二维层状材料的剥离及其复合物制备与性能研究
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摘要
石墨烯(G)与六方氮化硼(h-BN)具备相似的晶体结构，却有着各自独特的物理化学性能。将这两种二维材料进行插层复合，就使六方氮化硼与石墨烯具备互补的物化性质及电学，如半导体性、高温稳定性和高化学稳定性，可以作为碳材料的有效补充。本文利用化学溶剂法成功剥离得到单层、双层及多层六方氮化硼及石墨烯材料，并将六方氮化硼与石墨烯进行层与层交替叠加插层复合，形成类石墨烯半导体材料。此硼碳氮插层混合材料具有可调的能带结构，具备了半导体材料的基本特性，显示了良好的热稳定性同时还兼具石墨烯的坚韧性。另外，为了进一步探索六方氮化硼作为基体与纳米颗粒的掺杂制备生物复合材料。通过化学还原法得到纳米尺寸极小的纳米银颗粒负载于六方氮化硼材料表面，形成了纳米银/六方氮化硼复合物，这种新型复合材料具备优异的抗菌持久性能。
(1)采用化学溶剂法剥离将氮化硼与石墨粉末进行剥离，得到各自单层、双层及多层的二维超薄层状六方氮化硼及石墨烯材料。实验中根据表面张力在剥离过程中的影响，选择适宜的有机溶剂。通过对比不同有机溶剂下对六方氮化硼及石墨烯的剥离效果，得到剥离六方氮化硼的最佳有机溶剂为：异丙醇(IPA)；剥离石墨烯材料的有机溶剂为：二甲基甲酰胺(DMF)。在这两种溶剂中剥离后的六方氮化硼和石墨烯材料为较完整的六方晶体结构，并且通过控制离心速度得到不同层数的六方氮化硼及石墨烯材料。剥离后的六方氮化硼纳米材料直径尺寸约在500～800nm，石墨烯纳米材料约为600～900nm。这种方法优点在于方法简单，成本低，产量高，可实现产业化。
(2)将所得层状六方氮化硼与石墨烯材料再次溶于有机溶剂DMF中，进行一定强度的超声离心后得到了六方氮化硼/石墨烯插层混合物薄膜材料。由于在有机溶剂及机械超声作用下，破坏了原有材料各原子层间的范德华力，使得层状六方氮化硼与石墨烯各层之间重新插层排列以达到稳定状态，即这种新型复合材料的结构为六方氮化硼与石墨烯层层交替叠加类似“sandwich”的结构形式存在。利用各种不同表征手段证明了这种复合材料不仅具备六方氮化硼与石墨烯各自的物理化学性质，而且还具有其独特的电学性质，通过调整二者的掺入量比例来控制六方氮化硼/石墨烯混合物的光学带隙宽度。经电阻率、磁阻率及霍尔效应测试得出：六方氮化硼/石墨烯插层混合物具有一定的电阻率及霍尔效应现象，但与单纯石墨烯相比，其值并不是特别突出，说明六方氮化硼的引入促使此插层混合物的电学性质发生很大变化。
(3)通过选用VASP软件，对六方氮化硼/石墨烯插层混合物的插层机理、带隙变化规律的理论计算。石墨烯与六方氮化硼界面“振荡”的产生而导致各自对应电子改变，最后产生偶极现象而促使带隙发生变化。根据混合激子波函数的计算得出：单纯六方氮化硼具有较大带隙表现为绝缘体性质，当掺杂不同比例的石墨烯后使六方氮化硼的激子发生转移而导致其带隙随之分裂，进而在半导体或者半金属性之间变化。
(4)将剥离后的层状六方氮化硼作为基体，借助于微波辐射条件反应制备了纳米银颗粒，并均匀沉积在六方氮化硼表面形成纳米银/六方氮化硼复合材料。所得纳米银尺寸在5～10nm左右，无团聚现象。通过对此复合材料进行抗菌及杀菌性能测试后得出：纳米银/六方氮化硼复合物具有强烈的抗菌能力，杀菌率在99%以上。由此可以看出，此复合材料可应用于生物医药及防腐蚀防污涂层等领域。
本文通过化学溶剂法得到六方氮化硼/石墨烯插层混合材料，通过不同表征手段的测试，得到此插层材料具备其独特的物化性能及电学特性，由于六方氮化硼的插入导致石墨烯的带隙被打开，呈现半导体材料的特征，有望代替硅材料应用于微电子工业领域。另外，凭借微波辐射与化学还原反应相结合的方法合成了纳米银/六方氮化硼复合材料，这种新型材料具有良好的抗菌性能，可被用于生物医药、海洋工程防污防腐蚀等领域，由于纳米银插入到六方氮化硼各层之间，改变了原有存在的原子间范德华力，使得六方氮化硼的光学带隙也随之发生改变，从这个特征上出发，有可能实现此混合物在电学领域的应用。
Graphene (G) and hexagonal boron nitride (h-BN) have been received enormousattention due to their outstanding physical and mechanical properties. Owing to theirsimilar structures and distinct electronic properties, h-BN as the isoelectric analog ofgraphene that is considered as good candidate for fabricating h-BN/G composites withstackings structures, which could be a complete new compound and offer newfunctionalities, such as electron field, itinerant ferromagnetism, and half metallicity.So if h-BN hybridizes with graphene, it could be used in microelectronic applications,which may be a post-silicon solution. To further develop the layered h-BN as a carrierto fabricate nanoparticles/h-BN bio-composite material. We prepared the silver nano-particles depositing on the h-BN nanosheets by using chemical reduction method.This novel composite possesses excellent antibacterial effect and durability.
Here we demonstrate this concept for solids consisting of randomly stacked layers ofgraphene and hexagonal boron nitride (h-BN). Exfoliated h-BN and graphene weremixed, in various concentrations, to create artificially stacked h-BN/G solids. Thesevan der Waals stacked hybrid solid materials show interesting electrical, mechanicaland optical properties distinctly different from their starting parent layers. Theapproach could be used to create artificial materials, made from the van der Waalsstacking of robust atomic layers of different layered solids with vastly differentproperties.
(1) Dispersions of exfoliated h-BN layers and graphene have been prepared by liquidphase exfoliation method. Several organic solvents were selected to exfoliate boronnitride and graphite into2-D layered h-BN and graphene nanosheets. The resultsshow that the surface tension has a significant effect on exfoliation these twomaterials. The optimal solvent for exfoliation on h-BN is isopropanol (IPA) and forgraphene is dimethyl formamide (DMF). The crystal structures of exfoliated h-BNand graphene nanosheets are improved and satisfied. In addition, single-layer, double-layer and multi-layered h-BN and graphene were obtained by controllingcentrifugation speed. The diameter of h-BN nanosheets is about500~800nm, andgraphene nanosheets is around600~900nm. It is easier to be scable and high yield by using liquid phase exfoliation comparing to other methods, such as chemical vapordeposition (CVD).
(2) Layered hexagonal boron nitride and graphene dissovled in DMF, h-BN/graphenehybrid nanosheets was obtained after sonication and centrifugation. As the surfacetension and mechanical ultrasonication, the atomic van der Waals forces betweenlayered h-BN and graphene re-arranged which fabricate stacking sturctures of h-BNand graphene hybrid layer by layer. The physical, chemical and electrical propertieswere characterized. The resistivity, magnetoresistance and Hall Effect results showthat h-BN/graphene hybrid composites exhibit resistivity and Hall-effect phenomenon.
(3) The band gaps investigation of h-BN/G hybrid composites was conducted usingVASP (Vienna Ab-initio Simulation Package), a software package which relaxes alattice to its minimum energy configuration by means of density functional theory(DFT). The following two and three layer systems were studied: G/h-BN, G/h-BN/G,h-BN/G/h-BN, h-BN/h-BN/G, and G/G/h-BN. Ultimately, the minimum energystacking arrangements, inter-layer separations, and intra-layer lattice parameters werefound for each system. These maximally stable configurations were then analyzed fortheir structural and electronic properties. For the two-layer system, an AB stackingarrangement with boron, nitride overtop of carbon was found to be the most stable.Similarly, three-layer systems were found to be most stable with boron overtop ofcarbon (h-BN/G/h-BN system). In addition, the results suggest that h-BN layersadjacent to graphene do not significantly increase the band gap of the overall structure;we predict that the further addition of h-BN layers to h-BN/G/h-BN or h-BN/h-BN/G system would not significantly increase the band gaps of either.
(4) Layered hexagonal boron nitride nanosheets as substrate, the silver nano-particles(SNPs) was synthesized by using chemical reaction with microwave-assisted.From the TEM results show that the uniform silver nano-particles were deposited onthe surface of hexagonal boron nitride nanosheets to fabricate SNPs/h-BN composites.The size of silver nano-particles is about5~10nm, and no agglomeration phenomenon.The antimicrobial and bactericidal properties of SNPs/h-BN composite material wereinvestigated by inhibition zone. The results indicate that the SNPs/h-BN compositesexhibit strong antibacterial fuction, and the sterilization rate up to99%.In this paper, layered h-BN/G hybrid composites were fabricated by liquid phaseexfoliation method. It is expected that the novel material would replace siliconmaterials which is used in microelectronic divices; chemical reduction with microwave-assisted to synthesize nano-silver/h-Bncomposite. It is expected that thiscomposite material would be used for bio-medicine, marine engineering anti-corrosion and anti-fouling coating fields.
(1)采用化学溶剂法剥离将氮化硼与石墨粉末进行剥离，得到各自单层、双层及多层的二维超薄层状六方氮化硼及石墨烯材料。实验中根据表面张力在剥离过程中的影响，选择适宜的有机溶剂。通过对比不同有机溶剂下对六方氮化硼及石墨烯的剥离效果，得到剥离六方氮化硼的最佳有机溶剂为：异丙醇(IPA)；剥离石墨烯材料的有机溶剂为：二甲基甲酰胺(DMF)。在这两种溶剂中剥离后的六方氮化硼和石墨烯材料为较完整的六方晶体结构，并且通过控制离心速度得到不同层数的六方氮化硼及石墨烯材料。剥离后的六方氮化硼纳米材料直径尺寸约在500～800nm，石墨烯纳米材料约为600～900nm。这种方法优点在于方法简单，成本低，产量高，可实现产业化。
(2)将所得层状六方氮化硼与石墨烯材料再次溶于有机溶剂DMF中，进行一定强度的超声离心后得到了六方氮化硼/石墨烯插层混合物薄膜材料。由于在有机溶剂及机械超声作用下，破坏了原有材料各原子层间的范德华力，使得层状六方氮化硼与石墨烯各层之间重新插层排列以达到稳定状态，即这种新型复合材料的结构为六方氮化硼与石墨烯层层交替叠加类似“sandwich”的结构形式存在。利用各种不同表征手段证明了这种复合材料不仅具备六方氮化硼与石墨烯各自的物理化学性质，而且还具有其独特的电学性质，通过调整二者的掺入量比例来控制六方氮化硼/石墨烯混合物的光学带隙宽度。经电阻率、磁阻率及霍尔效应测试得出：六方氮化硼/石墨烯插层混合物具有一定的电阻率及霍尔效应现象，但与单纯石墨烯相比，其值并不是特别突出，说明六方氮化硼的引入促使此插层混合物的电学性质发生很大变化。
(3)通过选用VASP软件，对六方氮化硼/石墨烯插层混合物的插层机理、带隙变化规律的理论计算。石墨烯与六方氮化硼界面“振荡”的产生而导致各自对应电子改变，最后产生偶极现象而促使带隙发生变化。根据混合激子波函数的计算得出：单纯六方氮化硼具有较大带隙表现为绝缘体性质，当掺杂不同比例的石墨烯后使六方氮化硼的激子发生转移而导致其带隙随之分裂，进而在半导体或者半金属性之间变化。
(4)将剥离后的层状六方氮化硼作为基体，借助于微波辐射条件反应制备了纳米银颗粒，并均匀沉积在六方氮化硼表面形成纳米银/六方氮化硼复合材料。所得纳米银尺寸在5～10nm左右，无团聚现象。通过对此复合材料进行抗菌及杀菌性能测试后得出：纳米银/六方氮化硼复合物具有强烈的抗菌能力，杀菌率在99%以上。由此可以看出，此复合材料可应用于生物医药及防腐蚀防污涂层等领域。
本文通过化学溶剂法得到六方氮化硼/石墨烯插层混合材料，通过不同表征手段的测试，得到此插层材料具备其独特的物化性能及电学特性，由于六方氮化硼的插入导致石墨烯的带隙被打开，呈现半导体材料的特征，有望代替硅材料应用于微电子工业领域。另外，凭借微波辐射与化学还原反应相结合的方法合成了纳米银/六方氮化硼复合材料，这种新型材料具有良好的抗菌性能，可被用于生物医药、海洋工程防污防腐蚀等领域，由于纳米银插入到六方氮化硼各层之间，改变了原有存在的原子间范德华力，使得六方氮化硼的光学带隙也随之发生改变，从这个特征上出发，有可能实现此混合物在电学领域的应用。
Graphene (G) and hexagonal boron nitride (h-BN) have been received enormousattention due to their outstanding physical and mechanical properties. Owing to theirsimilar structures and distinct electronic properties, h-BN as the isoelectric analog ofgraphene that is considered as good candidate for fabricating h-BN/G composites withstackings structures, which could be a complete new compound and offer newfunctionalities, such as electron field, itinerant ferromagnetism, and half metallicity.So if h-BN hybridizes with graphene, it could be used in microelectronic applications,which may be a post-silicon solution. To further develop the layered h-BN as a carrierto fabricate nanoparticles/h-BN bio-composite material. We prepared the silver nano-particles depositing on the h-BN nanosheets by using chemical reduction method.This novel composite possesses excellent antibacterial effect and durability.
Here we demonstrate this concept for solids consisting of randomly stacked layers ofgraphene and hexagonal boron nitride (h-BN). Exfoliated h-BN and graphene weremixed, in various concentrations, to create artificially stacked h-BN/G solids. Thesevan der Waals stacked hybrid solid materials show interesting electrical, mechanicaland optical properties distinctly different from their starting parent layers. Theapproach could be used to create artificial materials, made from the van der Waalsstacking of robust atomic layers of different layered solids with vastly differentproperties.
(1) Dispersions of exfoliated h-BN layers and graphene have been prepared by liquidphase exfoliation method. Several organic solvents were selected to exfoliate boronnitride and graphite into2-D layered h-BN and graphene nanosheets. The resultsshow that the surface tension has a significant effect on exfoliation these twomaterials. The optimal solvent for exfoliation on h-BN is isopropanol (IPA) and forgraphene is dimethyl formamide (DMF). The crystal structures of exfoliated h-BNand graphene nanosheets are improved and satisfied. In addition, single-layer, double-layer and multi-layered h-BN and graphene were obtained by controllingcentrifugation speed. The diameter of h-BN nanosheets is about500~800nm, andgraphene nanosheets is around600~900nm. It is easier to be scable and high yield by using liquid phase exfoliation comparing to other methods, such as chemical vapordeposition (CVD).
(2) Layered hexagonal boron nitride and graphene dissovled in DMF, h-BN/graphenehybrid nanosheets was obtained after sonication and centrifugation. As the surfacetension and mechanical ultrasonication, the atomic van der Waals forces betweenlayered h-BN and graphene re-arranged which fabricate stacking sturctures of h-BNand graphene hybrid layer by layer. The physical, chemical and electrical propertieswere characterized. The resistivity, magnetoresistance and Hall Effect results showthat h-BN/graphene hybrid composites exhibit resistivity and Hall-effect phenomenon.
(3) The band gaps investigation of h-BN/G hybrid composites was conducted usingVASP (Vienna Ab-initio Simulation Package), a software package which relaxes alattice to its minimum energy configuration by means of density functional theory(DFT). The following two and three layer systems were studied: G/h-BN, G/h-BN/G,h-BN/G/h-BN, h-BN/h-BN/G, and G/G/h-BN. Ultimately, the minimum energystacking arrangements, inter-layer separations, and intra-layer lattice parameters werefound for each system. These maximally stable configurations were then analyzed fortheir structural and electronic properties. For the two-layer system, an AB stackingarrangement with boron, nitride overtop of carbon was found to be the most stable.Similarly, three-layer systems were found to be most stable with boron overtop ofcarbon (h-BN/G/h-BN system). In addition, the results suggest that h-BN layersadjacent to graphene do not significantly increase the band gap of the overall structure;we predict that the further addition of h-BN layers to h-BN/G/h-BN or h-BN/h-BN/G system would not significantly increase the band gaps of either.
(4) Layered hexagonal boron nitride nanosheets as substrate, the silver nano-particles(SNPs) was synthesized by using chemical reaction with microwave-assisted.From the TEM results show that the uniform silver nano-particles were deposited onthe surface of hexagonal boron nitride nanosheets to fabricate SNPs/h-BN composites.The size of silver nano-particles is about5~10nm, and no agglomeration phenomenon.The antimicrobial and bactericidal properties of SNPs/h-BN composite material wereinvestigated by inhibition zone. The results indicate that the SNPs/h-BN compositesexhibit strong antibacterial fuction, and the sterilization rate up to99%.In this paper, layered h-BN/G hybrid composites were fabricated by liquid phaseexfoliation method. It is expected that the novel material would replace siliconmaterials which is used in microelectronic divices; chemical reduction with microwave-assisted to synthesize nano-silver/h-Bncomposite. It is expected that thiscomposite material would be used for bio-medicine, marine engineering anti-corrosion and anti-fouling coating fields.
引文
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