CN102275977B - Preparation method of zinc oxide mesoscopic crystal with adjustable aspect ratio - Google Patents
Preparation method of zinc oxide mesoscopic crystal with adjustable aspect ratio Download PDFInfo
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- CN102275977B CN102275977B CN 201110201517 CN201110201517A CN102275977B CN 102275977 B CN102275977 B CN 102275977B CN 201110201517 CN201110201517 CN 201110201517 CN 201110201517 A CN201110201517 A CN 201110201517A CN 102275977 B CN102275977 B CN 102275977B
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Abstract
The invention provides a preparation method of a zinc oxide mesoscopic crystal with an adjustable aspect ratio, and the preparation method comprises the following steps: preparing a zinc salt aqueous solution with a concentration of 0.05-100 mg/mL, and heating under stirring to 70-95 DEG C; preparing a sodium hydroxide aqueous solution with a concentration of 5-300 mg/mL; dropwise adding the prepared sodium hydroxide aqueous solution to the zinc salt aqueous solution under a stirring condition to obtain a mixed solution; heating the mixed solution under stirring to 70-95 DEG C, and maintaining the constant temperature for 0.01-5 hours; separately centrifugally washing the mixed solution with deionized water and ethanol; and then drying the product obtained by centrifugal washing in a drying box at the temperature of 30-60 DEG C for 2-12 hours to obtain the zinc oxide mesoscopic crystal. The preparation method provided by the invention has low cost and simple process; the aspect ratio of the zinc oxide mesoscopic crystal can be adjusted and controlled by adjusting the concentrations of the zinc salt solution and the sodium hydroxide solution, heating temperature and heat-insulation time; and the prepared zinc oxide mesoscopic crystal has uniform size and regular shape.
Description
Technical field
The present invention relates to the preparation method that zinc oxide Jie sees crystal, particularly adjustable zinc oxide Jie of a kind of length-to-diameter ratio sees the preparation method of crystal.
Background technology
Zinc oxide is as a kind of important broad stopband N-shaped conductor oxidate, and energy gap is 3.7eV.Owing to having good chemistry and physical stability, zinc oxide obtains important application in various fields such as lithium ion battery, catalysis, Opto-Electronics Crystals, ultraviolet laser and gas sensitives as functional materials.There are some researches show, exist substantial connection between the performance of material and its pattern, the zinc oxide with specific morphology, size and structure can be because of the functionalization system of its unique further construction material of performance.In the decades in past, the synthetic aspect of the pattern of zinc oxide and size control has obtained very large achievement.Be situated between seeing crystal is to be assembled by certain mode by many nano particles, and its principal character is to have internal interface and the crystal grain trend is consistent, these characteristics determined be situated between and see crystal and have special physics-chem characteristic, have wide practical use.The report that relevant zinc oxide Jie sees crystal has appearred recently, the sight crystal all is synthetic under the condition of adding tensio-active agent (such as PVP) or organism (such as DMF) but the zinc oxide that these have been reported is situated between, tensio-active agent and organic interpolation have not only increased cost, also can see crystal to zinc oxide Jie pollutes, so that its Quality Down, and then affect its performance.Therefore, also do not have in the prior art a kind of can realize preparation size quickly and easily evenly, regular shape, monodispersity is good and length-to-diameter ratio is adjustable zinc oxide be situated between and see the preparation method of crystal.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide adjustable zinc oxide Jie of a kind of length-to-diameter ratio to see the preparation method of crystal, the zinc oxide that adopts present method to prepare is situated between, and the sight crystal has advantages of size uniform, regular shape, monodispersity is good and length-to-diameter ratio is adjustable.
To achieve these goals, the technical solution used in the present invention is:
The zinc oxide that a kind of length-to-diameter ratio is adjustable is situated between and sees the preparation method of crystal, comprises the steps:
Step 1: preparation zinc salt concentration is the zinc salt solution of 0.05～100mg/mL, and this zinc salt solution is heated to 70 ℃～95 ℃ under the condition that stirs;
Step 2: the preparation naoh concentration is the aqueous sodium hydroxide solution of 0.05～300mg/mL;
Step 3: the aqueous sodium hydroxide of step 2 preparation is joined in the zinc salt solution of step 1 preparation and obtain mixing solutions, the volume ratio of aqueous sodium hydroxide solution and zinc salt solution is 1: 2～2: 1, this dropwise adition process remain stirring, then mixing solutions is heated to 70 ℃～95 ℃ temperature ranges and keeps constant temperature 0.01h～5h under the condition that stirs, in mixing solutions, produce cotton-shaped suspended substance;
Step 4: the cotton-shaped suspended substance that step 3 is obtained is used first deionized water centrifuge washing 2～4 times under 6000rpm, each centrifuge washing 2-15min, then use dehydrated alcohol centrifuge washing 2～4 times under 6000rpm, each centrifuge washing 2-15min, at last with the dry 2h～12h in loft drier of the cotton-shaped suspended substance behind the centrifuge washing, drying temperature is 30 ℃～60 ℃, can obtain zinc oxide Jie and see crystal.
Zinc salt in the zinc salt solution of described step 1 preparation is Zn (NO
3)
2, Zn (CH
3COO)
2, ZnCL
2Or ZnSO
4In any one.
Preparation method of the present invention is with low cost, operation is simple, can regulate and control the length-to-diameter ratio that zinc oxide Jie sees crystal by adjusting zinc salt and concentration of sodium hydroxide solution, Heating temperature and soaking time, and the zinc oxide of preparing Jie sight crystalline size is even, regular shape.
Embodiment
The below is described in further details the present invention with embodiment.
Embodiment one
The present embodiment zinc oxide is situated between and sees the preparation method of crystal, comprises the steps:
Step 1: preparation 30mL concentration is the Zn (NO of 85mg/mL
3)
2The aqueous solution, and with Zn (NO
3)
2The aqueous solution is heated to 80 ℃ under the condition that stirs;
Step 2: preparation 30mL concentration is the aqueous sodium hydroxide solution of 60mg/mL;
Step 3: the aqueous sodium hydroxide of step 2 preparation is joined in the zinc salt solution of step 1 preparation and obtain mixing solutions, this dropwise adition process remain stirring, then mixing solutions is heated to 80 ℃ and be incubated 1h under the condition that stirs, in mixing solutions, produces cotton-shaped suspended substance;
Step 4: the cotton-shaped suspended substance that step 3 is obtained is used first deionized water centrifuge washing 3 times under 6000rpm, each centrifuge washing 8min, then use dehydrated alcohol centrifuge washing 3 times under 6000rpm, each centrifuge washing 8min, with the dry 10h under 40 ℃ of the product behind the centrifuge washing, can obtain zinc oxide Jie and see crystal at last.
Zinc oxide Jie that the present embodiment obtains sees crystal length and is about 270nm, and length-to-diameter ratio is about 5: 3.
Embodiment two
The present embodiment zinc oxide is situated between and sees the preparation method of crystal, comprises the steps:
Step 1: preparation 100mL concentration is the Zn (CH of 0.06mg/mL
3COO)
2The aqueous solution, and with Zn (CH
3COO)
2The aqueous solution is heated to 85 ℃ under the condition that stirs;
Step 2: preparation 100mL concentration is the aqueous sodium hydroxide solution of 0.08mg/mL;
Step 3: the aqueous sodium hydroxide of step 2 preparation is joined in the zinc salt solution of step 1 preparation and obtain mixing solutions, this dropwise adition process remain stirring, then mixing solutions is heated to 85 ℃ and be incubated 3h under the condition that stirs, in mixing solutions, produces cotton-shaped suspended substance;
Step 4: the cotton-shaped suspended substance that step 3 is obtained is used first deionized water centrifuge washing 2 times under 6000rpm, each centrifuge washing 15min, then use dehydrated alcohol centrifuge washing 3 times under 6000rpm, each centrifuge washing 8min, with the dry 12h under 30 ℃ of the product behind the centrifuge washing, can obtain zinc oxide Jie and see crystal at last.
Zinc oxide Jie that the present embodiment obtains sees crystal length and is about 260nm, and length-to-diameter ratio is about 2: 1.
Embodiment three
The present embodiment zinc oxide is situated between and sees the preparation method of crystal, comprises the steps:
Step 1: preparation 100mL concentration is the ZnCL of 100mg/mL
2The aqueous solution, and with ZnCL
2The aqueous solution is heated to 80 ℃ under the condition that stirs;
Step 2: preparation 100mL concentration is the aqueous sodium hydroxide solution of 300mg/mL;
Step 3: the aqueous sodium hydroxide of step 2 preparation is joined in the zinc salt solution of step 1 preparation and obtain mixing solutions, this dropwise adition process remain stirring, then mixing solutions is heated to 80 ℃ and be incubated 0.5h under the condition that stirs, in mixing solutions, produces cotton-shaped suspended substance;
Step 4: the cotton-shaped suspended substance that step 3 is obtained is used first deionized water centrifuge washing 3 times under 6000rpm, each centrifuge washing 8min, then use dehydrated alcohol centrifuge washing 4 times under 6000rpm, each centrifuge washing 2min, with the dry 10h under 40 ℃ of the product behind the centrifuge washing, can obtain zinc oxide Jie and see crystal at last.
Zinc oxide Jie that the present embodiment obtains sees crystal length and is about 800nm, and length-to-diameter ratio is about 3: 1.
Embodiment four
The present embodiment zinc oxide is situated between and sees the preparation method of crystal, comprises the steps:
Step 1: preparation 100mL concentration is the Zn (NO of 1mg/mL
3)
2The aqueous solution, and with Zn (NO
3)
2The aqueous solution is heated to 90 ℃ under the condition that stirs;
Step 2: preparation 100mL concentration is the aqueous sodium hydroxide solution of 0.8mg/mL;
Step 3: the aqueous sodium hydroxide of step 2 preparation is joined in the zinc salt solution of step 1 preparation and obtain mixing solutions, this dropwise adition process remain stirring, then mixing solutions is heated to 90 ℃ and be incubated 2h under the condition that stirs, in mixing solutions, produces cotton-shaped suspended substance;
Step 4: the cotton-shaped suspended substance that step 3 is obtained is used first deionized water centrifuge washing 3 times under 6000rpm, each centrifuge washing 9min, then use dehydrated alcohol centrifuge washing 2 times under 6000rpm, each centrifuge washing 15min, with the dry 2h under 60 ℃ of the product behind the centrifuge washing, can obtain zinc oxide Jie and see crystal at last.
Zinc oxide Jie that the present embodiment obtains sees crystal length and is about 1800nm, and length-to-diameter ratio is about 3: 1.
Embodiment five
The present embodiment zinc oxide is situated between and sees the preparation method of crystal, comprises the steps:
Step 1: preparation 200mL concentration is the Zn (NO of 1.2mg/mL
3)
2The aqueous solution, and with Zn (NO
3)
2The aqueous solution is heated to 95 ℃ under the condition that stirs;
Step 2: preparation 100mL concentration is the aqueous sodium hydroxide solution of 1mg/mL;
Step 3: the aqueous sodium hydroxide of step 2 preparation is joined in the zinc salt solution of step 1 preparation and obtain mixing solutions, this dropwise adition process remain stirring, then mixing solutions is heated to 95 ℃ and be incubated 0.01h under the condition that stirs, in mixing solutions, produces cotton-shaped suspended substance;
Step 4: the cotton-shaped suspended substance that step 3 is obtained is used first deionized water centrifuge washing 3 times under 6000rpm, each centrifuge washing 8min, then use dehydrated alcohol centrifuge washing 4 times under 6000rpm, each centrifuge washing 2min, with the dry 5h under 50 ℃ of the product behind the centrifuge washing, can obtain zinc oxide Jie and see crystal at last.
Zinc oxide Jie that the present embodiment obtains sees crystal length and is about 500nm, and length-to-diameter ratio is about 3: 2.
Embodiment six
The present embodiment zinc oxide is situated between and sees the preparation method of crystal, comprises the steps:
Step 1: preparation 50mL concentration is the ZnSO of 10mg/mL
4The aqueous solution, and with ZnSO
4The aqueous solution is heated to 70 ℃ under the condition that stirs;
Step 2: preparation 100mL concentration is the aqueous sodium hydroxide solution of 8mg/mL;
Step 3: the aqueous sodium hydroxide of step 2 preparation is joined in the zinc salt solution of step 1 preparation and obtain mixing solutions, this dropwise adition process remain stirring, then mixing solutions is heated to 70 ℃ and be incubated 5h under the condition that stirs, in mixing solutions, produces cotton-shaped suspended substance;
Step 4: the cotton-shaped suspended substance that step 3 is obtained is used first deionized water centrifuge washing 4 times under 6000rpm, each centrifuge washing 2min, then use dehydrated alcohol centrifuge washing 3 times under 6000rpm, each centrifuge washing 9min, with the dry 10h under 40 ℃ of the product behind the centrifuge washing, can obtain zinc oxide Jie and see crystal at last.
Zinc oxide Jie that the present embodiment obtains sees crystal length and is about 800nm, and length-to-diameter ratio is about 2: 1.
Claims (2)
1. the adjustable zinc oxide of a length-to-diameter ratio is situated between and sees the preparation method of crystal, comprises the steps:
Step 1: preparation zinc salt concentration is the zinc salt solution of 0.05～100mg/mL, and this zinc salt solution is heated to 70 ℃～95 ℃ under the condition that stirs;
Step 2: the preparation naoh concentration is the aqueous sodium hydroxide solution of 5～300mg/mL;
Step 3: the aqueous sodium hydroxide of step 2 preparation is joined in the zinc salt solution of step 1 preparation and obtain mixing solutions, the volume ratio of aqueous sodium hydroxide solution and zinc salt solution is 1: 2～2: 1, this dropwise adition process remain stirring, then mixing solutions is heated to 70 ℃～95 ℃ temperature ranges and keeps constant temperature 0.01h～5h under the condition that stirs, in mixing solutions, produce cotton-shaped suspended substance;
Step 4: the cotton-shaped suspended substance that step 3 is obtained is used first deionized water centrifuge washing 2～4 times under 6000rpm, each centrifuge washing 2-15min, then with dehydrated alcohol centrifuge washing 2～4 times under 6000rpm, each centrifuge washing 2-15min, then with the dry 2h～12h in loft drier of the cotton-shaped suspended substance behind the centrifuge washing, drying temperature is 30 ℃～60 ℃, can obtain zinc oxide Jie and see crystal.
2. method according to claim 1 is characterized in that: the zinc salt in the zinc salt solution of described step 1 preparation is Zn (NO
3)
2, Zn (CH
3COO)
2, ZnCl
2Or ZnSO
4In any one.
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| CN103771490B (en) * | 2014-01-04 | 2015-08-19 | 东华理工大学 | A kind of simple and easy stirring at room temperature prepares the method for micro-/ nano zinc oxide |
| CN105002552A (en) * | 2014-04-15 | 2015-10-28 | 昆明仁旺科技有限公司 | Iridium mesoscopic crystal synthesis method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5093099A (en) * | 1987-11-16 | 1992-03-03 | Kao Corporation | Flaky powder of zinc oxide and its composition for external use |
| CN101012555A (en) * | 2007-01-12 | 2007-08-08 | 刘津平 | Nano zinc oxide, solution preparation and method and device for film forming on metal or compound surface |
| CN101214990A (en) * | 2007-12-28 | 2008-07-09 | 中国科学院上海硅酸盐研究所 | Normal temperature synthesis method for nanometer zinc oxide |
-
2011
- 2011-07-19 CN CN 201110201517 patent/CN102275977B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5093099A (en) * | 1987-11-16 | 1992-03-03 | Kao Corporation | Flaky powder of zinc oxide and its composition for external use |
| CN101012555A (en) * | 2007-01-12 | 2007-08-08 | 刘津平 | Nano zinc oxide, solution preparation and method and device for film forming on metal or compound surface |
| CN101214990A (en) * | 2007-12-28 | 2008-07-09 | 中国科学院上海硅酸盐研究所 | Normal temperature synthesis method for nanometer zinc oxide |
Non-Patent Citations (2)
| Title |
|---|
| ZnO准一维纳米结构生长形态的演化机理;苏英杰等;《无机材料学报》;20091130;第24卷(第6期);第1141-1146页 * |
| 苏英杰等.ZnO准一维纳米结构生长形态的演化机理.《无机材料学报》.2009,第24卷(第6期),第1141-1146页. |
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