TWI603528B - Precursor composition and amorphous carbon material - Google Patents

Precursor composition and amorphous carbon material Download PDF

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TWI603528B
TWI603528B TW105127417A TW105127417A TWI603528B TW I603528 B TWI603528 B TW I603528B TW 105127417 A TW105127417 A TW 105127417A TW 105127417 A TW105127417 A TW 105127417A TW I603528 B TWI603528 B TW I603528B
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precursor composition
ranges
carbon material
oil
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TW201807874A (en
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yan-xu Chen
quan-neng Liao
guo-xu Lu
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Description

前驅組成物及非晶型碳材Precursor composition and amorphous carbon material

本發明是有關於一種負極用的非晶型碳材,特別是指一種用來形成負極用的非晶型碳材的前驅組成物。The present invention relates to an amorphous carbon material for a negative electrode, and more particularly to a precursor composition for forming an amorphous carbon material for a negative electrode.

中國大陸公告第102959771號專利案揭示一種鋰離子二次電池的負極碳材料用的原料油組合物。由該原料油組合物所形成的負極碳材料作為負極並應用至鋰離子二次電池中,可使該鋰離子二次電池具有快速充放電特性。The Chinese Patent Publication No. 102959771 discloses a raw material oil composition for a negative electrode carbon material of a lithium ion secondary battery. The negative electrode carbon material formed of the raw material oil composition is used as a negative electrode and applied to a lithium ion secondary battery, so that the lithium ion secondary battery can have rapid charge and discharge characteristics.

該原料油組合物是由以石油系重質油的殘油流化催化裂化裝置的塔底油、流化催化裂化裝置的塔底油,以及脫硫脫瀝油混合而成,其中,以該原料油組合物的總量為100wt%計,該殘油流化催化裂化裝置的塔底油的含量為10wt%至100wt%。該原料油組合物中的成分包含飽和成分、芳香族成分、樹脂成分及瀝青質成分。該原料油組合物的平均分子量範圍為400至600,且以該飽和成分、芳香族成分、樹脂成分及瀝青質成分的總量和為100wt%計,該飽和成分含量範圍為30wt%至50wt%,以及該芳香族成分含量範圍為50wt%至70wt%。The feedstock oil composition is a mixture of a bottom oil of a residual oil fluid catalytic cracking unit of a petroleum heavy oil, a bottom oil of a fluid catalytic cracking unit, and a desulfurization and deoiling oil. The total amount of the stock oil composition is 100% by weight, and the residual oil fluid catalytic cracking unit has a bottom oil content of 10% by weight to 100% by weight. The component in the stock oil composition contains a saturated component, an aromatic component, a resin component, and an asphaltene component. The stock oil composition has an average molecular weight ranging from 400 to 600, and the saturated component content ranges from 30% by weight to 50% by weight based on the total amount of the saturated component, the aromatic component, the resin component and the asphaltene component of 100% by weight. And the aromatic component content ranges from 50% by weight to 70% by weight.

雖透過該專利案的原料油組合物,可使該鋰離子二次電池具有快速充放電特性,但該鋰離子二次電池的電容量不佳且也未提及如何降低不可逆百分比。Although the lithium ion secondary battery can have rapid charge and discharge characteristics by the raw material oil composition of the patent, the lithium ion secondary battery has poor capacitance and does not mention how to reduce the irreversible percentage.

有鑑於此,提供一用於形成負極碳材料的原料油組合物,以使電池的電容量得以提升且不可逆百分比得以降低,是此技術領域相關技術人員可再突破的課題。In view of the above, it is a subject of those skilled in the art to provide a feedstock oil composition for forming a negative electrode carbon material to increase the capacity of the battery and reduce the irreversible percentage.

因此,本發明的第一目的,即在提供一種至少能克服先前技術的一缺點的前驅組成物。Accordingly, it is a first object of the present invention to provide a precursor composition that overcomes at least one of the disadvantages of the prior art.

於是,本發明前驅組成物用來形成負極用的非晶型碳材。該前驅組成物包含以該前驅組成物的總量為100wt%計,該碳元素含量範圍為84wt%至92.1wt%、該氫元素含量範圍為6wt%至10.3wt%、該氮元素含量範圍為0.59wt%至2wt%,及該硫元素含量範圍為0wt%至6wt%;該前驅組成物的重量平均分子量範圍為149至900,且分子量分佈指數範圍為1.33至6.87;以該前驅組成物的總量為100wt%計,該前驅組成物的灰分含量範圍為0wt%至0.0478wt%;以該前驅組成物的總量為100wt%計,該芳香烴含量範圍為15wt%至82wt%、該飽和烷烴含量範圍為12wt%至51wt%,且該環烷烴含量範圍為6wt%至34wt%。Thus, the precursor composition of the present invention is used to form an amorphous carbon material for a negative electrode. The precursor composition comprises, in a total amount of 100 wt% of the precursor composition, the carbon element content ranges from 84 wt% to 92.1 wt%, the hydrogen element content ranges from 6 wt% to 10.3 wt%, and the nitrogen element content ranges from 0.59 wt% to 2 wt%, and the sulfur element content ranges from 0 wt% to 6 wt%; the precursor composition has a weight average molecular weight ranging from 149 to 900, and a molecular weight distribution index ranging from 1.33 to 6.87; The precursor composition has an ash content ranging from 0% by weight to 0.0478% by weight based on 100% by weight of the total amount; and the aromatic hydrocarbon content is in the range of 15% by weight to 82% by weight based on the total amount of the precursor composition of 100% by weight. The alkane content ranges from 12 wt% to 51 wt%, and the naphthenic content ranges from 6 wt% to 34 wt%.

本發明的第二目的,即在提供一種非晶型碳材。A second object of the present invention is to provide an amorphous carbon material.

本發明非晶型碳材,利用上述的前驅組成物進行一處理所形成,其中,該處理包含一結焦程序及一煅燒程序。The amorphous carbon material of the present invention is formed by performing a treatment using the precursor composition described above, wherein the treatment comprises a coking process and a calcination process.

本發明的功效在於:透過調整碳元素含量、氫元素含量、氮元素含量、硫元素含量、該碳原子數目與氫原子數目的比值、重量平均分子量、分子量分佈指數、灰分含量、芳香烴含量、飽和烷烴含量,及環烷烴含量,使由該前驅組成物所形成的非晶型碳材應用至一電池作為負極時,可提升該電池的電容量及降低該電池的不可逆百分比。The effect of the present invention is to adjust the carbon content, the hydrogen element content, the nitrogen element content, the sulfur element content, the ratio of the number of carbon atoms to the number of hydrogen atoms, the weight average molecular weight, the molecular weight distribution index, the ash content, the aromatic hydrocarbon content, The saturated alkane content and the naphthenic content, when the amorphous carbon material formed by the precursor composition is applied to a battery as a negative electrode, can increase the capacity of the battery and reduce the irreversible percentage of the battery.

以下將就本發明內容進行詳細說明。The contents of the present invention will be described in detail below.

本發明將該前驅組成物進行元素分析,以取得碳元素、氫元素、氮元素及硫元素的含量。碳原子數目是利用經元素分析所得到的碳元素含量除以碳元素的原子量。氫原子數目是利用經元素分析所得到的氫元素含量除以氫元素的原子量。該分子量分佈指數指的是重量平均分子量(Mw)除以數目平均分子量(Mn)所得數值(Mw/Mn)。該灰分指的是該前驅組成物在氧氣的存在下進行燃燒後剩下不燃燒的物質的量。該芳香烴例如但不限於萘或蒽等。該飽和烷烴例如但不限於二十烷、三十烷或四十烷等。該環烷烴例如但不限於環戊烷或環己烷等。The precursor composition of the present invention is subjected to elemental analysis to obtain the contents of carbon, hydrogen, nitrogen and sulfur. The number of carbon atoms is obtained by dividing the carbon element content obtained by elemental analysis by the atomic weight of the carbon element. The number of hydrogen atoms is the atomic weight of the hydrogen element obtained by elemental analysis divided by the hydrogen element content. The molecular weight distribution index refers to a value (Mw/Mn) obtained by dividing the weight average molecular weight (Mw) by the number average molecular weight (Mn). The ash refers to the amount of non-combustible material remaining after the precursor composition is burned in the presence of oxygen. The aromatic hydrocarbon is, for example but not limited to, naphthalene or anthracene. The saturated alkane is, for example but not limited to, eicosane, triacontane or tetradecane. The cycloalkane is, for example but not limited to, cyclopentane or cyclohexane.

較佳地,該碳元素含量範圍為84wt%至92wt%及該氮元素含量範圍為0.59wt%至1wt%;該前驅組成物的灰分含量範圍為0.001wt%至0.0478wt%。Preferably, the carbon element content ranges from 84% by weight to 92% by weight and the nitrogen element content ranges from 0.59 wt% to 1 wt%; the precursor composition has an ash content ranging from 0.001 wt% to 0.0478 wt%.

較佳地,該碳元素含量範圍為91.0wt%至92.1wt%、該氫元素含量範圍為7.1wt%至7.5wt%、該氮元素含量範圍為0.62wt%至1.16wt%,及該硫元素含量範圍為0.045wt%至0.11wt%;該重量平均分子量範圍為541至900,且分子量分佈指數範圍為3.49至4.22;該前驅組成物的灰分含量範圍為0wt%至0.001wt%;該芳香烴含量範圍為64.8wt%至76.2wt%、該飽和烷烴含量範圍為12.4wt%至18.5wt%,且該環烷烴含量範圍為11.4wt%至20.1wt%。Preferably, the carbon element content ranges from 91.0 wt% to 92.1 wt%, the hydrogen element content ranges from 7.1 wt% to 7.5 wt%, the nitrogen element content ranges from 0.62 wt% to 1.16 wt%, and the sulfur element The content ranges from 0.045 wt% to 0.11 wt%; the weight average molecular weight ranges from 541 to 900, and the molecular weight distribution index ranges from 3.49 to 4.22; the precursor composition has an ash content ranging from 0 wt% to 0.001 wt%; the aromatic hydrocarbon The content ranges from 64.8 wt% to 76.2 wt%, the saturated alkane content ranges from 12.4 wt% to 18.5 wt%, and the naphthenic content ranges from 11.4 wt% to 20.1 wt%.

本發明前驅組成物為一種油料或混合多種油料調整出來,其中,該油料例如但不限於煉油產物或煉油副產物。該煉油產物或該煉油副產物是由一原油經物理分離處理及/或化學反應處理所獲得。詳細地說,該原油經分餾處理(例如常壓蒸餾程序)後會得到輕石油腦(又稱輕油)、重石油腦、煤油、柴油及殘渣油等初級油料,進一步依據所需選擇性地進行脫硫程序、加氫脫硫程序、裂解程序、重組程序、真空蒸餾程序、萃取程序或吹煉程序等精煉處理。該裂解程序例如觸媒裂解程序、熱裂解程序或氫化裂解程序等。The precursor composition of the present invention is adjusted as an oil or a mixture of a plurality of oil materials, such as, but not limited to, refinery products or refinery by-products. The refinery product or the refinery by-product is obtained by physical separation treatment and/or chemical reaction treatment of a crude oil. In detail, the crude oil is subjected to a fractionation treatment (for example, an atmospheric distillation process) to obtain primary oil materials such as light petroleum brain (also referred to as light oil), heavy petroleum brain, kerosene, diesel oil, and residual oil, and further selectively selected according to requirements. A refining process such as a desulfurization process, a hydrodesulfurization process, a cracking process, a recombination process, a vacuum distillation process, an extraction process, or a blowing process. The cleavage program is, for example, a catalytic cleavage program, a thermal lysis program or a hydrocracking program.

該煉油產物或該煉油副產物例如但不限於裂解燃料油(pyrolysis fuel oil,以下簡稱PFO)、經觸媒裂解程序取得的塔底渣油(residual of fluidized catalytic cracking,以下簡稱RFCC)、軟柏油、重質燃料油(heavy fuel oil,以下簡稱HFO)、硬柏油、經觸媒裂解程序取得的塔底渣油進行減壓蒸餾所得的油料 (以下簡稱減壓蒸餾RFCC)、裂解汽油(pyrolysis gasoline oil,以下簡稱PGO)、潤滑基礎油、脫硫渣油(residual of de-sulfur,以下簡稱RDS)、混合萃取油(combined extract,以下簡稱CE)、脫硫混合萃取油(hydrogenate desulfurization combined extract)、柏油(asphalt,又稱瀝青)或裂解渣油(residual of cracking,以下簡稱ROC)等。The refinery product or the refinery by-product such as, but not limited to, pyrolysis fuel oil (hereinafter referred to as PFO), residual of fluidized catalytic cracking (RFCC) obtained by catalytic cracking procedure, soft asphalt , heavy fuel oil (HFO), hard tar oil, oil obtained by vacuum distillation of bottom residue obtained by catalytic cracking procedure (hereinafter referred to as vacuum distillation RFCC), pyrolysis gasoline (pyrolysis gasoline) Oil, hereinafter referred to as PGO), lubricating base oil, residual of de-sulfur (hereinafter referred to as RDS), combined extract (hereinafter referred to as CE), and hydrogenate desulfurization combined extract (hydrogenate desulfurization combined extract) , asphalt (also known as asphalt) or residue of cracking (ROC).

該PFO是由原油經分餾處理取得重石油腦,再由該重石油腦經裂解程序所獲得。The PFO is obtained by fractional distillation of crude oil to obtain a heavy petroleum brain, which is obtained by a cracking procedure of the heavy petroleum brain.

該RFCC是由原油經分餾處理後殘留的殘渣油經真空蒸餾程序形成一真空製氣油(Vacuum Gas Oil),再由該真空製氣油依序經真空加氫脫硫程序及觸媒裂解程序後所獲得。The RFCC is a vacuum gas oil (Vacuum Gas Oil) formed by vacuum distillation of residual oil remaining after fractionation treatment, and then the vacuum gasification oil is sequentially subjected to a vacuum hydrodesulfurization process and a catalyst cracking procedure. Obtained later.

該軟柏油是由原油經分餾處理後殘留的殘渣油經真空蒸餾程序後殘留的塔底油。The soft asphalt is a bottom oil remaining after the residual oil remaining after the fractionation treatment of the crude oil is subjected to a vacuum distillation process.

該HFO是由PFO經過高溫吹除輕質成分所得。The HFO is obtained by blowing a light component from a PFO at a high temperature.

該硬柏油是由原油經分餾處理後殘留的殘渣油經真空蒸餾程序後殘留的塔底油,再經由萃取程序所獲得的萃餘油(即使用一萃取劑萃取出所要的油後,剩餘非在萃取劑中的油)。該萃取程序是以丙烷/丁烷作為萃取劑。The hard asphalt is a bottom oil remaining after the residual oil of the crude oil after fractionation treatment is subjected to a vacuum distillation process, and then the raffinate oil obtained by the extraction process (that is, after extracting the desired oil with an extractant, the remaining non- Oil in the extractant). The extraction procedure uses propane/butane as the extractant.

該減壓蒸餾RFCC是將上述RFCC進行真空蒸餾程序所獲得。The vacuum distillation RFCC is obtained by subjecting the above RFCC to a vacuum distillation process.

該PGO是由原油經分餾處理取得重石油腦,再由重石油腦經裂解程序所獲得。The PGO is obtained by fractional distillation of crude oil to obtain a heavy petroleum brain, and then obtained by a heavy petroleum brain by a cracking procedure.

該潤滑基礎油是由原油經分餾處理殘留的殘渣油經真空蒸餾程序形成一真空製氣油,再由該真空製氣油依序經真空加氫脫硫程序及萃取程序後所獲得。該萃取程序是利用糠醛作為萃取劑,以移除如環烷酸、多環芳香烴及雜環化合物等成分。該潤滑基礎油例如下述的第一潤滑基礎油或下述的第二潤滑基礎油等。The lubricating base oil is a vacuum gas-forming oil formed by vacuum distillation of residual oil remaining by fractional distillation, and then obtained by vacuum hydrogenation desulfurization procedure and extraction procedure. The extraction procedure utilizes furfural as an extractant to remove components such as naphthenic acids, polycyclic aromatic hydrocarbons, and heterocyclic compounds. The lubricating base oil is, for example, a first lubricating base oil described below or a second lubricating base oil described below.

該RDS是由原油經分餾處理後殘留的殘渣油經加氫脫硫程序後所獲得。該RDS例如下述的第一脫硫渣油或下述的第二脫硫渣油等。The RDS is obtained after the residual oil of the crude oil after fractionation treatment is subjected to a hydrodesulfurization process. The RDS is, for example, the first desulfurization residue described below or the second desulfurization residue described below.

該CE是由真空製氣油混合上述硬柏油的萃取油後,再經過萃取程序所獲得的萃取油(即使用一萃取劑萃取出來的油)。該萃取程序是利用糠醛作為萃取劑。The CE is an extraction oil obtained by mixing the above-mentioned hard asphalt oil with a vacuum gas oil and then subjected to an extraction process (that is, an oil extracted by using an extractant). The extraction procedure utilizes furfural as an extractant.

該脫硫混合萃取油是由CE經加氫脫硫程序所獲得。The desulfurization mixed extraction oil is obtained by CE hydrodesulfurization procedure.

該柏油是由原油經分餾處理殘留的殘渣油經真空蒸餾程序後殘留的塔底油,再經由吹煉程序後所獲得。The asphalt is obtained from a bottom oil remaining after the residual oil of the crude oil by fractional distillation and subjected to a vacuum distillation process, and then obtained through a blowing process.

該ROC是由原油經分餾處理殘留的殘渣油依序經真空加氫脫硫程序及裂解程序後所獲得。The ROC is obtained by sequentially subjecting the residual oil remaining by the fractionation treatment to a vacuum hydrodesulfurization procedure and a cracking procedure.

本發明列舉出該PFO、該RFCC、該HFO、該硬柏油、該PGO、該潤滑基礎油、該RDS、該CE、該脫硫混合萃取油、該柏油及該ROC的一種或數種組成態樣,但不限於該等組成態樣,且將該等態樣的碳元素(以下簡寫為C)含量(wt%)、氫元素(以下簡寫為H)含量(wt%)、氮元素(以下簡寫為N)含量(wt%)、硫元素(以下簡寫為S)含量(wt%)、碳原子數目與氫原子數目的比值(以下簡寫為C/H)、重量平均分子量(weight average molecular weight,以下簡寫為Mw)、數目平均分子量(number average molecular weight,以下簡寫為Mn)、峰平均分子量(peak average molecular weight,以下簡寫為Mp,為分子量分佈中最高峰的值)、分子量分佈指數(以下簡寫為Mw/Mn)、灰分含量、芳香烴(以下簡寫為Ca)含量(wt%)、飽和烷烴(以下簡寫為Cp)含量(wt%),及環烷烴(以下簡寫為Cn)含量(wt%),以表1及表2呈現。The present invention exemplifies one or several compositions of the PFO, the RFCC, the HFO, the hard asphalt, the PGO, the lubricating base oil, the RDS, the CE, the desulfurized mixed extraction oil, the asphalt, and the ROC. Such as, but not limited to, such a compositional form, and the carbon element (hereinafter abbreviated as C) content (wt%), hydrogen element (hereinafter abbreviated as H) content (wt%), and nitrogen element (hereinafter referred to as the equivalent) Abbreviated as N) content (wt%), sulfur element (hereinafter abbreviated as S) content (wt%), ratio of number of carbon atoms to number of hydrogen atoms (hereinafter abbreviated as C/H), weight average molecular weight (weight average molecular weight) , hereinafter abbreviated as Mw), number average molecular weight (hereinafter abbreviated as Mn), peak average molecular weight (hereinafter abbreviated as Mp, which is the highest peak value in the molecular weight distribution), and molecular weight distribution index (abbreviated as Mw) The following is abbreviated as Mw/Mn), ash content, aromatic hydrocarbon (hereinafter abbreviated as Ca) content (wt%), saturated alkane (hereinafter abbreviated as Cp) content (wt%), and naphthenic hydrocarbon (hereinafter abbreviated as Cn) content (hereinafter abbreviated as Cn) ( Wt%), presented in Tables 1 and 2.

表1 <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> --:表示未量測 </td><td> C </td><td> H </td><td> N </td><td> S </td><td> C/H </td><td> Mn </td></tr><tr><td> PFO </td><td> 90.99 </td><td> 8.30 </td><td> 0.63 </td><td> 0.15 </td><td> 0.91 </td><td> 152 </td></tr><tr><td> RFCC </td><td> 88.96 </td><td> 9.70 </td><td> 0.48 </td><td> 0.80 </td><td> 0.76 </td><td> 167 </td></tr><tr><td> HFO </td><td> 92.04 </td><td> 7.12 </td><td> 0.62 </td><td> 0.11 </td><td> 1.07 </td><td> 254 </td></tr><tr><td> 硬柏油 </td><td> 84.34 </td><td> 9.56 </td><td> 1.51 </td><td> 3.66 </td><td> 0.73 </td><td> 779 </td></tr><tr><td> PGO </td><td> 90.75 </td><td> 8.28 </td><td> 0.50 </td><td> 0.10 </td><td> 0.91 </td><td> 101 </td></tr><tr><td> 第一潤滑基礎油 </td><td> 88.44 </td><td> 8.91 </td><td> 0.61 </td><td> 6.06 </td><td> 0.82 </td><td> 192 </td></tr><tr><td> 第二潤滑基礎油 </td><td> 84.65 </td><td> 10.43 </td><td> 0.67 </td><td> 4.60 </td><td> 0.67 </td><td> 326 </td></tr><tr><td> 第一脫硫渣油 </td><td> 87.40 </td><td> 11.49 </td><td> 0.67 </td><td> 0.61 </td><td> 0.63 </td><td> 454 </td></tr><tr><td> CE </td><td> 84.23 </td><td> 8.99 </td><td> 1.36 </td><td> 6.28 </td><td> 0.78 </td><td> 234 </td></tr><tr><td> 脫硫混合萃取油 </td><td> 87.26 </td><td> 10.27 </td><td> 1.96 </td><td> 0.43 </td><td> 0.71 </td><td> 231 </td></tr><tr><td> 柏油 </td><td> 90.51 </td><td> 5.48 </td><td> 0.85 </td><td> -- </td><td> 1.38 </td><td> 189 </td></tr><tr><td> ROC </td><td> 91.28 </td><td> 8.08 </td><td> 0.61 </td><td> 0.79 </td><td> 0.94 </td><td> 133 </td></tr><tr><td> 第二脫硫渣油 </td><td> 86.25 </td><td> 12.40 </td><td> 0.99 </td><td> 0.43 </td><td> 0.58 </td><td> 474 </td></tr></TBODY></TABLE>Table 1         <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> --: indicates unmeasured</td><td> C </td><td > H </td><td> N </td><td> S </td><td> C/H </td><td> Mn </td></tr><tr><td> PFO </td><td> 90.99 </td><td> 8.30 </td><td> 0.63 </td><td> 0.15 </td><td> 0.91 </td><td> 152 < /td></tr><tr><td> RFCC </td><td> 88.96 </td><td> 9.70 </td><td> 0.48 </td><td> 0.80 </td> <td> 0.76 </td><td> 167 </td></tr><tr><td> HFO </td><td> 92.04 </td><td> 7.12 </td><td> 0.62 </td><td> 0.11 </td><td> 1.07 </td><td> 254 </td></tr><tr><td> Hard tar oil</td><td> 84.34 < /td><td> 9.56 </td><td> 1.51 </td><td> 3.66 </td><td> 0.73 </td><td> 779 </td></tr><tr> <td> PGO </td><td> 90.75 </td><td> 8.28 </td><td> 0.50 </td><td> 0.10 </td><td> 0.91 </td><td > 101 </td></tr><tr><td> First Lubricating Base Oil</td><td> 88.44 </td><td> 8.91 </td><td> 0.61 </td>< Td> 6.06 </td><td> 0.82 </td><td> 192 </td></tr><tr><td> Second Lubricating Base Oil</td><td> 84.65 </td> <td> 10.43 </td><td> 0.67 </td><td> 4.60 </td><td> 0.67 </td><td> 326 < /td></tr><tr><td> First Desulfurization Residue</td><td> 87.40 </td><td> 11.49 </td><td> 0.67 </td><td> 0.61 </td><td> 0.63 </td><td> 454 </td></tr><tr><td> CE </td><td> 84.23 </td><td> 8.99 </ Td><td> 1.36 </td><td> 6.28 </td><td> 0.78 </td><td> 234 </td></tr><tr><td> Desulfurization mixed extraction oil< /td><td> 87.26 </td><td> 10.27 </td><td> 1.96 </td><td> 0.43 </td><td> 0.71 </td><td> 231 </td ></tr><tr><td> tar</td><td> 90.51 </td><td> 5.48 </td><td> 0.85 </td><td> -- </td>< Td> 1.38 </td><td> 189 </td></tr><tr><td> ROC </td><td> 91.28 </td><td> 8.08 </td><td> 0.61 </td><td> 0.79 </td><td> 0.94 </td><td> 133 </td></tr><tr><td> second desulfurization residue</td><td > 86.25 </td><td> 12.40 </td><td> 0.99 </td><td> 0.43 </td><td> 0.58 </td><td> 474 </td></tr> </TBODY></TABLE>

表2 <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> --:表示未量測 </td><td> Mw </td><td> Mp </td><td> Mw/Mn </td><td> 灰分 </td><td> Ca </td><td> Cp </td><td> Cn </td></tr><tr><td> PFO </td><td> 653 </td><td> 97 </td><td> 4.30 </td><td> <0.001 </td><td> 63.1 </td><td> 20.4 </td><td> 16.5 </td></tr><tr><td> RFCC </td><td> 280 </td><td> 115 </td><td> 1.68 </td><td> 0.0035 </td><td> 39.9 </td><td> 35.0 </td><td> 25.2 </td></tr><tr><td> HFO </td><td> 886 </td><td> 329 </td><td> 3.49 </td><td> <0.001 </td><td> 64.8 </td><td> 18.5 </td><td> 16.7 </td></tr><tr><td> 硬柏油 </td><td> 2476 </td><td> 1093 </td><td> 3.53 </td><td> 0.0478 </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> PGO </td><td> 149 </td><td> 83 </td><td> 1.48 </td><td> <0.001 </td><td> 65.7 </td><td> 21.5 </td><td> 12.9 </td></tr><tr><td> 第一潤滑基礎油 </td><td> 255 </td><td> 269 </td><td> 1.33 </td><td> <0.001 </td><td> 49.4 </td><td> 30.5 </td><td> 20.1 </td></tr><tr><td> 第二潤滑基礎油 </td><td> 488 </td><td> 482 </td><td> 1.50 </td><td> <0.001 </td><td> 41.1 </td><td> 33.8 </td><td> 25.1 </td></tr><tr><td> 第一脫硫渣油 </td><td> 1154 </td><td> 918 </td><td> 2.54 </td><td> 0.0020 </td><td> 15.0 </td><td> 50.8 </td><td> 34.2 </td></tr><tr><td> CE </td><td> 329 </td><td> 314 </td><td> 1.41 </td><td> <0.001 </td><td> 40.8 </td><td> 33.1 </td><td> 26.1 </td></tr><tr><td> 脫硫混合萃取油 </td><td> 314 </td><td> 285 </td><td> 1.36 </td><td> <0.001 </td><td> 32.5 </td><td> 36.3 </td><td> 31.2 </td></tr><tr><td> 柏油 </td><td> 410 </td><td> 215 </td><td> 2.17 </td><td> -- </td><td> 82.1 </td><td> 12.1 </td><td> 5.8 </td></tr><tr><td> ROC </td><td> 189 </td><td> 112 </td><td> 1.42 </td><td> 0.1612 </td><td> 70.5 </td><td> 17.0 </td><td> 12.6 </td></tr><tr><td> 第二脫硫渣油 </td><td> 1686 </td><td> 608 </td><td> 3.56 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr></TBODY></TABLE>Table 2         <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> --: indicates unmeasured</td><td> Mw </td><td > Mp </td><td> Mw/Mn </td><td> ash</td><td> Ca </td><td> Cp </td><td> Cn </td></ Tr><tr><td> PFO </td><td> 653 </td><td> 97 </td><td> 4.30 </td><td> <0.001 </td><td> 63.1 </td><td> 20.4 </td><td> 16.5 </td></tr><tr><td> RFCC </td><td> 280 </td><td> 115 </td ><td> 1.68 </td><td> 0.0035 </td><td> 39.9 </td><td> 35.0 </td><td> 25.2 </td></tr><tr><td > HFO </td><td> 886 </td><td> 329 </td><td> 3.49 </td><td> <0.001 </td><td> 64.8 </td><td> 18.5 </td><td> 16.7 </td></tr><tr><td> Hard tar </td><td> 2476 </td><td> 1093 </td><td> 3.53 < /td><td> 0.0478 </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> PGO < /td><td> 149 </td><td> 83 </td><td> 1.48 </td><td> <0.001 </td><td> 65.7 </td><td> 21.5 </ Td><td> 12.9 </td></tr><tr><td> First Lubricating Base Oil</td><td> 255 </td><td> 269 </td><td> 1.33 < /td><td> <0.001 </td><td> 49.4 </td><td> 30.5 </td><td> 20.1 </td></tr><tr><td> Second Lubricating Base Oil</td><td> 488 </td><td> 482 </td><td> 1.50 </td><td> <0.001 </td><td> 41.1 </td> <td> 33.8 </td><td> 25.1 </td></tr><tr><td> First Desulfurization Residue</td><td> 1154 </td><td> 918 </ Td><td> 2.54 </td><td> 0.0020 </td><td> 15.0 </td><td> 50.8 </td><td> 34.2 </td></tr><tr>< Td> CE </td><td> 329 </td><td> 314 </td><td> 1.41 </td><td> <0.001 </td><td> 40.8 </td><td > 33.1 </td><td> 26.1 </td></tr><tr><td> Desulfurization mixed extraction oil</td><td> 314 </td><td> 285 </td>< Td> 1.36 </td><td> <0.001 </td><td> 32.5 </td><td> 36.3 </td><td> 31.2 </td></tr><tr><td> Asphalt</td><td> 410 </td><td> 215 </td><td> 2.17 </td><td> -- </td><td> 82.1 </td><td> 12.1 </td><td> 5.8 </td></tr><tr><td> ROC </td><td> 189 </td><td> 112 </td><td> 1.42 </td ><td> 0.1612 </td><td> 70.5 </td><td> 17.0 </td><td> 12.6 </td></tr><tr><td> second desulfurization residue< /td><td> 1686 </td><td> 608 </td><td> 3.56 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr></TBODY></TABLE>

一非晶型碳材利用本發明前驅組成物進行一處理所形成。該處理包含一結焦程序及一煅燒程序。該結焦程序目的在於使該前驅組成物結焦,而形成一結焦產物。該結焦程序包括一加熱步驟及一冷卻步驟。較佳地,該加熱步驟的操作溫度範圍為400℃至600℃。更佳地,該加熱步驟的操作溫度範圍為500℃至550℃。較佳地,該加熱步驟的操作時間範圍為1小時至16小時。更佳地,該加熱步驟的操作時間範圍為4小時至8小時。較佳地,該加熱步驟的操作壓力範圍為2atm至40atm。較佳地,該加熱步驟的升溫速率範圍為5℃/min至10℃/min。該冷卻步驟是自該加熱步驟的溫度降至一預定溫度。該預定溫度例如室溫。該煅燒程序目的在於使該結焦產物碳化,形成一非晶型碳材。該碳化過程會使得該結焦產物進行縮聚反應或/及脫氫反應或/及裂解反應,使該結焦產物的結構重新排列。較佳地,該煅燒程序的操作溫度範圍為1000℃至1200℃。較佳地,該煅燒程序的操作時間範圍為4小時以上。較佳地,該非晶型碳材具有一不大於0.01cm 3/g的孔體積。該處理還包含一在該煅燒程序後的研磨程序。該研磨程序的目的在於使該非晶型碳材的粒徑及/或形狀均一,形成一經研磨的非晶型碳材。該處理還包含一在該研磨程序後的粒徑分級程序。該粒徑分級程序目的在於將該經研磨的非晶型碳材依照不同粒徑進行分類,且將粒徑小於32μm的經研磨的非晶型碳材歸為一類。 An amorphous carbon material is formed by a treatment using the precursor composition of the present invention. The process includes a coking process and a calcination process. The coking process is intended to coke the precursor composition to form a coked product. The coking process includes a heating step and a cooling step. Preferably, the heating step has an operating temperature in the range of from 400 ° C to 600 ° C. More preferably, the heating step has an operating temperature in the range of from 500 ° C to 550 ° C. Preferably, the heating step has an operating time ranging from 1 hour to 16 hours. More preferably, the heating step has an operating time ranging from 4 hours to 8 hours. Preferably, the heating step has an operating pressure in the range of 2 atm to 40 atm. Preferably, the heating step has a heating rate in the range of 5 ° C / min to 10 ° C / min. The cooling step is to reduce the temperature from the heating step to a predetermined temperature. The predetermined temperature is, for example, room temperature. The calcination procedure aims to carbonize the coked product to form an amorphous carbon material. The carbonization process causes the coked product to undergo a polycondensation reaction and/or a dehydrogenation reaction and/or a cleavage reaction to rearrange the structure of the coked product. Preferably, the calcination procedure has an operating temperature in the range of from 1000 °C to 1200 °C. Preferably, the calcination procedure has an operating time range of more than 4 hours. Preferably, the amorphous carbon material has a pore volume of not more than 0.01 cm 3 /g. The process also includes a grinding procedure after the calcination process. The purpose of the polishing procedure is to uniformize the particle size and/or shape of the amorphous carbon material to form a ground amorphous carbon material. The process also includes a particle size fractionation procedure following the grinding procedure. The particle size fractionation program aims to classify the ground amorphous carbon material according to different particle diameters, and classify the ground amorphous carbon materials having a particle diameter of less than 32 μm into one class.

一負極包含一由一成膜組分所形成的導電膜。該成膜組分包含上述非晶型碳材及黏結劑。以該導電膜的總量為100wt%計,該非晶型碳材的含量範圍為90wt%至92wt%。該黏結劑例如但不限於聚偏二氟乙烯(polyvinylidenefluoride,簡稱PVDF)。該聚偏二氟乙烯例如吳羽化學工業社製且商品名為KF9200。以該導電膜的總量為100wt%計,該黏結劑的含量範圍為3wt%至7wt%。為使該導電膜具有更佳的導電度,較佳地,該成膜組分還包含助導劑。該助導劑例如但不限於導電碳材。該導電碳材例如但不限於購自Timcal且商品名為Super P的導電碳黑與KS-6的導電石墨。以該導電膜的總量為100wt%計,該助導劑的含量範圍為1wt%至4wt%。該導電膜的形成方式是將該成膜組分與一溶劑混合,並藉由成膜處理及乾燥處理來進行。該成膜處理例如但不限於塗佈方式。該溶劑例如但不限於N-甲基吡咯烷酮(N-methyl-2-pyrrolidone,簡稱NMP)。A negative electrode comprises a conductive film formed of a film-forming component. The film-forming component comprises the above amorphous carbon material and a binder. The amorphous carbon material is contained in an amount ranging from 90% by weight to 92% by weight based on 100% by weight of the total of the conductive film. The binder is, for example but not limited to, polyvinylidenefluoride (PVDF). The polyvinylidene fluoride is, for example, manufactured by Kureha Chemical Industry Co., Ltd. and traded under the trade name KF9200. The binder is contained in an amount ranging from 3 wt% to 7 wt%, based on 100% by weight of the total of the conductive film. In order to make the conductive film have better conductivity, preferably, the film-forming component further contains a co-ducing agent. The coagulant is for example but not limited to a conductive carbon material. The conductive carbon material is, for example but not limited to, conductive graphite obtained from Timcal and sold under the trade name Super P, and conductive graphite of KS-6. The content of the auxiliary agent ranges from 1% by weight to 4% by weight based on 100% by weight of the total of the conductive film. The conductive film is formed by mixing the film-forming component with a solvent and performing film formation treatment and drying treatment. The film forming process is, for example but not limited to, a coating method. The solvent is, for example but not limited to, N-methyl-2-pyrrolidone (NMP).

該負極還包含一用來承載該導電膜的導電載體。該導電載體例如但不限於銅箔。該負極的製作方法採以往用來製作負極的方法,舉例來說,使用塗佈機將該成膜組分塗佈在銅箔(厚度14微米)上,並在低於200℃的溫度下進行至少8小時以上的真空乾燥處理,即可獲得該負極。視後續尺寸等需求,進一步進行滾壓處理與裁切處理。The negative electrode further includes a conductive carrier for carrying the conductive film. The conductive carrier is for example but not limited to a copper foil. The negative electrode is produced by a conventional method for producing a negative electrode. For example, the film-forming component is coated on a copper foil (thickness: 14 μm) using a coater, and is carried out at a temperature lower than 200 ° C. The negative electrode can be obtained by vacuum drying treatment for at least 8 hours. Further, the rolling process and the cutting process are performed depending on the subsequent dimensions and the like.

該鋰電池包含上述負極。該鋰電池的製作方法採以往用來製作鋰電池的方法,舉例來說,於手套箱中,將一作為正極的鋰金屬薄片、上述負極、電解液及隔離膜組裝成 CR2032鈕扣型半電池。該電解液包含鋰鹽、溶劑及添加劑。該鋰鹽例如但不限於六氟磷酸鋰(lithium hexafluorophosphate,簡稱LiPF 6)。該溶劑例如但不限於碳酸乙烯酯(ethylene carbonate,簡稱EC)、碳酸二甲酯(dimethyl carbonate ,簡稱DMC),或碳酸甲乙酯(ethyl methyl carbonate,簡稱EMC)等。該添加劑例如但不限於碳酸亞乙烯酯(vinylene Carbonate,簡稱VC)。該隔離膜例如但不限於Celgard公司製的產品。 The lithium battery includes the above negative electrode. The lithium battery is produced by a method for producing a lithium battery. For example, in a glove box, a lithium metal foil as a positive electrode, the negative electrode, an electrolyte, and a separator are assembled into a CR2032 button type half-cell. The electrolyte contains a lithium salt, a solvent, and an additive. The lithium salt is, for example but not limited to, lithium hexafluorophosphate (LiPF 6 for short). The solvent is, for example but not limited to, ethylene carbonate (EC), dimethyl carbonate (DMC), or ethyl methyl carbonate (EMC). The additive is, for example but not limited to, vinylene carbonate (VC). The separator is, for example but not limited to, a product manufactured by Celgard.

本發明將就以下實施例來作進一步說明,但應瞭解的是,該實施例僅為例示說明之用,而不應被解釋為本發明實施之限制。The present invention will be further illustrated by the following examples, but it should be understood that this embodiment is intended to be illustrative only and not to be construed as limiting.

實施例1  前驅組成物Example 1 Precursor Composition

將2重量份的PFO與1重量份的第一脫硫渣油混合,形成本發明前驅組成物。2 parts by weight of PFO is mixed with 1 part by weight of the first desulfurized residual oil to form a precursor composition of the present invention.

實施例2至4及比較例1至9Examples 2 to 4 and Comparative Examples 1 to 9

實施例2至4及比較例1至9是以與實施例1相同的步驟來製備前驅組成物,不同的地方在於:改變原料的種類及其使用量,該原料的種類及其使用量如表3及表4。Examples 2 to 4 and Comparative Examples 1 to 9 were prepared in the same manner as in Example 1 except that the kind of the raw material and the amount thereof were changed, and the kind of the raw material and the amount thereof were as follows. 3 and Table 4.

C 、H 、N及 S含量分析:使用元素分析儀(廠牌:Elementar Analysensysteme;型號:GmbH)進行分析。Analysis of C, H, N and S content: analysis using an elemental analyzer (label: Elementar Analysensysteme; model: GmbH).

Mw分析:以膠體滲透層析儀(Gel Permeation Chromatography,廠牌:HP;型號:HP1090M),利用多種已知絕對分子量的聚苯乙烯當標準品,進行分析。Mw analysis: Gel permeation Chromatography (Gel Permeation Chromatography, brand: HP; model: HP1090M), using a variety of known absolute molecular weight polystyrene as a standard, analysis.

Mn分析:以膠體滲透層析儀(Gel Permeation Chromatography,廠牌:HP;型號: HP1090M),利用多種已知絕對分子量的聚苯乙烯當標準品,進行分析。Mn analysis: Gel permeation Chromatography (Gel Permeation Chromatography, brand: HP; model: HP1090M), using a variety of known absolute molecular weight polystyrene as a standard, analysis.

Mp分析:以膠體滲透層析儀(Gel Permeation Chromatography,廠牌:HP;型號: HP1090M),利用多種已知絕對分子量的聚苯乙烯當標準品,進行分析。Mp analysis: Gel permeation Chromatography (Gel Permeation Chromatography, brand: HP; model: HP1090M), using a variety of known absolute molecular weight polystyrene as a standard, analysis.

灰分分析:依據ASTMD482標準測手法進行分析。Ash analysis: analysis according to the ASTM D482 standard test method.

Ca、Cp及Cn含量分析:將0.25毫升的實施例1至3及比較例1至9的前驅組成物分別與0.5毫升的溶劑[包含CDCl 3及0.046 M 的三乙醯丙酮鐵(III)]混合並分別形成12個待測品。將該等待測品分別置入5 mm的試管中,並以 13C-核磁共振光譜儀(廠牌:Agilent;型號:400-MR DDR2)進行量測。該Ca為化學位移在105ppm至165ppm間的峰,該Cp及Cn為化學位移在0ppm至55ppm間的峰,其中,該Cp為尖峰,而Cn為駝峰。依據各峰的積分面積計算出Ca、Cp及Cn的含量。 Ca, Cp, and Cn content analysis: 0.25 ml of the precursor compositions of Examples 1 to 3 and Comparative Examples 1 to 9 were respectively added to 0.5 ml of a solvent [containing CDCl 3 and 0.046 M of triethylsulfonium iron (III)] Mix and form 12 test articles separately. The waiting samples were placed in a 5 mm test tube and measured by a 13 C-NMR spectrometer (label: Agilent; model: 400-MR DDR2). The Ca is a peak having a chemical shift between 105 ppm and 165 ppm, and the Cp and Cn are peaks having a chemical shift between 0 ppm and 55 ppm, wherein the Cp is a peak and Cn is a hump. The contents of Ca, Cp and Cn were calculated from the integrated areas of the peaks.

表3 <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> 實施例 </td><td> C </td><td> H </td><td> N </td><td> S </td><td> C/H </td><td> Mn </td><td> Mw </td></tr><tr><td> 1 </td><td> 2重量份 PFO </td><td> 1重量份 第一脫硫渣油 </td><td> 89.79 </td><td> 9.36 </td><td> 0.64 </td><td> 0.30 </td><td> 0.80 </td><td> 253 </td><td> 820 </td></tr><tr><td> 2 </td><td> 1重量份HFO </td><td> 92.04 </td><td> 7.12 </td><td> 0.62 </td><td> 0.11 </td><td> 1.07 </td><td> 254 </td><td> 886 </td></tr><tr><td> 3 </td><td> 1重量份 PGO </td><td> 1重量份 第一脫硫渣油 </td><td> 89.08 </td><td> 9.89 </td><td> 0.59 </td><td> 0.36 </td><td> 0.75 </td><td> 278 </td><td> 652 </td></tr><tr><td> 4 </td><td> 1重量份脫硫混合萃取油 </td><td> 87.26 </td><td> 10.27 </td><td> 1.96 </td><td> 0.43 </td><td> 0.71 </td><td> 231 </td><td> 314 </td></tr><tr><td> 比較例 </td><td> C </td><td> H </td><td> N </td><td> S </td><td> C/H </td><td> Mn </td><td> Mw </td></tr><tr><td> 1 </td><td> 1重量份第一潤滑基礎油 </td><td> 88.44 </td><td> 8.91 </td><td> 0.61 </td><td> 6.06 </td><td> 0.82 </td><td> 192 </td><td> 255 </td></tr><tr><td> 2 </td><td> 1重量份第二潤滑基礎油 </td><td> 84.65 </td><td> 10.43 </td><td> 0.67 </td><td> 4.60 </td><td> 0.67 </td><td> 326 </td><td> 488 </td></tr><tr><td> 3 </td><td> 1重量份第一脫硫渣油 </td><td> 87.40 </td><td> 11.49 </td><td> 0.67 </td><td> 0.61 </td><td> 0.63 </td><td> 454 </td><td> 1154 </td></tr><tr><td> 4 </td><td> 2重量份 PGO </td><td> 1重量份 第一脫硫渣油 </td><td> 89.63 </td><td> 9.35 </td><td> 0.56 </td><td> 0.27 </td><td> 0.80 </td><td> 219 </td><td> 484 </td></tr><tr><td> 5 </td><td> 1重量份 PFO </td><td> 1重量份 第一脫硫渣油 </td><td> 89.20 </td><td> 9.90 </td><td> 0.65 </td><td> 0.38 </td><td> 0.75 </td><td> 303 </td><td> 904 </td></tr><tr><td> 6 </td><td> 3重量份 PGO </td><td> 1重量份 第一脫硫渣油 </td><td> 89.91 </td><td> 9.08 </td><td> 0.54 </td><td> 0.23 </td><td> 0.83 </td><td> 189 </td><td> 400 </td></tr><tr><td> 7 </td><td> 1重量份 HFO </td><td> 1重量份 第一脫硫渣油 </td><td> 89.72 </td><td> 9.31 </td><td> 0.65 </td><td> 0.36 </td><td> 0.80 </td><td> 354 </td><td> 1020 </td></tr><tr><td> 8 </td><td> 1重量份CE </td><td> 84.23 </td><td> 8.99 </td><td> 1.36 </td><td> 6.28 </td><td> 0.78 </td><td> 234 </td><td> 329 </td></tr><tr><td> 9 </td><td> 1重量份 HFO </td><td> 1重量份 RFCC </td><td> 90.50 </td><td> 8.41 </td><td> 0.55 </td><td> 0.46 </td><td> 0.90 </td><td> 211 </td><td> 583 </td></tr></TBODY></TABLE>table 3         <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> Example</td><td> C </td><td> H </td ><td> N </td><td> S </td><td> C/H </td><td> Mn </td><td> Mw </td></tr><tr> <td> 1 </td><td> 2 parts by weight of PFO </td><td> 1 part by weight of the first desulfurized residue</td><td> 89.79 </td><td> 9.36 </td ><td> 0.64 </td><td> 0.30 </td><td> 0.80 </td><td> 253 </td><td> 820 </td></tr><tr><td > 2 </td><td> 1 part by weight HFO </td><td> 92.04 </td><td> 7.12 </td><td> 0.62 </td><td> 0.11 </td>< Td> 1.07 </td><td> 254 </td><td> 886 </td></tr><tr><td> 3 </td><td> 1 part by weight PGO </td>< Td> 1 part by weight of the first desulfurization residue</td><td> 89.08 </td><td> 9.89 </td><td> 0.59 </td><td> 0.36 </td><td> 0.75 </td><td> 278 </td><td> 652 </td></tr><tr><td> 4 </td><td> 1 part by weight of desulfurized mixed extraction oil</td ><td> 87.26 </td><td> 10.27 </td><td> 1.96 </td><td> 0.43 </td><td> 0.71 </td><td> 231 </td>< Td> 314 </td></tr><tr><td> Comparative Example </td><td> C </td><td> H </td><td> N </td><td> S </td><td> C/H </td><td> Mn </td><td> Mw </td></tr><tr><td> 1 </td><td> 1 part by weight of the first lubricating base oil</td><td> 88.44 </td><td> 8.91 </td><td> 0.61 </td><td> 6.06 </td ><td> 0.82 </td><td> 192 </td><td> 255 </td></tr><tr><td> 2 </td><td> 1 part by weight of the second lubrication foundation Oil</td><td> 84.65 </td><td> 10.43 </td><td> 0.67 </td><td> 4.60 </td><td> 0.67 </td><td> 326 < /td><td> 488 </td></tr><tr><td> 3 </td><td> 1 part by weight of the first desulfurization residue</td><td> 87.40 </td> <td> 11.49 </td><td> 0.67 </td><td> 0.61 </td><td> 0.63 </td><td> 454 </td><td> 1154 </td></ Tr><tr><td> 4 </td><td> 2 parts by weight of PGO </td><td> 1 part by weight of the first desulfurization residue</td><td> 89.63 </td><td > 9.35 </td><td> 0.56 </td><td> 0.27 </td><td> 0.80 </td><td> 219 </td><td> 484 </td></tr> <tr><td> 5 </td><td> 1 part by weight of PFO </td><td> 1 part by weight of the first desulfurized residue</td><td> 89.20 </td><td> 9.90 </td><td> 0.65 </td><td> 0.38 </td><td> 0.75 </td><td> 303 </td><td> 904 </td></tr><tr ><td> 6 </td><td> 3 parts by weight of PGO </td><td> 1 part by weight of the first desulfurization residue</td><td> 89.91 </td><td> 9.08 </ Td><td> 0.54 </td><t d> 0.23 </td><td> 0.83 </td><td> 189 </td><td> 400 </td></tr><tr><td> 7 </td><td> 1 Parts by weight HFO </td><td> 1 part by weight of the first desulfurization residue</td><td> 89.72 </td><td> 9.31 </td><td> 0.65 </td><td> 0.36 </td><td> 0.80 </td><td> 354 </td><td> 1020 </td></tr><tr><td> 8 </td><td> 1 part by weight CE </td><td> 84.23 </td><td> 8.99 </td><td> 1.36 </td><td> 6.28 </td><td> 0.78 </td><td> 234 < /td><td> 329 </td></tr><tr><td> 9 </td><td> 1 part by weight of HFO </td><td> 1 part by weight of RFCC </td><td > 90.50 </td><td> 8.41 </td><td> 0.55 </td><td> 0.46 </td><td> 0.90 </td><td> 211 </td><td> 583 </td></tr></TBODY></TABLE>

表4 <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> 實施例 </td><td> Mp </td><td> Mw/Mn </td><td> 灰分 </td><td> Ca </td><td> Cp </td><td> Cn </td></tr><tr><td> 1 </td><td> 2重量份 PFO </td><td> 1重量份 第一脫硫渣油 </td><td> 371 </td><td> 3.24 </td><td> <0.002 </td><td> 47.1 </td><td> 30.5 </td><td> 22.4 </td></tr><tr><td> 2 </td><td> 1重量份HFO </td><td> 329 </td><td> 3.49 </td><td> <0.001 </td><td> 64.8 </td><td> 18.5 </td><td> 16.7 </td></tr><tr><td> 3 </td><td> 1重量份 PGO </td><td> 1重量份 第一脫硫渣油 </td><td> 501 </td><td> 2.35 </td><td> <0.002 </td><td> 40.2 </td><td> 36.2 </td><td> 23.6 </td></tr><tr><td> 4 </td><td> 1重量份脫硫混合萃取油 </td><td> 285 </td><td> 1.36 </td><td> <0.001 </td><td> 32.5 </td><td> 36.3 </td><td> 31.2 </td></tr><tr><td> 比較例 </td><td> Mp </td><td> Mw/Mn </td><td> 灰分 </td><td> Ca </td><td> Cp </td><td> Cn </td></tr><tr><td> 1 </td><td> 1重量份第一潤滑基礎油 </td><td> 269 </td><td> 1.33 </td><td> <0.001 </td><td> 49.4 </td><td> 30.5 </td><td> 20.1 </td></tr><tr><td> 2 </td><td> 1重量份第二潤滑基礎油 </td><td> 482 </td><td> 1.50 </td><td> <0.001 </td><td> 41.1 </td><td> 33.8 </td><td> 25.1 </td></tr><tr><td> 3 </td><td> 1重量份第一脫硫渣油 </td><td> 918 </td><td> 2.54 </td><td> 0.0020 </td><td> 15.0 </td><td> 50.8 </td><td> 34.2 </td></tr><tr><td> 4 </td><td> 2重量份 PGO </td><td> 1重量份 第一脫硫渣油 </td><td> 361 </td><td> 2.21 </td><td> <0.002 </td><td> 48.8 </td><td> 31.2 </td><td> 20.0 </td></tr><tr><td> 5 </td><td> 1重量份 PFO </td><td> 1重量份 第一脫硫渣油 </td><td> 508 </td><td> 2.98 </td><td> <0.002 </td><td> 39.1 </td><td> 35.6 </td><td> 25.3 </td></tr><tr><td> 6 </td><td> 3重量份 PGO </td><td> 1重量份 第一脫硫渣油 </td><td> 292 </td><td> 2.12 </td><td> <0.002 </td><td> 53.0 </td><td> 28.8 </td><td> 18.2 </td></tr><tr><td> 7 </td><td> 1重量份 HFO </td><td> 1重量份 第一脫硫渣油 </td><td> 624 </td><td> 2.88 </td><td> <0.002 </td><td> 39.9 </td><td> 34.7 </td><td> 25.4 </td></tr><tr><td> 8 </td><td> 1重量份CE </td><td> 314 </td><td> 1.41 </td><td> <0.001 </td><td> 40.8 </td><td> 33.1 </td><td> 26.1 </td></tr><tr><td> 9 </td><td> 1重量份 HFO </td><td> 1重量份 RFCC </td><td> 222 </td><td> 2.76 </td><td> <0.0035 </td><td> 52.4 </td><td> 26.8 </td><td> 20.8 </td></tr></TBODY></TABLE>Table 4         <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> Example </td><td> Mp </td><td> Mw/Mn < /td><td> ash</td><td> Ca </td><td> Cp </td><td> Cn </td></tr><tr><td> 1 </td> <td> 2 parts by weight of PFO </td><td> 1 part by weight of the first desulfurized residue</td><td> 371 </td><td> 3.24 </td><td> <0.002 </ Td><td> 47.1 </td><td> 30.5 </td><td> 22.4 </td></tr><tr><td> 2 </td><td> 1 part by weight HFO </ Td><td> 329 </td><td> 3.49 </td><td> <0.001 </td><td> 64.8 </td><td> 18.5 </td><td> 16.7 </td ></tr><tr><td> 3 </td><td> 1 part by weight of PGO </td><td> 1 part by weight of the first desulfurization residue</td><td> 501 </td ><td> 2.35 </td><td> <0.002 </td><td> 40.2 </td><td> 36.2 </td><td> 23.6 </td></tr><tr>< Td> 4 </td><td> 1 part by weight of desulfurized mixed extraction oil</td><td> 285 </td><td> 1.36 </td><td> <0.001 </td><td> 32.5 </td><td> 36.3 </td><td> 31.2 </td></tr><tr><td> Comparative Example </td><td> Mp </td><td> Mw/ Mn </td><td> ash</td><td> Ca </td><td> Cp </td><td> Cn </td></tr><tr><td> 1 </ Td><td> 1 part by weight of the first lubricating base oil</td><td > 269 </td><td> 1.33 </td><td> <0.001 </td><td> 49.4 </td><td> 30.5 </td><td> 20.1 </td></tr ><tr><td> 2 </td><td> 1 part by weight of the second lubricating base oil</td><td> 482 </td><td> 1.50 </td><td> <0.001 </ Td><td> 41.1 </td><td> 33.8 </td><td> 25.1 </td></tr><tr><td> 3 </td><td> 1 part by weight first Sulfur residue oil</td><td> 918 </td><td> 2.54 </td><td> 0.0020 </td><td> 15.0 </td><td> 50.8 </td><td> 34.2 </td></tr><tr><td> 4 </td><td> 2 parts by weight of PGO </td><td> 1 part by weight of the first desulfurization residue</td><td> 361 </td><td> 2.21 </td><td> <0.002 </td><td> 48.8 </td><td> 31.2 </td><td> 20.0 </td></tr> <tr><td> 5 </td><td> 1 part by weight of PFO </td><td> 1 part by weight of the first desulfurization residue</td><td> 508 </td><td> 2.98 </td><td> <0.002 </td><td> 39.1 </td><td> 35.6 </td><td> 25.3 </td></tr><tr><td> 6 </ Td><td> 3 parts by weight of PGO </td><td> 1 part by weight of the first desulfurization residue</td><td> 292 </td><td> 2.12 </td><td> <0.002 </td><td> 53.0 </td><td> 28.8 </td><td> 18.2 </td></tr><tr><td> 7 </td><td> 1 part by weight of HFO </td><td> 1 part by weight Desulfurization Residue</td><td> 624 </td><td> 2.88 </td><td> <0.002 </td><td> 39.9 </td><td> 34.7 </td>< Td> 25.4 </td></tr><tr><td> 8 </td><td> 1 part by weight CE </td><td> 314 </td><td> 1.41 </td>< Td> <0.001 </td><td> 40.8 </td><td> 33.1 </td><td> 26.1 </td></tr><tr><td> 9 </td><td> 1 part by weight of HFO </td><td> 1 part by weight of RFCC </td><td> 222 </td><td> 2.76 </td><td> <0.0035 </td><td> 52.4 </ Td><td> 26.8 </td><td> 20.8 </td></tr></TBODY></TABLE>

應用例1   非晶型碳材及負極Application Example 1 Amorphous carbon material and negative electrode

將實施例1的前驅組成物以10℃/min的升溫速度加熱至500℃,並於一壓力為40atm的環境下,恆溫1小時,然後,冷卻至室溫,形成一結焦產物,且結焦產率為33%。接著,將該結焦產物加熱至1000℃,並恆溫4小時,形成該非晶型碳材。將該非晶型碳材以研磨機(廠牌:Retsch;型號:RM200 )進行研磨,接著以一篩網進行分級,取得D 50為20μm 至32μm的經研磨的非晶型碳材。將9.1克的經研磨的非晶型碳材、0.5克的聚偏二氟乙烯(吳羽化學工業社製,商品名為KF9200)及0.4的導電碳黑(購自Timcal且商品名為Super P)均勻混合,形成一成膜組分,再加入12克至15克的NMP均勻混合,形成一混合液。將該混合液塗佈於厚度為14μm的銅箔上,並於85℃進行0.5小時的乾燥處理,以移除NMP及水份,而形成一負極,其中,該負極包括銅箔及一形成在該銅箔上且厚度為20μm至22μm的導電膜,且該導電膜包含91wt%的該經研磨的非晶型碳材、5wt%的聚偏二氟乙烯,以及4wt%的導電碳黑。 The precursor composition of Example 1 was heated to 500 ° C at a temperature increase rate of 10 ° C / min, and kept at a constant pressure of 40 atm for 1 hour, and then cooled to room temperature to form a coking product, and coking was produced. The rate is 33%. Next, the coked product was heated to 1000 ° C and kept at a constant temperature for 4 hours to form the amorphous carbon material. The amorphous carbon material was ground by a grinder (manufactured by Retsch; model: RM200), and then classified by a sieve to obtain a ground amorphous carbon material having a D 50 of 20 μm to 32 μm. 9.1 g of the ground amorphous carbon material, 0.5 g of polyvinylidene fluoride (manufactured by Kureha Chemical Industry Co., Ltd., trade name: KF9200), and 0.4 conductive carbon black (purchased from Timcal and sold under the trade name Super P) The mixture is uniformly mixed to form a film-forming component, and 12 g to 15 g of NMP are further uniformly mixed to form a mixed solution. The mixture was applied to a copper foil having a thickness of 14 μm, and dried at 85 ° C for 0.5 hours to remove NMP and moisture to form a negative electrode, wherein the negative electrode included a copper foil and one formed thereon. The conductive film on the copper foil and having a thickness of 20 μm to 22 μm, and the conductive film contains 91% by weight of the ground amorphous carbon material, 5% by weight of polyvinylidene fluoride, and 4% by weight of conductive carbon black.

應用例2至15及應用例17及比較應用例1至15是以與應用例1相同的步驟來製備非晶型碳材及負極,不同的地方在於:改變前驅組成物的來源、改變結焦程序及煅燒程序的溫度、時間或壓力、改變非晶型碳材的D 50粒徑,改變成膜組分中各成分的種類及用量,如表3至表8。 Application Examples 2 to 15 and Application Example 17 and Comparative Application Examples 1 to 15 were the same procedures as in Application Example 1 to prepare an amorphous carbon material and a negative electrode, in which the source of the precursor composition was changed and the coking procedure was changed. And the temperature, time or pressure of the calcination procedure, changing the D 50 particle size of the amorphous carbon material, and changing the kind and amount of each component in the film-forming component, as shown in Tables 3 to 8.

應用例16是以與應用例1相同的步驟來製備非晶型碳材及負極,不同的地方在於:改變前驅組成物的來源、改變結焦程序及煅燒程序的溫度、時間或壓力、改變非晶型碳材的D 50粒徑,改變成膜組分中各成分的種類及用量,如表3至表4,其中,該應用例16的該非晶型碳材以衝突板式粉碎機(廠牌: NPK;型號:LJ-3)進行研磨,接著以粒徑分級機(廠牌: NPK;型號:MDS-3)進行分級,取得D 50為12.1μm的經研磨的非晶型碳材。 Application Example 16 was to prepare an amorphous carbon material and a negative electrode in the same manner as in Application Example 1, except that the source of the precursor composition was changed, the temperature, time or pressure of the coking process and the calcination procedure were changed, and the amorphous state was changed. The D 50 particle size of the carbon material is changed, and the type and amount of each component in the film forming component are changed, as shown in Tables 3 to 4, wherein the amorphous carbon material of the application example 16 is a collision plate type pulverizer (label: NPK; Model: LJ-3) was ground, and then classified by a particle size classifier (label: NPK; model: MDS-3) to obtain a ground amorphous carbon material having a D 50 of 12.1 μm.

表5 <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> 應用例 </td><td> 實施例 </td><td> 非晶型碳材 </td></tr><tr><td> 結焦程序 </td></tr><tr><td> 第一階段 </td><td> 第二階段 </td></tr><tr><td> 溫度(℃) </td><td> 時間(hr) </td><td> 壓力(atm) </td><td> 結焦產率(%) </td><td> 溫度(℃) </td><td> 時間(hr) </td><td> 壓力(atm) </td><td> 結焦產率(%) </td></tr><tr><td> 1 </td><td> 1 </td><td> 500 </td><td> 1 </td><td> 40 </td><td> 33 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 2 </td><td> 2 </td><td> 500 </td><td> 1 </td><td> 40 </td><td> 59 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 3 </td><td> 2 </td><td> 500 </td><td> 4 </td><td> 40 </td><td> 59 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 4 </td><td> 3 </td><td> 500 </td><td> 1 </td><td> 40 </td><td> 18 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 5 </td><td> 2 </td><td> 500 </td><td> 1 </td><td> 4~8 </td><td> 30 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 6 </td><td> 2 </td><td> 500 </td><td> 1 </td><td> 40 </td><td> 60 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 7 </td><td> 2 </td><td> 500 </td><td> 4 </td><td> 40 </td><td> 54 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 8 </td><td> 2 </td><td> 550 </td><td> 1 </td><td> 10 </td><td> 76 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 9 </td><td> 2 </td><td> 550 </td><td> 1 </td><td> 2 </td><td> 35 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 10 </td><td> 2 </td><td> 370 </td><td> 4 </td><td> 10 </td><td> -- </td><td> 500 </td><td> 4 </td><td> 2 </td><td> 43 </td></tr><tr><td> 11 </td><td> 2 </td><td> 370 </td><td> 8 </td><td> 10 </td><td> -- </td><td> 500 </td><td> 4 </td><td> 2 </td><td> 44 </td></tr><tr><td> 12 </td><td> 2 </td><td> 500 </td><td> 2 </td><td> 2 </td><td> 33 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 13 </td><td> 2 </td><td> 500 </td><td> 4 </td><td> 2 </td><td> 33 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 14 </td><td> 2 </td><td> 500 </td><td> 8 </td><td> 2 </td><td> 39 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 15 </td><td> 2 </td><td> 500 </td><td> 16 </td><td> 2 </td><td> 32 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 16 </td><td> 2 </td><td> 500 </td><td> 4 </td><td> 2 </td><td> 33 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 17 </td><td> 4 </td><td> 500 </td><td> 4 </td><td> 40 </td><td> 39 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr></TBODY></TABLE>table 5         <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> Application example</td><td> Example </td><td> Amorphous Carbon material</td></tr><tr><td> Coking procedure</td></tr><tr><td> First stage</td><td> Second stage</td>< /tr><tr><td> Temperature (°C) </td><td> Time (hr) </td><td> Pressure (atm) </td><td> Coking yield (%) </ Td><td> Temperature (°C) </td><td> Time (hr) </td><td> Pressure (atm) </td><td> Coking yield (%) </td></ Tr><tr><td> 1 </td><td> 1 </td><td> 500 </td><td> 1 </td><td> 40 </td><td> 33 < /td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 2 </td><td> 2 </td><td> 500 </td><td> 1 </td><td> 40 </td><td> 59 </td><td> -- < /td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 3 </td><td> 2 < /td><td> 500 </td><td> 4 </td><td> 40 </td><td> 59 </td><td> -- </td><td> -- < /td><td> -- </td><td> -- </td></tr><tr><td> 4 </td><td> 3 </td><td> 500 </ Td><td> 1 </td><td> 40 </td><td> 18 </td><td> -- </td><td> -- </td><td> -- < /td><td> -- </td></tr><tr><td> 5 </td><td> 2 </td><td> 500 </t d><td> 1 </td><td> 4~8 </td><td> 30 </td><td> -- </td><td> -- </td><td> - - </td><td> -- </td></tr><tr><td> 6 </td><td> 2 </td><td> 500 </td><td> 1 < /td><td> 40 </td><td> 60 </td><td> -- </td><td> -- </td><td> -- </td><td> - - </td></tr><tr><td> 7 </td><td> 2 </td><td> 500 </td><td> 4 </td><td> 40 </ Td><td> 54 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr> <tr><td> 8 </td><td> 2 </td><td> 550 </td><td> 1 </td><td> 10 </td><td> 76 </td ><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 9 </ Td><td> 2 </td><td> 550 </td><td> 1 </td><td> 2 </td><td> 35 </td><td> -- </td ><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 10 </td><td> 2 </td ><td> 370 </td><td> 4 </td><td> 10 </td><td> -- </td><td> 500 </td><td> 4 </td> <td> 2 </td><td> 43 </td></tr><tr><td> 11 </td><td> 2 </td><td> 370 </td><td> 8 </td><td> 10 </td><td> -- </td><td> 500 </td><td> 4 </td><td> 2 </td><td> 44 </td></tr><tr><td> 12 </td><td> 2 </td><td> 500 </td><td> 2 </td><td> 2 </td ><td> 33 </td>< Td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 13 </td> <td> 2 </td><td> 500 </td><td> 4 </td><td> 2 </td><td> 33 </td><td> -- </td>< Td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 14 </td><td> 2 </td>< Td> 500 </td><td> 8 </td><td> 2 </td><td> 39 </td><td> -- </td><td> -- </td>< Td> -- </td><td> -- </td></tr><tr><td> 15 </td><td> 2 </td><td> 500 </td><td > 16 </td><td> 2 </td><td> 32 </td><td> -- </td><td> -- </td><td> -- </td>< Td> -- </td></tr><tr><td> 16 </td><td> 2 </td><td> 500 </td><td> 4 </td><td> 2 </td><td> 33 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td>< /tr><tr><td> 17 </td><td> 4 </td><td> 500 </td><td> 4 </td><td> 40 </td><td> 39 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr></TBODY></ TABLE>

表6 <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> 應用例 </td><td> 非晶型碳材 </td><td> 黏結劑 (克) </td><td> 助導劑 (克) </td><td> 溶劑 (克) </td></tr><tr><td> 實施例 </td><td> 冷卻程序 </td><td> 煅燒程序 </td><td> 用量(克) </td><td> 粒徑 D<sub>50</sub> (μm) </td></tr><tr><td> 溫度(℃) </td><td> 時間(hr) </td><td> 溫度 (℃) </td><td> 時間 (hr) </td></tr><tr><td> 1 </td><td> 1 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 20至32 </td><td> 0.5 </td><td> 0.4 </td><td> 12至15 </td></tr><tr><td> 2 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 3 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 4 </td><td> 3 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 5 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 6 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 7 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 8 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 9 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 10 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 11 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 12 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 13 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 14 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 15 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 16 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 12.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 17 </td><td> 4 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 20至32 </td><td> 0.5 </td><td> 0.4 </td></tr></TBODY></TABLE>Table 6         <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> Application example</td><td> Amorphous carbon material</td><td> Adhesive (g) </td><td> Coagulant (g) </td><td> Solvent (g) </td></tr><tr><td> Example </td>< Td> Cooling procedure</td><td> Calcination procedure</td><td> Dosage (g) </td><td> Particle size D<sub>50</μ> (μm) </td>< /tr><tr><td> Temperature (°C) </td><td> Time (hr) </td><td> Temperature (°C) </td><td> Time (hr) </td> </tr><tr><td> 1 </td><td> 1 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 20 to 32 </td><td> 0.5 </td><td> 0.4 </td><td> 12 to 15 </td>< /tr><tr><td> 2 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 3 </td><td> 2 </td ><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td>< Td> 0.4 </td></tr><tr><td> 4 </td><td> 3 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 5 </td ><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </ Td></tr><tr><td> 6 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td>< Td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 7 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </ Td><td> 0.4 </td></tr><tr><td> 8 </td><td> 2 </td><td> 35 </td><td> 5 </td>< Td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 9 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </ Td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 10 </td><td> 2 </td><td> 35 </td>< Td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr ><tr><td> 11 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </ Td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 12 </td><td> 2 </td>< Td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 13 </td ><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td>< Td> 0.5 </td><td> 0.4 </td></tr><tr><td> 14 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr ><td> 15 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td>< Td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 16 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 12.1 </td><td> 0.5 </ Td><td> 0.4 </td></tr><tr><td> 17 </td><td> 4 </td><td> 35 </td><td> 5 </td>< Td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 20 to 32 </td><td> 0.5 </td><td> 0.4 </td>< /tr></TBODY></TABLE>

表7 <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> 比較應用例 </td><td> 比較例 </td><td> 結焦程序 </td></tr><tr><td> 第一階段 </td><td> 第二階段 </td></tr><tr><td> 溫度(℃) </td><td> 時間(hr) </td><td> 壓力(atm) </td><td> 結焦產率 (%) </td><td> 溫度(℃) </td><td> 時間(hr) </td><td> 壓力(atm) </td><td> 結焦產率 (%) </td></tr><tr><td> 1 </td><td> 1 </td><td> 500 </td><td> 1 </td><td> 40 </td><td> 46~54 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 2 </td><td> 2 </td><td> 500 </td><td> 1 </td><td> 40 </td><td> 46 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 3 </td><td> 3 </td><td> 500 </td><td> 1 </td><td> 40 </td><td> 29 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 4 </td><td> 1 </td><td> 500 </td><td> 4 </td><td> 40 </td><td> 49~55 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 5 </td><td> 3 </td><td> 500 </td><td> 4 </td><td> 40 </td><td> 26 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 6 </td><td> 3 </td><td> 400 </td><td> 4 </td><td> 40 </td><td> -- </td><td> 500 </td><td> 4 </td><td> 40 </td><td> 34 </td></tr><tr><td> 7 </td><td> 4 </td><td> 500 </td><td> 1 </td><td> 40 </td><td> 18~21 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 8 </td><td> 5 </td><td> 500 </td><td> 1 </td><td> 40 </td><td> 46 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 9 </td><td> 6 </td><td> 500 </td><td> 1 </td><td> 40 </td><td> 41 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 10 </td><td> 3 </td><td> 500 </td><td> 1 </td><td> 4~8 </td><td> 14 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 11 </td><td> 3 </td><td> 600 </td><td> 1 </td><td> 4~8 </td><td> 19 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 12 </td><td> 7 </td><td> 500 </td><td> 1 </td><td> 40 </td><td> 39 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 13 </td><td> 7 </td><td> 500 </td><td> 1 </td><td> 40 </td><td> 49 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 14 </td><td> 8 </td><td> 500 </td><td> 4 </td><td> 40 </td><td> 55 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 15 </td><td> 9 </td><td> 500 </td><td> 1 </td><td> 10 </td><td> 48 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr></TBODY></TABLE>Table 7         <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> Comparison Application </td><td> Comparison Example </td><td> Coking Procedure </td></tr><tr><td> The first stage</td><td> The second stage</td></tr><tr><td> Temperature (°C) </td>< Td> time (hr) </td><td> pressure (atm) </td><td> coking yield (%) </td><td> temperature (°C) </td><td> time ( Hr) </td><td> pressure (atm) </td><td> coking yield (%) </td></tr><tr><td> 1 </td><td> 1 < /td><td> 500 </td><td> 1 </td><td> 40 </td><td> 46~54 </td><td> -- </td><td> - - </td><td> -- </td><td> -- </td></tr><tr><td> 2 </td><td> 2 </td><td> 500 </td><td> 1 </td><td> 40 </td><td> 46 </td><td> -- </td><td> -- </td><td> - - </td><td> -- </td></tr><tr><td> 3 </td><td> 3 </td><td> 500 </td><td> 1 < /td><td> 40 </td><td> 29 </td><td> -- </td><td> -- </td><td> -- </td><td> - - </td></tr><tr><td> 4 </td><td> 1 </td><td> 500 </td><td> 4 </td><td> 40 </ Td><td> 49~55 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></ Tr><tr><td> 5 </td><td> 3 </td><td> 500 </td><td> 4 </td><td> 40 </td><td> 26 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></ Tr><tr><td> 6 </td><td> 3 </td><td> 400 </td><td> 4 </td><td> 40 </td><td> -- </td><td> 500 </td><td> 4 </td><td> 40 </td><td> 34 </td></tr><tr><td> 7 </td ><td> 4 </td><td> 500 </td><td> 1 </td><td> 40 </td><td> 18~21 </td><td> -- </ Td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 8 </td><td> 5 </ Td><td> 500 </td><td> 1 </td><td> 40 </td><td> 46 </td><td> -- </td><td> -- </ Td><td> -- </td><td> -- </td></tr><tr><td> 9 </td><td> 6 </td><td> 500 </td ><td> 1 </td><td> 40 </td><td> 41 </td><td> -- </td><td> -- </td><td> -- </ Td><td> -- </td></tr><tr><td> 10 </td><td> 3 </td><td> 500 </td><td> 1 </td> <td> 4~8 </td><td> 14 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 11 </td><td> 3 </td><td> 600 </td><td> 1 </td><td> 4~8 < /td><td> 19 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td></tr ><tr><td> 12 </td><td> 7 </td><td> 500 </td><td> 1 </td><td> 40 </td><td> 39 </ Td><td> -- </td>< Td> -- </td><td> -- </td><td> -- </td></tr><tr><td> 13 </td><td> 7 </td>< Td> 500 </td><td> 1 </td><td> 40 </td><td> 49 </td><td> -- </td><td> -- </td>< Td> -- </td><td> -- </td></tr><tr><td> 14 </td><td> 8 </td><td> 500 </td><td > 4 </td><td> 40 </td><td> 55 </td><td> -- </td><td> -- </td><td> -- </td>< Td> -- </td></tr><tr><td> 15 </td><td> 9 </td><td> 500 </td><td> 1 </td><td> 10 </td><td> 48 </td><td> -- </td><td> -- </td><td> -- </td><td> -- </td>< /tr></TBODY></TABLE>

表8 <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> 比較應用例 </td><td> 非晶型碳材 </td><td> 黏結劑 (克) </td><td> 助導劑 (克) </td><td> 溶劑 (克) </td></tr><tr><td> 比較例 </td><td> 冷卻程序 </td><td> 煅燒程序 </td><td> 用量 (克) </td><td> 粒徑 D<sub>50</sub> (μm) </td></tr><tr><td> 溫度(℃) </td><td> 時間(hr) </td><td> 溫度 (℃) </td><td> 時間 (hr) </td></tr><tr><td> 1 </td><td> 1 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 20至32 </td><td> 0.5 </td><td> 0.4 </td><td> 12至15 </td></tr><tr><td> 2 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 3 </td><td> 3 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 4 </td><td> 1 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 5 </td><td> 3 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 6 </td><td> 3 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 7 </td><td> 4 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 8 </td><td> 5 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 9 </td><td> 6 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 10 </td><td> 3 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 11 </td><td> 3 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 12 </td><td> 7 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 13 </td><td> 7 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 14 </td><td> 8 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 15 </td><td> 9 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr></TBODY></TABLE>Table 8         <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> Comparative Application </td><td> Amorphous Carbon Material</td><td > Adhesive (g) </td><td> Coagulant (g) </td><td> Solvent (g) </td></tr><tr><td> Comparative Example</td> <td> Cooling Procedure</td><td> Calcination Procedure</td><td> Dosage (g) </td><td> Particle Size D<sub>50</μ> (μm) </td> </tr><tr><td> Temperature (°C) </td><td> Time (hr) </td><td> Temperature (°C) </td><td> Time (hr) </td ></tr><tr><td> 1 </td><td> 1 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td > 4 </td><td> 9.1 </td><td> 20 to 32 </td><td> 0.5 </td><td> 0.4 </td><td> 12 to 15 </td> </tr><tr><td> 2 </td><td> 2 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 3 </td><td> 3 </ Td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td> <td> 0.4 </td></tr><tr><td> 4 </td><td> 1 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 5 </ Td><td> 3 </td> <td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td > 0.4 </td></tr><tr><td> 6 </td><td> 3 </td><td> 35 </td><td> 5 </td><td> 1000 < /td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 7 </td> <td> 4 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td > 0.5 </td><td> 0.4 </td></tr><tr><td> 8 </td><td> 5 </td><td> 35 </td><td> 5 < /td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr> <td> 9 </td><td> 6 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td > 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 10 </td><td> 3 </td><td> 35 < /td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td ></tr><tr><td> 11 </td><td> 3 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td > 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 12 </td><td> 7 < /td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td ><td> 0.4 </td></tr><tr><td> 13 </td><td> 7 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 < /td><td> 0.5 </td><td> 0.4 </td></tr><tr><td> 14 </td><td> 8 </td><td> 35 </td> <td> 5 </td><td> 1000 </td><td> 4 </td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></ Tr><tr><td> 15 </td><td> 9 </td><td> 35 </td><td> 5 </td><td> 1000 </td><td> 4 < /td><td> 9.1 </td><td> 0.5 </td><td> 0.4 </td></tr></TBODY></TABLE>

結焦產率:[結焦產物的重量/前驅組成物的重量]×100%。Coking yield: [weight of coked product / weight of precursor composition] × 100%.

非晶型碳材粒徑分析:將應用例1至17及比較應用例1至15的非晶型碳材以雷射粒徑分析儀進行分析(廠牌: Beckman;型號:LS13320)。Amorphous carbon material particle size analysis: The amorphous carbon materials of Application Examples 1 to 17 and Comparative Application Examples 1 to 15 were analyzed by a laser particle size analyzer (label: Beckman; model: LS13320).

第一圈充入電容量、第一圈放出電容量及不可逆百分比分析:為方便描述,該等分析以應用例1做為代表進行說明,而其餘的應用例及比較應用例皆以相同方式進行組裝及量測。將一作為正極的鋰金屬薄片、一應用例1的負極、電解液,及隔離膜(廠牌:Celgard;材質:聚丙烯及聚乙烯)組裝成CR2032鈕扣型半電池,其中,該電解液包含99wt%的1M LiPF 6溶液及1wt%的碳酸亞乙烯酯。該LiPF 6溶液包含LiPF 6、EC、EMC及DMC,其中,EC:EMC:DMC的體積比為1:1:1。將該CR2032鈕扣型半電池利用充放電機(廠牌:ARBIN;型號:BT2043)於室溫(25℃)下進行量測,且量測條件為在CC/CV模式下0.1C充電到0V;cut-off 電流0.01C;在CC模式下,0.1C放電至1.8V。該不可逆百分比為[(第一圈充入電容量-第一圈放出電容量)/第一圈充入電容量]×100%。 The first ring is charged into the capacity, the first ring discharge capacity and the irreversible percentage analysis: for convenience of description, the analysis is described by using the application example 1, and the remaining application examples and comparative application examples are assembled in the same manner. And measurement. A lithium metal foil as a positive electrode, a negative electrode of an application example 1, an electrolyte, and a separator (label: Celgard; material: polypropylene and polyethylene) are assembled into a CR2032 button type half-cell, wherein the electrolyte contains 99 wt% of a 1 M LiPF 6 solution and 1 wt% of vinylene carbonate. The LiPF 6 solution contains LiPF 6 , EC, EMC, and DMC, wherein the volume ratio of EC:EMC:DMC is 1:1:1. The CR2032 button type half-cell is measured by a charge and discharge machine (label: ARBIN; model: BT2043) at room temperature (25 ° C), and the measurement condition is that 0.1 C is charged to 0 V in CC/CV mode; The cut-off current is 0.01C; in CC mode, 0.1C is discharged to 1.8V. The irreversible percentage is [(first ring charging capacity - first ring discharging capacity) / first ring charging capacity] x 100%.

表9 <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> 應用例 </td><td> 實施例 </td><td> 第一圈放出電容量(mAh/g) </td><td> 不可逆百分比 (%) </td><td> 比較應用例 </td><td> 比較例 </td><td> 第一圈放出電容量 (mAh/g) </td><td> 不可逆百分比 (%) </td></tr><tr><td> 1 </td><td> 1 </td><td> 291 </td><td> 27.9 </td><td> 1 </td><td> 1 </td><td> 344 </td><td> 39.4 </td></tr><tr><td> 2 </td><td> 2 </td><td> 242 </td><td> 26.5 </td><td> 2 </td><td> 2 </td><td> 320 </td><td> 40.6 </td></tr><tr><td> 3 </td><td> 2 </td><td> 265 </td><td> 25.7 </td><td> 3 </td><td> 3 </td><td> 317 </td><td> 30.3 </td></tr><tr><td> 4 </td><td> 3 </td><td> 266 </td><td> 29.1 </td><td> 4 </td><td> 1 </td><td> 330 </td><td> 40.0 </td></tr><tr><td> 5 </td><td> 2 </td><td> 240 </td><td> 22.3 </td><td> 5 </td><td> 3 </td><td> 265 </td><td> 36.5 </td></tr><tr><td> 6 </td><td> 2 </td><td> 242 </td><td> 26.5 </td><td> 6 </td><td> 3 </td><td> 288 </td><td> 36.7 </td></tr><tr><td> 7 </td><td> 2 </td><td> 265 </td><td> 25.7 </td><td> 7 </td><td> 4 </td><td> 295 </td><td> 33.4 </td></tr><tr><td> 8 </td><td> 2 </td><td> 273 </td><td> 27.1 </td><td> 8 </td><td> 5 </td><td> 285 </td><td> 33.3 </td></tr><tr><td> 9 </td><td> 2 </td><td> 272 </td><td> 27.4 </td><td> 9 </td><td> 6 </td><td> 273 </td><td> 32.1 </td></tr><tr><td> 10 </td><td> 2 </td><td> 288 </td><td> 26.6 </td><td> 10 </td><td> 3 </td><td> 295 </td><td> 33.3 </td></tr><tr><td> 11 </td><td> 2 </td><td> 279 </td><td> 26.4 </td><td> 11 </td><td> 3 </td><td> 302 </td><td> 38.9 </td></tr><tr><td> 12 </td><td> 2 </td><td> 251 </td><td> 28.3 </td><td> 12 </td><td> 7 </td><td> 266 </td><td> 30.2 </td></tr><tr><td> 13 </td><td> 2 </td><td> 284 </td><td> 27.3 </td><td> 13 </td><td> 7 </td><td> 266 </td><td> 30.2 </td></tr><tr><td> 14 </td><td> 2 </td><td> 282 </td><td> 26.8 </td><td> 14 </td><td> 8 </td><td> 282 </td><td> 40.4 </td></tr><tr><td> 15 </td><td> 2 </td><td> 267 </td><td> 28.1 </td><td> 15 </td><td> 9 </td><td> 265 </td><td> 36.5 </td></tr><tr><td> 16 </td><td> 2 </td><td> 279 </td><td> 21.5 </td><td>   </td><td>   </td><td>   </td><td>   </td></tr><tr><td> 17 </td><td> 4 </td><td> 283 </td><td> 29.3 </td><td>   </td><td>   </td><td>   </td><td>   </td></tr></TBODY></TABLE>Table 9         <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> Application </td><td> Example </td><td> First lap Release capacity (mAh/g) </td><td> irreversible percentage (%) </td><td> Comparison application example</td><td> Comparison example</td><td> Release of the first circle Capacitance (mAh/g) </td><td> irreversible percentage (%) </td></tr><tr><td> 1 </td><td> 1 </td><td> 291 </td><td> 27.9 </td><td> 1 </td><td> 1 </td><td> 344 </td><td> 39.4 </td></tr><tr ><td> 2 </td><td> 2 </td><td> 242 </td><td> 26.5 </td><td> 2 </td><td> 2 </td>< Td> 320 </td><td> 40.6 </td></tr><tr><td> 3 </td><td> 2 </td><td> 265 </td><td> 25.7 </td><td> 3 </td><td> 3 </td><td> 317 </td><td> 30.3 </td></tr><tr><td> 4 </td ><td> 3 </td><td> 266 </td><td> 29.1 </td><td> 4 </td><td> 1 </td><td> 330 </td>< Td> 40.0 </td></tr><tr><td> 5 </td><td> 2 </td><td> 240 </td><td> 22.3 </td><td> 5 </td><td> 3 </td><td> 265 </td><td> 36.5 </td></tr><tr><td> 6 </td><td> 2 </td ><td> 242 </td><td> 26.5 </td><td> 6 </td><td> 3 </td><td> 288 </td><td> 36.7 </td>< /tr><tr>< Td> 7 </td><td> 2 </td><td> 265 </td><td> 25.7 </td><td> 7 </td><td> 4 </td><td> 295 </td><td> 33.4 </td></tr><tr><td> 8 </td><td> 2 </td><td> 273 </td><td> 27.1 </ Td><td> 8 </td><td> 5 </td><td> 285 </td><td> 33.3 </td></tr><tr><td> 9 </td>< Td> 2 </td><td> 272 </td><td> 27.4 </td><td> 9 </td><td> 6 </td><td> 273 </td><td> 32.1 </td></tr><tr><td> 10 </td><td> 2 </td><td> 288 </td><td> 26.6 </td><td> 10 </ Td><td> 3 </td><td> 295 </td><td> 33.3 </td></tr><tr><td> 11 </td><td> 2 </td>< Td> 279 </td><td> 26.4 </td><td> 11 </td><td> 3 </td><td> 302 </td><td> 38.9 </td></tr ><tr><td> 12 </td><td> 2 </td><td> 251 </td><td> 28.3 </td><td> 12 </td><td> 7 </ Td><td> 266 </td><td> 30.2 </td></tr><tr><td> 13 </td><td> 2 </td><td> 284 </td>< Td> 27.3 </td><td> 13 </td><td> 7 </td><td> 266 </td><td> 30.2 </td></tr><tr><td> 14 </td><td> 2 </td><td> 282 </td><td> 26.8 </td><td> 14 </td><td> 8 </td><td> 282 </ Td><td> 40.4 </td></tr><tr><td> 15 </td><td> 2 </td><td> 267 </td><td> 28.1 </td>< Td> 15 </td><td> 9 </td><td> 265 </td><td> 36.5 </td></tr><tr><td> 16 </td><td> 2 </td><td> 279 </ Td><td> 21.5 </td><td> </td><td> </td><td> </td><td> </td></tr><tr><td> 17 < /td><td> 4 </td><td> 283 </td><td> 29.3 </td><td> </td><td> </td><td> </td><td > </td></tr></TBODY></TABLE>

參閱表9,應用例1至17的第一圈放出電容量範圍為240mAh/g至291mAh/g,且不可逆百分比範圍為21.5%至29.1%,而比較應用例1至15的第一圈放出電容量範圍為265mAh/g至344mAh/g,且不可逆百分比範圍為30.0%至40.6%。Referring to Table 9, the first loop discharge capacity of Application Examples 1 to 17 ranges from 240 mAh/g to 291 mAh/g, and the irreversible percentage ranges from 21.5% to 29.1%, while the first loop of the application examples 1 to 15 is discharged. The capacity ranges from 265 mAh/g to 344 mAh/g, and the irreversible percentage ranges from 30.0% to 40.6%.

綜上所述,本發明透過調整碳元素含量、氫元素含量、氮元素含量、硫元素含量、該碳原子數目與氫原子數目的比值、重量平均分子量、分子量分佈指數、灰分含量、芳香烴含量、飽和烷烴含量,及環烷烴含量,使由該前驅組成物所形成的非晶型碳材應用至一電池作為負極時,可降低該電池的不可逆百分比,故確實能達成本發明的目的。In summary, the present invention adjusts the carbon content, the hydrogen element content, the nitrogen element content, the sulfur element content, the ratio of the number of carbon atoms to the number of hydrogen atoms, the weight average molecular weight, the molecular weight distribution index, the ash content, and the aromatic hydrocarbon content. The saturated alkane content and the naphthenic content can reduce the irreversible percentage of the battery when the amorphous carbon material formed from the precursor composition is applied to a battery as a negative electrode, so that the object of the present invention can be achieved.

惟以上所述者,僅為本發明的實施例而已,當不能以此限定本發明實施的範圍,凡是依本發明申請專利範圍及專利說明書內容所作的簡單的等效變化與修飾,皆仍屬本發明專利涵蓋的範圍內。However, the above is only the embodiment of the present invention, and the scope of the invention is not limited thereto, and all the simple equivalent changes and modifications according to the scope of the patent application and the patent specification of the present invention are still Within the scope of the invention patent.

Claims (6)

一種前驅組成物,用來形成負極用的非晶型碳材,包含: 以該前驅組成物的總量為100wt%計,該碳元素含量範圍為84wt%至92.1wt%、該氫元素含量範圍為6wt%至10.3wt%、該氮元素含量範圍為0.59wt%至2wt%,及該硫元素含量範圍為0wt%至6wt%; 該前驅組成物的重量平均分子量範圍為149至900,且分子量分佈指數範圍為1.33至6.87; 以該前驅組成物的總量為100wt%計,該前驅組成物的灰分含量範圍為0wt%至0.0478wt%; 以該前驅組成物的總量為100wt%計,該芳香烴含量範圍為15wt%至82wt%、該飽和烷烴含量範圍為12wt%至51wt%,且該環烷烴含量範圍為6wt%至34wt%。A precursor composition for forming an amorphous carbon material for a negative electrode, comprising: the carbon element content ranging from 84% by weight to 92.1% by weight, based on the total amount of the precursor composition: 100% by weight, the hydrogen element content range 6wt% to 10.3wt%, the nitrogen element content ranges from 0.59wt% to 2wt%, and the sulfur element content ranges from 0wt% to 6wt%; the precursor composition has a weight average molecular weight ranging from 149 to 900, and the molecular weight The distribution index ranges from 1.33 to 6.87; the precursor composition has an ash content ranging from 0 wt% to 0.0478 wt%, based on the total amount of the precursor composition of 100 wt%; and the total amount of the precursor composition is 100 wt%, The aromatic hydrocarbon content ranges from 15 wt% to 82 wt%, the saturated alkane content ranges from 12 wt% to 51 wt%, and the naphthenic content ranges from 6 wt% to 34 wt%. 如請求項1所述的前驅組成物,其中,該碳元素含量範圍為84wt%至92wt%及該氮元素含量範圍為0.59wt%至1wt%;該前驅組成物的灰分含量範圍為0.001wt%至0.0478wt%。The precursor composition according to claim 1, wherein the carbon element content ranges from 84% by weight to 92% by weight and the nitrogen element content ranges from 0.59% by weight to 1% by weight; the precursor composition has an ash content ranging from 0.001% by weight. To 0.0478 wt%. 如請求項1所述的前驅組成物,其中,該碳元素含量範圍為91.0wt%至92.1wt%、該氫元素含量範圍為7.1wt%至7.5wt%、該氮元素含量範圍為0.62wt%至1.16wt%,及該硫元素含量範圍為0.045wt%至0.11wt%;該重量平均分子量範圍為541至900,且分子量分佈指數範圍為3.49至4.22;該前驅組成物的灰分含量範圍為0wt%至0.001wt%;該芳香烴含量範圍為64.8wt%至76.2wt%、該飽和烷烴含量範圍為12.4wt%至18.5wt%,且該環烷烴含量範圍為11.4wt%至20.1wt%。The precursor composition according to claim 1, wherein the carbon element content ranges from 91.0 wt% to 92.1 wt%, the hydrogen element content ranges from 7.1 wt% to 7.5 wt%, and the nitrogen element content ranges from 0.62 wt%. To 1.16 wt%, and the sulfur element content ranges from 0.045 wt% to 0.11 wt%; the weight average molecular weight ranges from 541 to 900, and the molecular weight distribution index ranges from 3.49 to 4.22; the precursor composition has an ash content ranging from 0 wt. % to 0.001 wt%; the aromatic hydrocarbon content ranges from 64.8 wt% to 76.2 wt%, the saturated alkane content ranges from 12.4 wt% to 18.5 wt%, and the naphthenic content ranges from 11.4 wt% to 20.1 wt%. 一種非晶型碳材,利用如請求項1至3任一項所述的前驅組成物進行一處理所形成,其中,該處理包含一結焦程序及一煅燒程序。An amorphous carbon material formed by performing a treatment using the precursor composition according to any one of claims 1 to 3, wherein the treatment comprises a coking process and a calcination process. 如請求項4所述的非晶型碳材,其中,該結焦程序包括一加熱步驟及一冷卻步驟,該加熱步驟的操作溫度範圍為400℃至600℃,該加熱步驟的操作時間範圍為1小時至16小時。The amorphous carbon material according to claim 4, wherein the coking process comprises a heating step and a cooling step, the heating step has an operating temperature range of 400 ° C to 600 ° C, and the heating step has an operating time range of 1 Hours to 16 hours. 如請求項5所述的非晶型碳材,其中,該加熱步驟的操作溫度範圍為500℃至550℃,該加熱步驟的操作時間範圍為4小時至8小時。The amorphous carbon material according to claim 5, wherein the heating step has an operating temperature ranging from 500 ° C to 550 ° C, and the heating step has an operating time ranging from 4 hours to 8 hours.
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