WO2023058500A1 - 炭素質材料、蓄電デバイス用負極、蓄電デバイス、及び炭素質材料の製造方法 - Google Patents
炭素質材料、蓄電デバイス用負極、蓄電デバイス、及び炭素質材料の製造方法 Download PDFInfo
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- WO2023058500A1 WO2023058500A1 PCT/JP2022/035918 JP2022035918W WO2023058500A1 WO 2023058500 A1 WO2023058500 A1 WO 2023058500A1 JP 2022035918 W JP2022035918 W JP 2022035918W WO 2023058500 A1 WO2023058500 A1 WO 2023058500A1
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 229920001542 oligosaccharide Polymers 0.000 description 1
- 150000002482 oligosaccharides Chemical class 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 239000001254 oxidized starch Substances 0.000 description 1
- 235000013808 oxidized starch Nutrition 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 239000011301 petroleum pitch Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical group [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical group O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 150000004714 phosphonium salts Chemical class 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 125000004437 phosphorous atom Chemical group 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920005596 polymer binder Polymers 0.000 description 1
- 239000002491 polymer binding agent Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229920002742 polystyrene-block-poly(ethylene/propylene) -block-polystyrene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 229940116317 potato starch Drugs 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000007348 radical reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229940100486 rice starch Drugs 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 229920001935 styrene-ethylene-butadiene-styrene Polymers 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical group C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- 125000005497 tetraalkylphosphonium group Chemical group 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- USFPINLPPFWTJW-UHFFFAOYSA-N tetraphenylphosphonium Chemical class C1=CC=CC=C1[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 USFPINLPPFWTJW-UHFFFAOYSA-N 0.000 description 1
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical group O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 1
- WLPUWLXVBWGYMZ-UHFFFAOYSA-N tricyclohexylphosphine Chemical compound C1CCCCC1P(C1CCCCC1)C1CCCCC1 WLPUWLXVBWGYMZ-UHFFFAOYSA-N 0.000 description 1
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 1
- FIQMHBFVRAXMOP-UHFFFAOYSA-N triphenylphosphane oxide Chemical compound C=1C=CC=CC=1P(C=1C=CC=CC=1)(=O)C1=CC=CC=C1 FIQMHBFVRAXMOP-UHFFFAOYSA-N 0.000 description 1
- OUYCCCASQSFEME-UHFFFAOYSA-N tyrosine Natural products OC(=O)C(N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-UHFFFAOYSA-N 0.000 description 1
- 239000004474 valine Substances 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 229940100445 wheat starch Drugs 0.000 description 1
- 238000004846 x-ray emission Methods 0.000 description 1
- 239000000811 xylitol Substances 0.000 description 1
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 1
- 235000010447 xylitol Nutrition 0.000 description 1
- 229960002675 xylitol Drugs 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/42—Powders or particles, e.g. composition thereof
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Definitions
- Patent Document 3 a carbonaceous material adjusted to contain a specific amount of various elements other than the carbon element.
- the nitrogen element content is 1.0% by mass or more
- the hydrogen element content is 0.1% by mass or less
- the phosphorus element content is 0.5% by mass by fluorescent X-ray analysis.
- the carbonaceous material according to [1] which has a carbon interplanar spacing (d 002 ) of 3.65 ⁇ or more as measured by X-ray diffraction.
- the carbonaceous material according to [1] or [2] which has an elemental oxygen content of less than 1.0% by mass as determined by elemental analysis.
- the upper limit of the carbon spacing (d 002 ) is from the viewpoint that by appropriately reducing d 002 , the volume of the carbonaceous material can be appropriately reduced, the effective capacity per volume can be increased, and the discharge capacity per volume can be easily increased. is preferably 4.00 ⁇ or less, more preferably 3.95 ⁇ or less, still more preferably 3.90 ⁇ or less, and even more preferably 3.85 ⁇ or less.
- the carbon spacing (d 002 ) is measured by X-ray diffraction using the Bragg formula, specifically by the method described in Examples.
- the carbon spacing (d 002 ) is adjusted to the above range by adjusting the amount of nitrogen-containing compound that can be added when producing the carbonaceous material, adjusting the temperature and time of heat treatment, etc. be able to.
- the half width value of the peak near 1650 cm -1 is the value of the electrode produced using the carbonaceous material. It is preferably 98 cm ⁇ 1 or more, more preferably 100 cm ⁇ 1 or more, still more preferably 101 cm ⁇ 1 or more, still more preferably 102 cm ⁇ 1 or more, from the viewpoint of easily increasing the discharge capacity per weight.
- the peak around 1650 cm ⁇ 1 is a Raman peak generally called G band, and is a peak caused by disorder/defect of graphite structure.
- the electrode density of the negative electrode obtained by using the carbonaceous material can be easily increased, and as a result, the discharge capacity per volume as well as the discharge capacity per weight can be easily increased.
- the ratio D 80 /D 20 of D 80 to D 20 in the volume-based particle size distribution of the carbonaceous material measured by the laser diffraction scattering particle size distribution measurement method is preferable. is 3.5 or more, more preferably 4.0 or more, still more preferably 4.5 or more, even more preferably 5.0 or more, especially preferably 5.5 or more, and especially more preferably 6.0 or more, From the same point of view, it is preferably 18 or less, more preferably 16 or less, and even more preferably 15 or less.
- D 80 /D 20 is a volume-based particle size distribution measured by a laser diffraction/scattering particle size distribution measurement method. In the particle size distribution, the particle diameter at which the cumulative volume is 80% is D 80 , and the particle diameter at which the cumulative volume is 20% is D 20 .
- Phosphonium salts include, for example, tetraalkylphosphonium salts and tetraphenylphosphonium salts. These salts may be, for example, halides, sulfates, phosphates, and acetates.
- phosphorus-containing compounds phosphoric acid and ammonium dihydrogen phosphate, which have a high intramolecular phosphorus content, are preferable from the viewpoint that a large amount of elemental phosphorus is easily incorporated into the carbonaceous material.
- the phosphorus-containing compound is preferably a compound having a volatilization temperature of preferably 100° C. or higher, more preferably 150° C. or higher, from the viewpoint of reaction with the saccharide compound during the heat treatment process.
- the production method further includes a compound having a saccharide skeleton and a nitrogen-containing Before the step (1) of mixing the compounds to obtain a mixture, at the same time as the step (1), or after the step (1), a step (b) of gelatinizing the compound having a saccharide skeleton may be further included.
- the step (b) is further performed, the cavities contained in the compound having a saccharide skeleton used as the raw material are closed, and as a result, the density of the finally obtained electrode formed from the carbonaceous material is easily increased, and the volume per unit It becomes easy to increase the discharge capacity of the battery.
- the carbonaceous material of the present invention is suitable, for example, as a carbonaceous material for a power storage device mounted on a vehicle such as an automobile (typically a non-aqueous electrolyte secondary battery for driving a vehicle).
- the vehicle is not particularly limited, and can be a vehicle commonly known as an electric vehicle, a hybrid vehicle with a fuel cell or an internal combustion engine, etc., but at least a power supply device equipped with the above battery. , an electric drive mechanism driven by power supply from the power supply device, and a control device for controlling the same.
- the vehicle may further include a power generating brake or a regenerative brake, and a mechanism for converting braking energy into electricity to charge the non-aqueous electrolyte secondary battery.
- the average particle size (particle size distribution) of carbide was measured by the following method. 5 mg of the sample was added to a 2 mL aqueous solution containing 5% by mass of a surfactant (“Toriton X100” manufactured by Wako Pure Chemical Industries, Ltd.), treated with an ultrasonic cleaner for 10 minutes or more, and dispersed in the aqueous solution. The particle size distribution was measured using this dispersion. The particle size distribution was measured using a particle size/particle size distribution analyzer (“Microtrac MT3300EXII” manufactured by Microtrac Bell Co., Ltd.). D50 is the particle diameter at which the cumulative volume is 50%, and this value was used as the average particle diameter.
- Argon ion laser light wavelength 532 nm
- Laser power on sample 100-300 W/cm 2
- Resolution 5-7 cm -1
- Measurement range 150-4000 cm -1
- Measurement mode XY Averaging Exposure time: 20 seconds
- Accumulation times 2 times Peak intensity measurement: Baseline correction Polynom-3rd order automatic correction Peak search & fitting processing GaussLoren
- Example 1 100 parts by mass of starch (cornstarch), 11.6 parts by mass of melamine (0.15 mol per mol of starch monosaccharide unit), 7.6 parts by mass of adipic acid (0.08 part per 1 mol of starch monosaccharide unit) mol) and 4 parts by mass of ammonium dihydrogen phosphate (0.06 mol per 1 mol of starch monosaccharide unit) were placed in a sample bottle and shaken to obtain a mixture (step 1 and step a). The resulting mixture was heated to 600° C. in a nitrogen gas atmosphere. At this time, the rate of temperature increase up to 600° C. was 600° C./hour (10° C./min).
- a carbonization treatment was performed by heat-treating at 600° C. for 30 minutes in a nitrogen gas stream to obtain a carbide (step 2).
- the amount of nitrogen gas supplied was 0.5 L/min per 10 g of starch.
- the obtained charcoal was divided into two, and each was pulverized using a ball mill under different conditions to obtain a pulverized charcoal having a D50 of 9 ⁇ m and a pulverized charcoal having a D50 of 2 ⁇ m (Step 3). .
- pulverized charcoal with D50 of 9 ⁇ m, pulverized charcoal with D50 of 2 ⁇ m and polystyrene (manufactured by Sekisui Plastics Co., Ltd., average particle size 400 ⁇ m) were added in a mass ratio of 1:2:0.3. was placed in a 100 ml container and mixed by shaking at 2 Hz for 5 minutes. The resulting mixture was heated to 1250° C. and subjected to a high-temperature firing treatment of heat treatment at 1250° C. for 30 minutes to obtain a carbonaceous material (Step 4). At this time, the rate of temperature increase up to 1250° C. was 600° C./hour (10° C./min). The temperature elevation and heat treatment described above were performed under a nitrogen gas stream. The amount of nitrogen gas supplied was 3 L/min per 5 g of pulverized carbide.
- Example 2 Steps 1 to 3 and step a were carried out in the same manner as in Example 1 to obtain a ground carbide having a D 50 of 9 ⁇ m and a ground carbide having a D 50 of 2 ⁇ m.
- Step 4 was carried out in the same manner as in Example 1, except that ABS resin (manufactured by Sekisui Plastics Co., Ltd., average particle size 100 ⁇ m) was mixed with the obtained pulverized carbide instead of polystyrene, and the carbonaceous material was obtained. Obtained.
- ABS resin manufactured by Sekisui Plastics Co., Ltd., average particle size 100 ⁇ m
- Example 3 Steps 1 to 3 and step a were carried out in the same manner as in Example 1 to obtain a ground carbide having a D 50 of 9 ⁇ m and a ground carbide having a D 50 of 2 ⁇ m.
- Step 4 was carried out in the same manner as in Example 1, except that instead of polystyrene, polymethyl methacrylate (PMMA, manufactured by Kuraray Co., Ltd., average particle size 300 ⁇ m) was mixed with the obtained pulverized carbide to obtain a carbonaceous material. Obtained.
- PMMA polymethyl methacrylate
- Example 4 Steps 1 to 3 and step a were carried out in the same manner as in Example 1 to obtain a ground carbide having a D 50 of 9 ⁇ m and a ground carbide having a D 50 of 2 ⁇ m. Then, the ground char with a D50 of 9 ⁇ m, the ground char with a D50 of 2 ⁇ m and polystyrene are placed in a 100 ml vessel in a mass ratio of 1:2:0.3 and shaken at 2 Hz for 5 minutes. mixed by The resulting mixture was heated to 1280° C. and subjected to a high-temperature firing treatment of heat treatment at 1280° C. for 11.25 minutes to obtain a carbonaceous material (Step 4).
- the rate of temperature increase up to 1280° C. was 600° C./hour (10° C./min).
- the temperature elevation and heat treatment described above were performed under a nitrogen gas stream.
- the amount of nitrogen gas supplied was 3 L/min per 5 g of pulverized carbide.
- Example 5 Steps 1 to 3 and step a were carried out in the same manner as in Example 1 to obtain a ground carbide having a D 50 of 9 ⁇ m and a ground carbide having a D 50 of 2 ⁇ m.
- the pulverized charcoal with D50 of 9 ⁇ m and the pulverized charcoal with D50 of 2 ⁇ m were placed in a 100 ml container so as to have a mass ratio of 1:2, and were mixed by shaking at 2 Hz for 5 minutes.
- the obtained mixture was heated to 1250° C. and subjected to a high-temperature firing treatment step of heat-treating at 1250° C. for 30 minutes.
- step 4 the temperature was lowered to 900° C., and a gasified volatile organic substance (hexane) was supplied at a concentration of 0.5 vol % at 900° C. for 30 minutes to obtain a carbonaceous material (step 4).
- a gasified volatile organic substance hexane
- the rate of temperature increase to 1250° C. and the rate of temperature decrease to 900° C. were 600° C./hour (10° C./min).
- the above temperature rise, temperature drop and heat treatment were performed under a nitrogen gas stream.
- the amount of nitrogen gas supplied was 3 L/min per 5 g of pulverized carbide.
- Example 7 100 parts by mass of starch (cornstarch), 11.6 parts by mass of melamine (0.15 mol per mol of starch monosaccharide unit), 7.6 parts by mass of adipic acid (0.08 part per 1 mol of starch monosaccharide unit) mol) and 6 parts by mass of ammonium dihydrogen phosphate (0.08 mol per 1 mol of starch monosaccharide unit) were placed in a sample bottle and shaken to obtain a mixture (step 1 and step a). The resulting mixture was heated to 600° C. in a nitrogen gas atmosphere. At this time, the rate of temperature increase up to 600° C. was 600° C./hour (10° C./min).
- a carbonization treatment was performed by heat-treating at 600° C. for 30 minutes in a nitrogen gas stream to obtain a carbide (step 2).
- the amount of nitrogen gas supplied was 0.5 L/min per 10 g of starch.
- the obtained charcoal was divided into two, and each was pulverized using a ball mill under different conditions to obtain a pulverized charcoal having a D50 of 9 ⁇ m and a pulverized charcoal having a D50 of 2 ⁇ m (Step 3). .
- the pulverized charcoal with D50 of 9 ⁇ m and the pulverized charcoal with D50 of 2 ⁇ m were placed in a 100 ml container so as to have a mass ratio of 1:2, and were mixed by shaking at 2 Hz for 5 minutes.
- the obtained mixture was heated to 1250° C. and subjected to a high temperature firing treatment step of heat treatment at 1250° C. for 10 minutes.
- the temperature was lowered to 900° C., and the gasified volatile organic matter (hexane) was supplied at a concentration of 0.5 vol % at 900° C. for 30 minutes to obtain a carbonaceous material (step 4).
- the rate of temperature increase to 1250° C. and the rate of temperature decrease to 900° C. were 600° C./hour (10° C./min).
- the above temperature rise, temperature drop and heat treatment were performed under a nitrogen gas stream.
- the amount of nitrogen gas supplied was 3 L/min per 5 g of pulverized carbide.
- Example 8 In step 4 of Example 5, the carbonaceous material was produced in the same manner as in Example 5 except that propane was supplied instead of hexane and the high temperature heat treatment step was performed, and then step 4 was performed at 800 ° C. for 30 minutes. Obtained.
- Steps 1 to 3 and step a were performed in the same manner as in Example 1 to obtain a ground carbide having a D 50 of 9 ⁇ m and a ground carbide having a D 50 of 2 ⁇ m (Step 3).
- the pulverized charcoal with D50 of 9 ⁇ m and the pulverized charcoal with D50 of 2 ⁇ m were placed in a 100 ml container so as to have a mass ratio of 1:2, and were mixed by shaking at 2 Hz for 5 minutes.
- the resulting mixture was heated to 1250° C. and subjected to a high-temperature firing treatment of heat treatment at 1250° C. for 30 minutes to obtain a carbonaceous material (Step 4).
- the rate of temperature increase up to 1250° C. was 600° C./hour (10° C./min).
- the temperature elevation and heat treatment described above were performed under a nitrogen gas stream.
- the amount of nitrogen gas supplied was 3 L/min per 5 g of pulverized carbide.
- Example 10 A carbonaceous material was obtained in the same manner as in Example 9, except that in step 4 of Example 9, the heat treatment at 1250° C. for 10 minutes was performed instead of the heat treatment at 1250° C. for 30 minutes.
- Comparative example 1 100 parts by mass of starch (cornstarch) was heated to 600° C. in a nitrogen gas atmosphere. At this time, the rate of temperature increase up to 600° C. was 600° C./hour (10° C./min). Then, a carbonization treatment was performed by heat-treating at 600° C. for 30 minutes in a nitrogen gas stream to obtain a carbide. At this time, the amount of nitrogen gas supplied was 0.5 L/min per 10 g of starch. After that, the obtained carbide was pulverized with a ball mill to obtain a pulverized carbide having a D 50 of 5.5 ⁇ m. The obtained pulverized carbide was heated to 1200° C.
- Comparative example 2 100 parts by mass of glucose and 36 parts by mass of ammonium chloride were mixed in a mortar. The resulting mixture was heated to 1000° C. in a nitrogen gas atmosphere. At this time, the rate of temperature increase up to 1000° C. was 240° C./hour (4° C./min). Then, a carbonization treatment was performed by heat treatment at 1000° C. for 60 minutes in a nitrogen gas stream to obtain a carbide (first firing). At this time, the amount of nitrogen gas supplied was 1 L/min per 5 g of glucose. After that, the obtained carbide was pulverized with a ball mill to obtain pulverized carbide. Next, the pulverized carbide was heated to 1200° C.
- the amount of nitrogen gas supplied was 0.5 L/min per 10 g of starch.
- the obtained carbide was pulverized with a ball mill to obtain a pulverized carbide having a D 50 of 5.5 ⁇ m (Step 3).
- the resulting pulverized carbide was heated to 1100° C. and subjected to a high-temperature firing treatment step (step 4) of heat treatment at 1100° C. for 60 minutes to obtain a carbonaceous material.
- the rate of temperature increase up to 1250° C. was 600° C./hour (10° C./min).
- the temperature elevation and heat treatment described above were performed under a nitrogen gas stream.
- the amount of nitrogen gas supplied was 3 L/min per 5 g of pulverized carbide.
- Comparative Example 4 A carbonaceous material was obtained in the same manner as in Comparative Example 3, except that 4 parts by mass of ammonium dihydrogen phosphate was added in step a in step 1 of Comparative Example 3.
- step a of step 1 of Comparative Example 4 instead of 4 parts by mass of ammonium dihydrogen phosphate, 6 parts by mass of ammonium dihydrogen phosphate (0.08 mol per 1 mol of starch monosaccharide unit) was mixed. A carbonaceous material was obtained in the same manner as in Comparative Example 4 except for the above.
- Comparative Example 7 (Comparative Example 7) In Comparative Example 4, instead of raising the temperature of the pulverized carbide to 1100° C. and performing heat treatment at 1100° C. for 60 minutes, the pulverized carbide was heated to 1150° C. and heat treated at 1150° C. for 10 minutes. A carbonaceous material was obtained in the same manner as in Comparative Example 4 except for the above.
- Comparative Example 8 In Comparative Example 4, instead of raising the temperature of the pulverized carbide to 1100° C. and heat-treating it at 1100° C. for 60 minutes, the pulverized carbide was heated to 1200° C., and as soon as the temperature reached 1200° C. A carbonaceous material was obtained in the same manner as in Comparative Example 4 except that the heating was stopped so as to lower the temperature and the heat treatment was performed.
- a carbonization treatment was performed by heat-treating at 600° C. for 30 minutes in a nitrogen gas stream to obtain a carbide (step 2).
- the amount of nitrogen gas supplied was 0.5 L/min per 10 g of starch.
- the obtained carbide was pulverized with a ball mill to obtain a pulverized carbide having a D 50 of 5.5 ⁇ m (Step 3).
- the obtained pulverized carbide was heated to 1200° C. and subjected to a high-temperature firing treatment of heat treatment at 1200° C. for 60 minutes to obtain a carbonaceous material (Step 4).
- the rate of temperature increase up to 1200° C. was 600° C./hour (10° C./min).
- the temperature elevation and heat treatment described above were performed under a nitrogen gas stream.
- the amount of nitrogen gas supplied was 3 L/min per 5 g of pulverized carbide.
- a negative electrode was produced according to the following procedure. 95 parts by mass of carbonaceous material, 2 parts by mass of conductive carbon black (“Super-P (registered trademark)” manufactured by TIMCAL), 1 part by mass of carboxymethyl cellulose (CMC), 2 parts by mass of styrene-butadiene rubber (SBR) and water 90 parts by mass were mixed to obtain a slurry. The obtained slurry was applied to a copper foil having a thickness of 15 ⁇ m, dried and then pressed to obtain an electrode having a diameter of 14 mm and a thickness of 45 ⁇ m.
- conductive carbon black (“Super-P (registered trademark)” manufactured by TIMCAL)
- CMC carboxymethyl cellulose
- SBR styrene-butadiene rubber
- the electrode prepared above was used as a working electrode, and metallic lithium was used as a counter electrode and a reference electrode.
- ethylene carbonate, dimethyl carbonate, and ethyl methyl carbonate were mixed and used at a volume ratio of 1:1:1.
- 1 mol/L of LiPF 6 was dissolved in this solvent and used as an electrolyte.
- a polypropylene film was used as the separator.
- a coin cell was fabricated in a glove box under an argon atmosphere.
- a charging/discharging test was performed on the lithium secondary battery having the above configuration using a charging/discharging test apparatus (manufactured by Toyo System Co., Ltd., "TOSCAT").
- Doping with lithium was performed at a rate of 70 mA/g with respect to the mass of the active material, and doping was performed to 1 mV with respect to the potential of lithium. Further, a constant voltage of 1 mV was applied against the lithium potential, and doping was terminated when the rate reached 2 mA/g with respect to the mass of the active material. The capacity at this time was defined as the charge capacity. Next, dedoping is performed at a rate of 70 mA / g with respect to the mass of the active material until the lithium potential becomes 1.5 V, and the charged capacity at this time is the initial charge capacity (mAh), and the discharged capacity is the initial discharge capacity. (mAh).
- the obtained initial charge capacity and initial discharge capacity were divided by the weight of the negative electrode, respectively, and the obtained values were defined as charge capacity per weight (mAh/g) and discharge capacity per weight (mAh/g) ( Evaluation of initial charge/discharge). Also, the percentage of the value obtained by dividing the initial discharge capacity by the initial charge capacity was defined as the current efficiency (%).
- Capacity retention rate and total efficiency after repeated charging and discharging ⁇ Capacity retention rate after repeated charging and discharging>
- the discharge capacity obtained after repeating the above initial charge/discharge evaluation conditions 10 times was taken as the discharge capacity after repeated charge/discharge.
- nitrogen element content, hydrogen element content, oxygen element content (elemental analysis), oxygen element content (XPS), phosphorus element content , the carbon spacing (d 002 ), the half width of the peak near 1360 cm ⁇ 1 , and the half width of the peak near 1650 cm ⁇ 1 are shown in Tables 1 and 2.
- Table 2 also shows the discharge capacity and current efficiency per weight, and the capacity retention rate and total efficiency after repeated charging and discharging, which were measured for the obtained battery.
- the batteries produced using the carbonaceous material of each example had a high discharge capacity per weight and exhibited excellent current efficiency. In addition, even after 10 times of repeated charging and discharging, the discharge capacity was high, and the capacity retention rate and overall efficiency were also high. On the other hand, the batteries manufactured using the carbonaceous materials of the respective comparative examples, which do not satisfy the predetermined nitrogen element content, hydrogen element content, and/or phosphorus element content, have sufficiently high discharge capacities per weight. Otherwise, the current efficiency was not sufficiently high, and the capacity retention rate after 10 times of repeated charging and discharging further decreased, resulting in a low overall efficiency.
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Abstract
Description
〔1〕元素分析による、窒素元素含有量が1.0質量%以上であり、水素元素含有量が0.1質量%以下であり、蛍光X線分析によるリン元素含有量が0.5質量%以上2.0質量%以下である、炭素質材料。
〔2〕X線回折測定による炭素面間隔(d002)が3.65Å以上である、〔1〕に記載の炭素質材料。
〔3〕元素分析による酸素元素含有量が1.0質量%未満である、〔1〕又は〔2〕に記載の炭素質材料。
〔4〕XPSによる酸素元素含有量が18質量%未満である、〔1〕~〔3〕のいずれかに記載の炭素質材料。
〔5〕レーザーラマン分光法により観測されるラマンスペクトルにおいて、1360cm-1付近のピークの半値幅の値が210cm-1以上である、〔1〕~〔4〕のいずれかに記載の炭素質材料。
〔6〕蓄電デバイスの負極用炭素質材料である、〔1〕~〔5〕のいずれかに記載の炭素質材料。
〔7〕〔1〕~〔6〕のいずれかに記載の炭素質材料を含む、蓄電デバイス用負極。
〔8〕〔7〕に記載の蓄電デバイス用負極を含む、蓄電デバイス。
〔9〕以下の工程:
(1)糖類骨格を有する化合物、及び窒素含有化合物を混合して混合物を得る工程、
(2)前記混合物を、不活性ガス雰囲気下、500~900℃で熱処理して炭化物を得る工程、
(3)前記炭化物を粉砕及び/又は分級する工程、及び
(4)粉砕及び/又は分級された前記炭化物を、不活性ガス雰囲気下、1200~1600℃で熱処理して炭素質材料を得る工程
を少なくとも含み、
(a)前記工程(4)における熱処理よりも前に、糖類骨格を有する化合物、該化合物を含む混合物、又は、該混合物の炭化物と、リン含有化合物とを混合する工程
を含む、〔1〕~〔6〕のいずれかに記載の炭素質材料の製造方法。
〔10〕前記工程(4)を揮発性有機物の存在下で行う、または、前記工程(4)の後に、揮発性有機物の存在下でさらなる熱処理を行う工程(5)をさらに含む、〔9〕に記載の製造方法。
XPSで分析される酸素元素含有量は炭素質材料の最表面に含まれる酸素元素の量を表しており、最表面に存在する官能基量に対応する。最表面の酸素元素含有量が少ないと、初期の段階から電解液やLiとの反応を抑制しやすく、特に初期の充放電における電流効率を向上させやすい。XPS分析による酸素元素含有量は小さい程よく、その下限は0質量%以上である。炭素質材料のXPS分析による酸素元素含有量は、炭素質材料を製造する際に添加され得る窒素含有化合物を増やすことにより低減することができ、添加され得るリン含有化合物の添加量、熱処理を施す温度、時間を調整する等によっても、上記の範囲に調整することができる。
(1)糖類骨格を有する化合物、及び窒素含有化合物を混合して混合物を得る工程、
(2)前記混合物を、不活性ガス雰囲気下、500~900℃で熱処理して炭化物を得る工程、
(3)前記炭化物を粉砕及び/又は分級する工程、及び
(4)粉砕及び/又は分級された前記炭化物を、不活性ガス雰囲気下、1200~1600℃で熱処理して炭素質材料を得る工程
を少なくとも含み、
(a)上記工程(4)における熱処理よりも前に、糖類骨格を有する化合物、該化合物を含む混合物、又は、該混合物の炭化物と、リン含有化合物とを混合する工程
を含む。本発明は、上記の炭素質材料の製造方法も提供する。
工程(1)の前に、糖類骨格を有する化合物に、該化合物の質量に対して5~50質量%の水を混合し、50~200℃の温度で1分~5時間加熱する工程(b1)、
工程(1)の前に、糖類骨格を有する化合物に、衝撃、圧潰、摩擦、及び/又はせん断の作用を有する機械的処理を施す工程(c1)、
工程(1)と同時に、もしくは工程(1)の後に、糖類骨格を有する化合物を含む混合物に、糖類骨格を有する化合物の質量に対して5~50質量%の水を混合し、50~200℃の温度で1分~5時間加熱する工程(b2)、及び/又は、
工程(1)と同時に、もしくは工程(1)の後に、糖類骨格を有する化合物を含む混合物に、衝撃、圧潰、摩擦、及び/又はせん断の作用を有する機械的処理を施す工程(c2)。
株式会社堀場製作所製、酸素・窒素・水素分析装置EMGA-930を用いて、不活性ガス溶解法に基づいて元素分析を行った。
当該装置の検出方法は、酸素:不活性ガス融解-非分散型赤外線吸収法(NDIR)、窒素:不活性ガス融解-熱伝導法(TCD)、水素:不活性ガス融解-非分散型赤外線吸収法(NDIR)であり、校正は、(酸素・窒素)Niカプセル、TiH2(H標準試料)、SS-3(O標準試料)、SiN(N標準試料)で行い、前処理として250℃、約10分で水分量を測定した試料20mgをNiカプセルに取り、元素分析装置内で30秒脱ガスした後に測定した。試験は3検体で分析し、平均値を分析値とした。上記のようにして、試料中の水素、酸素及び窒素元素含有量を得た。
株式会社リガク製。ZSX Primus-μを用いて、蛍光X線分析法に基づいて分析を行った。
上部照射方式用ホルダーを用い、試料測定面積を直径30mmの円周内とした。被測定試料2.0gとポリマーバインダ2.0g(Chemplex社製 Spectro Blend44μ Powder)とを乳鉢で混合し、成形機に入れた。成形機に15tonの荷重を1分間かけて、直径40mmのペレットを作製した。作製したペレットをポリプロピレン製のフィルムで包み、試料ホルダーに設置して測定を行った。X線源は30kV、100mAに設定した。リンKα線の強度からリン元素含有量を求めるため、分光結晶にGe(111)、検出器にガスフロー型比例係数管を使用し、2θが137~144°の範囲を、走査速度4°/分で測定した。
「株式会社リガク製MiniFlexII」を用い、後述する実施例及び比較例で調製した炭素質材料の粉体を試料ホルダーに充填し、Niフィルターにより単色化したCuKα線を線源とし、X線回折図形を得た。回折図形のピーク位置は重心法(回折線の重心位置を求め、これに対応する2θ値でピーク位置を求める方法)により求め、標準物質用高純度シリコン粉末の(111)面の回折ピークを用いて補正した。CuKα線の波長λを0.15418nmとし、以下に記すBraggの公式によりd002を算出した。
炭化物の平均粒子径(粒度分布)は、以下の方法により測定した。試料5mgを界面活性剤(和光純薬工業株式会社製「ToritonX100」)が5質量%含まれた2mL水溶液に投入し、超音波洗浄器で10分以上処理し、水溶液中に分散させた。この分散液を用いて粒度分布を測定した。粒度分布測定は、粒子径・粒度分布測定装置(マイクロトラック・ベル株式会社製「マイクロトラックMT3300EXII」)を用いて行った。D50は、累積体積が50%となる粒子径であり、この値を平均粒子径として用いた。
ラマン分光器(ナノフォトン社製「レーザーラマン顕微鏡Ramanforce」)を用い、炭素質材料である測定対象粒子を観測台ステージ上にセットし、対物レンズの倍率を20倍とし、ピントを合わせ、アルゴンイオンレーザ光を照射しながら測定した。測定条件の詳細は以下のとおりである。得られたラマンスペクトルから、1360cm-1付近のピークの半値幅、及び1650cm-1付近のピークの半値幅を決定した。
アルゴンイオンレーザ光の波長:532nm
試料上のレーザーパワー:100-300W/cm2
分解能:5-7cm-1
測定範囲:150-4000cm-1
測定モード:XY Averaging
露光時間:20秒
積算回数:2回
ピーク強度測定:ベースライン補正 Polynom-3次で自動補正
ピークサーチ&フィッテイング処理 GaussLoren
走査型X線光電子分光分析装置(アルバック・ファイ株式会社製「PHI Quantera SXM」)を用いて各炭素質材料のC1s、P2p、O1s、N1s由来のピークを観測し、元素組成比を確認した。詳細な測定条件は以下の通りである。
X線源:単色化 Al Kα(1486.6eV)
X線ビーム径 :200μmφ(50W,15kV)
測定範囲:1000μm(ヨコ)×300μm(タテ)
信号の取り込み角:45°
帯電中和条件:中和電子銃,Ar+イオン銃
圧力:1x10-6Pa
測定方法:通常測定
デンプン(コーンスターチ)100質量部とメラミン11.6質量部(デンプン単糖ユニット1モルに対して0.15モル)、アジピン酸7.6質量部(デンプン単糖ユニット1モルに対して0.08モル)、リン酸二水素アンモニウム4質量部(デンプン単糖ユニット1モルに対して0.06モル)をサンプル瓶にいれ振り混ぜることで混合物を得た(工程1及び工程a)。得られた混合物を、窒素ガス雰囲気中、600℃まで昇温した。この際、600℃までの昇温速度は600℃/時間(10℃/分)とした。次いで、窒素ガス気流下、600℃で30分間熱処理する炭化処理を行うことにより炭化物を得た(工程2)。この際、窒素ガスの供給量は、デンプン10gあたり0.5L/分であった。その後、得られた炭化物を2つに分け、それぞれを異なる条件でボールミルを用いて粉砕することにより、D50が9μmの粉砕した炭化物とD50が2μmの粉砕した炭化物を得た(工程3)。次に、D50が9μmの粉砕した炭化物、D50が2μmの粉砕した炭化物およびポリスチレン(積水化成品工業株式会社製、平均粒子径400μm)を、質量比1:2:0.3となるように100mlの容器にいれ、2Hzで5分間振とうすることにより混合した。得られた混合物を、1250℃まで昇温し、1250℃で30分間熱処理する高温焼成処理を行うことにより炭素質材料を得た(工程4)。この際、1250℃までの昇温速度は600℃/時間(10℃/分)とした。上記の昇温及び熱処理は窒素ガス気流下で行った。窒素ガスの供給量は、粉砕した炭化物5gあたり3L/分であった。
実施例1と同様に工程1~3及び工程aを行い、D50が9μmの粉砕した炭化物とD50が2μmの粉砕した炭化物を得た。得られた粉砕した炭化物に、ポリスチレンに代えて、ABS樹脂(積水化成品工業株式会社製、平均粒子径100μm)を混合した以外は実施例1と同様にして工程4を行い、炭素質材料を得た。
実施例1と同様に工程1~3及び工程aを行い、D50が9μmの粉砕した炭化物とD50が2μmの粉砕した炭化物を得た。得られた粉砕した炭化物に、ポリスチレンに代えて、ポリメチルメタクリレート(PMMA、株式会社クラレ製、平均粒子径300μm)を混合した以外は実施例1と同様にして工程4を行い、炭素質材料を得た。
実施例1と同様に工程1~3及び工程aを行い、D50が9μmの粉砕した炭化物とD50が2μmの粉砕した炭化物を得た。次に、D50が9μmの粉砕した炭化物、D50が2μmの粉砕した炭化物およびポリスチレンを、質量比1:2:0.3となるように100mlの容器にいれ、2Hzで5分間振とうすることにより混合した。得られた混合物を1280℃まで昇温し、1280℃で11.25分間熱処理する高温焼成処理を行うことにより炭素質材料を得た(工程4)。この際、1280℃までの昇温速度は600℃/時間(10℃/分)とした。上記の昇温及び熱処理は窒素ガス気流下で行った。窒素ガスの供給量は、粉砕した炭化物5gあたり3L/分であった。
実施例1と同様に工程1~3及び工程aを行い、D50が9μmの粉砕した炭化物とD50が2μmの粉砕した炭化物を得た。次に、D50が9μmの粉砕した炭化物とD50が2μmの粉砕した炭化物とを質量比1:2となるように100mlの容器にいれ、2Hzで5分間振とうすることにより混合した。得られた混合物を1250℃まで昇温し、1250℃で30分間熱処理する高温焼成処理工程を行った。その後800℃まで降温させ、ガス化させた揮発性有機物(ヘキサン)を0.5vol%濃度で800℃で30分間供給し、炭素質材料を得た(工程4)。この際、1250℃までの昇温速度及び800℃までの降温速度は600℃/時間(10℃/分)とした。上記の昇温、降温及び熱処理は窒素ガス気流下で行った。窒素ガスの供給量は、粉砕した炭化物5gあたり3L/分であった。
実施例1と同様に工程1~3及び工程aを行い、D50が9μmの粉砕した炭化物とD50が2μmの粉砕した炭化物を得た。次に、D50が9μmの粉砕した炭化物とD50が2μmの粉砕した炭化物を質量比1:2となるように100mlの容器にいれ、2Hzで5分間振とうすることにより混合した。得られた混合物を1250℃まで昇温し、1250℃で30分間熱処理する高温焼成処理工程を行った。その後900℃まで降温させ、ガス化させた揮発性有機物(ヘキサン)を0.5vol%濃度で900℃で30分間供給し、炭素質材料を得た(工程4)。この際、1250℃までの昇温速度及び900℃までの降温速度は600℃/時間(10℃/分)とした。上記の昇温、降温及び熱処理は窒素ガス気流下で行った。窒素ガスの供給量は、粉砕した炭化物5gあたり3L/分であった。
デンプン(コーンスターチ)100質量部とメラミン11.6質量部(デンプン単糖ユニット1モルに対して0.15モル)、アジピン酸7.6質量部(デンプン単糖ユニット1モルに対して0.08モル)、リン酸二水素アンモニウム6質量部(デンプン単糖ユニット1モルに対して0.08モル)をサンプル瓶にいれ振り混ぜることで混合物を得た(工程1及び工程a)。得られた混合物を、窒素ガス雰囲気中、600℃まで昇温した。この際、600℃までの昇温速度は600℃/時間(10℃/分)とした。次いで、窒素ガス気流下、600℃で30分間熱処理する炭化処理を行うことにより炭化物を得た(工程2)。この際、窒素ガスの供給量は、デンプン10gあたり0.5L/分であった。その後、得られた炭化物を2つに分け、それぞれを異なる条件でボールミルを用いて粉砕することにより、D50が9μmの粉砕した炭化物とD50が2μmの粉砕した炭化物を得た(工程3)。次に、D50が9μmの粉砕した炭化物とD50が2μmの粉砕した炭化物とを質量比1:2となるように100mlの容器にいれ、2Hzで5分間振とうすることにより混合した。得られた混合物を1250℃まで昇温し、1250℃で10分間熱処理する高温焼成処理工程を行った。その後900℃まで降温させ、ガス化させた揮発性有機物(ヘキサン)を0.5vol%濃度で900℃で30分間供し、炭素質材料を得た(工程4)。この際、1250℃までの昇温速度及び900℃までの降温速度は600℃/時間(10℃/分)とした。上記の昇温、降温及び熱処理は窒素ガス気流下で行った。窒素ガスの供給量は、粉砕した炭化物5gあたり3L/分であった。
実施例5の工程4において、ヘキサンに代えてプロパンを供給して高温熱処理工程を行った後、800℃30分間、工程4を行ったこと以外は実施例5と同様にして、炭素質材料を得た。
実施例1と同様に工程1~3及び工程aを行い、D50が9μmの粉砕した炭化物とD50が2μmの粉砕した炭化物を得た(工程3)。次に、D50が9μmの粉砕した炭化物とD50が2μmの粉砕した炭化物とを質量比1:2となるように100mlの容器にいれ、2Hzで5分間振とうすることにより混合した。得られた混合物を、1250℃まで昇温し、1250℃で30分間熱処理する高温焼成処理を行うことにより炭素質材料を得た(工程4)。この際、1250℃までの昇温速度は600℃/時間(10℃/分)とした。上記の昇温及び熱処理は窒素ガス気流下で行った。窒素ガスの供給量は、粉砕した炭化物5gあたり3L/分であった。
実施例9の工程4において、1250℃で30分間の熱処理に代えて、1250℃で10分間の熱処理を行ったこと以外は実施例9と同様にして、炭素質材料を得た。
デンプン(コーンスターチ)100質量部を、窒素ガス雰囲気中、600℃まで昇温した。この際、600℃までの昇温速度は600℃/時間(10℃/分)とした。次いで、窒素ガス気流下、600℃で30分間熱処理する炭化処理を行うことにより炭化物を得た。この際、窒素ガスの供給量は、デンプン10gあたり0.5L/分であった。その後、得られた炭化物をボールミルで粉砕することにより、D50が5.5μmの粉砕した炭化物を得た。得られた粉砕した炭化物を、1200℃まで昇温し、1200℃で60分間熱処理する高温焼成処理を行うことにより炭素質材料を得た。この際、1200℃までの昇温速度は600℃/時間(10℃/分)とした。上記の昇温及び熱処理は窒素ガス気流下で行った。窒素ガスの供給量は、粉砕した炭化物5gあたり3L/分であった。
グルコース100質量部と塩化アンモニウム36質量部を乳鉢で混合した。得られた混合物を、窒素ガス雰囲気中、1000℃まで昇温した。この際、1000℃までの昇温速度は240℃/時間(4℃/分)とした。次いで、窒素ガス気流下、1000℃で60分間熱処理して炭化処理を行なうことにより炭化物を得た(第1焼成)。この際、窒素ガスの供給量は、グルコース5gあたり1L/分であった。その後、得られた炭化物をボールミルで粉砕することにより、粉砕炭化物を得た。次に、粉砕炭化物を、1200℃まで昇温し、1200℃で60分間熱処理する高温焼成処理を行うことにより炭素質材料を得た(第2焼成)。この際、1200℃までの昇温速度は600℃/時間(10℃/分)とした。上記の昇温及び熱処理は窒素ガス気流下で行った。窒素ガスの供給量は、粉砕炭化物5gあたり3L/分であった。
デンプン(コーンスターチ)100質量部とメラミン11.6質量部(デンプン単糖ユニット1モルに対して0.15モル)、アジピン酸7.6質量部(デンプン単糖ユニット1モルに対して0.08モル)をサンプル瓶にいれ振り混ぜることで混合物を得た(工程1)。得られた混合物を、窒素ガス雰囲気中、600℃まで昇温した。この際、600℃までの昇温速度は600℃/時間(10℃/分)とした。次いで、窒素ガス気流下、600℃で30分間熱処理する炭化処理を行うことにより炭化物を得た(工程2)。この際、窒素ガスの供給量は、デンプン10gあたり0.5L/分であった。その後、得られた炭化物をボールミルで粉砕することにより、D50が5.5μmの粉砕した炭化物を得た(工程3)。得られた粉砕した炭化物を1100℃まで昇温し、1100℃で60分間熱処理する高温焼成処理工程(工程4)を行い、炭素質材料を得た。この際、1250℃までの昇温速度は600℃/時間(10℃/分)とした。上記の昇温及び熱処理は窒素ガス気流下で行った。窒素ガスの供給量は、粉砕した炭化物5gあたり3L/分であった。
比較例3の工程1中の工程aで、リン酸二水素アンモニウム4質量部を加えたこと以外は比較例3と同様にして、炭素質材料を得た。
比較例4の工程1中の工程aで、リン酸二水素アンモニウム4質量部に代えて、リン酸二水素アンモニウム2質量部(デンプン単糖ユニット1モルに対して0.03モル)を混合したこと以外は比較例4と同様にして、炭素質材料を得た。
比較例4の工程1中の工程aで、リン酸二水素アンモニウム4質量部に代えて、リン酸二水素アンモニウム6質量部(デンプン単糖ユニット1モルに対して0.08モル)を混合したこと以外は比較例4と同様にして、炭素質材料を得た。
比較例4において、粉砕した炭化物を1100℃まで昇温し1100℃で60分間の熱処理を行ったことに代えて、粉砕した炭化物を1150℃まで昇温し、1150℃で10分間の熱処理を行ったこと以外は比較例4と同様にして、炭素質材料を得た。
比較例4において、粉砕した炭化物を1100℃まで昇温し1100℃で60分間の熱処理を行ったことに代えて、粉砕した炭化物を1200℃まで昇温し、1200℃に達するとすぐに温度が下がるように加熱を停止して、熱処理を行ったこと以外は比較例4と同様にして、炭素質材料を得た。
デンプン(コーンスターチ)10gとメラミン0.2g(デンプン単糖ユニット1モルに対して0.026モル)、アジピン酸0.76g(デンプン単糖ユニット1モルに対して0.08モル)、リン酸二水素アンモニウム0.4g(デンプン単糖ユニット1モルに対して0.06モル)をサンプル瓶に入れ振り混ぜることで混合物を得た(工程1及び工程a)。得られた混合物を、窒素ガス雰囲気中、600℃まで昇温した。この際、600℃までの昇温速度は600℃/時間(10℃/分)とした。次いで、窒素ガス気流下、600℃で30分間熱処理する炭化処理を行うことにより炭化物を得た(工程2)。この際、窒素ガスの供給量は、デンプン10gあたり0.5L/分であった。その後、得られた炭化物をボールミルで粉砕することにより、D50が5.5μmの粉砕した炭化物を得た(工程3)。得られた粉砕した炭化物を、1200℃まで昇温し、1200℃で60分間熱処理する高温焼成処理を行うことにより炭素質材料を得た(工程4)。この際、1200℃までの昇温速度は600℃/時間(10℃/分)とした。上記の昇温および熱処理は窒素ガス気流下で行った。窒素ガスの供給量は、粉砕した炭化物5gあたり3L/分であった。
各実施例及び比較例で得た炭素質材料をそれぞれ用いて、以下の手順に従って負極を作製した。
炭素質材料95質量部、導電性カーボンブラック(TIMCAL製「Super-P(登録商標)」)2質量部、カルボキシメチルセルロース(CMC)1質量部、スチレン・ブタジエン・ラバー(SBR)2質量部及び水90質量部を混合し、スラリーを得た。得られたスラリーを厚さ15μmの銅箔に塗布し、乾燥後プレスして、直径14mmで打ち抜き厚さ45μmの電極を得た。
上記で作製した電極を作用極とし、金属リチウムを対極及び参照極として使用した。溶媒として、エチレンカーボネートとジメチルカーボネートとエチルメチルカーボネートを、体積比で1:1:1となるように混合して用いた。この溶媒に、LiPF6を1mol/L溶解し、電解質として用いた。セパレータにはポリプロピレン膜を使用した。アルゴン雰囲気下のグローブボックス内でコインセルを作製した。
上記構成のリチウム二次電池について、充放電試験装置(東洋システム株式会社製、「TOSCAT」)を用いて、充放電試験を行った。リチウムのドーピングは、活物質質量に対し70mA/gの速度で行い、リチウム電位に対して1mVになるまでドーピングした。さらにリチウム電位に対して1mVの定電圧を印加して、活物質質量に対し2mA/gの速度になった段階でドーピングを終了した。このときの容量を充電容量とした。次いで、活物質質量に対し70mA/gの速度で、リチウム電位に対して1.5Vになるまで脱ドーピングを行い、このとき充電した容量を初期充電容量(mAh)、放電した容量を初期放電容量(mAh)とした。得られた初期充電容量と初期放電容量を、それぞれ負極の重量で除して、得られた値を重量あたりの充電容量(mAh/g)と重量あたりの放電容量(mAh/g)とした(初期充放電の評価)。また、初期放電容量を、初期充電容量で除して、得られた値の百分率を電流効率(%)とした。
〈繰返しの充放電後の容量維持率〉
上記の初期充放電評価条件を10回繰り返し実施した後に得られた放電容量を繰返しの充放電後の放電容量とした。また、以下の式により繰返しの充放電後の容量維持率を算出した。
繰返しの充放電後の容量維持率(%)=繰返しの充放電後の放電容量(mAh/g)/初期放電容量(mAh/g)×100
以下の式により繰り返しの充放電後の全効率を算出した。全効率は初回の充放電による劣化および繰り返しの充放電による劣化の両方を示す指標となる。
全効率(%)=繰返しの充放電後の容量維持率(%)×電流効率(%)/100
Claims (10)
- 元素分析による、窒素元素含有量が1.0質量%以上であり、水素元素含有量が0.1質量%以下であり、蛍光X線分析によるリン元素含有量が0.5質量%以上2.0質量%以下である、炭素質材料。
- X線回折測定による炭素面間隔(d002)が3.65Å以上である、請求項1に記載の炭素質材料。
- 元素分析による酸素元素含有量が1.0質量%未満である、請求項1又は2に記載の炭素質材料。
- XPSによる酸素元素含有量が18質量%未満である、請求項1~3のいずれかに記載の炭素質材料。
- レーザーラマン分光法により観測されるラマンスペクトルにおいて、1360cm-1付近のピークの半値幅の値が210cm-1以上である、請求項1~4のいずれかに記載の炭素質材料。
- 蓄電デバイスの負極用炭素質材料である、請求項1~5のいずれかに記載の炭素質材料。
- 請求項1~6のいずれかに記載の炭素質材料を含む、蓄電デバイス用負極。
- 請求項7に記載の蓄電デバイス用負極を含む、蓄電デバイス。
- 以下の工程:
(1)糖類骨格を有する化合物、及び窒素含有化合物を混合して混合物を得る工程、
(2)前記混合物を、不活性ガス雰囲気下、500~900℃で熱処理して炭化物を得る工程、
(3)前記炭化物を粉砕及び/又は分級する工程、及び
(4)粉砕及び/又は分級された前記炭化物を、不活性ガス雰囲気下、1200~1600℃で熱処理して炭素質材料を得る工程
を少なくとも含み、
(a)前記工程(4)における熱処理よりも前に、糖類骨格を有する化合物、該化合物を含む混合物、又は、該混合物の炭化物と、リン含有化合物とを混合する工程
を含む、請求項1~6のいずれかに記載の炭素質材料の製造方法。 - 前記工程(4)を揮発性有機物の存在下で行う、または、前記工程(4)の後に、揮発性有機物の存在下でさらなる熱処理を行う工程(5)をさらに含む、請求項9に記載の製造方法。
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WO2019009333A1 (ja) | 2017-07-06 | 2019-01-10 | 株式会社クラレ | 非水電解質二次電池の負極活物質用の炭素質材料、非水電解質二次電池用負極、非水電解質二次電池ならびに炭素質材料の製造方法 |
WO2019009332A1 (ja) | 2017-07-06 | 2019-01-10 | 株式会社クラレ | 非水電解質二次電池の負極活物質用の炭素質材料、非水電解質二次電池用負極、非水電解質二次電池ならびに炭素質材料の製造方法 |
WO2019235469A1 (ja) * | 2018-06-05 | 2019-12-12 | 日本電気株式会社 | 還元型グラフェン系材料 |
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2022
- 2022-09-27 WO PCT/JP2022/035918 patent/WO2023058500A1/ja active Application Filing
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- 2022-09-27 JP JP2023552814A patent/JPWO2023058500A1/ja active Pending
- 2022-09-27 WO PCT/JP2022/035912 patent/WO2023058499A1/ja active Application Filing
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Publication number | Priority date | Publication date | Assignee | Title |
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JP2009200014A (ja) | 2008-02-25 | 2009-09-03 | Sumitomo Bakelite Co Ltd | 二次電池用炭素材、二次電池用電極、および二次電池 |
JP2018095517A (ja) * | 2016-12-14 | 2018-06-21 | 昭和電工株式会社 | 黒鉛材料、黒鉛材料の製造方法及び二次電池 |
WO2019009333A1 (ja) | 2017-07-06 | 2019-01-10 | 株式会社クラレ | 非水電解質二次電池の負極活物質用の炭素質材料、非水電解質二次電池用負極、非水電解質二次電池ならびに炭素質材料の製造方法 |
WO2019009332A1 (ja) | 2017-07-06 | 2019-01-10 | 株式会社クラレ | 非水電解質二次電池の負極活物質用の炭素質材料、非水電解質二次電池用負極、非水電解質二次電池ならびに炭素質材料の製造方法 |
WO2019235469A1 (ja) * | 2018-06-05 | 2019-12-12 | 日本電気株式会社 | 還元型グラフェン系材料 |
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TW202330397A (zh) | 2023-08-01 |
WO2023058499A1 (ja) | 2023-04-13 |
KR20240072176A (ko) | 2024-05-23 |
TW202333408A (zh) | 2023-08-16 |
JPWO2023058499A1 (ja) | 2023-04-13 |
KR20240072175A (ko) | 2024-05-23 |
JPWO2023058500A1 (ja) | 2023-04-13 |
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