CN102502887A - Method for preparing cobalt sulfide nanocrystals by hydrothermal-assisted sonochemistry - Google Patents

Method for preparing cobalt sulfide nanocrystals by hydrothermal-assisted sonochemistry Download PDF

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CN102502887A
CN102502887A CN2011103756765A CN201110375676A CN102502887A CN 102502887 A CN102502887 A CN 102502887A CN 2011103756765 A CN2011103756765 A CN 2011103756765A CN 201110375676 A CN201110375676 A CN 201110375676A CN 102502887 A CN102502887 A CN 102502887A
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ultrasonic
deionized water
reaction
cobalt sulfide
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CN102502887B (en
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曹丽云
李碧
李意峰
黄剑锋
吴建鹏
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QIDONG SHENGHAN MEDICAL TECHNOLOGY Co.,Ltd.
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Shaanxi University of Science and Technology
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Abstract

The invention provides a method for preparing cobalt sulfide nanocrystals by hydrothermal-assisted sonochemistry. The method comprises the steps of: adding cobalt nitrate hexahydrate to deionized water to obtain a solution A; adding EDTA (Ethylene Diamine Tetraacetic Acid) to the solution A and stirring to obtain a solution B; adding an H2S solution to the solution B to obtain a solution C; adding (NH4)2S to deionized water to obtain a solution D; oscillating the solution C in an ultrasonic cleaner, and simultaneously dropwise adding the solution D; adding the solution obtained after an ultrasonic reaction to a hydrothermal kettle for sealed reacting; after the reaction is finished, taking out the hydrothermal kettle, cooling to room temperature, separating the product, washing with deionized water and absolute ethanol respectively and drying to obtain black cobalt sulfide nanocrystals. According to the invention, prepared cobalt sulfide nanocrystals are controllable in appearance and are of a nanorod structure with a diameter about 10 nm; and the preparing process is simple, the operation is convenient, the temperature is low, the energy consumption is low and the preparing cost is lower.

Description

The auxiliary sonochemistry of a kind of hydro-thermal prepares the method for cobalt sulfide nanocrystalline
Technical field
The invention belongs to the sulfide nano-material technical field, be specifically related to the method that the auxiliary sonochemistry of a kind of hydro-thermal prepares cobalt sulfide nanocrystalline.
Background technology
Transient metal sulfide nano material as a kind of nontoxic, environmental protection; Cobaltous sulfide also has the due non-linear nature of nano material, fluorescent characteristic, quantum size effect and other important physical chemical property except having special 3d valence electron shell structure.Because such characteristic, make nano Co S material that more superior physics, chemistry, optics, pigment performance and purposes more widely arranged.Find after deliberation; The energy gap of cobalt sulfide nano particle is approximately 3.91eV [S.P.Tandon; J.P.Gupta.Measurement of Forbidden Energy Gap of Semiconductors by Diffuse Reflectance Technique.Physica Status Solidi (b), 1970,381 (1): 363-367]; The cobaltous sulfide nano material will be at [the M.S.Sadjadi that is widely used aspect these such as high energy density cells, solar energy electric material; A.Pourahmad, Sh.Sohrabnezhad, K.Zare.Formation of NiS and CoS semiconductor nanoparticles inside mordenite-type zeolite.Materials Letters; 2007,61 (14-15): 2923-2926].
Sonochemical method is to utilize acoustic cavitation can quicken or control chemical reaction, improves reaction yield and causes new chemical reaction, and be a kind of novel method for preparing nano material that occurs in recent years.Utilize sonochemical method to prepare cobalt sulfide nanocrystalline,, will be about micron-sized zone at yardstick and produce the high temperature and high pressure [M.Behboudnia of moment mainly due to cavitation effect of ultrasonic waves; M.H.Majlesara, B.Khanbabaee.Preparation of ZnS nanorods by ultrasonic waves [J] .Materials Science and Engineering B, 2005; 122 (2): 160-163]; In addition, when UW acted on solution, mechanics effect can pass through stirring action; Promote interionic to interact, thereby promote that chemical reaction fully carries out; The intensive shockwave that the acoustic cavitation effect produces has suppressed the formation of big micelle; Calorifics effect can promote the CoS cohesion; But chemical effect promotes oxidn reduction reaction, thus to CoS nanocrystalline be formed with good promoter action.
Hydrothermal method also be development in recent years than faster more a kind of method, research system generally is in imperfect nonequilibrium situations, the high-temperature high-pressure state in the thermal and hydric environment makes important interionic reaction accelerate, and has saved reaction so greatly and has carried out the needed time
Summary of the invention
The objective of the invention is to propose the method that the auxiliary sonochemistry of a kind of hydro-thermal prepares cobalt sulfide nanocrystalline.This method is simple to operate, the cobalt sulfide nanocrystalline well-crystallized of gained, and particle size dispersion is better.
For achieving the above object, the technical scheme that the present invention adopts is:
1) gets the analytical pure cobalt nitrate hexahydrate (Co (NO of 1.16g-5.80g 3) 26H 2O) place Erlenmeyer flask, in Erlenmeyer flask, add deionized water, stir, be configured to the red clear solution A of 40mL;
2) get 0.58g-2.90g YD 30 (EDTA) add stir in the solution A solution B;
3) mass concentration that in solution B, adds 0.5-4.0mL is 2% H 2S solution, stir solution C;
4) get (NH of 0.14mL-0.68mL 4) 2S places small beaker, and adds the solution D that deionized water is configured to 40mL;
5) solution C is put into ultrasonic cleaner and shake, dropwise add solution D simultaneously, set ultrasonic time 10-60min, ultrasonic power 200-500W, ultrasonic temperature 20-80 ℃;
6) solution behind the ultrasonic reaction is added in the water heating kettle, controlling its packing ratio is 50%-80%, and sealing afterwards is at 170-210 ℃ of reaction 6-24h;
7) after reaction finishes, the water heating kettle taking-up is cooled to room temperature, after product was separated, the product after the separation cleaned with deionized water and absolute ethyl alcohol respectively, and the baking oven of putting into 80 ℃ carries out drying, obtains the cobalt sulfide nanocrystalline of black.
Because the sonochemistry energy produces in the reaction process HTHP, intensive shockwave and high speed jet, having hindered particle becomes big micelle, and the criticality of thermal and hydric environment impels the crystallinity of crystal grain better, makes that the product crystallinity of gained is fine.The cobalt sulfide nanocrystalline pattern of this method preparation is controlled, is the nano bar-shape structure, and diameter is about 10nm; And preparation technology is simple, and is easy to operate, and temperature is low, and energy consumption is little, and preparation cost is lower.
Description of drawings
Fig. 1 is the transmission electron micrograph of the cobalt sulfide nanocrystalline of the embodiment of the invention 1 preparation.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done further explain.
Embodiment 1:
1) gets the analytical pure cobalt nitrate hexahydrate (Co (NO of 2.32g 3) 26H 2O) place Erlenmeyer flask, in Erlenmeyer flask, add deionized water, stir, be configured to the red clear solution A of 40mL;
2) get 1.16g YD 30 (EDTA) add stir in the solution A solution B;
3) mass concentration that in solution B, adds 2.0mL is 2% H 2S solution, stir solution C;
4) get (NH of 0.28mL 4) 2S places small beaker, and adds the solution D that deionized water is configured to 40mL;
5) solution C is put into ultrasonic cleaner and shake, dropwise add solution D simultaneously, set ultrasonic time 30min, ultrasonic power 300W, 80 ℃ of ultrasonic temperature;
6) solution behind the ultrasonic reaction is added in the water heating kettle, controlling its packing ratio is 8%, and sealing afterwards is at 190 ℃ of reaction 24h;
7) after reaction finishes, the water heating kettle taking-up is cooled to room temperature, after product was separated, the product after the separation cleaned with deionized water and absolute ethyl alcohol respectively, and the baking oven of putting into 80 ℃ carries out drying, obtains the cobalt sulfide nanocrystalline of black.
The cobalt sulfide nanocrystalline of gained is observed with transmission electron microscope, can be found out that prepared sample is the nano bar-shape structure, diameter is (Fig. 1) about 10nm.
Embodiment 2:
1) gets the analytical pure cobalt nitrate hexahydrate (Co (NO of 1.16g 3) 26H 2O) place Erlenmeyer flask, in Erlenmeyer flask, add deionized water, stir, be configured to the red clear solution A of 40mL;
2) get 0.58g YD 30 (EDTA) add stir in the solution A solution B;
3) mass concentration that in solution B, adds 0.5mL is 2% H 2S solution, stir solution C;
4) get (NH of 0.14mL 4) 2S places small beaker, and adds the solution D that deionized water is configured to 40mL;
5) solution C is put into ultrasonic cleaner and shake, dropwise add solution D simultaneously, set ultrasonic time 60min, ultrasonic power 500W, 50 ℃ of ultrasonic temperature;
6) solution behind the ultrasonic reaction is added in the water heating kettle, controlling its packing ratio is 80%, and sealing afterwards is at 180 ℃ of reaction 18h;
7) after reaction finishes, the water heating kettle taking-up is cooled to room temperature, after product was separated, the product after the separation cleaned with deionized water and absolute ethyl alcohol respectively, and the baking oven of putting into 80 ℃ carries out drying, obtains the cobalt sulfide nanocrystalline of black.
Embodiment 3:
1) gets the analytical pure cobalt nitrate hexahydrate (Co (NO of 5.80g 3) 26H 2O) place Erlenmeyer flask, in Erlenmeyer flask, add deionized water, stir, be configured to the red clear solution A of 40mL;
2) get 2.90g YD 30 (EDTA) add stir in the solution A solution B;
3) mass concentration that in solution B, adds 4.0mL is 2% H 2S solution, stir solution C;
4) get (NH of 0.68mL 4) 2S places small beaker, and adds the solution D that deionized water is configured to 40mL;
5) solution C is put into ultrasonic cleaner and shake, dropwise add solution D simultaneously, set ultrasonic time 15min, ultrasonic power 200W, 40 ℃ of ultrasonic temperature;
6) solution behind the ultrasonic reaction is added in the water heating kettle, controlling its packing ratio is 50%, and sealing afterwards is at 170 ℃ of reaction 20h;
7) after reaction finishes, the water heating kettle taking-up is cooled to room temperature, after product was separated, the product after the separation cleaned with deionized water and absolute ethyl alcohol respectively, and the baking oven of putting into 80 ℃ carries out drying, obtains the cobalt sulfide nanocrystalline of black.
Embodiment 4:
1) gets the analytical pure cobalt nitrate hexahydrate (Co (NO of 3.25g 3) 26H 2O) place Erlenmeyer flask, in Erlenmeyer flask, add deionized water, stir, be configured to the red clear solution A of 40mL;
2) get 2.30g YD 30 (EDTA) add stir in the solution A solution B;
3) mass concentration that in solution B, adds 1.0mL is 2% H 2S solution, stir solution C;
4) get (NH of 0.55mL 4) 2S places small beaker, and adds the solution D that deionized water is configured to 40mL;
5) solution C is put into ultrasonic cleaner and shake, dropwise add solution D simultaneously, set ultrasonic time 20min, ultrasonic power 400W, 20 ℃ of ultrasonic temperature;
6) solution behind the ultrasonic reaction is added in the water heating kettle, controlling its packing ratio is 60%, and sealing afterwards is at 200 ℃ of reaction 6h;
7) after reaction finishes, the water heating kettle taking-up is cooled to room temperature, after product was separated, the product after the separation cleaned with deionized water and absolute ethyl alcohol respectively, and the baking oven of putting into 80 ℃ carries out drying, obtains the cobalt sulfide nanocrystalline of black.
Embodiment 5:
1) gets the analytical pure cobalt nitrate hexahydrate (Co (NO of 4.60g 3) 26H 2O) place Erlenmeyer flask, in Erlenmeyer flask, add deionized water, stir, be configured to the red clear solution A of 40mL;
2) get 1.65g YD 30 (EDTA) add stir in the solution A solution B;
3) mass concentration that in solution B, adds 3.0mL is 2% H 2S solution, stir solution C;
4) get (NH of 0.32mL 4) 2S places small beaker, and adds the solution D that deionized water is configured to 40mL;
5) solution C is put into ultrasonic cleaner and shake, dropwise add solution D simultaneously, set ultrasonic time 40min, ultrasonic power 500W, 60 ℃ of ultrasonic temperature;
6) solution behind the ultrasonic reaction is added in the water heating kettle, controlling its packing ratio is 70%, and sealing afterwards is at 210 ℃ of reaction 6h;
7) after reaction finishes, the water heating kettle taking-up is cooled to room temperature, after product was separated, the product after the separation cleaned with deionized water and absolute ethyl alcohol respectively, and the baking oven of putting into 80 ℃ carries out drying, obtains the cobalt sulfide nanocrystalline of black.
Embodiment 6:
1) gets the analytical pure cobalt nitrate hexahydrate (Co (NO of 5.00g 3) 26H 2O) place Erlenmeyer flask, in Erlenmeyer flask, add deionized water, stir, be configured to the red clear solution A of 40mL;
2) get 0.80g YD 30 (EDTA) add stir in the solution A solution B;
3) mass concentration that in solution B, adds 0.8mL is 2% H 2S solution, stir solution C;
4) get (NH of 0.22mL 4) 2S places small beaker, and adds the solution D that deionized water is configured to 40mL;
5) solution C is put into ultrasonic cleaner and shake, dropwise add solution D simultaneously, set ultrasonic time 50min, ultrasonic power 300W, 70 ℃ of ultrasonic temperature;
6) solution behind the ultrasonic reaction is added in the water heating kettle, controlling its packing ratio is 60%, and sealing afterwards is at 200 ℃ of reaction 10h;
7) after reaction finishes, the water heating kettle taking-up is cooled to room temperature, after product was separated, the product after the separation cleaned with deionized water and absolute ethyl alcohol respectively, and the baking oven of putting into 80 ℃ carries out drying, obtains the cobalt sulfide nanocrystalline of black.

Claims (1)

1. a hydro-thermal assists sonochemistry to prepare the method for cobalt sulfide nanocrystalline, it is characterized in that:
1) gets the analytical pure cobalt nitrate hexahydrate (Co (NO of 1.16g-5.80g 3) 26H 2O) place Erlenmeyer flask, in Erlenmeyer flask, add deionized water, stir, be configured to the red clear solution A of 40mL;
2) get 0.58g-2.90g YD 30 (EDTA) add stir in the solution A solution B;
3) mass concentration that in solution B, adds 0.5-4.0mL is 2% H 2S solution, stir solution C;
4) get (NH of 0.14mL-0.68mL 4) 2S places small beaker, and adds the solution D that deionized water is configured to 40mL;
5) solution C is put into ultrasonic cleaner and shake, dropwise add solution D simultaneously, set ultrasonic time 10-60min, ultrasonic power 200-500W, ultrasonic temperature 20-80 ℃;
6) solution behind the ultrasonic reaction is added in the water heating kettle, controlling its packing ratio is 50%-80%, and sealing afterwards is at 170-210 ℃ of reaction 6-24h;
7) after reaction finishes, the water heating kettle taking-up is cooled to room temperature, after product was separated, the product after the separation cleaned with deionized water and absolute ethyl alcohol respectively, and the baking oven of putting into 80 ℃ carries out drying, obtains the cobalt sulfide nanocrystalline of black.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107857305A (en) * 2017-12-20 2018-03-30 南京隆信达新材料科技有限公司 Ternary FexCo1‑xS2The synthetic method of powder
CN108821348A (en) * 2018-09-17 2018-11-16 陕西科技大学 A kind of cobalt sulfide nanometer sheet material and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101746837A (en) * 2009-12-24 2010-06-23 东北师范大学 Preparation method of cobalt sulfide micro tube with hiberarchy structure
CN101786671A (en) * 2009-10-30 2010-07-28 陕西科技大学 Method for preparing bar-shaped cobalt sulfide nanocrystalline

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101786671A (en) * 2009-10-30 2010-07-28 陕西科技大学 Method for preparing bar-shaped cobalt sulfide nanocrystalline
CN101746837A (en) * 2009-12-24 2010-06-23 东北师范大学 Preparation method of cobalt sulfide micro tube with hiberarchy structure

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
WENJUN DONG ET AL.: "Hydrothermal synthesis and structure evolution of hierarchical cobalt sulfide nanostructures", 《DALTON TRANS》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107857305A (en) * 2017-12-20 2018-03-30 南京隆信达新材料科技有限公司 Ternary FexCo1‑xS2The synthetic method of powder
CN108821348A (en) * 2018-09-17 2018-11-16 陕西科技大学 A kind of cobalt sulfide nanometer sheet material and preparation method thereof
CN108821348B (en) * 2018-09-17 2021-02-19 陕西科技大学 Cobalt sulfide nanosheet material and preparation method thereof

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Address before: 808, 8 / F, building B, building a, B, business center, gangzhilong science and Technology Park, No.6 Qinglong Road, Qinghua community, Longhua street, Shenzhen City, Guangdong Province

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