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Synthesizing method for zinc oxide nanometer materials
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A technology of zinc oxide nano and synthesis method, which is applied in the direction of zinc oxide/zinc hydroxide, etc., can solve the problems of reducing the specific surface area of nano ZnO, easy agglomeration of nano ZnO, and difficulty in working at the same time, so as to achieve simple operation and easy industrialization Effect
Active Publication Date: 2015-03-25
江苏汇诚医疗科技有限公司
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[0002] Zinc oxide (ZnO) is an important semiconductor material. In the liquid-phase synthesis process of nano-scale ZnO, single-chain surfactants (such as CTAB, SDS, SDBS) and water-soluble polymers (such as PVP, PEG ) as a dispersant, the obtained nano-ZnO can remove the protective agent after washing, but the nano-ZnO without protective layer is easy to agglomerate in use, thereby significantly reducing the specific surface area of nano-ZnO
At the same time, the use of common surfactants or dispersants is difficult to simultaneously control the synthesis of ZnO morphology and maintain a high specific surface area.
Method used
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example 1
[0030] Example 1: 10g of 2,8,14,20-tetraalkyl-resorcinol calix[4]-5,11,17,23-sodium tetramethanesulfonate, 72.7g of zinc nitrate and 583.8g of Add concentrated ammonia water into 37805g water to dissolve, mix and dissolve, heat to 97-101°C to achieve reflux, keep warm for 3-4 hours, and centrifuge to obtain a solid.
[0031] Dry the solid in a vacuum oven at 50-70° C. for 12-14 hours to obtain 30.9 g of nanometer zinc oxide.
example 2
[0032] Example 2: 10g of 2,8,14,20-tetrapropyl-resorcinol calix[4]-5,11,17,23-sodium tetramethanesulfonate, 73g of zinc acetate and 583.5g of concentrated Add ammonia water to 37810g water to dissolve, mix and dissolve, heat to 97-101°C to achieve reflux, keep warm for 3-4 hours, and then centrifuge to obtain a solid.
[0033] Dry the solid in a vacuum oven at 50-70° C. for 12-14 hours to obtain 31.3 g of nanometer zinc oxide.
example 3
[0034] Example 3: 10g of 2,8,14,20-tetrahexyl-resorcinol calix[4]-5,11,17,23-sodium tetramethanesulfonate, 75g of zinc sulfate and 583.5g of concentrated ammonia Add it into 37810g water to dissolve, mix and dissolve, heat to 97-101°C to achieve reflux, keep warm for 3-4 hours, and centrifuge to obtain a solid.
[0035] Dry the solid in a vacuum oven at 50-70° C. for 12-14 hours to obtain 32.2 g of nanometer zinc oxide.
[0036] 3. Product identification:
[0037] 1, Figure 1 to Figure 5 The FE-SEM, TEM and HR-TEM photos of the ZnO dumbbell balls were given.
[0038] from Figures 1 to 5 It can be seen that by adopting the process of the present invention, the obtained zinc oxide material has a nanostructure.
[0039] 2. Put the purified ZnO powder into a corundum crucible and place it in a muffle furnace, and calcinate at 500-800°C for 5-8 hours to obtain mesoporous ZnO micro-nano crystals. Then proceed to product identification:
[0040] Image 6 , 7 The FE...
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Abstract
The invention relates to a synthesizing method for zinc oxide nanometer materials, particularly to a synthesizing method for zinc oxide nanometer mesoporous materials. The method comprises the steps: mixing zinc salt and stronger ammonia water to settled solution in a backflow way at the ordinary pressure; using a micelle formed by a calix[4]resorcinol methanesulfinic acid sodium type surface active agent as a template; carrying out the fixing and the gathering of zinc ions by the electrostatic attraction of hydrophilic group sulfoacid anions of the surface active agent to zinc ammonia complex anions; depositing ZnO nanometer particles during the procedure of the ammonia gas removal by the way of backflow, and forming dumbbell-shaped ZnO nanometer particles. Because the calix[4]resorcinol methanesulfinic acid sodium type surface active agent and the micelle thereof are in big-calix cavity, multi-head and multi-tail structures, the formation of the dumbbell-shaped particles can be participated in a frame way during the synthesizing procedure of the ZnO nanometers. The method is easy to operate, and is suitable for industrialization.
Description
technical field [0001] The invention relates to a synthesis method of zinc oxide nanometer mesoporous material. Background technique [0002] Zinc oxide (ZnO) is an important semiconductor material. In the liquid-phase synthesis process of nano-scale ZnO, single-chain surfactants (such as CTAB, SDS, SDBS) and water-soluble polymers (such as PVP, PEG ) as a dispersant, the obtained nano-ZnO can remove the protective agent after washing, but the nano-ZnO without protective layer is easy to agglomerate in use, thereby significantly reducing the specific surface area of nano-ZnO. At the same time, the use of common surfactants or dispersants is difficult to simultaneously control the synthesis of ZnO morphology and maintain a high specific surface area. Contents of the invention [0003] The purpose of the present invention is to propose a synthesis method capable of controlling the morphology and size of the prepared nano-ZnO and obtaining a zinc oxide nano-material with a...
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