CN100402161C - Method for preparing nano-film on ceramic glazed tiles and nano-film coating machine - Google Patents
Method for preparing nano-film on ceramic glazed tiles and nano-film coating machine Download PDFInfo
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- 239000002120 nanofilm Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000009501 film coating Methods 0.000 title claims abstract description 15
- 238000007654 immersion Methods 0.000 claims abstract description 19
- 238000007598 dipping method Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims description 17
- 239000010408 film Substances 0.000 claims description 13
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- 239000010409 thin film Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 abstract description 21
- 239000011248 coating agent Substances 0.000 abstract description 17
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000011449 brick Substances 0.000 abstract description 2
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 230000000844 anti-bacterial effect Effects 0.000 description 5
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- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- -1 Polypropylene Polymers 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- CUJRVFIICFDLGR-UHFFFAOYSA-N acetylacetonate Chemical compound CC(=O)[CH-]C(C)=O CUJRVFIICFDLGR-UHFFFAOYSA-N 0.000 description 2
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
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- 229920002379 silicone rubber Polymers 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 1
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- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及一种在陶瓷釉面砖上制备纳米薄膜的方法及纳米薄膜镀膜机，属于陶瓷釉面砖技术领域，制备纳米薄膜的方法是将陶瓷釉面砖附设在溶胶浸池壁上，向溶胶浸池中充入溶胶，然后再从溶胶浸池底部将溶胶放出，陶瓷釉面砖表面即附上一层溶胶膜，将附有溶胶膜的陶瓷釉面砖进行干燥后处理，即可使陶瓷釉面砖上附上一层纳米薄膜。纳米薄膜镀膜机有一用边框和密封门构成的溶胶浸池，密封门内侧面上设有陶瓷釉面砖固定件，边框的下边框上设有溶胶进出口。本发明在陶瓷釉面砖上制备纳米薄膜的方法，科学合理，简单易行；配用的纳米薄膜镀膜机结构简单，使用方便，操作容易，利于获得高质量的均匀镀膜。本发明方法也可以在平板玻璃上进行单面镀膜。
The invention relates to a method for preparing a nano-film on ceramic glazed tiles and a nano-film coating machine, belonging to the technical field of ceramic glazed tiles. The method for preparing a nano-film is to attach ceramic glazed tiles to the wall of a sol immersion tank, and pour into the sol immersion tank The sol is filled in the sol, and then the sol is released from the bottom of the sol dipping tank, and a layer of sol film is attached to the surface of the ceramic glazed tile. After drying the ceramic glazed tile with the sol film, the ceramic glazed tile can be attached. A layer of nano film. The nano film coating machine has a sol immersion tank composed of a frame and a sealed door. The inner side of the sealed door is provided with a ceramic glazed brick fixing piece, and the lower frame of the frame is provided with a sol inlet and outlet. The method for preparing nano-film on ceramic glazed tiles of the present invention is scientific and reasonable, simple and easy to implement; the nano-film coating machine used is simple in structure, easy to use and easy to operate, and is beneficial to obtain high-quality uniform coating. The method of the present invention can also be used for single-sided coating on flat glass.
Description
技术领域 technical field
本发明涉及一种在陶瓷釉面砖上制备纳米薄膜的方法及纳米薄膜镀膜机，属于陶瓷釉面砖技术领域。The invention relates to a method for preparing a nano-film on ceramic glazed tiles and a nano-film coating machine, belonging to the technical field of ceramic glazed tiles.
背景技术 Background technique
陶瓷釉面砖包括陶瓷内墙砖、外墙砖及陶瓷地砖等，是建筑上常用的传统装饰装修材料，例如陶瓷内墙砖主要用于厨房及卫生间的墙面，能保持室内美观和整洁，容易清洗。如果在陶瓷表面上镀一层纳米薄膜，赋予传统陶瓷新的功能，则能大大增加其使用价值，如进行TiO2镀膜，可以起到抗菌、自洁、净化室内空气的作用。目前，在其它基材基体上镀敷TiO2纳米薄膜采用的是溶胶凝胶法，使用浸渍提拉技术，是将清洁的基板浸入溶胶中，然后以一定的速度将基板垂直提起至脱离液面，溶胶在基板表面形成凝胶薄膜，经过干燥及热处理得到相应的功能膜，适宜双面镀膜。但是在实践应用中发现在陶瓷砖表面镀膜存在如下问题：(1)由于陶瓷侧面及背面具有一定吸水率，不能与溶胶接触，因此无法采用通常的浸渍提拉溶胶凝胶法进行大面积镀膜；(2)将溶胶采用涂刷、喷涂、滚涂、刮涂、印刷等镀膜方法时，镀膜厚度的均匀性不好掌握，由于TiO2的折射率很高，厚度的微小变化也会出现异常干涉色，致使镀膜质量不易保证。Ceramic glazed tiles include ceramic interior wall tiles, exterior wall tiles and ceramic floor tiles, etc., which are traditional decoration materials commonly used in buildings. For example, ceramic interior wall tiles are mainly used for the walls of kitchens and bathrooms, which can keep the interior beautiful and tidy, and are easy to cleaning. If a layer of nano-film is coated on the surface of ceramics to endow traditional ceramics with new functions, its use value can be greatly increased. For example, TiO 2 coating can play the role of antibacterial, self-cleaning, and indoor air purification. At present, the sol-gel method is used to plate TiO2 nano-films on other substrates. Using the dipping and pulling technology, the clean substrate is immersed in the sol, and then the substrate is lifted vertically to the liquid level at a certain speed. , The sol forms a gel film on the surface of the substrate, and the corresponding functional film is obtained after drying and heat treatment, which is suitable for double-sided coating. However, in practical application, it is found that there are the following problems in the coating on the surface of ceramic tiles: (1) because the side and back of the ceramic have a certain water absorption rate and cannot be in contact with the sol, it is impossible to use the usual dipping and pulling sol-gel method for large-area coating; (2) When the sol is coated by brushing, spraying, rolling, scraping, printing and other coating methods, the uniformity of the coating thickness is not easy to grasp. Because the refractive index of TiO 2 is very high, there will be abnormal interference in small changes in the thickness Color, resulting in coating quality is not easy to guarantee.
发明内容 Contents of the invention
本发明的目的在于提供一种在陶瓷釉面砖上制备纳米薄膜的方法，科学合理，简单易行；同时提供配用的纳米薄膜镀膜机，结构简单，使用方便，操作容易。The purpose of the present invention is to provide a method for preparing nano-film on ceramic glazed tiles, which is scientific, reasonable, simple and easy to implement; meanwhile, it provides a matching nano-film coating machine, which is simple in structure, convenient to use and easy to operate.
本发明所述的在陶瓷釉面砖上制备纳米薄膜的方法，是将陶瓷釉面砖附设在溶胶浸池壁上，向溶胶浸池中充入溶胶，然后再从溶胶浸池底部将溶胶放出，陶瓷釉面砖表面即附上一层溶胶膜，将附有溶胶膜的陶瓷釉面砖进行干燥、热处理等后处理，即可使陶瓷釉面砖上附上一层纳米薄膜。The method for preparing nano-film on ceramic glazed tiles according to the present invention is to attach ceramic glazed tiles to the wall of the sol immersion tank, fill the sol immersion tank with sol, and then release the sol from the bottom of the sol immersion tank. A layer of sol film is attached to the surface of the glazed tile, and a layer of nano film can be attached to the ceramic glazed tile after drying and heat treatment of the ceramic glazed tile with the sol film.
可以将陶瓷釉面砖附设在溶胶浸池的密封门内侧，简单易行。Ceramic glazed tiles can be attached to the inner side of the sealed door of the sol dipping tank, which is simple and easy.
溶胶凝胶法的浸渍提拉过程是液体静止、基板向上运动，形成双面镀膜，与溶胶凝胶法的浸渍提拉法相比，本发明方法采用了逆向思维的方式，固定陶瓷釉面砖不动，使溶胶液体液面平稳地向下流动，形成镀膜。通过控制溶胶的浓度或粘度及液体的流动速度，可以获得不同膜厚的均匀薄膜，也可以通过多次镀膜获得较厚的薄膜，解决了陶瓷釉面砖大面积镀膜的问题。The dipping and pulling process of the sol-gel method is that the liquid is still and the substrate moves upward to form a double-sided coating. Compared with the dipping and pulling method of the sol-gel method, the method of the present invention adopts a reverse thinking method to fix the ceramic glazed tiles. , so that the liquid surface of the sol liquid flows down smoothly to form a coating. By controlling the concentration or viscosity of the sol and the flow rate of the liquid, uniform films with different film thicknesses can be obtained, and thicker films can also be obtained through multiple coatings, which solves the problem of large-area coatings on ceramic glazed tiles.
配合上述方法，所用纳米薄膜镀膜机，有一用边框和密封门构成的溶胶浸池，密封门内侧面上设有陶瓷釉面砖固定件，以便将陶瓷釉面砖固定在上面，如插槽、托板和别钩等，在边框的下边框上设溶胶进出口。溶胶进出口也可以是分别设置，溶胶进口可以设在上部或顶部。In conjunction with the above method, the nano-film coating machine used has a sol immersion tank composed of a frame and a sealed door, and ceramic glazed tile fixing parts are arranged on the inner side of the sealed door to fix the ceramic glazed tiles on it, such as slots, supporting plates And do not hook etc., establish sol import and export on the lower frame of frame. The inlet and outlet of the sol can also be set separately, and the inlet of the sol can be set on the upper part or the top.
其中的密封门可以是游离的门，也可以是固定在边框上的开关门，由折页轴连接等。The airtight door can be a free door, or a switch door fixed on the frame, connected by hinge shafts, etc.
将釉面砖固定到密封门内侧面上，关上门，釉面砖构成了一部分溶胶浸池壁，这时，从溶胶进出口向溶胶浸池内加入溶胶，至液面与釉面砖的上边缘齐平，当液面稳定后，再从溶胶进出口放掉溶胶，溶胶浸池内的液面稳定平稳下降，在釉面砖上附上一层均匀的溶胶膜，经过烘干等后处理即可使陶瓷釉面砖上附上一层纳米薄膜。结构简单，使用方便，操作容易。Fix the glazed tiles on the inner side of the sealed door, close the door, and the glazed tiles constitute a part of the wall of the sol immersion pool. At this time, add sol from the sol inlet and outlet to the sol immersion pool until the liquid level is flush with the upper edge of the glazed tiles. When the liquid level is stable, release the sol from the sol inlet and outlet, and the liquid level in the sol dipping tank will drop steadily, and a uniform layer of sol film will be attached on the glazed tiles. After drying and other post-processing, the ceramic glazed tiles Attach a layer of nano film on it. The structure is simple, the use is convenient, and the operation is easy.
在边框的上边框上设通气口，保证溶胶的加入、排出畅通，防止产生气泡，促进均匀镀膜。也可以不设上边框，上部敞口即可。Vents are provided on the upper frame of the frame to ensure the smooth addition and discharge of the sol, prevent the generation of air bubbles, and promote uniform coating. It is also possible not to set the upper frame, and the upper part is open.
在溶胶浸池边框与密封门内侧之间加设密封圈，增强密封性能，密封圈可以设在边框上，也可以设在密封门内侧，保证边框与密封门间的良好密封即可。密封圈可用硅橡胶或耐酸耐温的橡胶制作，Add a sealing ring between the frame of the sol dipping tank and the inside of the sealing door to enhance the sealing performance. The sealing ring can be set on the frame or inside the sealing door to ensure a good seal between the frame and the sealing door. The sealing ring can be made of silicon rubber or acid-resistant and temperature-resistant rubber.
将密封门设计有相对的两个，甚至可以设计为相对的两对，提高镀膜效率。There are two opposite airtight doors, or even two opposite pairs, to improve the coating efficiency.
在溶胶浸池的底部连接液位计，便于溶胶液位观察，方便准确操作。A liquid level gauge is connected to the bottom of the sol immersion tank to facilitate the observation of the sol liquid level and convenient and accurate operation.
本发明中，溶胶可以是行业通用的镀膜溶胶，也可以是新研制的镀膜溶胶。加入溶胶操作可以附设储液罐，采取压力注入方法。溶胶流出时的速度通过进出口的口径大小控制。镀膜后的干燥、热处理等后续处理同其它镀膜方法一样。与现有技术相同的技术内容不再赘述。In the present invention, the sol can be a common coating sol in the industry, or a newly developed coating sol. The operation of adding sol can be equipped with a liquid storage tank, and the method of pressure injection can be adopted. The speed when the sol flows out is controlled by the diameter of the inlet and outlet. Subsequent treatments such as drying and heat treatment after coating are the same as other coating methods. The same technical content as the prior art will not be repeated.
以300×450mm的超平陶瓷釉面砖为例试验，成功地在陶瓷釉面砖表面上镀出了表面光亮、无干涉色的纳米TiO2抗菌薄膜。Taking the 300×450mm ultra-flat ceramic glazed tile as an example test, a nano-TiO 2 antibacterial film with bright surface and no interference color was successfully plated on the surface of the ceramic glazed tile.
本发明在陶瓷釉面砖上制备纳米薄膜的方法，科学合理，简单易行；配用的纳米薄膜镀膜机结构简单，使用方便，操作容易，利于获得高质量的均匀镀膜。本发明方法也可以在平板玻璃上进行单面镀膜。The method for preparing nano film on ceramic glazed tiles of the present invention is scientific, reasonable, simple and easy to implement; the matched nano film coating machine is simple in structure, easy to use and easy to operate, and is beneficial to obtain high-quality uniform coating film. The method of the present invention can also be used for single-sided coating on flat glass.
附图说明 Description of drawings
图1、本发明纳米薄膜镀膜机一实施例结构示意图。Fig. 1, the structure diagram of an embodiment of the nano film coating machine of the present invention.
图中：1、通气口 2、聚丙烯上边框 3、硅橡胶密封圈 4、密封门 5、聚丙烯下边框 6、溶胶进出口 7、溶胶浸池 8、液位计。In the figure: 1. Air vent 2. Polypropylene upper frame 3. Silicone rubber sealing ring 4. Sealed door 5. Polypropylene lower frame 6. Sol inlet and outlet 7. Sol immersion tank 8. Liquid level gauge.
具体实施方式 Detailed ways
结合上述实施例附图对本发明作进一步说明。The present invention will be further described in conjunction with the accompanying drawings of the above-mentioned embodiments.
如图所示，本发明所述的纳米薄膜镀膜机，有一用边框2、5等和密封门4构成的溶胶浸池7，密封门有相对的一对，用折页固定在边框上，密封门4内侧面上设有陶瓷釉面砖固定插槽，边框的下边框5上设有溶胶进出口6，边框的上边框2上设有通气口1，边框上固定有密封圈3，溶胶浸池7的底部连接有简易的透明管液位计8。As shown in the figure, the nano film coating machine of the present invention has a sol immersion tank 7 composed of frames 2, 5, etc. and a sealed door 4, and the sealed door has a pair opposite, fixed on the frame with a hinge, sealed The inner side of the door 4 is provided with ceramic glazed brick fixing slots, the lower frame 5 of the frame is provided with a sol inlet and outlet 6, the upper frame 2 of the frame is provided with a vent 1, and the frame is fixed with a sealing ring 3, and the sol dipping tank The bottom of 7 is connected with simple and easy transparent tube liquid level gauge 8.
操作过程1：Operation process 1:
采用钛酸丁酯为原料，乙醇EtOH为溶剂，按Ti(OBu)4∶EtOH∶H2O∶HNO3∶酰丙酮AcAc＝1∶18∶2∶0.2∶0.5的摩尔配比制备稳定的溶胶，其中，酰丙酮AcAc为抑制剂，可延缓钛酸丁酯的强烈水解。把300×450mm陶瓷釉面砖清洗干净、烘干后安装在密封门上，将门关上压紧。溶胶通过进出口进入溶胶浸池，当液位与釉面砖上边缘齐平时，停止加入溶胶，液面稳定后，通过溶胶进出口以一定速度排出。打开密封门，取下釉面砖，在80℃温度下烘干2小时，在马弗炉中以3-5℃的升温速度升温至500℃，保温1小时，然后自然降温至室温，即获得锐钛矿型纳米TiO2薄膜，得到表面光亮、无干涉色的纳米TiO2抗菌薄膜抗菌釉面砖。Using butyl titanate as raw material and ethanol EtOH as solvent, a stable sol was prepared according to the molar ratio of Ti(OBu) 4 : EtOH: H 2 O : HNO 3 : Acylacetone AcAc=1:18:2:0.2:0.5 , among them, acetylacetonate AcAc is an inhibitor, which can delay the strong hydrolysis of butyl titanate. Clean and dry the 300×450mm ceramic glazed tiles and install them on the airtight door, close the door and press it tightly. The sol enters the sol immersion tank through the inlet and outlet. When the liquid level is equal to the upper edge of the glazed tile, stop adding the sol. After the liquid level is stable, it is discharged through the sol inlet and outlet at a certain speed. Open the airtight door, remove the glazed tiles, dry them at 80°C for 2 hours, heat them up to 500°C at a rate of 3-5°C in a muffle furnace, keep them warm for 1 hour, and then cool them down to room temperature naturally to obtain sharpness. Titanium-type nano- TiO2 thin film, to obtain nano- TiO2 antibacterial film antibacterial glazed tiles with bright surface and no interference color.
操作过程2：Operation process 2:
采用四氯化钛为原料，无水乙醇为溶剂，按1∶40的体积比，将四氯化钛在搅拌条件下逐滴加入到乙醇中，密闭陈化一周后得到稳定的溶胶。把300×450mm陶瓷釉面砖清洗干净、烘干，安装在密封门上，将门关上压紧。溶胶通过进出口进入溶胶浸池，达到设定高度后停止加溶胶，液面稳定后，通过溶胶进出口以一定速度放出。打开密封门，取下釉面砖，在80℃温度下烘干，在500℃温度下热处理1小时，得到表面光亮、无干涉色的纳米TiO2抗菌薄膜釉面砖。Titanium tetrachloride is used as raw material, absolute ethanol is used as solvent, and titanium tetrachloride is added dropwise to ethanol with stirring at a volume ratio of 1:40, and a stable sol is obtained after airtight aging for one week. Clean and dry the 300×450mm ceramic glazed tiles, install them on the airtight door, close the door and press it tightly. The sol enters the sol immersion tank through the inlet and outlet, stops adding sol after reaching the set height, and releases the sol at a certain speed through the inlet and outlet after the liquid level is stable. Open the sealed door, remove the glazed tiles, dry them at 80°C, and heat them at 500°C for 1 hour to obtain glazed tiles with nano- TiO2 antibacterial film with bright surface and no interference color.
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| CNB2005101046041A CN100402161C (en) | 2005-12-23 | 2005-12-23 | Method for preparing nano-film on ceramic glazed tiles and nano-film coating machine |
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| CNB2005101046041A CN100402161C (en) | 2005-12-23 | 2005-12-23 | Method for preparing nano-film on ceramic glazed tiles and nano-film coating machine |
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| CN1986080A CN1986080A (en) | 2007-06-27 |
| CN100402161C true CN100402161C (en) | 2008-07-16 |
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| CN103643225B (en) * | 2013-11-27 | 2015-11-11 | 中国科学院上海硅酸盐研究所 | A kind of chemical bath legal system is for the method for large size cadmium sulphide membrane |
| CN105457844B (en) * | 2015-12-24 | 2019-01-11 | 中国科学院宁波材料技术与工程研究所 | A kind of device of liquid level sedimentation plated film |
| CN113860921A (en) * | 2021-09-24 | 2021-12-31 | 腾盛科技创新服务(揭阳)有限公司 | Ceramic material with excellent antibacterial property and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4779562A (en) * | 1986-03-19 | 1988-10-25 | Fujitsu Limited | Apparatus for depositing mono-molecular layer |
| CN2504001Y (en) * | 2001-09-22 | 2002-08-07 | 洛阳玻璃股份有限公司 | Sol-gel coating equipment |
| CN1436590A (en) * | 2002-02-06 | 2003-08-20 | 云南大学 | Photocatalytic superhydrophilic composite titanium dioxide and tin dioxide film |
| JP2005161268A (en) * | 2003-12-05 | 2005-06-23 | Fuji Xerox Co Ltd | Coating method for resin dispersion liquid, coating device for resin dispersion liquid and manufacturing method for fixing belt |
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2005
- 2005-12-23 CN CNB2005101046041A patent/CN100402161C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4779562A (en) * | 1986-03-19 | 1988-10-25 | Fujitsu Limited | Apparatus for depositing mono-molecular layer |
| CN2504001Y (en) * | 2001-09-22 | 2002-08-07 | 洛阳玻璃股份有限公司 | Sol-gel coating equipment |
| CN1436590A (en) * | 2002-02-06 | 2003-08-20 | 云南大学 | Photocatalytic superhydrophilic composite titanium dioxide and tin dioxide film |
| JP2005161268A (en) * | 2003-12-05 | 2005-06-23 | Fuji Xerox Co Ltd | Coating method for resin dispersion liquid, coating device for resin dispersion liquid and manufacturing method for fixing belt |
Non-Patent Citations (2)
| Title |
|---|
| 溶胶－凝胶法TiO*光催化膜的制备与研究. 李霞，张梅梅.山东轻工业学院学报，第15卷第4期. 2001 |
| 溶胶－凝胶法TiO*光催化膜的制备与研究. 李霞，张梅梅.山东轻工业学院学报，第15卷第4期. 2001 * |
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| CN1986080A (en) | 2007-06-27 |
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