CN1388066A - Solid-phase low-temperature thermal decomposition and synthesis process of preparing crystalline and amorphous superfine zine oxide powder - Google Patents
Solid-phase low-temperature thermal decomposition and synthesis process of preparing crystalline and amorphous superfine zine oxide powder Download PDFInfo
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- CN1388066A CN1388066A CN 02132486 CN02132486A CN1388066A CN 1388066 A CN1388066 A CN 1388066A CN 02132486 CN02132486 CN 02132486 CN 02132486 A CN02132486 A CN 02132486A CN 1388066 A CN1388066 A CN 1388066A
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Abstract
本发明属于精细无机化学材料制备领域,涉及对溶胶－凝胶经高温热解Zn(OH)2制备ZnO方法的改进,它是将固态的金属锌盐与碳酸氢钠按一定比例混合,在一定的温度下热分解,制备超微ZnO粉末。根据分解温度的不同,分别合成非晶态、晶态ZnO。本发明的固相低温热分解合成晶态和非晶态超微氧化锌粉末的制备方法设备简单、操作简单、成本低、产率高,产率95%以上。所得晶态ZnO粒径均匀,且在10－50nm范围内能很好的控制,非晶态ZnO具有较强的紫外发射。本发明广泛用于电子、日化、建材、涂料、橡胶制品,特别作为电子材料,广泛用于化学传感器,高频压电共振腔、光电池、紫外发光器件等,是重要的精细化工材料。The invention belongs to the field of preparation of fine inorganic chemical materials, and relates to the improvement of the method for preparing ZnO from sol-gel through high-temperature pyrolysis of Zn(OH) 2 . Thermal decomposition at a certain temperature to prepare ultrafine ZnO powder. According to different decomposition temperatures, amorphous and crystalline ZnO were synthesized respectively. The preparation method of the present invention for synthesizing crystalline and amorphous ultrafine zinc oxide powders by solid-phase low-temperature thermal decomposition has simple equipment, simple operation, low cost, and high yield, which is more than 95%. The particle size of the obtained crystalline ZnO is uniform and can be well controlled in the range of 10-50nm, and the amorphous ZnO has strong ultraviolet emission. The invention is widely used in electronics, daily chemicals, building materials, coatings, rubber products, especially as electronic materials, widely used in chemical sensors, high-frequency piezoelectric resonant cavities, photocells, ultraviolet light-emitting devices, etc., and is an important fine chemical material.
Description
Technical field: the invention belongs to fine inorganic chemical material preparation field, relate to sol-gel through high temperature pyrolysis Zn (OH)
2The improvement of preparation ZnO method.
Background technology: in the method that is usually used in preparing the ultra micro ZnO powder at present is that sol-gel is through high temperature pyrolysis Zn (OH)
2Preparation ZnO.As the domestic urea water solution of having developed, this method is the raw material synthesis of nano-zinc oxide with urea, zinc nitrate.This method requires processing condition to keep suitable reacting dynamics condition for guaranteeing quality product.
Summary of the invention: in order to solve the optimization processing condition in the above-mentioned technology, keep keeping higher zinc hydroxide supersaturation ratio everywhere in the reactor, and heat up, cooling has bigger speed, thereby make operation easier big, the problem of preparation condition harshness.The objective of the invention is to explore the preparation method who sets up synthetic crystalline state of simple, easy to operate, low-cost, the easy-operating solid-phase low-temperature thermolysis of a kind of equipment and amorphous superfine zine oxide powder, its making step is as at first forming compound by a certain percentage with solid-state metal zinc salt and sodium bicarbonate, compound is carried out thermolysis under certain temperature and certain hour, be prepared into non-crystalline state, crystalline state ultra micro ZnO powder respectively.
The present invention has adopted the solid state heat decomposition technique to solve that background technology zinc hydroxide supersaturation ratio height, intensification, rate of temperature fall are big, operation is difficult, the harsh problem of preparation condition.The preparation method that the equipment that the invention provides is simple, low-cost, crystalline state and amorphous superfine zine oxide powder are synthesized in preparation solid-phase low-temperature easy to operate thermolysis, gained crystalline state ZnO particle diameter is even, and energy better controlled in the 10-50nm scope, non-crystalline state ZnO has stronger ultraviolet emission.The productive rate height can reach productive rate more than 95%.Ultra micro ZnO powder of the present invention is widely used in electronics, daily use chemicals, building materials, coating, rubber item, especially as electronic material, is widely used in chemical sensor, and high frequency piezoelectric resonant chamber, photocell, ultra-violet light-emitting device etc. are important fine chemistry industry materials.
Description of drawings:
Fig. 1 is an x-ray diffraction pattern of the present invention
Fig. 2 is a transmission electron microscope picture of the present invention
Fig. 3 is a photoluminescence spectrum of the present invention
Embodiment is as shown in the figure:
Among Fig. 1 (a) be the present invention at 250 ℃ of heat treated x-ray diffraction patterns, be that the present invention is at 160 ℃ of heat treated x-ray diffraction patterns (b)
Among Fig. 2 (a), be that the present invention is at 200 ℃, 250 ℃ heat treated transmission electron microscope pictures (b); (c) be that the present invention is at 160 ℃ of heat treated transmission electron microscope pictures
(a) is the photoluminescence spectrum of the present invention when 160 ℃ of thermal treatment among Fig. 3, (b) is the photoluminescence spectrum of the present invention when 250 ℃ of thermal treatment
Embodiment 1: the preparation of non-crystalline state ultra micro ZnO: take by weighing 2g Zn (CH
3COO) 2H
2O and 2gNHCO
3Place mortar, thorough mixing.Mixture is placed on the quartz boat, at N
2Flow down in tube furnace 160 ℃ of thermal treatments 3 hours, the cooling washing, 90 ℃ of dryings of product 3 hours, white ZnOH
2O 0.86g, productive rate 95.3%.Temperature in the stove can be 150-170 ℃ of selection, and heat treatment period can be selected at 1-5 hour.Prepare non-crystalline state ultra micro ZnO this moment.
Embodiment 2: the preparation of crystalline state nano-ZnO: take by weighing 2g Zn (CH
3COO) 2H
2O and 2gNHCO
3Place mortar, thorough mixing.Mixture is placed on the quartz boat, at N
2Flow down in tube furnace 250 ℃ of thermal treatments 3 hours, the cooling washing, 90 ℃ of dryings of product 3 hours, canescence 25nm ZnO 0.69g, productive rate 94%.Temperature in the stove can be 180-300 ℃ of selection, and heat treatment period can be selected at 1-5 hour.Prepare crystalline state ultra micro ZnO this moment.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02132486 CN1388066A (en) | 2002-06-25 | 2002-06-25 | Solid-phase low-temperature thermal decomposition and synthesis process of preparing crystalline and amorphous superfine zine oxide powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02132486 CN1388066A (en) | 2002-06-25 | 2002-06-25 | Solid-phase low-temperature thermal decomposition and synthesis process of preparing crystalline and amorphous superfine zine oxide powder |
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| CN1388066A true CN1388066A (en) | 2003-01-01 |
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| CN 02132486 Pending CN1388066A (en) | 2002-06-25 | 2002-06-25 | Solid-phase low-temperature thermal decomposition and synthesis process of preparing crystalline and amorphous superfine zine oxide powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CZ296748B6 (en) * | 2004-03-10 | 2006-06-14 | Univerzita Palackého | Process for preparing amorphous ferric oxide |
| CN101743340B (en) * | 2007-07-17 | 2012-02-29 | 默克专利有限公司 | Organometallic zinc compound for preparing zinc oxide films |
-
2002
- 2002-06-25 CN CN 02132486 patent/CN1388066A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CZ296748B6 (en) * | 2004-03-10 | 2006-06-14 | Univerzita Palackého | Process for preparing amorphous ferric oxide |
| CN101743340B (en) * | 2007-07-17 | 2012-02-29 | 默克专利有限公司 | Organometallic zinc compound for preparing zinc oxide films |
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