CN105565365A - Flower-like zinc oxide crystal preparation method - Google Patents
Flower-like zinc oxide crystal preparation method Download PDFInfo
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- CN105565365A CN105565365A CN201410520036.2A CN201410520036A CN105565365A CN 105565365 A CN105565365 A CN 105565365A CN 201410520036 A CN201410520036 A CN 201410520036A CN 105565365 A CN105565365 A CN 105565365A
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Abstract
The invention relates to a flower-like zinc oxide crystal preparation method, wherein the amount of the reactant and the PH value of the mixing liquid are controlled, different precursors are obtained through a hydrothermal method, and then the product is sintered to obtain the flower-like zinc oxide crystal with the uniform size distribution. According to the present invention, the method has characteristics of simple, fast and safe operation, low cost, and good repeatability; the obtained flower-like zinc oxide crystal is expected to have good application prospects in the fields of chemical sensing, photocatalytic degradation of organic dyes, and energy storage.
Description
Technical field
The invention belongs to the preparation of the oxide compound of zinc, relate to a kind of preparation method of flower shape zinc oxide crystal.The method utilizes hydro-thermal reaction, and at control reactant concn, on the basis in temperature of reaction and reaction times, obtain the flower shape zinc oxide crystal of pattern and size uniformity, this material is expected to be applied to catalyzed reaction and photodegradation organic dye further.
Background technology
Zinc oxide is a kind of important metal oxide semiconductor, its bandwidth is 3.7 ev, excited state bandwidth is 60meV, this character of zinc oxide determines it has huge application potential (Dai, Z.R. in optics, solar cell, piezoelectric nano engine, gas sensor etc.; Pan, Z.W.; Wang, Z.L.Adv.Funct.Mater.2003,13,9-24.).
In the last few years, the zinc oxide of different micro nano structure was successfully obtained, the nano wire of such as zinc oxide, nanometer rod, nanotube, nanometer sheet, hollow ball and other pattern (Huang, M.H.; Mao, S.; Feick, H.; Yan, H.Q.; Wu, Y.Y.; Kind, H.; Weber, E.; Russo, R.; Yang, P.D.Science2001,292,1897-1899.).The self aggregation of nanometer assembled unit becomes complicated structure and has been proved to be a kind of effectively synthesis mode.A lot of researchist pays close attention to the preparation synthesis upper (B.X.Li, Y.F.Wang, J.Phys.Chem.C114 (2010) 890-896.) of three-layer laminated structure.Compare with low-dimensional materials, zinc oxide laminate structure due to 3D structure has high specific surface area and in catalyzed reaction, avoids the advantage of self aggregation, outstanding photochemical catalysis performance (Y.L.Lai can be provided, M.Meng, Y.F.Yu, Appl.Catal.B:Environ.100 (2010) 491-501.).
Summary of the invention
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of preparation method of flower shape zinc oxide crystal, is characterized in that comprising the steps:
(1) take suitable quantity of water soluble zinc salt and 1 ~ 10g oxysuccinic acid, add in 100 ~ 200ml distilled water, under being placed in 10 ~ 100 DEG C of environment, induction stirring 5 ~ 30min obtains A liquid.
(2) gel B is formed under A liquid being placed in 50 ~ 150 DEG C of environment.
(3) take 1.0 ~ 20.0g potassium hydroxide, join in the middle of B, induction stirring 10 ~ 30min obtains C.
(4) C is transferred in 100 ~ 250ml reactor, maintain the temperature at 10 ~ 150 DEG C and leave standstill 1 ~ 24h.
(5) by the solid product distilled water wash that obtains in reactor 1 ~ 3 time, obtain product and keep 20 ~ 120 DEG C, dry 12 ~ 24h.
(6) final product is obtained after being kept by the product obtained after drying 100 ~ 500 DEG C to calcine 1 ~ 5h in retort furnace.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of flower shape zinc oxide crystal in embodiment 1;
Fig. 2 is the XRD figure sheet of flower shape zinc oxide crystal in embodiment 2;
Embodiment:
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
Embodiment 1
1. claim 1.83g zinc acetate and 2.68g oxysuccinic acid, add in 100ml distilled water, under being placed in 60 DEG C of environment, induction stirring 30min obtains A liquid.
2. gel B is formed under A liquid being placed in 100 DEG C of environment.
3. take 5.6g potassium hydroxide, join in the middle of B, induction stirring 20min obtains C.
4. C is transferred in 100ml reactor, maintain the temperature at 140 DEG C of standing 12h.
5. by the solid product distilled water wash that obtains in reactor 3 times, obtain product and keep 60 DEG C, dry 12h.
6. final product is obtained after being kept by the product obtained after drying 250 DEG C to calcine 3h in retort furnace.
Embodiment 2
1. final product is obtained after being kept by the product obtained after drying 350 DEG C to calcine 2h in retort furnace.
2. claim 1.83g zinc acetate and 2.68g oxysuccinic acid, add in 100ml distilled water, under being placed in 60 DEG C of environment, induction stirring 30min obtains A liquid.
3. gel B is formed under A liquid being placed in 100 DEG C of environment.
4. take 0.7g potassium hydroxide, join in the middle of B, induction stirring 20min obtains C.
5. C is transferred in 100ml reactor, maintain the temperature at 140 DEG C of standing 12h.
6. by the solid product distilled water wash that obtains in reactor 3 times, obtain product and keep 60 DEG C, dry 12h.
7. final product is obtained after being kept by the product obtained after drying 250 DEG C to calcine 3h in retort furnace.
Embodiment 3
1. claim 1.83g zinc acetate and 2.68g oxysuccinic acid, add in 100ml distilled water, under being placed in 60 DEG C of environment, induction stirring 30min obtains A liquid.
2. gel B is formed under A liquid being placed in 100 DEG C of environment.
3. take 1.4g potassium hydroxide, join in the middle of B, induction stirring 20min obtains C.
4. C is transferred in 100ml reactor, maintain the temperature at 140 DEG C of standing 12h.
5. by the solid product distilled water wash that obtains in reactor 3 times, obtain product and keep 60 DEG C, dry 12h.
6. final product is obtained after being kept by the product obtained after drying 250 DEG C to calcine 3h in retort furnace.
Embodiment 4
1. claim 1.83g zinc acetate and 2.68g oxysuccinic acid, add in 100ml distilled water, under being placed in 60 DEG C of environment, induction stirring 30min obtains A liquid.
2. gel B is formed under A liquid being placed in 100 DEG C of environment.
3. take 2.8g potassium hydroxide, join in the middle of B, induction stirring 20min obtains C.
4. C is transferred in 100ml reactor, maintain the temperature at 140 DEG C of standing 12h.
5. by the solid product distilled water wash that obtains in reactor 3 times, obtain product and keep 60 DEG C, dry 12h.
6. final product is obtained after being kept by the product obtained after drying 250 DEG C to calcine 3h in retort furnace.
Embodiment 5
1. claim 1.83g zinc acetate and 2.68g oxysuccinic acid, add in 100ml distilled water, under being placed in 60 DEG C of environment, induction stirring 30min obtains A liquid.
2. gel B is formed under A liquid being placed in 100 DEG C of environment.
3. take 7.2g potassium hydroxide, join in the middle of B, induction stirring 20min obtains C.
4. C is transferred in 100ml reactor, maintain the temperature at 140 DEG C of standing 12h.
5. by the solid product distilled water wash that obtains in reactor 3 times, obtain product and keep 60 DEG C, dry 12h.
6. final product is obtained after being kept by the product obtained after drying 250 DEG C to calcine 3h in retort furnace.
Embodiment 6
1. claim 1.83g zinc acetate and 2.68g oxysuccinic acid, add in 100ml distilled water, under being placed in 60 DEG C of environment, induction stirring 30min obtains A liquid.
2. gel B is formed under A liquid being placed in 100 DEG C of environment.
3. take 11.2g potassium hydroxide, join in the middle of B, induction stirring 20min obtains C.
4. C is transferred in 100ml reactor, maintain the temperature at 140 DEG C of standing 12h.
5. by the solid product distilled water wash that obtains in reactor 3 times, obtain product and keep 60 DEG C, dry 12h.
6. final product is obtained after being kept by the product obtained after drying 250 DEG C to calcine 3h in retort furnace.
Claims (4)
1. a preparation method for flower shape zinc oxide crystal, is characterized in that comprising the following steps:.
(1) take suitable quantity of water soluble zinc salt and 1 ~ 10g oxysuccinic acid, add in 100 ~ 200ml distilled water, under being placed in 10 ~ 100 DEG C of environment, induction stirring 5 ~ 30min obtains A liquid.
(2) gel B is formed under A liquid being placed in 50 ~ 150 DEG C of environment.
(3) take 1.0 ~ 20.0g potassium hydroxide, join in the middle of B, induction stirring 10 ~ 30min obtains C.
(4) C is transferred in 100 ~ 250ml reactor, maintain the temperature at 10 ~ 150 DEG C and leave standstill 1 ~ 24h.
(5) by the solid product distilled water wash that obtains in reactor 1 ~ 3 time, obtain product and keep 20 ~ 120 DEG C, dry 12 ~ 24h.
(6) product obtained after drying is kept 100 ~ 500 DEG C in retort furnace, after calcining 1 ~ 5h, obtain final product.
2., by the preparation method of flower shape zinc oxide crystal described in claim 1, it is characterized in that: the water-soluble zinc salt described in described step (1) can be zinc sulfate, zinc nitrate, zinc chloride.
3., by the preparation method of flower shape zinc oxide crystal described in claim 1, it is characterized in that: the potassium hydroxide amount described in described step (3) need ensure that its pH value adding rear solution is between 8-14.
4., by the preparation method of flower shape zinc oxide crystal described in claim 1, it is characterized in that: described in described step (6), the temperature rise rate of retort furnace should control at 1 ~ 5 DEG C/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106673053A (en) * | 2017-01-05 | 2017-05-17 | 温州生物材料与工程研究所 | Method for preparing sodium-doped zinc oxide nano-powder |
| CN107916433A (en) * | 2016-10-09 | 2018-04-17 | 中国科学院大连化学物理研究所 | The preparation of micro nano structure zinc electrode and zinc electrode and application |
| CN110124657A (en) * | 2019-06-14 | 2019-08-16 | 辽宁大学 | K ion doping ZnO catalysis material and its preparation method and application |
-
2014
- 2014-09-28 CN CN201410520036.2A patent/CN105565365A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107916433A (en) * | 2016-10-09 | 2018-04-17 | 中国科学院大连化学物理研究所 | The preparation of micro nano structure zinc electrode and zinc electrode and application |
| CN106673053A (en) * | 2017-01-05 | 2017-05-17 | 温州生物材料与工程研究所 | Method for preparing sodium-doped zinc oxide nano-powder |
| CN110124657A (en) * | 2019-06-14 | 2019-08-16 | 辽宁大学 | K ion doping ZnO catalysis material and its preparation method and application |
| CN110124657B (en) * | 2019-06-14 | 2021-07-20 | 辽宁大学 | K ion doped ZnO photocatalytic material and preparation method and application thereof |
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Application publication date: 20160511 |