ES2667211T3 - Recubrimiento de carbono amorfo de partículas carbonosas a partir de dispersiones que incluyen compuestos orgánicos anfifílicos - Google Patents

Recubrimiento de carbono amorfo de partículas carbonosas a partir de dispersiones que incluyen compuestos orgánicos anfifílicos Download PDF

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ES2667211T3
ES2667211T3 ES15719635.3T ES15719635T ES2667211T3 ES 2667211 T3 ES2667211 T3 ES 2667211T3 ES 15719635 T ES15719635 T ES 15719635T ES 2667211 T3 ES2667211 T3 ES 2667211T3
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amphiphilic organic
carbonaceous particles
synthetic
carbon coating
graphite
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Julie MICHAUD
Michael Spahr
Simone ZÜRCHER
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Imerys Graphite and Carbon Switzerland SA
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Abstract

Procedimiento para preparar partículas carbonosas modificadas en la superficie en el que dichas partículas carbonosas están recubiertas con una capa superficial de carbono amorfo, que comprende a. dispersar partículas carbonosas junto con un compuesto orgánico anfifílico, en el que el compuesto orgánico anfifílico es una lignina sulfatada, una sal de lignosulfonato, o mezclas de los mismos, y en el que las partículas carbonosas y el compuesto orgánico anfifílico se dispersan en presencia de un disolvente, b. secar por pulverización la dispersión, y c. efectuar la carbonización de las partículas secadas por pulverización que comprenden el compuesto orgánico anfifílico en la superficie de dichas partículas.

Description

imagen1
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imagen7
imagen8
imagen9
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imagen11
imagen12
imagen13
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imagen15
imagen16
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Material de partida
Grafito sintético No. 1 Grafito sintético No. 2 Grafito sintético No. 3 Grafito sintético No. 4 Grafito sintético No. 5 Grafito sintético No. 6
Tamaño de partícula
imagen18 imagen19 imagen20 imagen21 imagen22 imagen23
D10 (µm)
1.2 1.6 3.1 3.2 5.1 3.7
D5O (µm)
2.4 3.4 8.0 10.0 17.9 8.8
D90 (µm)
4.7 6.5 17.2 24.2 35.8 17.9
BET SSA (m2 g -1)
26 20 12 12 8.5 9.5
Densidad de xileno (g cm-3)
2.255 2.255 2.255 2.255 2.252 2.260
Densidad de Scott (g cm-3)
0.07 0.07 0.1 0.14 0.18 0.09
Distancia entre capas c/2 (nm)
0.3357 0.3357 0.3358 .3358 0.3358 0.3356
Tamaño de cristalita de Lc (nm)
60 75 126 131 147 175
[004]/[110] (intensidad de picos)
6.7 8.4 12.7 14.8 12.6 12.8
[004]/[110] (área de picos)
11.0 13.2 15.8 19.6 16.6 17.1
Porosidad (%)
60 imagen24 66 72 72 77
Pérdida de masa de recubrimiento de carbono pirolizado (resultado TGA) [%]
0.1 0.1 0.1 0.1 0.1 0.1
Q3 (S=0.8) en [%]
8.0 imagen25 imagen26 20.8 imagen27 imagen28
ks,p = Q3
1590 imagen29 imagen30 4160 imagen31 imagen32
(S=0.8)/(2.26-densidad de xileno)
imagen33 imagen34 imagen35 imagen36 imagen37 imagen38
Q3 (AR=0.8) en [%]
79.5 imagen39 imagen40 88.5 imagen41 imagen42
kAR,ρ = Q3 (AR=0.8)/(2.26densidad de xileno)
15900 imagen43 imagen44 17700 imagen45 imagen46
Capacidad reversible a 10 mA/g (Ah kg-1)
361 358 364 364 355 366
Propiedades de los materiales de coque de partida Las propiedades de los materiales de coque de partida se muestran en la Tabla 3.
19
Tabla 3: Propiedades de los materiales de coque de partida
Material de partida
Coque de petróleo Coque de acetileno
Tamaño de partícula
imagen47 imagen48
D10 (µm)
1.1 3.8
D50 (µm)
3.2 9.0
D90 (µm)
6.1 16.2
BET SSA (m2 g -1)
34.1 19
Densidad de Xileno (g cm-3)
2.071 1.534
Densidad de Scott (g cm-3)
0.151 0.44
Distancia entre capas c/2 (nm)
0.350 0.356
Tamaño de cristalina Lc (nm)
2.7 2
Porosidad (%)
67 56
Pérdida de masa de recubrimiento de carbono pirolizado (resultado TGA) [%]
0.0 -a
Q3 (S=0.8) en [%]
4.6 4.5
ks,p = Q3 (S=0.8)/(2.1-densidad de xileno)
160 8
Q3 (AR=0.8) en [%]
76.7 82.3
kAR,ρ = Q3 (AR=0.8)/( 2.1-densidad de xileno)
2646 145
Capacidad reversible en 10 mA/g (Ah kg-1)
256 590
aLa pérdida de masa de carbono pirolizado no puede determinarse a partir de muestras de coque de acetileno ya que algunas reacciones superficiales en el instrumento causan un ligero aumento en la masa (aproximadamente 1%) a temperaturas de hasta 450°C.
Propiedades de materiales recubiertos con núcleo de grafito
Las propiedades de materiales recubiertos a modo de ejemplo con un núcleo de grafito de acuerdo con la presente invención se muestran en la Tabla 4. Tabla 4: Propiedades de materiales recubiertos con núcleo de grafito
20
Ejemplo
1 2 3 4 5 6 7 8 9
Material de partida
Gráfico sintético No. 3 Gráfico sintético No. 2 Gráfico sintético No. 6 Gráfico sintético No. 3 Gráfico sintético No. 1 Gráfico sintético No. 3 Gráfico sintético No. 5 Gráfico sintético No. 4/LB2053 Gráfico sintético No. 3/Si
Tamaño de partícula
imagen49 imagen50 imagen51 imagen52 imagen53 imagen54 imagen55 imagen56 imagen57
D10 (µm)
8.1 9.2 9.1 10.9 6.7 12.7 7.7 10.3 7.5
D50 (µm)
21.6 17.5 19.2 21.4 16.4 23.9 19.8 20.7 16.5
D90 (µm)
40.7 30.8 24.5 38.3 32.2 41.1 41.6 34.9 31.1
BET SSA (m2 g -1)
3.7 3.8 3.6 5.5 11.3 1.3 3.4 5.7 5.0
Densidad de xileno (g cm-3)
2.184 2.069 2.169 2.181 2.197 2.044 2.156 2.147 2.197
Densidad de Scott (g cm-3)
0.25 imagen58 0.23 0.18 0.34 0.36 0.30 0.35 imagen59
Distancia entre capas c/2 (nm)
0.3358 0.3361 0.3357 0.3358 0.3359 0.3360 0.3358 0.3358 0.3358
Tamaño de cristalita Lc (nm)
96 48 127 84 48 60 122 131 103
[004]/[110] (intensidad)
1.3 1.0 1.5 1.1 0.9 1.2 2.2 1.8 1.5
[004]/[110] (área)
2.0 1.5 2.2 1.8 1.6 1.7 3.6 2.9 2.4
Porosidad (%)
76 imagen60 79 80 79 80 79 74 76
Pérdida de masa de recubrimiento de carbono pirolizado (resultado TGA) [%]
5.8 15.1 6.7 6.9 5.4 20.0 5.9 8.4 5.2
Q3 (S=0.8) en [%]
7.8 28.5 7.8 30.3 4.2 43.9 40.4 1.6 9.4
ks,p = Q3 (S=0.8)/(2.26densidad de xileno)
102 150 89 383 69 203 388 23.6 150
Q3 (AR=0.8) en [%]
81.8 76.6 78.6 77.9 23.3 84.8 98.3 44.5 75.8
21
Ejemplo
1 2 3 4 5 6 7 8 9
Material de partida
Gráfico sintético No. 3 Gráfico sintético No. 2 Gráfico sintético No. 6 Gráfico sintético No. 3 Gráfico sintético No. 1 Gráfico sintético No. 3 Gráfico sintético No. 5 Gráfico sintético No. 4/LB2053 Gráfico sintético No. 3/Si
kAR,ρ = Q3 (AR=0.8)/(2.26densidad de xileno)
1077 402 904 985 389 392 945 635 1202
Capacidad reversible a 10 mA/g (Ah kg-1)
356 311 346 346 345 325 346 351 423
Reducción relativa en capacidad irrreversible
28 59 2 5 45 (9%) 2 1* 21†
(%) en comparación con el grafito en bruto
imagen61 imagen62 imagen63 imagen64 imagen65 imagen66 imagen67 imagen68 imagen69
*La reducción relativa se compara con el KS 25 en bruto, la gravitación microcoloidal contribuiría considerablemente a la capacidad irreversible. Por lo tanto, la reducción relativa debería ser mayor que la mostrada. †La reducción relativa se compara con una mezcla de grafito en bruto y nanosilicio.
Propiedades de materiales recubiertos con núcleo de carbono no grafítico Las propiedades de los materiales revestidos con un núcleo de carbono no grafítico de acuerdo con la presente invención se muestran en la Tabla 5. Tabla 5: Propiedades de materiales recubiertos con núcleo de carbono no grafítico
Ejemplo
10 11 12 13 14
Material de partida
Coque de petróleo Coque de acetileno Coque de petróleo/ negro de lámpara Coque de petróleo/nanotubos de carbono Coque de petróleo/nanopolvo de estaño 60-80 nm
Tamaño de partícula
imagen70 imagen71 imagen72 imagen73 imagen74
D10 (µm)
6.7 6.6 6.0 11.0 5.7
D50 (µm)
13.2 13.8 13.8 24.5 13.7
D90 (µm)
24.9 26.2 27.4 44.5 27.9
BET SSA (m2 g -1)
5.4 1.6 14.7 11.7 9
22
Ejemplo
10 11 12 13 14
Material de partida
Coque de petróleo Coque de acetileno Coque de petróleo/ negro de lámpara Coque de petróleo/nanotubos de carbono Coque de petróleo/nanopolvo de estaño 60-80 nm
Densidad de xileno (g cm-3)
2.024 1.96 2.032 2.089 2.123
Densidad de Scott (g cm3)
0.4 imagen75 n.d. n.d. n.d.
Distancia entre capas c/2 (nm)
0.350 0.349 0.352 0.349 0.347
Tamaño de cristalita Lc (nm)
3.4 5.3 2.6 3.6 5.3
Porosidad (%)
74 60 n.d. n.d. n.d.
Pérdida de masa de recubrimiento de carbono pirolizado (resultado TGA) [%]
7 -a n.d. n.d. n.d.
Q3 (S=0.8) en [%]
4.7 7.4 n.d. n.d. n.d.
ks,p = Q3 (S=0.8)/(2.1densidad de xileno)
62 53 n.d. n.d. n.d.
Q3 (AR=0.8) en [%]
55.2 74.4 n.d. n.d. n.d.
kAR,ρ = Q3 (AR=0.8)/(2.1densidad de xileno)
725 531 n.d. n.d. n.d.
Capacidad reversible en 10 mA/g (Ah kg-1)
240 162 254 233 227
Reducción relativa en capacidad irreversible en (%) en comparación con el grafito en bruto
35 47 30 46 40
aLa naturaleza química de las partículas de coque de acetileno de núcleo es demasiado similar al recubrimiento de carbono amorfo y, por lo tanto, no se puede distinguir la reactividad con el oxígeno del recubrimiento y la partícula central. Por lo tanto, no es posible determinar la pérdida de masa del revestimiento de carbono pirolizado.
Se observa que el coque de acetileno revestido de carbono amorfo mostró una densidad de xileno ligeramente superior en comparación con el material de partida. Esto parece ser causado por la grafitización parcial ya que el material fue carbonizado a 1800°C.
Propiedades de materiales recubiertos alternativos (ejemplos comparativos)
Las propiedades comparativas de materiales recubiertos alternativos conocidos de la técnica anterior se muestran en la Tabla 6.
23
Tabla 6: Propiedades de materiales recubiertos alternativos
Ejemplo Comparativo
1 2 3 4
imagen76
Grafito natural recubierto Mesocarbono grafitado microesferas de mesocarbono grafitado Grafito recubierto con CVD†
Tamaño de partícula
imagen77 imagen78 imagen79 imagen80
D10 (µm)
9 7 12 7
D50 (µm)
18 14 23 16
D90 (µm)
31 27 41 32
BET SSA (m2 g -1)
2 1 1.8 3.8
Densidad de xileno (g cm-3)
2.244 2.247 2.233 2.218
Densidad de Scott (g cm-3)
0.63 0.66 1.115 0.258
Distancia entre capas c/2 (nm)
220 83 120 139
Tamaño de cristalita Lc (nm)
0.3361 0.3361 0.3359 0.3357
[004]/[110] (intensidad)
5.8 1.9 2.7 9.7
[004]/[110] (área)
8.2 3.0 4.1 10.5
Porosidad (%)
57 59 39 71
Pérdida de masa de recubrimiento de carbono pirolizado (resultado TGA) [%]
0.2 0.0 0.0 0.7
Q3 (S=0.8) en [%]
20.3 7.2 3.6 20.1
ks,p = Q3 (S=0.8)/(2.26-densidad de xileno)
1271 553 134 4026
Q3 (AR=0.8) en [%]
93 85.6 83 89
kAR,ρ = Q3 (AR=0.8)/(2.26-densidad de xileno)
5841 6580 3070 17700
Capacidad reversible en 10 mA/g (Ah kg-1)
353 326 imagen81 356
†Se utilizó un método de laboratorio de deposición química en fase de vapor (CVD) con acetileno para recubrir el grafito sintético TIMREX KS 5-25 a una temperatura de tratamiento de 1050°C. Se utilizó una mezcla de gas de acetileno en nitrógeno (relación 1:3) con un tiempo de tratamiento de 30 minutos
24
imagen82

Claims (1)

  1. imagen1
    imagen2
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