CN111644634A - Method for preparing two-dimensional metal through hot pressing based on solution processing - Google Patents
Method for preparing two-dimensional metal through hot pressing based on solution processing Download PDFInfo
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 29
- 239000002184 metal Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000007731 hot pressing Methods 0.000 title claims abstract description 6
- 238000010129 solution processing Methods 0.000 title claims abstract 3
- 235000012431 wafers Nutrition 0.000 claims abstract description 86
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 66
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 66
- 239000010703 silicon Substances 0.000 claims abstract description 66
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 58
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 8
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 8
- NWAHZABTSDUXMJ-UHFFFAOYSA-N platinum(2+);dinitrate Chemical compound [Pt+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O NWAHZABTSDUXMJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 239000006185 dispersion Substances 0.000 claims abstract description 5
- 239000002243 precursor Substances 0.000 claims abstract description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000011521 glass Substances 0.000 claims description 20
- 238000004321 preservation Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 abstract description 23
- 239000000463 material Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000002135 nanosheet Substances 0.000 description 29
- 229910000831 Steel Inorganic materials 0.000 description 18
- 239000010959 steel Substances 0.000 description 18
- 239000010931 gold Substances 0.000 description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 10
- 229920000742 Cotton Polymers 0.000 description 7
- 239000002086 nanomaterial Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 229910052709 silver Inorganic materials 0.000 description 5
- 239000004332 silver Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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Abstract
本发明涉及一种基于溶液加工的热压制备二维金属的方法，属于材料科学与工程技术和化学领域。本发明方法所用到的原料为金属前驱体溶液或金属粉体颗粒，包括硝酸银溶液，氯金酸溶液，硝酸铂溶液，金属铌粉体颗粒等，再加入适量乙醇来配成分散液，在一定温度和一定压力下，将夹在两个硅片之间的分散液重塑为二维金属。本发明具有制备工艺简单、效率高、性能好、成本低等优点。
The invention relates to a method for preparing two-dimensional metal by hot pressing based on solution processing, and belongs to the fields of material science and engineering technology and chemistry. The raw materials used in the method of the invention are metal precursor solutions or metal powder particles, including silver nitrate solution, chloroauric acid solution, platinum nitrate solution, metal niobium powder particles, etc., and then an appropriate amount of ethanol is added to prepare a dispersion liquid. Under a certain temperature and pressure, the dispersion liquid sandwiched between two silicon wafers is reshaped into a two-dimensional metal. The invention has the advantages of simple preparation process, high efficiency, good performance, low cost and the like.
Description
(2)技术领域(2) Technical field
本发明涉及热压制备二维材料的方法，属于材料科学与工程技术和化学领域。The invention relates to a method for preparing two-dimensional materials by hot pressing, and belongs to the fields of material science and engineering technology and chemistry.
(3)背景技术(3) Background technology
与块状金属相比，二维纳米结构的超薄金属材料一般能表现出让人难以预料的物理化学特性，更会在超导、磁性存储、光学设备、催化等工业领域大放光彩。金属银、金、铂等一直是许多研究工作中重要研究对象之一，它们的纳米结构具有非常良好的塑性、导电性、化学稳定性和抗菌抗氧化性等优点，使其在集成电路、印刷电子、表面拉曼增强、绿色家具、能源、医疗、催化、电镀等工业领域有着非常广阔的应用前景：其中，二维金属纳米结构的制备和共性能探究是今年来研究的热议课题，同时，伴随柔性电子技术的火热以及其在人们生活服务中越多元化的应用，高质量、超薄、大面积尺寸、晶体结构优良的金属纳米片成为金属的纳米结构制备研究工作中更高的期求。Compared with bulk metals, ultra-thin metal materials with two-dimensional nanostructures generally exhibit unpredictable physical and chemical properties, and will shine in industrial fields such as superconductivity, magnetic storage, optical devices, and catalysis. Metal silver, gold, platinum, etc. have always been one of the important research objects in many research works. Their nanostructures have the advantages of very good plasticity, electrical conductivity, chemical stability, antibacterial and antioxidative properties, which make them widely used in integrated circuits, printing, etc. Electronics, surface Raman enhancement, green furniture, energy, medical, catalysis, electroplating and other industrial fields have very broad application prospects. Among them, the preparation and co-property exploration of two-dimensional metal nanostructures is a hot topic of research this year. With the popularity of flexible electronic technology and its more diversified applications in people's life services, high-quality, ultra-thin, large-area size, and excellent crystal structure metal nanosheets have become a higher expectation in the research work on the preparation of metal nanostructures. .
目前，二维金属纳米结构的制备合成工作主要围绕着化学法展开，已发展成熟的合成路线有电化学沉积法、模板生长法、快速还原法以及湿化学等方法，以此类方法制备获得的金属纳米片多在数十纳米厚度间，很难在厚度上实现进一步的突破，且化学合成路线操作复杂冗长，实验过程中的各类辅助试剂也限制了获得高纯净的金属纳米片的绝对性，因此，设计新的合成路线已是亟需面对的挑战。At present, the preparation and synthesis of two-dimensional metal nanostructures mainly revolves around chemical methods. The mature synthetic routes include electrochemical deposition, template growth, rapid reduction and wet chemistry. Metal nanosheets are mostly tens of nanometers in thickness, and it is difficult to achieve further breakthroughs in thickness. The chemical synthesis route is complicated and lengthy, and various auxiliary reagents in the experimental process also limit the absoluteness of obtaining high-purity metal nanosheets. Therefore, designing new synthetic routes is an urgent challenge.
本发明结合金属材料特有的物理性能，根据二维金属纳米结构，制备方案为：准备原材料的乙醇分散液，并将其置于两个表面高度抛光的衬底之间，形成三明治结构，接着向该三明治结构施加一定的压力和温度，并保温保压一定时间，待冷却到室温后，即可获得附着在沉底表面的二维材料。本方案通过机械热压延展法，利用金属等材料在一定温度下会产生形变的特点，对具有金属延展特性的材料进高温高压处理，来制备二维超薄纳米结构。The present invention combines the unique physical properties of metal materials, and according to the two-dimensional metal nanostructure, the preparation scheme is as follows: prepare an ethanol dispersion of the raw material, and place it between two substrates with highly polished surfaces to form a sandwich structure, and then add it to the A certain pressure and temperature are applied to the sandwich structure, and the heat preservation and pressure are maintained for a certain period of time. After cooling to room temperature, a two-dimensional material attached to the surface of the sinking bottom can be obtained. In this scheme, two-dimensional ultra-thin nanostructures are prepared by using the mechanical hot-rolling stretching method, using the characteristics of metals and other materials that will deform at a certain temperature, and subjecting materials with metal ductility characteristics to high-temperature and high-pressure treatment.
通过本发明可以制备出具有超薄结构的金属纳米片，如银纳米片的厚度可达到1.7nm，且纳米片完整性好，表面光滑，原子相清晰规整，结构取向一致，且为单晶结构。这种具有超薄结构的纳米片还能表现出一定的特殊光学现象，如第一次在金属银中检测到两个尖锐的PL峰。The invention can prepare metal nanosheets with ultra-thin structure, for example, the thickness of silver nanosheets can reach 1.7 nm, and the nanosheets have good integrity, smooth surface, clear and regular atomic phase, consistent structure orientation, and single crystal structure. . The nanosheets with ultrathin structure can also exhibit certain special optical phenomena, such as the detection of two sharp PL peaks in metallic silver for the first time.
综上所述，本发明所提出的热压法制备二维金属的方法，具有工艺流程短、生产效率高、成分控制灵活等优势。To sum up, the method for preparing two-dimensional metal by hot pressing proposed in the present invention has the advantages of short process flow, high production efficiency, flexible composition control and the like.
(4)发明内容(4) Contents of the invention
1、本发明的目标1. Object of the present invention
通过本发明可以制备出具有超薄结构的金属纳米片，如银纳米片的厚度可达到1.7nm，且纳米片完整性好，表面光滑，原子相清晰规整，结构取向一致，且为单晶结构。这种具有超薄结构的纳米片还能表现出一定的特殊光学现象，如第一次在金属银中检测到两个尖锐的PL峰。The invention can prepare metal nanosheets with ultra-thin structure, for example, the thickness of silver nanosheets can reach 1.7 nm, and the nanosheets have good integrity, smooth surface, clear and regular atomic phase, consistent structure orientation, and single crystal structure. . The nanosheets with ultrathin structure can also exhibit certain special optical phenomena, such as the detection of two sharp PL peaks in metallic silver for the first time.
2、本技术的发明要点2. The main points of the invention of this technology
本发明要点如下：The main points of the present invention are as follows:
(1)将金属前驱体溶液或金属粉体颗粒(硝酸银溶液、氯金酸溶液、硝酸铂溶液、金属 Nb粉体颗粒)与乙醇按照一定比例配置成0.5mg/ml～2mg/ml的分散液。(1) Disperse the metal precursor solution or metal powder particles (silver nitrate solution, chloroauric acid solution, platinum nitrate solution, metal Nb powder particles) and ethanol according to a certain proportion to a dispersion of 0.5mg/ml ~ 2mg/ml liquid.
(2)取30～40微升配好的溶液滴在硅片上，静置5分钟。(2) Drop 30-40 microliters of the prepared solution on the silicon wafer and let it stand for 5 minutes.
(3)将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度为200℃～400℃，压力为0.7Gpa～0.8Gpa，保温保压20～50min。(3) Place two silicon wafers and glass wafers into a "sandwich" structure and place them on a hot press, the temperature is 200℃～400℃, the pressure is 0.7Gpa～0.8Gpa, and the heat preservation and pressure are maintained for 20～50min.
(4)待温度降至室温后，打开热压机，得到二维化的产物。(4) After the temperature drops to room temperature, the hot press is turned on to obtain a two-dimensional product.
本发明提出的热压法制备二维金属的方法，其优点是：工艺流程短、生产效率高、成分控制灵活，为低成本、高质量和高产量的二维金属、氧化物和聚合物的生产开辟了新的途径，促进了其基础科学研究和工业应用。The method for preparing two-dimensional metal by hot pressing method proposed in the present invention has the advantages of short process flow, high production efficiency, flexible composition control, and is suitable for low-cost, high-quality and high-yield two-dimensional metals, oxides and polymers. Production opens up new avenues for its basic scientific research and industrial applications.
(5)本发明的附图(5) Drawings of the present invention
图1为本发明方法制备的二维单晶Ag的高倍TEM图。FIG. 1 is a high magnification TEM image of two-dimensional single crystal Ag prepared by the method of the present invention.
图2为本发明方法制备的二维单晶Ag的低倍TEM图。FIG. 2 is a low magnification TEM image of the two-dimensional single crystal Ag prepared by the method of the present invention.
(6)本发明实施例(6) Embodiments of the present invention
以下介绍本发明方法的实施例：Embodiments of the inventive method are introduced below:
实施例1Example 1
二维Ag纳米片的制备Preparation of two-dimensional Ag nanosheets
将硝酸银溶液与乙醇按照一定比例配置成0.5mg/ml的溶液，取两块厚度为0.7mm的硅片放在10cm*10cm的钢片上，再用移液枪取30-40微升配置好的溶液滴在硅片上，静置5分钟。将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度设置为200℃，压力为0.73Gpa，保压20min。待温度降至室温后，打开热压机，得到二维化的产物Ag。The silver nitrate solution and ethanol are prepared into a solution of 0.5mg/ml according to a certain ratio, and two silicon wafers with a thickness of 0.7mm are placed on a steel sheet of 10cm*10cm, and then 30-40 microliters are prepared with a pipette gun. The solution was dropped on the silicon wafer and left to stand for 5 minutes. Two silicon wafers and glass wafers were placed in a "sandwich" structure, placed on a hot press, the temperature was set to 200 °C, the pressure was 0.73 Gpa, and the pressure was maintained for 20 min. After the temperature dropped to room temperature, the hot press was turned on to obtain a two-dimensional product Ag.
实施例2Example 2
二维Ag纳米片的制备Preparation of two-dimensional Ag nanosheets
先取硝酸银溶液0.5g，将其加热分解后得到的产物与乙醇按照一定比例配置成0.5mg/ml 的溶液，取两块厚度为0.7mm的硅片放在10cm*10cm的钢片上，再用移液枪取30-40微升配置好的溶液滴在硅片上，静置5分钟。将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度设置为200℃，压力为0.73Gpa，保压20min。待温度降至室温后，打开热压机，得到二维化的产物Ag。First take 0.5g of silver nitrate solution, heat and decompose the product obtained after heating and decompose it and prepare a solution of 0.5mg/ml with ethanol according to a certain ratio, take two silicon wafers with a thickness of 0.7mm and place them on a 10cm*10cm steel sheet, and then use Pipette 30-40 microliters of the prepared solution onto the silicon wafer and let it stand for 5 minutes. Two silicon wafers and glass wafers were placed in a "sandwich" structure, placed on a hot press, the temperature was set to 200 °C, the pressure was 0.73 Gpa, and the pressure was maintained for 20 min. After the temperature dropped to room temperature, the hot press was turned on to obtain a two-dimensional product Ag.
实施例3Example 3
二维Ag纳米片的制备Preparation of two-dimensional Ag nanosheets
将硝酸银溶液与乙醇按照一定比例配置成1mg/ml的溶液，取两块厚度为0.7mm的硅片放在10cm*10cm的钢片上，再用移液枪取30-40微升配置好的溶液滴在硅片上，静置5分钟。将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度设置为200℃，压力为0.73Gpa，保压20min。待温度降至室温后，打开热压机，得到二维化的产物Ag。The silver nitrate solution and ethanol are prepared into a solution of 1 mg/ml according to a certain proportion, and two silicon wafers with a thickness of 0.7 mm are placed on a steel sheet of 10 cm*10 cm, and then 30-40 microliters of the prepared solution are taken with a pipette gun. The solution was dropped on the silicon wafer and left to stand for 5 minutes. Two silicon wafers and glass wafers were placed in a "sandwich" structure, placed on a hot press, the temperature was set to 200 °C, the pressure was 0.73 Gpa, and the pressure was maintained for 20 min. After the temperature dropped to room temperature, the hot press was turned on to obtain a two-dimensional product Ag.
实施例4Example 4
二维Ag纳米片的制备Preparation of two-dimensional Ag nanosheets
将硝酸银溶液与乙醇按照一定比例配置成1.5mg/ml的溶液，取两块厚度为0.7mm的硅片放在10cm*10cm的钢片上，再用移液枪取30-40微升配置好的溶液滴在硅片上，静置5分钟。将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度设置为250℃，压力为0.73Gpa，保压20min。待温度降至室温后，打开热压机，得到二维化的产物Ag。The silver nitrate solution and ethanol are prepared into a solution of 1.5mg/ml according to a certain proportion, and two silicon wafers with a thickness of 0.7mm are placed on a 10cm*10cm steel plate, and then 30-40 microliters are prepared with a pipette gun. The solution was dropped on the silicon wafer and left to stand for 5 minutes. Two silicon wafers and glass wafers were placed in a "sandwich" structure, placed on a hot press, the temperature was set to 250 °C, the pressure was 0.73 Gpa, and the pressure was maintained for 20 min. After the temperature dropped to room temperature, the hot press was turned on to obtain a two-dimensional product Ag.
实施例5Example 5
二维金属Au纳米片的制备Preparation of two-dimensional metallic Au nanosheets
将氯金酸溶液与乙醇按照一定比例配置成0.5mg/ml溶液，取两块厚度为0.7mm的硅片放在10cm*10cm的钢片上，再用移液枪取30-40微升配置好的溶液滴在硅片上，静置5分钟。将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度设置为280℃，压力为0.7Gpa，保压30min。待温度降至室温后，打开热压机，得到二维化的产物Au。Prepare chloroauric acid solution and ethanol according to a certain ratio to a 0.5mg/ml solution, take two silicon wafers with a thickness of 0.7mm and place them on a 10cm*10cm steel plate, and then use a pipette to take 30-40 microliters to prepare The solution was dropped on the silicon wafer and left to stand for 5 minutes. Two silicon wafers and glass wafers were placed in a "sandwich" structure, placed on a hot press, the temperature was set to 280°C, the pressure was 0.7Gpa, and the pressure was maintained for 30min. After the temperature dropped to room temperature, the hot press was turned on to obtain the two-dimensional product Au.
实施例6Example 6
二维金属Au纳米片的制备Preparation of two-dimensional metallic Au nanosheets
将氯金酸溶液与乙醇按照一定比例配置成1mg/ml的溶液，取两块厚度为0.7mm的硅片放在10cm*10cm的钢片上，再用移液枪取30-40微升配置好的溶液滴在硅片上，静置5分钟。将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度设置为280℃，压力为0.7Gpa，保压40min。待温度降至室温后，打开热压机，得到二维化的产物Au。Prepare chloroauric acid solution and ethanol into a 1mg/ml solution according to a certain ratio, take two silicon wafers with a thickness of 0.7mm and place them on a 10cm*10cm steel plate, and then use a pipette gun to take 30-40 microliters to prepare The solution was dropped on the silicon wafer and left to stand for 5 minutes. Two silicon wafers and glass wafers were placed in a "sandwich" structure, placed on a hot press, the temperature was set to 280°C, the pressure was 0.7Gpa, and the pressure was maintained for 40min. After the temperature dropped to room temperature, the hot press was turned on to obtain the two-dimensional product Au.
实施例7Example 7
二维金属Au纳米片的制备Preparation of two-dimensional metallic Au nanosheets
将氯金酸溶液与乙醇按照一定比例配置成1.5mg/ml的溶液，取两块厚度为0.7mm的硅片放在10cm*10cm的钢片上，再用移液枪取30-40微升配置好的溶液滴在硅片上，静置5分钟。将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度设置为300℃，压力为0.7Gpa，保压40min。待温度降至室温后，打开热压机，得到二维化的产物Au。Prepare chloroauric acid solution and ethanol into a 1.5mg/ml solution according to a certain ratio, take two silicon wafers with a thickness of 0.7mm and place them on a 10cm*10cm steel plate, and then use a pipette to take 30-40 microliters of configuration. The good solution was dropped on the silicon wafer and left to stand for 5 minutes. Two silicon wafers and glass wafers were placed in a "sandwich" structure, placed on a hot press, the temperature was set to 300°C, the pressure was 0.7Gpa, and the pressure was maintained for 40min. After the temperature dropped to room temperature, the hot press was turned on to obtain the two-dimensional product Au.
实施例8Example 8
二维金属Pt纳米片的制备Preparation of two-dimensional metallic Pt nanosheets
将硝酸铂溶液与乙醇按照一定的比例配置成0.5mg/ml溶液，取两块厚度为0.7mm的硅片放在10cm*10cm的钢片上，并用棉签蘸取乙醇擦拭硅片，再用移液枪取30-40微升配置好的溶液滴在硅片上，静置5分钟。将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度设置为200℃，压力为0.73Gpa，保压40min。待温度降至室温后，打开热压机，得到二维化的产物Pt。Prepare a 0.5mg/ml solution of platinum nitrate solution and ethanol according to a certain ratio, take two silicon wafers with a thickness of 0.7mm and place them on a 10cm*10cm steel plate, and wipe the silicon wafer with a cotton swab dipped in ethanol, and then pipette The gun takes 30-40 microliters of the prepared solution and drops it on the silicon wafer, and let it stand for 5 minutes. Two silicon wafers and glass wafers were placed in a "sandwich" structure, placed on a hot press, the temperature was set to 200 °C, the pressure was 0.73 Gpa, and the pressure was maintained for 40 min. After the temperature dropped to room temperature, the hot press was turned on to obtain the two-dimensional product Pt.
实施例9Example 9
二维金属Pt纳米片的制备Preparation of two-dimensional metallic Pt nanosheets
将硝酸铂溶液与乙醇按照一定的比例配置成1mg/ml的溶液，取两块厚度为0.7mm的硅片放在10cm*10cm的钢片上，再用移液枪取30-40微升配置好的溶液滴在硅片上，静置5分钟。将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度设置为200℃，压力为0.73Gpa，保压40min。待温度降至室温后，打开热压机，得到二维化的产物Pt。The platinum nitrate solution and ethanol are prepared into a solution of 1 mg/ml according to a certain ratio, and two silicon wafers with a thickness of 0.7 mm are placed on a steel sheet of 10 cm*10 cm, and then 30-40 microliters are prepared with a pipette gun. The solution was dropped on the silicon wafer and left to stand for 5 minutes. Two silicon wafers and glass wafers were placed in a "sandwich" structure, placed on a hot press, the temperature was set to 200 °C, the pressure was 0.73 Gpa, and the pressure was maintained for 40 min. After the temperature dropped to room temperature, the hot press was turned on to obtain the two-dimensional product Pt.
实施例10Example 10
二维金属Pt纳米片的制备Preparation of two-dimensional metallic Pt nanosheets
将硝酸铂溶液与乙醇按照一定的比例配置成1.5mg/ml的溶液，取两块厚度为0.7mm的硅片放在10cm*10cm的钢片上，再用移液枪取30-40微升配置好的溶液滴在硅片上，静置5分钟。将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度设置为200℃，压力为0.73 Gpa，保压40min。待温度降至室温后，打开热压机，得到二维化的产物Pt。The platinum nitrate solution and ethanol are prepared into a solution of 1.5mg/ml according to a certain proportion, and two silicon wafers with a thickness of 0.7mm are placed on a 10cm*10cm steel plate, and then 30-40 microliters are prepared with a pipette gun. The good solution was dropped on the silicon wafer and left to stand for 5 minutes. Two silicon wafers and glass wafers were placed in a "sandwich" structure, placed on a hot press, the temperature was set to 200 °C, the pressure was 0.73 Gpa, and the pressure was maintained for 40 min. After the temperature dropped to room temperature, the hot press was turned on to obtain the two-dimensional product Pt.
实施例11Example 11
二维金属Nb纳米片的制备Preparation of two-dimensional metallic Nb nanosheets
取少量Nb粉体颗粒,将其与乙醇按照一定的比例配置成0.5mg/ml的溶液，取两块厚度为 0.7mm的硅片放在10cm*10cm的钢片上，再用移液枪取30-40微升配置好的溶液滴在硅片上，静置5分钟。将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度设置为300℃，压力为0.8Gpa，保温保压30min。待温度降至室温后，打开热压机，得到二维化的产物Nb。Take a small amount of Nb powder particles, mix it with ethanol according to a certain ratio to form a 0.5mg/ml solution, take two silicon wafers with a thickness of 0.7mm and place them on a 10cm*10cm steel sheet, and then use a pipette gun to take 30 - 40 microliters of the prepared solution was dropped on the silicon wafer and allowed to stand for 5 minutes. Two silicon wafers and glass wafers were placed in a "sandwich" structure, placed on a hot press, the temperature was set to 300°C, the pressure was 0.8Gpa, and the temperature was maintained at 30min. After the temperature dropped to room temperature, the hot press was turned on to obtain the two-dimensional product Nb.
实施例12Example 12
二维金属Nb纳米片的制备Preparation of two-dimensional metallic Nb nanosheets
取少量Nb粉体颗粒,将其与乙醇按照一定的比例配置成1mg/ml的溶液，取两块厚度为 0.7mm的硅片放在10cm*10cm的钢片上，并用棉签蘸取乙醇擦拭硅片，再用移液枪取30-40 微升配置好的溶液滴在硅片上，静置5分钟。将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度设置为300℃，压力为0.8Gpa，保温保压40min。待温度降至室温后，打开热压机，得到二维化的产物Nb。Take a small amount of Nb powder particles, mix it with ethanol according to a certain ratio to make a 1mg/ml solution, take two silicon wafers with a thickness of 0.7mm and place them on a 10cm*10cm steel sheet, and use a cotton swab dipped in ethanol to wipe the silicon wafer , and then use a pipette to take 30-40 microliters of the prepared solution and drop it on the silicon wafer, and let it stand for 5 minutes. Two silicon wafers and glass wafers were placed in a "sandwich" structure, placed on a hot press, the temperature was set to 300°C, the pressure was 0.8Gpa, and the temperature was maintained at 40min. After the temperature dropped to room temperature, the hot press was turned on to obtain the two-dimensional product Nb.
实施例13Example 13
二维金属Nb纳米片的制备Preparation of two-dimensional metallic Nb nanosheets
取少量Nb粉体颗粒,将其与乙醇按照一定的比例配置成2mg/ml的溶液，取两块厚度为 0.7mm的硅片放在10cm*10cm的钢片上，再用移液枪取30-40微升配置好的溶液滴在硅片上，静置5分钟。将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度设置为300℃，压力为0.8Gpa，保温保压30min。待温度降至室温后，打开热压机，得到二维化的产物Nb。Take a small amount of Nb powder particles, mix it with ethanol according to a certain ratio to make a 2mg/ml solution, take two silicon wafers with a thickness of 0.7mm and place them on a 10cm*10cm steel sheet, and then use a pipette gun to take 30- 40 microliters of the prepared solution was dropped on the silicon wafer and allowed to stand for 5 minutes. Two silicon wafers and glass wafers were placed in a "sandwich" structure, placed on a hot press, the temperature was set to 300°C, the pressure was 0.8Gpa, and the temperature was maintained at 30min. After the temperature dropped to room temperature, the hot press was turned on to obtain the two-dimensional product Nb.
实施例14Example 14
二维Ag纳米片的制备Preparation of two-dimensional Ag nanosheets
将硝酸银溶液与乙醇按照一定的比例配置成1mg/ml的溶液，取两块厚度为0.7mm的硅片放在10cm*10cm的钢片上，并用棉签蘸取乙醇擦拭硅片，再用移液枪取30-40微升配置好的溶液滴在硅片上，静置5分钟。将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度设置为250℃，压力为0.73Gpa，保压30min。待温度降至室温后，打开热压机，得到二维化的产物Ag。The silver nitrate solution and ethanol are prepared into a 1mg/ml solution according to a certain ratio, and two silicon wafers with a thickness of 0.7mm are placed on a 10cm*10cm steel plate, and the silicon wafer is wiped with a cotton swab dipped in ethanol, and then pipetted. The gun takes 30-40 microliters of the prepared solution and drops it on the silicon wafer, and let it stand for 5 minutes. Two silicon wafers and glass wafers were placed in a "sandwich" structure, placed on a hot press, the temperature was set to 250 °C, the pressure was 0.73 Gpa, and the pressure was maintained for 30 min. After the temperature dropped to room temperature, the hot press was turned on to obtain a two-dimensional product Ag.
实施例15Example 15
二维金属Au纳米片的制备Preparation of two-dimensional metallic Au nanosheets
将氯金酸溶液与乙醇按照一定比例配置成1mg/ml的溶液，取两块厚度为0.7mm的硅片放在10cm*10cm的钢片上，并用棉签蘸取乙醇擦拭硅片，再用移液枪取30-40微升配置好的溶液滴在硅片上，静置5分钟。将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度设置为240℃，压力为0.7Gpa，保压40min。待温度降至室温后，打开热压机，得到二维化的产物Au。The chloroauric acid solution and ethanol are prepared into a 1mg/ml solution according to a certain proportion, and two silicon wafers with a thickness of 0.7mm are placed on a 10cm*10cm steel plate, and the silicon wafer is wiped with a cotton swab dipped in ethanol, and then pipetted. The gun takes 30-40 microliters of the prepared solution and drops it on the silicon wafer, and let it stand for 5 minutes. Two silicon wafers and glass wafers were placed in a "sandwich" structure, placed on a hot press, the temperature was set to 240°C, the pressure was 0.7Gpa, and the pressure was maintained for 40min. After the temperature dropped to room temperature, the hot press was turned on to obtain the two-dimensional product Au.
实施例16Example 16
二维金属Au纳米片的制备Preparation of two-dimensional metallic Au nanosheets
将氯金酸溶液与乙醇按照一定比例配置成1.5mg/ml的溶液，取两块厚度为0.7mm的硅片放在10cm*10cm的钢片上，并用棉签蘸取乙醇擦拭硅片，再用移液枪取30-40微升配置好的溶液滴在硅片上，静置5分钟。将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度设置为300℃，压力为0.7Gpa，保压40min。待温度降至室温后，打开热压机，得到二维化的产物Au。The chloroauric acid solution and ethanol are prepared into a solution of 1.5mg/ml according to a certain ratio, and two silicon wafers with a thickness of 0.7mm are placed on a 10cm*10cm steel sheet, and a cotton swab is dipped in ethanol to wipe the silicon wafer. The liquid gun takes 30-40 microliters of the prepared solution and drops it on the silicon wafer, and let it stand for 5 minutes. Two silicon wafers and glass wafers were placed in a "sandwich" structure, placed on a hot press, the temperature was set to 300°C, the pressure was 0.7Gpa, and the pressure was maintained for 40min. After the temperature dropped to room temperature, the hot press was turned on to obtain the two-dimensional product Au.
实施例17Example 17
二维金属Nb纳米片的制备Preparation of two-dimensional metallic Nb nanosheets
取少量Nb粉体颗粒,将其与乙醇按照一定的比例配置成2mg/ml的溶液，取两块厚度为 0.7mm的硅片放在10cm*10cm的钢片上，并用棉签蘸取乙醇擦拭硅片，再用移液枪取30-40 微升配置好的溶液滴在硅片上，静置5分钟。将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度设置为250℃，压力为0.8Gpa，保温保压40min。待温度降至室温后，打开热压机，得到二维化的产物Nb。Take a small amount of Nb powder particles, mix it with ethanol according to a certain ratio to make a 2mg/ml solution, take two silicon wafers with a thickness of 0.7mm and place them on a 10cm*10cm steel sheet, and use a cotton swab dipped in ethanol to wipe the silicon wafer , and then use a pipette to take 30-40 microliters of the prepared solution and drop it on the silicon wafer, and let it stand for 5 minutes. Two silicon wafers and glass wafers were placed in a "sandwich" structure, placed on a hot press, the temperature was set to 250°C, the pressure was 0.8Gpa, and the temperature was maintained at 40min. After the temperature dropped to room temperature, the hot press was turned on to obtain the two-dimensional product Nb.
实施例18Example 18
二维金属Pt纳米片的制备Preparation of two-dimensional metallic Pt nanosheets
将硝酸铂溶液与乙醇按照一定的比例配置成1.5mg/ml的溶液，取两块厚度为0.7mm的硅片放在10cm*10cm的钢片上，并用棉签蘸取乙醇擦拭硅片，再用移液枪取30-40微升配置好的溶液滴在硅片上，静置5分钟。将两片硅片和玻璃片放置成“三明治”结构，放在热压机上，温度设置为250℃，压力为0.73Gpa，保压50min。待温度降至室温后，打开热压机，得到二维化的产物Pt。The platinum nitrate solution and ethanol are prepared into a solution of 1.5mg/ml according to a certain ratio, and two silicon wafers with a thickness of 0.7mm are placed on a steel sheet of 10cm*10cm, and a cotton swab is dipped in ethanol to wipe the silicon wafer. The liquid gun takes 30-40 microliters of the prepared solution and drops it on the silicon wafer, and let it stand for 5 minutes. Two silicon wafers and glass wafers were placed in a "sandwich" structure, placed on a hot press, the temperature was set to 250 °C, the pressure was 0.73 Gpa, and the pressure was maintained for 50 min. After the temperature dropped to room temperature, the hot press was turned on to obtain the two-dimensional product Pt.
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