Preparation, modification and application of laser-induced graphene
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摘要: 激光诱导是一种新型的石墨烯制备技术(Laser induced graphene，LIG)，该工艺是通过高能束辐照含碳基底实现三维网络结构石墨烯的快速生成。与传统的石墨烯制备工艺相比，LIG制备技术具有快速制备、可图案化、环境友好、微观形貌可控和成分可控等特点，因此受到了广泛的关注。本文总结了LIG近年的研究进展，包括前驱体的成分调控、光源的选择和LIG的微结构控制。同时也探究了近年来LIG的原位和非原位的修饰改性方法，阐述了LIG在柔性储能电极和传感器领域的应用，并对LIG在集能源、传感和检测一体化设备方向的发展进行展望。Abstract: Laser-induced graphene (LIG) is a novel graphene preparation technique, which is a process for the rapid transformation of three-dimensional network-structured graphene by irradiating carbon-containing substrates with high-energy beams. Compared with the conventional graphene preparation process, LIG has attracted broad research interest because of its rapid preparation, designable patterning, environmental friendliness, controlled microscopic morphology, and controlled composition. This review summarizes the synthesis process of LIG, including the composition of precursors, the selection of light sources, and the structural modulation of LIG. It also explores the in-situ and non-in-situ modification methods of LIG in recent years, describes the applications of LIG in the field of flexible electrodes and sensors, and provides an outlook on the development of LIG in the direction of integrated energy, sensing, and detection devices.
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Key words:
- LIG /
- in-situ doping /
- composite /
- flexible electrode /
- sensors
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图 1 (a) 激光诱导聚酰亚胺(PI)生成激光诱导石墨烯(LIG)；(b) LIG薄膜的SEM图像(插图为相应的高倍SEM图像)；(c) PI薄膜和 LIG粉末的XRD图谱；(d) PI薄膜和LIG的拉曼光谱；(e) LIG的HRTEM图像；(f) LIG薄片边缘扫描透射显微镜(STEM)图像[31]
Figure 1. (a) Laser induced graphene (LIG) formation on polyimide (PI) by laser-induced; (b) SEM image of LIG thin films (Inset is the corresponding higher magnification SEM image); (c) XRD patterns of PI film and LIG powder; (d) Raman spectra of PI film and LIG; (e) HRTEM image of LIG; (f) Scanning transmission microscope (STEM) images of the edge of LIG sheet[31]
图 2 (a) 激光诱导聚砜(PSU)类聚合物转变成LIG的原理图[34]；(b) 椰子和面包表面转换为字母“R”形状的LIG[37]；(c) 聚苯并噁嗪基LIG的制备示意图[38]
Figure 2. (a) Schematic of PSU class polymers LIG via laser induction[34]; (b) LIG conversion of coconut and bread surfaces into letter "R" shape[37]; (c) Schematic illustration for the preparation of poly(Ph-ddm)-based LIG[38]
DDM—4, 4-diaminodiphenyl methane
图 3 (a) 森林状石墨烯薄膜的结构及其宽带光吸收和高光热转换的理论机制[52]；(b) LIG泡沫的制造和加工[53]；(c) 3D “R”形状的LIG泡沫[53]；(d) 光纤激光加工示意图[53]；(e) 叠层制造和光纤雕刻结合打印的3D LIG泡沫[53]；(f) 基于LIG的增材制造技术的示意图[54]；(g) 打印整个石墨烯涡轮机的分布流程[54]；(h) 全石墨烯宏观结构(AGM)的激光辅助生长示意图[55]；(i) 含20层LIG泡沫的AGM立方体(插图是AGM立方体的放大截面SEM图像)[55]
Figure 3. (a) Structure of forest-like graphene film and the theoretical mechanism of broadband light absorption and high photothermal conversion[52]; (b) Manufacturing and processing of LIG foam[53]; (c) 3D "R" shape of the milled LIG foam[53]; (d) Schematic of fiber laser milling process[53]; (e) 3D LIG foam printed by the combination of laminated object manufacturing and fiber laser milling[53]; (f) Schematic diagram of additive manufacturing technology based on LIG[54]; (g) Step-by-step process for printing a whole graphene turbine[54]; (h) Schematic illustration of laser-assisted growth of all-graphene macrostructures (AGM) [55]; (i) Cube of AGM with 20-layer LIG foam (The inset is the enlarged cross-sectional SEM image of the AGM cube)[55]
EG—Ethylene glycol
图 4 (a) 激光诱导PI生成LIG纤维(LIGF)的示意图[56]；(b) “R”形图案的LIGF[56]；(c) LIGF的SEM图像(插图为TEM图像)[56]；(d) PI生产激光诱导石墨烯电子器件的路线图[60]；(e) LIGF电子器件(LIGFE)的光学图像[60]；(f) 柔性LIGFE照片[60]
Figure 4. (a) Schematic diagram of laser induced PI generation of LIG fibers (LIGF)[56]; (b) "R" shape patterned LIGF[56]; (c) SEM image of LIGF (Inset is the TEM image) [56]; (d) Roadmap of producing laser-induced graphene fiber electronics (LIGFE) from PI[60]; (e) Optical photo of LIGFE[60]; (f) Digital photographs of flexible LIGFE[60]
图 5 (a) 从单层LIG (s-LIG)到致密LIG (d-LIG)的制备过程示意图[64]；(b) s-LIG 和d-LIG-2.4的XPS图谱[64]；(c) d-LIG-2.4中氮气峰的解卷积[64]；(d) 通过激光诱导在PI/聚磷酸铵(APP)薄膜上制造的掺磷石墨烯(LIPG)[68]；(e) 在可控气室中制造LIG[69]；((f), (g)) 在不同气体环境下制备的LIG样品的XPS图谱[69]；((h)~(k)) 在不同气体环境下制备的LIG样品的俯视图扫描电镜图像[69]
Figure 5. (a) Diagram of the preparation process for the transition from single LIG (s-LIG) to dense LIG (d-LIG) [64]; (b) XPS spectra of s-LIG and d-LIG-2.4[64]; (c) Deconvolution of nitrogen peak for d-LIG-2.4[64]; (d) Phosphorus-doped graphene (LIPG) fabricated on PI/ammonium polyphosphate (APP) film by laser induction[68]; (e) Abrication of LIG in a controlled gas chamber[69]; ((f), (g)) XPS spectra of LIG samples made under different gas atmospheres[69]; ((h)~(k)) Top view SEM images of LIG samples prepared under different gas atmospheres [69]
图 6 (a) 激光诱导含金属配合物的聚酰亚胺(MC-PI)薄膜形成金属氧化物(MO)-LIG[93]；((b)~(d)) MO-LIG的SEM图像[93]；((e)~(j)) LIG中的结晶金属氧化物的高分辨TEM图像[93]；(k) LIG/Cu的合成方法[94]；((i), (m)) LIG/Cu的TEM图像和高分辨TEM图像[94]
Figure 6. (a) Formation of metal oxide (MO)-LIG by laser induction on metal-complex-containing polyimide (MC-PI) film[93]; ((b)-(d)) SEM images of MO-LIG [93]; ((e)-(j)) High-resolution TEM images showing crystalline metal oxide in LIG[93]; (k) Synthetic scheme of the preparation of LIG/Cu[94]; ((i), (m)) TEM image and high-resolution TEM image of LIG/Cu[94]
PAA—Poly(amic acid); NPs—Nanoparticle; d—Lattice fringe spacing
图 7 (a) LIG-MnO2、LIG-FeOOH、LIG-聚苯胺(PANI)超级电容器(SC)的结构示意图[100]；(b) 微型超级电容器(MSC)器件的数码图像[100]；(c) LIG-MnO2的横断面扫描电镜图像[100]；(d) LIG-MnO2-2.5 h、LIG-PANI-15和LIG-FeOOH//LIG-MnO2的Ragone图[100]；(e) LIG-SC和堆叠的LIG-SC的制造示意图[102]；(f) LIG-SC柔性测试图[102]；(g) 激光诱导PI两侧形成石墨烯的横截面SEM图像[102]；(h) LIG的SEM图像[102]；(i) LIG的TEM图像(插图为高分辨TEM图像)[102]；(j) LIG-SC和LIG-MSC的Ragone图谱[102]
Figure 7. (a) Schematic structure of LIG-MnO2, LIG-FeOOH, LIG-polyaniline (PANI) supercapacitors (SC)[100]; (b) Digital photograph of one microsupercapacitor (MSC) device[100]; (c) Cross-sectional SEM image of LIG-MnO2[100]; (d) Ragone plots of LIG-MnO2-2.5 h, LIG-PANI-15, and LIG-FeOOH//LIG-MnO2; (e) Manufacturing schematic diagram of LIG-SC and stacked LIG-SC[100]; (f) LIG-SC flexible testing diagram[102]; (g) Cross sectional SEM image of a PI substrate with both sides laser induced to form graphene[102]; (h) SEM image of the LIG film[102]s; (i) TEM image of a LIG thin film (Inset is HRTEM image of LIG)[102]; (j) Ragone plots of single LIG-SC and LIG-MSC[102]
PVA—Poly(vinyl alcohol)
图 8 (a) Kevlar纤维向LIG转变的示意图；(b) LIG-Kevlar气体传感器对不同NO2浓度的响应曲线；(c) LIG-Kevlar气体传感器在100 ppm NO2浓度下的3次循环响应曲线；(d) 用于心电图(ECG)测量的LIG-Kevlar电极的示意图；(e) 用LIG-Kevlar电极测量手臂的心电图信号；(f) 放大后心电信号[109]
Figure 8. (a) Schematic illustration showing the transformation of Kevlar to LIG; (b) Response curves of the LIG-Kevlar textile gas sensor to different NO2 concentrations; (c) Three-cycle response curves of the LIG-Kevlar gas sensor upon exposure to 100 ppm of NO2; (d) Schematic illustration showing the LIG-Kevlar textile electrode for electrocardiogram (ECG) measurement; (e) ECG signals from the arms measured by LIG-Kevlar textile electrodes; (f) Magnified ECG signal[109]
图 9 (a) LIG具有发射和检测声音的能力；(b) 在10 kHz和20 kHz时，声压与输入功率的关系图(方块是实验结果，直线是理论结果)；(c) 不同功率激光器产生的 LIG 输出声压级(SPL)与频率的关系(4条曲线均以1 W的输入功率进行归一化处理)；(d) 测试人员佩戴了LIG人工喉；(e) LIG的阻值随测试者喉咙振动而变化[114]
Figure 9. (a) LIG has the ability of emitting and detecting sound; (b) Plot of the sound pressure versus the input power at 10 kHz and 20 kHz (The square is the experimental result and the line is the theoretical result); (c) Output sound pressure level (SPL) versus the frequency of LIG generated by the laser with different power (The four curves are normalized with the input power of 1 W); (d) Tester wearing the LIG artificial throat; (e) LIG's resistance changes towards the throat vibrations of the tester[114]
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