Liquid plasmas and their applications in nanomaterial synthesis
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摘要:
液相等离子体是冷等离子体的一个新分支，具有温度低、传质传热快、常压操作、反应活性高等特点。基于液相等离子体的过程强化技术在纳米材料制备、挥发性有机物降解、杀菌消毒、化学合成等领域有广泛的应用前景。以液相等离子体中纳米材料的制备为研究对象，介绍了反应体系可能存在的活性粒子、检测方法和反应机理；对常见的反应器结构进行归纳整理，按照放电是否在电解液内部进行将其分为非浸没式和浸没式液相等离子体两大类，并列举了几种典型的反应器结构；介绍了几类利用液相等离子体技术制备纳米材料的典例，并对该领域的研究现状做了总结；对该领域亟需解决的问题与发展方向进行讨论与展望。
Abstract:As a new branch in non-thermal plasmas, plasma-liquid technology is characterized by low temperature, mass and heat transfer effectiveness, atmospheric-pressure operation and high reactivity. Process intensification techniques based on liquid plasmas have wide applications in nanofabrication, volatile organic compounds decomposition, sterilization and disinfection, chemical synthesis, etc. Taking the synthesis of nanomaterials by the liquid plasma as the research object, firstly, the reactive radicals that may exist in the system are introduced, together with the relevant characterization methods and possible reaction mechanisms; afterwards, the most widely adopted plasma-liquid systems are illustrated, which can be divided into non-immersed systems and immersed systems according to whether plasma is formed within the bulk of electrolytes; furthermore, several typical examples of nanomaterials synthesized by the plasma-liquid method are presented, with a summary of the state-of-art research in this field, finally, the challenges and development trends are discussed.
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Key words:
- liquid plasmas /
- plasma equipment /
- nanotechnology /
- plasma-liquid interaction /
- nanomaterials
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图 2 液相等离子体制备贵金属机理示意图
Figure 2. Mechanism schematic diagram of liquid phase plasma system preparation of metal
图 7 液相等离子体制备纳米材料典例
Figure 7. Typical examples of preparation of nanomaterials by liquid plasma
表 1 液相等离子体中常见自由基的检测方法及相关反应
Table 1. Detection methods and related reactions of common free radicals in liquid plasma
species detection method advantages and disadvantages correlation reaction references hydrogen peroxide
(H2O2)(1) titanium sulfate reagent colorimetry
(2) colorimetric or fluorometric analysis(1) less interference, good stability, but limited sensitivity(2) many interference factors (such as air, pH, solvent, etc.), but high sensitivity, lower detection limit～10×10−6 OH + H2O·→ H2O2+ H2O2+2H++2e−→H2O2H2O2+H++e−→H2O+OH [17][18][19] hydrogen
atom (H)(1) EPR technology
(2) isotope labeling(1) high sensitivity, low detection limit, easy decomposition of the product, requiring excess capture agent(2) the source, distribution and chemical reaction of H atoms can be explored, but it is usually used in conjunction with the EPR method H++e−→H [20][21][22] hydroxyl radicals
(OH·)(1) EPR technology(2) HPLC method
(3) spectrophotometry(1) high sensitivity and low detection limit, the most ideal method for the determination of hydroxyl radicals, the instrument is expensive, the choice of capture agent is critical(2) easy to implement, but its sensitivity and accuracy are still insufficient(3) easy to operate, has high selectivity, and is not easily affected by other ions at specific wavelengths; insufficient accuracy and sensitivity, requires the capture agent or the adduct product with the hydroxyl to have characteristic fluorescence H2O→H+OH·
OH·+H++e−→H2O[23][24][25][26] superoxide anion
(O2−)(1) EPR technology
(2) fluorescent probe method(1) high sensitivity, low detection limit, expensive instrument(2) easy to operate, lower instrument price, but the sensitivity is low, and it is interfered by particles like H2O2, OH· 2O+H2O+e−→H2O+O2− [27][28][29] ozone
(O3)(1) spectrophotometry
(2) fluorescent probe method(1) the operation is simple and fast, but the sensitivity is low, and it will be interfered by other oxidants(2) good selectivity, but it needs to be in a specific pH range; when pH ≥ 10, the probe will be destroyed in H2O2 O3+2H++2e−→O2+H2O [30][31][32] nitric oxide
(NO)(1) EPR technology(2) spectrophotometry
(3) fluorescent probe method(1) high sensitivity, low detection limit, wide application, but need to avoid oxidation of Fe2+ particles in the reagent(2) easy to operate, instrument is relatively cheap, and the aqueous solution to be tested needs to be acidified in advance before the test(3) has good selectivity, but the pH of the aqueous solution to be tested needs to be higher than 5.5 4NO+2O2+2H2O→
4NO2−+4H+[33][34][35][36] nitrite (NO2−) (1) spectrophotometry
(2) HPLC method(1) the operation is simple and fast, but the sensitivity is low, and it will be interfered by other oxidants(2) easy to implement, but its sensitivity and accuracy are still insufficient 2HNO2→NO+NO2+H2ONO2−+H+→HNO2 [37]
[38]nitrate
(NO3−)(1) spectrophotometry
(2) HPLC method(1) the operation is simple and fast, but the sensitivity is low, and it will be interfered by other oxidants(2) easy to implement, but its sensitivity and accuracy are still insufficient NO2−+ OH·→NO3− [39][40][41] peroxynitrite
(ONOO−)(1) colorimetric or fluorometric analysis(2) chemical reaction(3) fluorescent probe method (1) multiple interference factors, extremely sensitive to light-induced oxidation, and specificity problems(2) the existence of ONOO− can only be indirectly proved by the concentration decay of NO2− and H2O2, and the accuracy is insufficient (3) low selectivity, interfered by particles like H2O2 and HClO, in the absence ofHClO, the selectivity is enhanced NO2−+H2O2→ONOO−+H2OONOO−→NO3− [42][43][44] peroxynitric
acid (O2NOOH)(1) HPLC method (1) easy to detect, but the sensitivity is low, the detection environment requires low temperature and low pH value NO3−+H2O2→
O2NOO−+H2O[45] singlet oxygen
(1O2)(1) EPR technology
(2) fluorescent probe method(1) good selectivity, high sensitivity, not affected by other free radicals, the detection reagent has a strong pungent odor and is easily oxidized in the air(2) the probe acts as a photosensitizer to generate singlet oxygen, and the probe is destroyed in hydrogen peroxide O2+e−→1O2+e−21O2+2H+→H2O2+O21O2+H2O2→OH·+OH−+O2 [46][47][48][49] 
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表 2 基于液相等离子体技术合成纳米材料
Table 2. Synthesis of nanomaterials based on liquid phase plasma technology
nanomaterials examples liquid plasma type references precious metal element Au contact glow discharge [56] microplasma discharge [63, 94] two-electrode pulsed plasma [76-81] Ag arc discharge [55, 84] Pd gas-liquid interface plasma [82] Pt flat electrode plasma [62] microplasma discharge [83] precious metal alloy Au - Ag alloy two-electrode plasma [54] microplasma discharge [60] Au - Pt alloy two-electrode pulsed plasma [85] metal element Ni solution glow discharge [57] Cu submerged arc discharge [86] Fe high voltage cathodic polarized discharge [58] Mn solution discharge [72] Sn dielectric barrier discharge [75] metal alloy Fe – Ni alloy solution discharge [59] Ni – Cu alloy dielectric barrier discharge [74] oxide CuO/ZnO two-electrode pulsed plasma [87] ZnO contact glow discharge [88] Cu2O microplasma discharge [95] TiO2 gliding arc discharge [52] defective TiO2 submerged pulse discharge [89] carbon material carbon nanotubes alternating current arc discharge [78] graphene submerged arc discharge [90-91] submerged arc discharge [79] silicon material Si dielectric barrier discharge [73] composite material carbon – metal nano contact glow discharge [92] carbon – non-metal nano solution discharge [93] plasma induced cathode discharge [96]
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