CN107935020A - A kind of Cu2The controllable method for preparing of O nanofibers - Google Patents
A kind of Cu2The controllable method for preparing of O nanofibers Download PDFInfo
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- 239000002121 nanofiber Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000010949 copper Substances 0.000 claims abstract description 44
- 108010010803 Gelatin Proteins 0.000 claims abstract description 32
- 229920000159 gelatin Polymers 0.000 claims abstract description 32
- 239000008273 gelatin Substances 0.000 claims abstract description 32
- 235000019322 gelatine Nutrition 0.000 claims abstract description 32
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 32
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 229940095064 tartrate Drugs 0.000 claims abstract description 11
- 150000001879 copper Chemical class 0.000 claims abstract description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000002906 tartaric acid Nutrition 0.000 claims abstract description 7
- 239000011975 tartaric acid Substances 0.000 claims abstract description 7
- 239000011858 nanopowder Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 230000035484 reaction time Effects 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 2
- 229910001431 copper ion Inorganic materials 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims 2
- 230000000996 additive effect Effects 0.000 claims 2
- VZOPRCCTKLAGPN-ZFJVMAEJSA-L potassium;sodium;(2r,3r)-2,3-dihydroxybutanedioate;tetrahydrate Chemical group O.O.O.O.[Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O VZOPRCCTKLAGPN-ZFJVMAEJSA-L 0.000 claims 1
- 229940074446 sodium potassium tartrate tetrahydrate Drugs 0.000 claims 1
- -1 tartrate anion Chemical class 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 17
- 239000002086 nanomaterial Substances 0.000 abstract description 7
- 108090000623 proteins and genes Proteins 0.000 abstract description 5
- 102000004169 proteins and genes Human genes 0.000 abstract description 5
- 229910052802 copper Inorganic materials 0.000 abstract description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 2
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000003301 hydrolyzing effect Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 26
- 239000000835 fiber Substances 0.000 description 5
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical group [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 5
- 229940074439 potassium sodium tartrate Drugs 0.000 description 5
- 239000000376 reactant Substances 0.000 description 5
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 5
- 238000007792 addition Methods 0.000 description 3
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 3
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229940112669 cuprous oxide Drugs 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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Abstract
一种Cu2O纳米纤维的可控制备方法，涉及利用明胶模板可控制备Cu2O纳米纤维技术领域。可溶性铜盐、酒石酸或酒石酸盐和明胶通过水热反应获得Cu2O纳米粉体，通过调控作为模板的明胶的添加量以及反应体系的pH值，以控制产物的形态，并获得高质量的Cu2O纳米纤维。本发明以铜盐为铜原料，酒石酸或酒石酸盐为还原剂，以A型明胶水解得到的线性蛋白质分子为模板，通过水热法来制备高质量Cu2O纳米纤维。和已经报道的一维Cu2O纳米材料合成方法相比较，该法具有原理简单、环境友好和产量高等优点。本发明以明胶为模板，通过低温水热法成功获得了高质量的Cu2O纳米纤维，为一维Cu2O纳米材料的制备提供了一种新的途径。
A controllable preparation method of Cu 2 O nanofibers relates to the technical field of controllable preparation of Cu 2 O nanofibers using gelatin templates. Soluble copper salt, tartaric acid or tartrate and gelatin are hydrothermally reacted to obtain Cu 2 O nanopowder. By adjusting the amount of gelatin added as a template and the pH value of the reaction system, the morphology of the product is controlled and high-quality Cu 2O nanofibers. In the invention, copper salt is used as copper raw material, tartaric acid or tartrate is used as reducing agent, and linear protein molecules obtained by hydrolyzing type A gelatin are used as templates to prepare high-quality Cu 2 O nanofibers through a hydrothermal method. Compared with the reported synthesis methods of one-dimensional Cu 2 O nanomaterials, this method has the advantages of simple principle, environmental friendliness and high yield. The invention uses gelatin as a template to successfully obtain high-quality Cu 2 O nanofibers through a low-temperature hydrothermal method, providing a new approach for the preparation of one-dimensional Cu 2 O nanometer materials.
Description
技术领域technical field
本发明涉及利用明胶模板可控制备Cu2O纳米纤维技术领域，具体是涉及一种Cu2O纳米纤维的可控制备方法。The invention relates to the technical field of controllable preparation of Cu 2 O nanofibers by using a gelatin template, in particular to a controllable preparation method of Cu 2 O nanofibers.
背景技术Background technique
氧化亚铜(Cu2O)是一种p型的窄禁带宽度(禁带宽度为2.2eV)的半导体材料。由于其可吸收位于可见光区的能量，具有良好的吸收率，而被广泛的应用于光催化、太阳能电池、气敏元件等领域。Cuprous oxide (Cu 2 O) is a p-type semiconductor material with a narrow bandgap (2.2eV). Because it can absorb energy in the visible light region and has good absorptivity, it is widely used in photocatalysis, solar cells, gas sensors and other fields.
Cu2O纳米材料形态各异，诸如立方体、八面体、十二面体和十四面体等Cu2O多面体、Cu2O纳米线和纳米管等都有许多报道和研究。研究指出，一维Cu2O纳米材料由于其特殊的几何形状、大的长径比及纳米材料所具有的量子尺寸效应、表面效应，己引起人们的广泛关注。当前，人们在制备一维尺度的Cu2O纳米材料方面主要还是采用氧化铝模板法，该方法虽具有通用性，但制备过程复杂且获得的产物纯度不高。Cu 2 O nanomaterials have various shapes, such as Cu 2 O polyhedrons such as cubes, octahedrons, dodecahedrons and tetradecahedrons, Cu 2 O nanowires and nanotubes, etc., have been reported and studied in many ways. Studies have pointed out that one-dimensional Cu 2 O nanomaterials have attracted widespread attention due to their special geometric shape, large aspect ratio, quantum size effect and surface effect of nanomaterials. At present, the alumina template method is mainly used in the preparation of one-dimensional Cu 2 O nanomaterials. Although this method is versatile, the preparation process is complicated and the purity of the obtained product is not high.
明胶(Gelatin)是一种动物胶精制品，其水解产物也是一种长链的高分子蛋白质(Protein,Pr)，已被证明可作为模板有效控制合成Fe3O4多孔纤维。本发明利用明胶来制备高质量Cu2O纳米纤维。Gelatin (Gelatin) is a refined product of animal glue, and its hydrolyzed product is also a long-chain polymer protein (Protein, Pr), which has been proved to be effective as a template for the controlled synthesis of Fe 3 O 4 porous fibers. The present invention utilizes gelatin to prepare high-quality Cu 2 O nanofibers.
发明内容Contents of the invention
本发明要解决的技术问题为提供一种工艺简单、成本低、适合工业化应用的Cu2O纳米纤维的可控制备方法。The technical problem to be solved by the present invention is to provide a controllable preparation method of Cu 2 O nanofibers with simple process, low cost and suitable for industrial application.
为了实现上述目的，本发明所采用的技术方案为：一种Cu2O纳米纤维的可控制备方法，可溶性铜盐、酒石酸或酒石酸盐和明胶通过水热反应获得Cu2O纳米粉体，通过调控作为模板的明胶的添加量以及反应体系的pH值，以控制产物的形态，并获得高质量的Cu2O纳米纤维。In order to achieve the above object, the technical solution adopted in the present invention is: a controllable preparation method of Cu 2 O nanofibers, soluble copper salt, tartaric acid or tartrate and gelatin are hydrothermally reacted to obtain Cu 2 O nano powders, by Regulate the amount of gelatin added as a template and the pH value of the reaction system to control the shape of the product and obtain high-quality Cu 2 O nanofibers.
作为本发明的Cu2O纳米纤维的可控制备方法的优选技术方案，可控制备方法步骤如下：As a preferred technical solution of the controllable preparation method of Cu2O nanofibers of the present invention, the steps of the controllable preparation method are as follows:
1)、将可溶性铜盐和酒石酸或酒石酸盐溶液加入至一定体积的去离子水中配成溶液；1), adding soluble copper salt and tartaric acid or tartrate solution to a certain volume of deionized water to form a solution;
2)、将明胶加入到上述溶液中，稍许加热使其完全溶液，得到一种胶体溶液；2), adding gelatin to the above solution, heating it slightly to make it completely dissolved, and obtaining a colloidal solution;
3)、上述溶液用NaOH溶液调节其pH值后转入反应釜中，进行水热反应，反应结束取出反应物，经洗涤便可获得目标产物。3), the above-mentioned solution is adjusted its pH value with NaOH solution, and then transferred to a reaction kettle for hydrothermal reaction. After the reaction, the reactant is taken out, and the target product can be obtained after washing.
作为本发明的Cu2O纳米纤维的可控制备方法的进一步优选：As a further preferred method for the controllable preparation of Cu2O nanofibers of the present invention :
步骤1)中铜盐选自CuSO4.5H2O或Cu(NO3)2，酒石酸盐选自酒石酸钾钠；步骤1)中铜离子和酒石酸根之间的摩尔比为1：1～3，溶液中铜盐的摩尔浓度为0.02～0.06mol/L。In step 1), the copper salt is selected from CuSO 4 .5H 2 O or Cu(NO 3 ) 2 , and the tartrate is selected from potassium sodium tartrate; the molar ratio between copper ion and tartrate in step 1) is 1:1-3 , the molar concentration of the copper salt in the solution is 0.02-0.06 mol/L.
步骤2)中作为模板的明胶的添加量为2～40g/L，依步骤1)中配成的溶液体积计。The amount of gelatin used as a template in step 2) is 2-40 g/L, based on the volume of the solution prepared in step 1).
步骤3)中用NaOH溶液调节其pH值为5～12；步骤3)中水热反应的温度为130～150℃，反应时间为6～24h。In step 3), NaOH solution is used to adjust its pH value to 5-12; in step 3), the temperature of hydrothermal reaction is 130-150°C, and the reaction time is 6-24h.
本发明以铜盐为铜原料，酒石酸或酒石酸盐为还原剂，以A型明胶水解得到的线性蛋白质分子(Protein,Pr)为模板，通过水热法来制备高质量Cu2O纳米纤维。和已经报道的一维Cu2O纳米材料合成方法相比较，该法具有原理简单、环境友好和产量高等优点。In the present invention, copper salt is used as copper raw material, tartaric acid or tartrate is used as reducing agent, and linear protein molecule (Protein, Pr) obtained by hydrolyzing type A gelatin is used as template to prepare high-quality Cu 2 O nanofibers through a hydrothermal method. Compared with the reported synthesis methods of one-dimensional Cu 2 O nanomaterials, this method has the advantages of simple principle, environmental friendliness and high yield.
相对于现有技术，本发明的有益效果还表现如下：Compared with prior art, beneficial effect of the present invention also shows as follows:
1)、本发明以明胶为模板，通过低温水热法成功获得了高质量的Cu2O纳米纤维，为一维Cu2O纳米材料的制备提供了一种新的途径。1) The present invention uses gelatin as a template to successfully obtain high-quality Cu 2 O nanofibers through a low-temperature hydrothermal method, which provides a new way for the preparation of one-dimensional Cu 2 O nanomaterials.
2)、反应过程中通过添加适量的明胶模板，调控反应体系的pH大小，获得的产物形态新颖，具有质量高和产量大等优点，且可获得高质量的Cu2O纳米纤维。2) During the reaction process, by adding an appropriate amount of gelatin template and adjusting the pH of the reaction system, the obtained product has a novel shape, high quality and large yield, and high-quality Cu 2 O nanofibers can be obtained.
3)、本发明的Cu2O纳米纤维制备工艺流程简单、无需贵重设备、成本低，可以宏量制备高品质Cu2O纳米纤维。3) The preparation process of Cu 2 O nanofibers of the present invention is simple, does not require expensive equipment, and has low cost, and can produce high-quality Cu 2 O nanofibers in large quantities.
附图说明Description of drawings
图1为实施例1中得到产物的形态和化学组成；Fig. 1 is the form and chemical composition that obtains product in embodiment 1;
图2为实施例1中得到产物的物相和微观结构分析；Fig. 2 is the phase and microstructure analysis of product obtained in embodiment 1;
图3为实施例1中得到产物的可见光吸收光谱；Fig. 3 is the visible light absorption spectrum that obtains product in embodiment 1;
图4为不同明胶添加量下得到产物的形态；Fig. 4 obtains the form of product under different gelatin additions;
图5为不同反应时间下得到产物的形态；Fig. 5 is the form that obtains product under different reaction times;
图6为不同pH下得到产物的形态。Figure 6 shows the morphology of the products obtained at different pHs.
具体实施方式Detailed ways
以下结合实施例和附图对本发明的一种Cu2O纳米纤维的可控制备方法作出进一步的详述。本发明方法所得沉淀物的相结构、形貌、化学组成采用X射线粉末衍射(XRD，D3500)和场发射扫描电子显微镜(FE-SEM，SU8010)来表征和分析。A controllable preparation method of Cu 2 O nanofibers of the present invention will be further described in detail below with reference to the examples and accompanying drawings. The phase structure, morphology and chemical composition of the precipitate obtained by the method of the present invention are characterized and analyzed by X-ray powder diffraction (XRD, D3500) and field emission scanning electron microscope (FE-SEM, SU8010).
实施例1：高质量CuO2纳米纤维的制备与表征。Example 1: Preparation and characterization of high-quality CuO nanofibers.
1)、将1mmol的Cu(NO3)2和1mmol的酒石酸钾钠溶解于50mL去离子水中，加入明胶1g加热溶解后，用NaOH溶液将其pH调节到7～8左右。1) Dissolve 1 mmol of Cu(NO 3 ) 2 and 1 mmol of potassium sodium tartrate in 50 mL of deionized water, add 1 g of gelatin and heat to dissolve, then adjust the pH to about 7-8 with NaOH solution.
2)、将上述溶液装入反应釜中，在140℃烘箱中反应16h后冷却，取出反应物并经洗涤、烘干处理。2) Put the above solution into a reaction kettle, react in an oven at 140°C for 16 hours, then cool down, take out the reactants and wash and dry them.
图1为在该实施例下得到的产物的形态和化学组成。可以看出，产物的形状为纤维状，长度约为十几微米，纤维直径约为60nm，单根纤维主要由Cu、O和少量的C组成。图2为该产物的结构和光学性能分析结果。结合图1和图2结果可以得出，实施例1获得的为高质量的CuO2纳米纤维，CuO2纳米纤维结晶度很高。同时，具有优异的可见光吸收性能(见图3)，通过估算可以得出CuO2纳米纤维的禁带宽度约为2.0eV，略小于Cu2O块体带隙2.2eV。Fig. 1 is the morphology and the chemical composition of the product obtained under this embodiment. It can be seen that the shape of the product is fibrous, the length is about ten microns, the fiber diameter is about 60nm, and a single fiber is mainly composed of Cu, O and a small amount of C. Figure 2 shows the structural and optical performance analysis results of the product. Combining the results in Figure 1 and Figure 2, it can be concluded that the CuO 2 nanofibers obtained in Example 1 are high-quality CuO 2 nanofibers, and the CuO 2 nanofibers have a high degree of crystallinity. At the same time, it has excellent visible light absorption performance (see Figure 3), and it can be estimated that the band gap of CuO 2 nanofibers is about 2.0eV, which is slightly smaller than the band gap of Cu 2 O bulk 2.2eV.
实施例2：明胶模板使用量对产物形态的影响。Example 2: The influence of the amount of gelatin template used on the shape of the product.
1)、将1mmol的Cu(NO3)2和1mmol的酒石酸钾钠溶解于50mL去离子水中，明胶的添加量分别为0g、0.5g、1.5g和2g，用NaOH溶液将其pH调节到7～8左右；1), 1 mmol of Cu(NO 3 ) 2 and 1 mmol of potassium sodium tartrate were dissolved in 50 mL of deionized water, the amount of gelatin added was 0 g, 0.5 g, 1.5 g and 2 g respectively, and the pH was adjusted to 7 with NaOH solution ~8 or so;
2)、将上述各溶液装入反应釜中，在140℃烘箱中反应16h后冷却，取出反应物并经洗涤、烘干处理。2) Put the above-mentioned solutions into a reaction kettle, react in an oven at 140°C for 16 hours, then cool down, take out the reactants and wash and dry them.
图4为不同明胶添加量下得到的产物的形态(a、b、c、d依次表示明胶的添加量分别为0g、0.5g、1.5g和2g)。可以得出，不添加明胶时，得到的产物为八面体CuO2颗粒，随着明胶使用量的增加，纤维状的CuO2产物开始增多。然而，明胶量增加到一定时(超过1.5g，见图4d)，纤维发生团聚。Fig. 4 is the form of the product obtained under different gelatin additions (a, b, c, d represent the additions of gelatin respectively 0g, 0.5g, 1.5g and 2g). It can be concluded that when no gelatin is added, the obtained product is octahedral CuO 2 particles, and with the increase of gelatin usage, the fibrous CuO 2 product begins to increase. However, when the amount of gelatin was increased to a certain level (over 1.5 g, see Figure 4d), the fibers agglomerated.
实施例3：反应时间对产物形态的影响。Embodiment 3: the influence of reaction time on product morphology.
1)、将1mmol的Cu(NO3)2和1mmol的酒石酸钾钠溶解于50mL去离子水中，明胶的添加量为1g，用NaOH溶液将其pH调节到7～8左右；1) Dissolve 1 mmol of Cu(NO 3 ) 2 and 1 mmol of potassium sodium tartrate in 50 mL of deionized water, add 1 g of gelatin, and adjust the pH to about 7 to 8 with NaOH solution;
2)、将上述各溶液装入反应釜中，在140℃烘箱中，反应时间分别为6h、12h和24h，冷却后取出反应物并经洗涤、烘干处理。2) Put the above-mentioned solutions into a reaction kettle, and place them in an oven at 140°C for 6 hours, 12 hours and 24 hours respectively. After cooling, take out the reactants and wash and dry them.
图5为不同反应时间下得到的产物的形态(a、b、c依次表示反应时间分别为6h、12h和24h)。可以看出，反应时间对产物的形态影响不大，反应时间过长时，将使得纤维直径增加。Figure 5 is the form of the product obtained under different reaction times (a, b, c successively represent that the reaction time is 6h, 12h and 24h respectively). It can be seen that the reaction time has little effect on the morphology of the product, and if the reaction time is too long, the fiber diameter will increase.
实施例4：反应体系pH大小对产物形态的影响规律。Example 4: The influence rule of the pH of the reaction system on the product form.
1)、将3mmol的CuSO4.5H2O和9mmol的酒石酸钾钠溶解于50mL去离子水中，明胶的添加量为1g，用NaOH溶液将其pH调节为6、9和12；1), 3 mmol of CuSO 4 .5H 2 O and 9 mmol of potassium sodium tartrate were dissolved in 50 mL of deionized water, the amount of gelatin added was 1 g, and the pH was adjusted to 6, 9 and 12 with NaOH solution;
2)、将上述各溶液装入反应釜中，在150℃烘箱中，反应时间分别为20h，冷却后取出反应物并经洗涤、烘干处理。2) Put the above-mentioned solutions into a reaction kettle, and place them in an oven at 150°C for 20 hours. After cooling, take out the reactants and wash and dry them.
图6为不同pH下得到的产物的形态(a、b、c依次表示pH调节至6、9和12)。可以看出，反应溶液pH大小对产物的形态的影响较大，pH小于7或高于9时，纤维状产物都较少。Figure 6 is the morphology of the products obtained at different pH (a, b, c successively represent the pH adjusted to 6, 9 and 12). It can be seen that the pH of the reaction solution has a great influence on the morphology of the product, and when the pH is less than 7 or higher than 9, the fibrous products are less.
综合上述各实施例及其相应结果可以得出结论：高质量的纤维状Cu2O制备的主要影响因素是：明胶模板的用量、反应温度、溶液的pH大小以及反应时间等，当调控到合适的参数后，才能成功获得高质量的Cu2O纳米纤维。因此，和已有的制备Cu2O方法相比，本发明方法又具有明显的可控特征。Based on the above examples and corresponding results, it can be concluded that the main factors affecting the preparation of high-quality fibrous Cu 2 O are: the amount of gelatin template, reaction temperature, pH of the solution, and reaction time. High-quality Cu 2 O nanofibers can be successfully obtained only after the parameters are selected. Therefore, compared with the existing method for preparing Cu 2 O, the method of the present invention has obvious controllable characteristics.
以上内容仅仅是对本发明的构思所作的举例和说明，所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，只要不偏离发明的构思或者超越本权利要求书所定义的范围，均应属于本发明的保护范围。The above content is only an example and description of the concept of the present invention. Those skilled in the art make various modifications or supplements to the described specific embodiments or replace them in similar ways, as long as they do not deviate from the concept of the invention. Or beyond the scope defined in the claims, all should belong to the protection scope of the present invention.
Claims (7)
- A kind of 1. Cu2The controllable method for preparing of O nanofibers, it is characterised in that soluble copper salt, tartaric acid or tartrate and Gelatin obtains Cu by hydro-thermal reaction2O nano-powders, the additive amount and reaction system of the gelatin of template are used as by regulation and control PH value, in the form of controlling product, and obtains the Cu of high quality2O nanofibers.
- 2. controllable method for preparing as claimed in claim 1, it is characterised in that step is as follows：1) soluble copper salt and tartaric acid or tartrate solution, are added into the wiring solution-forming into the deionized water of certain volume；2), gelatin is added in above-mentioned solution, slightly heating makes its perfect solution, obtains a kind of colloidal solution；3), above-mentioned solution is transferred in reaction kettle after adjusting its pH value with NaOH solution, carries out hydro-thermal reaction, and reaction terminates to take out anti- Thing is answered, it is washed to obtain target product.
- 3. controllable method for preparing as claimed in claim 2, it is characterised in that mantoquita is selected from CuSO in step 1)4.5H2O or Cu (NO3)2, tartrate is selected from sodium potassium tartrate tetrahydrate.
- 4. controllable method for preparing as claimed in claim 3, it is characterised in that in step 1) between copper ion and tartrate anion Molar ratio is 1：1~3, the molar concentration of mantoquita is 0.02~0.06mol/L in solution.
- 5. controllable method for preparing as claimed in claim 4, it is characterised in that the additive amount of the middle gelatin as template of step 2) For 2~40g/L, according to the liquor capacity meter being made into step 1).
- 6. controllable method for preparing as claimed in claim 2, it is characterised in that adjusting its pH value with NaOH solution in step 3) is 5~12.
- 7. controllable method for preparing as claimed in claim 2, it is characterised in that in step 3) temperature of hydro-thermal reaction for 130~ 150 DEG C, the reaction time is 6~24h.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102464357A (en) * | 2010-11-04 | 2012-05-23 | 中国科学院合肥物质科学研究院 | Iron ferric oxide nanofibers, preparation method and application thereof |
-
2018
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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Non-Patent Citations (2)
| Title |
|---|
| XIAO-LIN LUO ET AL.: "Hydrothermal synthesis of morphology controllable Cu2O and their catalysis in thermal decomposition of ammonium perchlorate", 《JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY》 * |
| 阮青锋等: "不同形态Cu2O枝晶的可控制备及形成机理", 《人工晶体学报》 * |
Cited By (1)
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|---|---|---|---|---|
| CN109485084A (en) * | 2018-12-29 | 2019-03-19 | 合肥学院 | Method for synthesizing cuprous oxide powder with controllable form and application |
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