂減壓環境為133Pa(1torr)以下之環境。
熱處理前述非晶質多孔質碳時,需在非氧化性環境或減壓環境進行,但該情況之非氧化性環境如上述,意指氬氣環境或氮氣環境等,所謂減壓環境如上述意指133Pa(1torr)以下之環境。另外,熱處理溫度只要為非晶質碳結晶化之溫度以上即沒有問題,但就順利且短時間形成層狀構造(結晶化)而言,較好為800℃以上,更好為2000℃以上之溫度。但,由於溫度過高產生能量之浪費,故較好在熱處理溫度為2500℃以下進行。
首先,如圖1(a)所示,以90:10之重量比混合作為碳前驅物之聚醯胺酸樹脂(醯亞胺系樹脂)1,與作為鑄型粒子之氧化鎂(MgO,平均結晶粒徑100nm)2。接著,如圖1(b)所示,在氮氣環境中於1000℃熱處理該混合物1小時,使聚醯胺酸樹脂熱分解而獲得具備碳質壁3之燒成物。接著,如圖1(c)所示,以1mol/l之比例添加之硫酸溶液洗淨所得燒成物,使MgO完全溶出而獲得具有多數微孔4之非晶質多孔質碳5。最後,在氮氣環境中於2500℃熱處理該非晶質多孔質碳1小時,獲得多孔質碳。
以下稱如此製作之多孔質碳為本發明碳A1。
本發明碳A1之STEM(掃描透過電子顯微鏡)照片示於圖2。由圖2可了解,本發明碳A1之碳部分之至少一部分成為層狀,據此,可知碳部分之至少一部分結晶性發達。亦即,可知本發明碳A1之碳質壁3之至少一部分之結晶性發達。又,鄰接層之層間距離由於為0.33nm左右,故若為11層構造,則成層狀之碳部分之厚度成為3.3nm(0.33nm×[11-1])。且,可見到本發明碳A1成三次元網目構造(海綿狀之碳形狀),且上述介孔為開氣孔,成為氣孔部分連續之構成。
除了熱處理非晶質之多孔質碳時之溫度設為2000℃以外,餘如上述實施例1般製備多孔質碳。
以下稱如此製備之多孔質碳為本發明碳A2。
本發明碳A2之STEM照片示於圖3。由圖3可知,本發明碳A2之碳部分之至少一部分成層狀,據此,可知碳部分之至少一部分之結晶性發達。且,可見到本發明碳A2成三次元網目構造(海綿狀之碳形狀),而且,上述介孔為開氣孔,成為氣孔部分連續之構成。
除了熱處理非晶質之多孔質碳時之溫度設為1400℃以外,餘如上述實施例1般製備多孔質碳。
以下稱如此製作之多孔質碳為本發明碳A3。
除了熱處理非晶質之多孔質碳時之溫度設為900℃以外,餘如上述實施例1般製備多孔質碳。
以下稱如此製作之多孔質碳為本發明碳A4。
本發明碳A4之STEM(掃描透過電子顯微鏡)照片示於圖4。由圖4可了解,本發明碳A4之碳部分之至少一部分成層狀,據此,可知碳部分之至少一部分之結晶性發達。且,可見到本發明碳A4成三次元網目構造(海綿狀之碳形狀),而且,上述介孔為開氣孔,成為氣孔部分連續之構成。
除了使用活性碳(和光純藥工業股份有限公司製造之試藥)代替非晶質之多孔質碳作為熱處理前之碳材料,且在2000℃熱處理該活性碳以外,餘如上述實施例1般製備多孔質碳。
以下稱如此製作之多孔質碳為比較用碳Z1。
除使用活性碳(和光純藥工業股份有限公司製造之試藥)代替非晶質之多孔質碳作為熱處理前之碳材料,且在1400℃熱處理該活性碳以外,餘如上述實施例1般製備多
孔質碳。
以下稱如此製作之多孔質碳為比較用碳Z2。
除使用活性碳(和光純藥工業股份有限公司製造之試藥)代替非晶質之多孔質碳作為熱處理前之碳材料,且該活性碳未經熱處理以外,餘如上述實施例1般製備多孔質碳。
以下稱如此製作之多孔質碳為比較用碳Z3。
調查上述本發明碳A1~A4中之相對壓力與N2吸附量之關係(吸附等溫線),其結果示於圖5。
本實驗係使用比表面積測定裝置(Bellsorp 18,日本Bell(股)),以氮吸附法測定。試料係取樣約0.1g於試料盒中,在裝置之試料前處理部中,在約300℃進行脫氣處理約5小時後進行測定。
由圖5可了解,使相對壓力在0~0.1之範圍內見到本發明碳A3、A4之N2氣體吸附量變多,相對地,本發明碳A2與本發明碳A3、A4相比,N2氣體吸附量減少,且本發明碳A1幾乎不吸附N2氣體。另一方面,相對壓力超過0.1之範圍時,雖然本發明碳A1、A2相較於本發明碳A3、A4,N2氣體之吸附量少,但確認充分吸附N2氣體。進行下述實驗2以調查獲得該實驗結果之理由。
針對上述本發明碳A1~A4及比較碳Z1~Z3,求得BET比表面積、介孔容量、及微孔容量,其結果示於表1。又,BET比表面積係由吸附等溫線之結果,使用BET法算出。另外,以BJH(Berret-Joyner-Halenda)法調查介孔容量。另外,以HK(Horbath-Kawazoe)法調查微孔容量。
如由表1所了解,使用多孔質碳作為熱處理前之碳材料,且在900℃或1400℃對其熱處理之本發明碳A3、A4,在相對壓力較高時之氣體吸附能高之介孔,與面向該介孔之位置配置之在相對壓力較低時之氣體吸附能高之微孔之容量均大。因此,本發明碳A3、A4無論相對壓力高或低,氣體吸附能均高,相對於此,使用多孔質碳作為熱處理前之碳材料,在2000℃對其熱處理之本發明碳A2,相較於本發明碳A3、
A4,由於介孔與微孔之容量稍小,故無論相對壓力高或低,氣體吸附能均稍低。且,使用多孔質碳作為熱處理前之碳材料,在2500℃對其熱處理之本發明碳A1,不僅與本發明碳A3、A4相比而且與本發明碳A2相比,介孔與微孔之容量均小,尤其,微孔容量顯著變小。因此,無論相對壓力高或低,氣體吸附能均降低,尤其,由於微孔容量顯著變小,故相對壓力低時之氣體吸附能特別低。
另外,與比較碳Z1、Z2及比較碳Z3相較時,可知藉由熱處理,會使微孔顯著減少。相對於此,若比較本發明碳A2、A3、A4,可知由於具有介孔,即使熱處理溫度上升,仍可抑制微孔之減少。但,熱處理溫度提高至2500℃之本發明碳A1見到微孔減少。
基於以上理由,認為係成為如實驗1之結果者。
由上述,本發明碳A1、A2相較於本發明碳A3、A4,氣體吸附能雖降低,但相較於使用活性碳作為熱處理前之碳材料,對其熱處理時,認為氣體吸附能特別高。理由認為是,使用活性碳作為熱處理前之碳材料,將其在2000℃熱處理之比較碳Z1由於介孔與微孔之容量極小,故氣體吸附能顯著降低。
由上述,本發明碳A1、A2中,儘管至少一部份碳結晶化,但因具有介孔而維持了多孔質狀態,故認為可更充分發揮氣體吸附能等之碳所具有之優點。
又,本發明碳A2與本發明碳A3、A4相比,由於介孔與微孔之容量稍小,故BET比表面積亦稍小。且,本發
明碳A1由於介孔與微孔容量更小,故BET比表面積更小。但,相較於介孔與微孔之容量極小之比較碳Z1,本發明碳A1、A2之比表面積仍格外的大。
此外,為實現氣體吸附能之提高等,介孔容量宜較大,但並不限於本發明碳A1之0.55ml/g以上者,亦可為0.2ml/g以上。又,成為如此小之介孔容量認為係在超過2500℃之溫度熱處理多孔質碳之情況。
針對本發明碳A1、A2、A4之容積密度加以調查,其結果示於表2。
由表2可了解,本發明碳A1、A2相較於本發明碳A4,可見到容積密度較大,尤其,見到本發明碳A1之容積密度較大。此係如上述,本發明碳A1、A2相較於本發明碳A4,介孔與微孔之容量小(碳部分之容積較大),尤其,認為本發明碳A1係起因於介孔與微孔之容積極小者。
以BJH法調查本發明碳A1、A2、A4之氣孔尺寸分佈(介孔尺寸分佈),其結果示於圖6~圖8(圖6為本發明碳A1,圖7為本發明碳A2,圖8為本發明碳A4)。
如由圖6~圖8所了解,由於本發明碳A1、A2、A4中之介孔尺寸之峰為3~5nm,故可知隨著熱處理溫度之不同,介孔尺寸之峰並未變化。
調查上述本發明碳A1~A4及比較碳Z1~Z3之比電阻,其結果示於表3。實驗係於以重量比80:20之比例物理性混合各種碳與作為黏結劑之聚四氟乙烯(Dupont公司製造之Teflon(註冊商標)6J)所得混合物中添加作為溶劑之丙酮,且加工成薄片狀。在120℃下乾燥5小時使溶劑乾燥,製備100mm×100mm×1mm之薄片。接著,使用四端子法測定該薄片之比電阻。
如由表3所了解,針對使用多孔質碳作為熱處理前之碳材料時進行調查時,見到相對於熱處理溫度為2000℃以上之本發明碳A1、A2之比電阻為2.0~3.1×101Ω.cm,熱處理溫度未達2000℃之本發明碳A3、A4之比電阻為1.0×105~3.5×105Ω.cm。因此,可知本發明碳A1、A2相較於本發明碳A3、A4其比電阻顯著較小。
另一方面,針對使用活性碳作為熱處理前之碳材料之情況調查時,相對於熱處理溫度為2000℃以上之比較碳Z1之比電阻為8.0×102Ω.cm,見到熱處理溫度未達2000℃之比較碳Z2、Z3之比電阻為3.8×104~2.4×105Ω.cm。因此,比較碳Z1相較於比較碳Z2、Z3,為比電阻較小。但,可知與本發明碳A1、A2相較時比電阻較大。其理由並不確定,但認為原因係相對於本發明碳A1、A2存在有充分介孔,且層狀構造發達,比較碳Z1幾乎沒有介孔,且幾乎未發展層狀構造所致。
又,比電阻愈小愈好,但未必須為3.1×101Ω.cm以下,若為1.0×102Ω.cm以下亦可使用於各領域中。
進行本發明碳A1與本發明碳A4之X射線繞射(線源為CuKα),其結果示於圖9。
如由圖9所了解,可見到本發明碳A1在布拉格(Bragg)角度(2θ±0.2°)=26.45°下,石墨之峰(002面)顯著,相對於此,本發明碳A4在布拉格角度=26.45°下,石墨之
峰(002面)看不太到。因此,可知本發明碳A1之碳已石墨化,但本發明碳A4之碳尚未石墨化。
又,由X射線繞射結果之峰之半高寬值,使用Scherrer之式求得微結晶尺寸後,微結晶直徑約為30nm。
本發明之氣體吸附材料可使用作為非水電解質電池之負極材料、電容之電極材料等。
1‧‧‧聚醯胺酸樹脂(醯亞胺系樹脂)
2‧‧‧氧化鎂
3‧‧‧碳質壁
4‧‧‧介孔
5‧‧‧多孔質碳
圖1為顯示本發明之製造步驟之圖,該圖(a)為顯示混合聚醯胺酸樹脂與氧化鎂之狀態之說明圖,該圖(b)為顯示熱處理混合物之狀態之說明圖,該圖(c)為顯示多孔質碳之說明圖。
圖2為本發明碳A1之STEM(掃描透過電子顯微鏡)照片。
圖3為本發明碳A2之STEM照片。
圖4為本發明碳A4之STEM照片。
圖5為顯示本發明碳A1~A4之相對壓力與N2吸附量之關係之圖表。
圖6為顯示本發明碳A1之細孔徑與其比例之關係之圖表。
圖7為顯示本發明碳A2之細孔徑與其比例之關係之圖表。
圖8為顯示本發明碳A4之細孔徑與其比例之關係之圖表。
圖9為本發明碳A1及本發明之碳A4之X射線繞射圖。
Claims (16)
- 一種多孔質碳,其特徵為具備有介孔(mesoporous)與構成該介孔之外圍輪廓之碳質壁,且上述碳質壁存在有形成層狀構造之部分,其中前述介孔之尺寸為2~50nm,容積密度為0.14g/cc以上且1.0g/cc以下,前述碳質壁形成三次元網目構造。
- 如申請專利範圍第1項之多孔質碳,其比表面積為200m2/g以上。
- 如申請專利範圍第1項之多孔質碳,其中上述介孔為開氣孔,且成為氣孔部分連續之構成。
- 如申請專利範圍第1~3項中任一項之多孔質碳,其中上述介孔之容量為0.2ml/g以上。
- 如申請專利範圍第1~3項中任一項之多孔質碳,其中形成上述層狀構造之部分的厚度為1nm以上且100nm以下。
- 一種多孔質碳,其特徵為具備有介孔與構成該介孔之外圍輪廓之碳質壁,其對於CuKα線(波長1.541埃)之X射線繞射光譜中,在布拉格(Bragg)角度2θ之26.45°具有峰,其中前述介孔之尺寸為2~50nm,容積密度為0.14g/cc以上且1.0g/cc以下,前述碳質壁形成三次元網目構造。
- 如申請專利範圍第6項之多孔質碳,其比表面積為200m2/g以上。
- 如申請專利範圍第6或7項之多孔質碳,其中上述 介孔為開氣孔,且成為氣孔部分連續的構成。
- 如申請專利範圍第6或7項之多孔質碳,其中上述介孔之容量為0.2ml/g以上。
- 如申請專利範圍第6或7項之多孔質碳,其中上述碳質壁存在有形成層狀構造之部分。
- 如申請專利範圍第6或7項之多孔質碳,其比電阻為1.0×102Ω.cm以下。
- 一種多孔質碳,其特徵為具備介孔及構成該介孔之外圍輪廓之碳質壁,且比電阻為1.0×102Ω.cm以下,其中前述介孔之尺寸為2~50nm,容積密度為0.14g/cc以上且1.0g/cc以下,前述碳質壁形成三次元網目構造。
- 如申請專利範圍第12項之多孔質碳,其比表面積為200m2/g以上。
- 如申請專利範圍第12或13項之多孔質碳,其中上述介孔為開氣孔,且成為氣孔部分連續的構成。
- 如申請專利範圍第12或13項之多孔質碳,其中上述介孔之容量為0.2ml/g以上。
- 如申請專利範圍第12或13項之多孔質碳,其中上述碳質壁存在有形成層狀構造之部分。
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JP2011051830A JP5860600B2 (ja) | 2011-03-09 | 2011-03-09 | 多孔質炭素 |
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JP2015172161A (ja) * | 2014-03-12 | 2015-10-01 | 東洋炭素株式会社 | 多孔質炭素シート |
JP6175014B2 (ja) * | 2014-03-12 | 2017-08-02 | 東洋炭素株式会社 | 多孔質炭素及び多孔質炭素を用いた吸着/脱離装置 |
EP3165506A4 (en) * | 2014-07-03 | 2018-03-14 | Toray Industries, Inc. | Porous carbon material and method for manufacturing porous carbon material |
WO2016009935A1 (ja) * | 2014-07-15 | 2016-01-21 | 東レ株式会社 | 金属空気電池用電極材料 |
KR102405638B1 (ko) * | 2014-07-15 | 2022-06-07 | 도레이 카부시키가이샤 | 전극 재료 및 그것을 사용한 리튬 이온 전지 또는 리튬 이온 캐패시터 |
KR20170056582A (ko) * | 2014-09-17 | 2017-05-23 | 도레이 카부시키가이샤 | 전기 화학 커패시터용 전극 재료, 전기 화학 커패시터용 전극 도공액, 전기 화학 커패시터용 전극 및 전기 화학 커패시터 |
WO2016132903A1 (ja) * | 2015-02-19 | 2016-08-25 | 株式会社リコー | 非水電解液蓄電素子 |
CN111261871B (zh) * | 2015-03-11 | 2022-09-30 | 株式会社理光 | 非水电解液蓄电元件 |
KR102054609B1 (ko) * | 2016-03-11 | 2019-12-10 | 닛산 지도우샤 가부시키가이샤 | 연료 전지용 탄소 분말, 그리고 당해 연료 전지용 탄소 분말을 사용하는 촉매, 전극 촉매층, 막 전극 접합체 및 연료 전지 |
WO2020004674A1 (ja) * | 2018-06-29 | 2020-01-02 | 東洋炭素株式会社 | 多孔質炭素の製造方法及びこの製造方法により製造された多孔質炭素を含む電極及び触媒担体 |
EP3978112A4 (en) * | 2019-06-03 | 2023-06-21 | Toyo Tanso Co., Ltd. | SUPPORTED PLATINUM CATALYST, FUEL CELL CATHODE, FUEL CELL AND METHOD FOR PRODUCING SUPPORTED PLATINUM CATALYST |
KR20230095966A (ko) * | 2020-10-02 | 2023-06-29 | 디킨슨 코포레이션 | 페리모픽 물질의 확장 가능한 합성 |
CN112158836B (zh) * | 2020-10-13 | 2021-12-07 | 扬州工业职业技术学院 | 一种黄棕壤衍生多孔碳材料的制备方法 |
WO2023189050A1 (ja) * | 2022-03-28 | 2023-10-05 | リンテック株式会社 | 平板状多孔質炭素材料、平板状多孔質炭素材料の製造方法、及び前駆体 |
CN115548265A (zh) * | 2022-09-01 | 2022-12-30 | 天津大学 | 自支撑三维多孔碳内嵌纳米晶活性物质复合泡沫的制备方法 |
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US11584651B2 (en) | 2023-02-21 |
EP2684843A4 (en) | 2014-09-03 |
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