CN100404142C - Ultrasonic spray pyrolysis nozzle - Google Patents
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- CN100404142C CN100404142C CNB2006100148907A CN200610014890A CN100404142C CN 100404142 C CN100404142 C CN 100404142C CN B2006100148907 A CNB2006100148907 A CN B2006100148907A CN 200610014890 A CN200610014890 A CN 200610014890A CN 100404142 C CN100404142 C CN 100404142C
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- 238000003764 ultrasonic spray pyrolysis Methods 0.000 title abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 32
- 239000003595 mist Substances 0.000 claims abstract description 20
- 238000005507 spraying Methods 0.000 claims description 4
- 230000006698 induction Effects 0.000 claims 2
- 239000010408 film Substances 0.000 abstract description 23
- 239000010409 thin film Substances 0.000 abstract description 14
- 238000002360 preparation method Methods 0.000 abstract description 7
- 239000000758 substrate Substances 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000009172 bursting Effects 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 9
- 239000012159 carrier gas Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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Abstract
本发明涉及一种超声喷雾热分解喷头，特别是一种导雾管上半部分加有储液瓶、喷嘴直径由大到小有一个渐变的过程的超声喷雾热分解喷头，可以广泛地应用于薄膜材料、特别是透明导电氧化物薄膜的制备方面。现有技术存在衬底炸裂、喷嘴堵塞导致根本无法成膜的缺陷；为此，本发明提出了一种超声喷雾热分解喷头新的技术方案，其特点在于：喷嘴上增加了一个储液瓶，储液瓶包含有进气导管和排液导管，进气导管与水平面的夹角θ为10-350°，排液管口设置一个阀门。本发明的有益效果是：通过储液瓶和调节进气口的倾斜角度使得大半径雾滴和液态物质不再影响成膜，通过改变喷嘴形状可有效的获得大面积、均匀的薄膜。The invention relates to an ultrasonic spray pyrolysis nozzle, in particular to an ultrasonic spray pyrolysis nozzle with a liquid storage bottle added to the upper half of the mist guide tube and a gradual change in nozzle diameter from large to small, which can be widely used in Preparation of thin film materials, especially transparent conductive oxide thin films. In the existing technology, there are defects such as substrate bursting and nozzle clogging, which make it impossible to form a film at all; for this reason, the present invention proposes a new technical solution for an ultrasonic spray pyrolysis nozzle, which is characterized in that a liquid storage bottle is added to the nozzle, The liquid storage bottle includes an air inlet conduit and a liquid discharge conduit, the angle θ between the air inlet conduit and the horizontal plane is 10-350°, and a valve is arranged at the outlet of the liquid outlet. The beneficial effects of the present invention are: through the liquid storage bottle and the adjustment of the inclination angle of the air inlet, the large-radius mist and liquid substances no longer affect the film formation, and the large-area and uniform film can be effectively obtained by changing the shape of the nozzle.
Description
技术领域 technical field
本发明涉及一种超声喷雾热分解喷头，特别是一种导雾管上半部分加有储液瓶、喷嘴直径由大到小有一个渐变的过程的超声喷雾热分解喷头，可以广泛地应用于薄膜材料、特别是透明导电氧化物薄膜的制备方面，属于薄膜材料沉积技术领域。The invention relates to an ultrasonic spray pyrolysis nozzle, in particular to an ultrasonic spray pyrolysis nozzle with a liquid storage bottle added to the upper half of the mist guide tube and a gradual change in nozzle diameter from large to small, which can be widely used in The invention relates to the preparation of thin film materials, especially transparent conductive oxide thin films, and belongs to the technical field of thin film material deposition.
背景技术 Background technique
随着薄膜材料和薄膜器件日益广泛的应用，薄膜的制备显得越来越重要。超声雾化热分解法已成为一种常用的薄膜制备技术，超声喷雾热分解工艺是将低分子有机盐的水溶液进行雾化，并由载气输送至高温衬底，使其发生热分解而生成薄膜。其原料价格低廉，无毒无害，反应物容易处理；超声喷雾热解对环境要求很低，无需真空，沉积温度也不高(在420℃左右)，工艺控制十分简单，其成本远远低于其它成膜方法；此外，用超声喷雾热分解法制备薄膜，容易实现掺杂，特别是用于多元薄膜的制备以及对薄膜进行掺杂；还适用于大面积生长，并且可生长出与其它方法相媲美的高质量薄膜等优点而倍受研究者的青睐。With the increasingly wide application of thin film materials and thin film devices, the preparation of thin films is becoming more and more important. Ultrasonic atomization pyrolysis has become a commonly used thin film preparation technology. The ultrasonic spray pyrolysis process is to atomize the aqueous solution of low molecular organic salt, and transport it to the high-temperature substrate by the carrier gas, so that it can be thermally decomposed to form film. Its raw materials are cheap, non-toxic and harmless, and the reactants are easy to handle; ultrasonic spray pyrolysis has very low environmental requirements, no vacuum is needed, and the deposition temperature is not high (about 420 ° C), the process control is very simple, and its cost is far lower In addition, the preparation of thin films by ultrasonic spray pyrolysis is easy to achieve doping, especially for the preparation of multi-component thin films and the doping of thin films; it is also suitable for large-area growth, and can be grown with other The advantages of high-quality thin films comparable to other methods are favored by researchers.
通常，对于超声喷雾热分解这种技术，影响薄膜质量主要有两个方面：Generally, for the technology of ultrasonic spray pyrolysis, there are two main aspects that affect the quality of the film:
1.雾化器产生雾滴粒子的大小和均匀程度。这主要由雾化器的性能决定。1. The size and uniformity of the droplet particles produced by the atomizer. This is mainly determined by the performance of the atomizer.
2.喷头：其中喷头是获得高质量薄膜的关键。前驱溶液经雾化器作用后形成雾滴，雾滴在载气的携带过程中相互之间的碰撞以及与导管壁的碰撞使得雾滴半径不断增大，在导管壁上有部分半径较大的液滴形成；由于导管外壁的温度要低于雾滴的温度，这使得接近导管壁的雾滴在壁上凝结。这些大半径雾滴逐渐形成液滴。另外，要获取大面积的高质量薄膜，必须使雾气的喷射范围尽可能大，而且均匀。工业上通常采用高压来解决这个问题。但雾气与液体和气体不同，是介于液体和气体之间一种物质状态，它不像液体或气体那样可以承受极大的压强而仍然保持原来的状态，雾气在压强稍大时就开始液化。2. Nozzle: Among them, the nozzle is the key to obtain high-quality film. The precursor solution forms mist droplets after the atomizer, and the collisions between the mist droplets and the collision with the conduit wall during the carrying process of the carrier gas make the radius of the mist droplets continuously increase, and there are some larger radius areas on the conduit wall. Droplet formation; since the temperature of the outer wall of the conduit is lower than that of the mist droplets, this causes the droplets close to the conduit wall to condense on the wall. These large-radius droplets gradually form into droplets. In addition, in order to obtain a large-area high-quality film, the spraying range of the mist must be as large as possible and uniform. The industry usually adopts high pressure to solve this problem. However, mist is different from liquid and gas. It is a state of matter between liquid and gas. Unlike liquid or gas, it can withstand great pressure and still maintain its original state. Mist begins to liquefy when the pressure is slightly higher. .
上面两种情况下的液化现象产生的液滴，一方面沿着喷头直接滴至衬底，严重影响薄膜结构和表面形貌(如附图1)，甚至使衬底炸裂导致根本无法成膜；另一方面，在较高温的喷嘴处蒸发结晶，导致喷嘴堵塞，使得实验无法进行。The droplets produced by the liquefaction phenomenon in the above two cases, on the one hand, drop directly to the substrate along the nozzle, which seriously affects the film structure and surface morphology (as shown in Figure 1), and even causes the substrate to burst, making it impossible to form a film at all; On the other hand, evaporative crystallization at the higher temperature nozzles resulted in clogging of the nozzles, making the experiment impossible.
因此，本设计集中在改变喷头结构：上半部分的结构称之为储液瓶，由于储液瓶可以消除液态物质沿喷头流至衬底以及这种喷嘴可以减小雾气在喷嘴处的液化，从理论上可以消除大半径雾滴和液态物质对实验的影响，同时可以增大薄膜的生长面积和改善薄膜的均匀性；下半部分是由导雾管到喷口处(喷嘴)，其内径由大到小，再由小到大有一个渐变的过程，此设计部分是让雾气尽可能散开，形成大面积均匀的薄膜。Therefore, this design focuses on changing the structure of the nozzle: the structure of the upper part is called a liquid storage bottle, because the liquid storage bottle can eliminate the flow of liquid substances along the nozzle to the substrate and this nozzle can reduce the liquefaction of the mist at the nozzle. It can theoretically eliminate the influence of large-radius droplets and liquid substances on the experiment, and at the same time increase the growth area of the film and improve the uniformity of the film; the lower part is from the mist guide to the nozzle (nozzle), and its inner diameter is There is a gradual process from large to small, and then from small to large. Part of this design is to spread the mist as much as possible to form a large-area uniform film.
发明内容 Contents of the invention
现有技术存在衬底炸裂、喷嘴堵塞导致根本无法成膜的缺陷；本发明的目的，是克服现有技术的缺陷，为此，本发明公开提出一种可以有效地抑制雾气的凝结和液化、消除液滴对薄膜生长所导致的严重影响、使得超声喷雾热分解法成为更加实用和有效的一种薄膜制备方法的喷头设计方案，本发明具体的技术方案是：The existing technology has the defects of substrate bursting and nozzle clogging, which lead to the inability to form a film at all; the purpose of the present invention is to overcome the defects of the prior art. Therefore, the present invention discloses a method that can effectively inhibit the condensation and liquefaction of mist Eliminate the serious impact of droplets on film growth, making the ultrasonic spray pyrolysis method a more practical and effective nozzle design for a film preparation method. The specific technical solutions of the present invention are:
这种超声喷雾热分解喷头，它包括一个喷嘴和储液瓶，其特点在于：喷嘴上增加了一个储液瓶，储液瓶包含有进气导管和排液导管，进气导管与水平面的夹角θ为10-350°，排液管口设置一个阀门。This ultrasonic spray pyrolysis nozzle includes a nozzle and a liquid storage bottle, and its characteristic is that a liquid storage bottle is added to the nozzle, and the liquid storage bottle includes an air inlet conduit and a liquid discharge conduit, and the clamp between the air inlet conduit and the horizontal plane The angle θ is 10-350°, and a valve is arranged at the outlet of the discharge pipe.
本发明的有益效果是：通过储液瓶和调节进气口的倾斜角度使得大半径雾滴和液态物质不再影响成膜，通过改变喷嘴形状可有效的获得大面积、均匀的薄膜。The beneficial effects of the present invention are: through the liquid storage bottle and the adjustment of the inclination angle of the air inlet, the large-radius mist and liquid substances no longer affect the film formation, and the large-area and uniform film can be effectively obtained by changing the shape of the nozzle.
附图说明 Description of drawings
图1：用普通喷头制备薄膜的表面形貌Figure 1: The surface morphology of the film prepared with a common nozzle
图2：用储液瓶和改变喷嘴形状的喷头制备薄膜的表面形貌Figure 2: Surface topography of thin films prepared with a reservoir bottle and a spray head that changes the shape of the nozzle
图3：普通喷头示意图Figure 3: Schematic diagram of a common nozzle
图4：本发明喷头的结构示意图Figure 4: Schematic diagram of the structure of the nozzle of the present invention
图5：本发明喷头的喷嘴结构示意图Figure 5: Schematic diagram of the nozzle structure of the nozzle of the present invention
图中：1.储液瓶 2.进气导管 3.排液导管 4.阀门 5.喷嘴 6.导雾管 7.喷口直径 8.喷口 α.夹角(导雾管向喷口过度的角度变化) d.导雾管向喷口过度处最小直径In the figure: 1.
具体实施方式 Detailed ways
下面结合附图对本发明的具体实施方式作进一步说明：The specific embodiment of the present invention will be further described below in conjunction with accompanying drawing:
这种超声喷雾热分解喷头，它包括一个喷嘴和储液瓶，其特征在于：喷嘴5上增加了一个储液瓶1，储液瓶包含有进气导管2和排液导管3，进气导管与水平面的夹角θ为10-350°，排液管口设置一个阀门4。This ultrasonic spray pyrolysis nozzle includes a nozzle and a liquid storage bottle, and is characterized in that: a
导雾管6逐渐变细、再逐渐变粗成喷口，变化角度α在10-90°内，其最细处直径d范围在0.05-100mm，而最下端喷口8的直径7是1-500mm。The mist guide pipe 6 gradually becomes thinner and thicker to become a spout, the angle of change α is within 10-90°, the diameter d of the thinnest part is in the range of 0.05-100mm, and the diameter 7 of the bottom spout 8 is 1-500mm.
储液瓶可以是椭圆形、圆形或者顶部变化光滑的其它形状。The reservoir bottle can be oval, round, or other shape with a smooth top change.
这种喷头的设计方法与传统的不同。传统喷头一般如图3，我们的喷头在设计理念上有很大的突破，通过采用储液瓶和改变喷嘴的形状可以有效地改善薄膜的均匀性和质量，同时也可增大成膜面积。The design method of this nozzle is different from the traditional one. The traditional nozzle is generally shown in Figure 3. Our nozzle has a great breakthrough in the design concept. By using the liquid storage bottle and changing the shape of the nozzle, the uniformity and quality of the film can be effectively improved, and the film forming area can also be increased.
实施例Example
采用超声喷雾热分解法，用带有储液瓶和改变喷嘴形状的喷头制备ZnO薄膜，以0.4sccm的载气流量、1.5mm孔径的喷嘴，调整衬底与喷头间的距离，在普通玻璃衬底上可获得面积为25cm2的均匀薄膜，薄膜表面形貌较好(见图2)。Ultrasonic spray pyrolysis method was used to prepare ZnO film with a nozzle with a liquid storage bottle and a nozzle shape changed. With a carrier gas flow rate of 0.4 sccm and a nozzle with a diameter of 1.5 mm, the distance between the substrate and the nozzle was adjusted. A uniform film with an area of 25 cm 2 can be obtained on the bottom, and the surface morphology of the film is good (see Figure 2).
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| CNB2006100148907A CN100404142C (en) | 2006-07-24 | 2006-07-24 | Ultrasonic spray pyrolysis nozzle |
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| CNB2006100148907A CN100404142C (en) | 2006-07-24 | 2006-07-24 | Ultrasonic spray pyrolysis nozzle |
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| CN100404142C true CN100404142C (en) | 2008-07-23 |
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| CN105057154B (en) * | 2015-08-14 | 2017-06-16 | 重庆理工大学 | A kind of free-standing multi-source copolymerization Jiao ultrasonic spray pyrolysis spraying reaction chamber |
| CN109706433B (en) * | 2018-12-04 | 2021-06-29 | 南京工业大学 | A kind of ultrasonic spray deposition thin film device and method |
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| CN1040932A (en) * | 1988-09-08 | 1990-04-04 | 清华大学 | Preparation of Ultrafine Powder by Ultrasonic Atomization |
| CN1083908A (en) * | 1992-09-07 | 1994-03-16 | 西门子公司 | water-steam separator |
| CN1250823A (en) * | 1998-10-14 | 2000-04-19 | 中国科学院新疆物理研究所 | Atomizing thermolysis process for preparing film |
| CN1259405A (en) * | 1999-08-30 | 2000-07-12 | 上海交通大学 | Transparent conductive film and reflection reduction film spray coating equipment and method |
| JP2004267893A (en) * | 2003-03-07 | 2004-09-30 | Samco International Inc | Atomizer for forming ceramic thin film and thin film manufacturing method using the atomizer |
| CN1692987A (en) * | 2005-04-26 | 2005-11-09 | 南开大学 | Special nozzle for preparing transparent conductive film by ultrasonic rapid deposition method |
| CN1783433A (en) * | 2004-12-03 | 2006-06-07 | 中国科学院上海硅酸盐研究所 | Process for preparing nitrigen-aluminium co-blended hole zinc oxide thin film material |
| WO2006073171A1 (en) * | 2005-01-07 | 2006-07-13 | Kabushiki Kaisha Kobe Seiko Sho | Thermal spraying nozzle device and thermal spraying equipment |
-
2006
- 2006-07-24 CN CNB2006100148907A patent/CN100404142C/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1040932A (en) * | 1988-09-08 | 1990-04-04 | 清华大学 | Preparation of Ultrafine Powder by Ultrasonic Atomization |
| CN1083908A (en) * | 1992-09-07 | 1994-03-16 | 西门子公司 | water-steam separator |
| CN1250823A (en) * | 1998-10-14 | 2000-04-19 | 中国科学院新疆物理研究所 | Atomizing thermolysis process for preparing film |
| CN1259405A (en) * | 1999-08-30 | 2000-07-12 | 上海交通大学 | Transparent conductive film and reflection reduction film spray coating equipment and method |
| JP2004267893A (en) * | 2003-03-07 | 2004-09-30 | Samco International Inc | Atomizer for forming ceramic thin film and thin film manufacturing method using the atomizer |
| CN1783433A (en) * | 2004-12-03 | 2006-06-07 | 中国科学院上海硅酸盐研究所 | Process for preparing nitrigen-aluminium co-blended hole zinc oxide thin film material |
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