CN106977100A - The good frit for porcelain enamel with steel plate adherence - Google Patents
The good frit for porcelain enamel with steel plate adherence Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/06—Frit compositions, i.e. in a powdered or comminuted form containing halogen
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2207/00—Compositions specially applicable for the manufacture of vitreous enamels
- C03C2207/04—Compositions specially applicable for the manufacture of vitreous enamels for steel
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Abstract
本发明公开了一种与钢板密着性良好的搪瓷釉料，按重量百分比计，由以下组分构成：SiO2 50～65％、Al2O3 20～30％、B2O3 4～15％、Na2O 1.2～1.5％、K2O 1.3～1.6％、EuO2 1～10％、EuF3 2～5％。本发明在常规搪瓷釉料中加入EuO2和EuF3可以提高釉料的硬度以及与钢板的密着性，还能有效防止鱼鳞爆的发生。The invention discloses an enamel glaze with good adhesion to a steel plate, which is composed of the following components by weight percentage: SiO 2 50-65%, Al 2 O 3 20-30%, B 2 O 3 4-15% %, Na 2 O 1.2-1.5%, K 2 O 1.3-1.6%, EuO 2 1-10%, EuF 3 2-5%. In the present invention, adding EuO 2 and EuF 3 to the conventional enamel glaze can improve the hardness of the glaze and the adhesion with the steel plate, and can effectively prevent fish scale explosion.
Description
技术领域technical field
本发明涉及一种釉料，具体涉及一种与钢板密着性良好的搪瓷釉料。The invention relates to a glaze, in particular to an enamel glaze with good adhesion to a steel plate.
背景技术Background technique
搪瓷涂覆法是将玻璃料涂覆在钢板表面，经过高温焙烧，使搪瓷层与钢板基体发生交互作用，形成致密且与基体结合牢固的涂层工艺。搪瓷釉料与一般陶瓷釉料不同，其突出的特点是具有玻璃特性，搪瓷釉料不仅表面光滑美观，而且具有非常优良的耐蚀性、耐磨性、耐高温、不导电性等特殊性能。在金属基体表面烧制一层搪瓷层能够有效提高其使用寿命，并且可以解决不锈钢钢板不能同时具备的高温力学性能和抗高温腐蚀性能的矛盾。常规的搪瓷涂层都较薄，主要起保护基体金属的作用。The enamel coating method is to coat the glass frit on the surface of the steel plate and bake it at a high temperature to make the enamel layer interact with the steel plate substrate to form a dense coating process that is firmly combined with the substrate. Enamel glazes are different from general ceramic glazes in that they have glass properties. Enamel glazes not only have a smooth and beautiful surface, but also have very good corrosion resistance, wear resistance, high temperature resistance, and non-conductivity. Firing a layer of enamel on the surface of the metal substrate can effectively improve its service life, and can solve the contradiction between high-temperature mechanical properties and high-temperature corrosion resistance that stainless steel plates cannot have at the same time. Conventional enamel coatings are thin and mainly protect the base metal.
钢板与搪瓷是两种不同组成、不同结构、性能各异的材料，钢板与瓷釉结合不牢固，密着性差，容易脱落。硬度是表征材料软硬程度的一种性能，影响搪瓷层硬度的因素有很多，搪瓷层的组成和搪瓷层与金属基板的密着强度等。搪瓷层强度与密着性具有一定的相关性。Steel plate and enamel are two kinds of materials with different compositions, different structures, and different properties. The combination of steel plate and enamel is not firm, the adhesion is poor, and it is easy to fall off. Hardness is a property that characterizes the softness and hardness of the material. There are many factors that affect the hardness of the enamel layer, such as the composition of the enamel layer and the adhesion strength between the enamel layer and the metal substrate. There is a certain correlation between the strength of the enamel layer and the adhesion.
发明内容Contents of the invention
本发明要解决的技术问题是提供一种与钢板密着性良好的搪瓷釉料，该釉料硬度高，与不锈钢板的密着性好，还能有效防止鱼鳞爆的出现。The technical problem to be solved by the present invention is to provide an enamel glaze with good adhesion to the steel plate. The glaze has high hardness, good adhesion to the stainless steel plate, and can effectively prevent fish scale explosion.
本发明提供的技术方案是提供一种与钢板密着性良好的搪瓷釉料，按重量百分比计，由以下组分构成：The technical solution provided by the present invention is to provide a kind of enamel glaze with good adhesion to the steel plate, which is composed of the following components in terms of weight percentage:
SiO2 50～65％、Al2O3 20～30％、B2O3 4～15％、Na2O 1.2～1.5％、K2O 1.3～1.6％、EuO2 1～10％、EuF3 2～5％。SiO 2 50-65%, Al 2 O 3 20-30%, B 2 O 3 4-15%, Na 2 O 1.2-1.5%, K 2 O 1.3-1.6%, EuO 2 1-10%, EuF 3 2 to 5%.
SiO2是基体剂，能够形成搪瓷的骨架。Si-O键键力强，骨架完整，热稳定性、耐化学腐蚀性能好。SiO 2 is a matrix agent that can form the skeleton of enamel. The Si-O bond has strong bond strength, complete skeleton, good thermal stability and chemical corrosion resistance.
Al2O3使得搪瓷釉料在烧成温度下粘度增大，晶核形成顺利，晶体长大受阻，形成大量的微晶结构，提高搪瓷层的硬度。Al 2 O 3 makes the viscosity of the enamel glaze increase at the firing temperature, the crystal nucleus is formed smoothly, the crystal growth is hindered, a large number of microcrystalline structures are formed, and the hardness of the enamel layer is improved.
B2O3具有较小的表面张力和低的弹性模数，因而有利于促进熔体的流动性，提高搪瓷的光泽度、细腻度和弹性。还具有熔点低，发挥助溶剂的作用。B 2 O 3 has small surface tension and low elastic modulus, which is beneficial to promote the fluidity of the melt and improve the gloss, fineness and elasticity of enamel. It also has a low melting point and plays the role of a cosolvent.
K2O、Na2O为碱金属氧化物，是极强的助溶剂。K 2 O and Na 2 O are alkali metal oxides and are extremely strong co-solvents.
EuO2中的Eu4+会取代SiO2中的Si4+，而Eu4+4f电子层能量与其6S层电子能量相当，电子容易在这两个电子层间运动，使Eu-O键具有一定的柔韧性。因此，在搪瓷层冷却时，钢板基层释放出氢气时，Eu-O键可以伸长，晶体空间增加，可以给释放的氢气提供聚集空间，可有效防止鱼鳞爆。Eu 4+ in EuO 2 will replace Si 4+ in SiO 2 , and the energy of the Eu 4+ 4f electron shell is equivalent to its 6S shell electron energy, and the electrons are easy to move between these two electron shells, making the Eu-O bond have a certain of flexibility. Therefore, when the enamel layer is cooled and hydrogen gas is released from the base plate of the steel plate, the Eu-O bond can be elongated, and the crystal space increases, which can provide gathering space for the released hydrogen gas, which can effectively prevent fish scales from bursting.
EuO2在烧成时可提高搪瓷层粘度，晶核顺利形成，阻止晶体长大，形成大量的微晶结构。EuF3的加入可以在烧成冷却过程中使搪瓷层熔体粘度迅速增大，大大提高搪瓷层内微细晶体。两者同时加入，可以大大提高了搪瓷层的硬度。EuO 2 can increase the viscosity of the enamel layer during firing, and the crystal nuclei can be formed smoothly, preventing crystal growth and forming a large number of microcrystalline structures. The addition of EuF 3 can increase the melt viscosity of the enamel layer rapidly during the firing and cooling process, and greatly increase the fine crystals in the enamel layer. Adding both at the same time can greatly increase the hardness of the enamel layer.
EuO2和EuF3的存在大大提高了FeO在搪瓷层的溶解，成为界面反应的催化剂，使界面反应加快，促进FeO与搪瓷层中硅酸盐反应生成硅酸铁化合物，硅酸铁化合物形成锚状，使得搪瓷层紧紧地抓牢在基体上，增加了搪瓷层与基体的密着性。The presence of EuO 2 and EuF 3 greatly improves the dissolution of FeO in the enamel layer, and becomes a catalyst for the interface reaction, which accelerates the interface reaction and promotes the reaction between FeO and silicate in the enamel layer to form iron silicate compounds, which form anchors. shape, so that the enamel layer is firmly grasped on the substrate, increasing the adhesion between the enamel layer and the substrate.
作为优选，各组分的重量百分比为：SiO2 60％、Al2O3 25％、B2O3 7.2％、Na2O1.3％、K2O 1.5％、EuO2 2％、EuF3 3％。Preferably, the weight percentage of each component is: SiO 2 60%, Al 2 O 3 25%, B 2 O 3 7.2%, Na 2 O 1.3%, K 2 O 1.5%, EuO 2 2%, EuF 3 3%.
上述搪瓷釉料按照以下步骤进行制备：Above-mentioned enamel glaze is prepared according to the following steps:
1)称取配方量的SiO2、Al2O3和B2O3预先混合球磨，混合均匀度≥99.5％；1) Pre-mixed and ball-milled SiO 2 , Al 2 O 3 and B 2 O 3 in the formula amount, and the mixing uniformity is ≥99.5%;
2)将其他原料加入步骤1)的混合物料中，混合球磨，混合均匀度≥98％；2) Add other raw materials into the mixed material in step 1), mix and ball mill, and the mixing uniformity is ≥98%;
3)将步骤2)的混合物料送入转炉或池炉中熔制，温度控制在1250～1280℃；3) Send the mixed material in step 2) into a converter or a pool furnace for melting, and control the temperature at 1250-1280°C;
4)待物料完全熔融后打钎，将熔融的液态玻璃快速拉成1.2～1.5m的玻璃丝进行检测，在玻璃丝的1m内有2～3个节即为熔制完成；4) Brazing is performed after the material is completely melted, and the molten liquid glass is quickly pulled into a glass filament of 1.2-1.5m for inspection. If there are 2-3 knots within 1m of the glass filament, the melting is completed;
5)将熔制好的玻璃液体快速倒入水中激淬，滤干后即得。5) Quickly pour the melted glass liquid into water to quench it, filter it dry and get it.
与现有技术相比，本发明在常规搪瓷釉料中加入EuO2和EuF3可以提高釉料的硬度以及与钢板的密着性，还能有效防止鱼鳞爆的发生。Compared with the prior art, the present invention adds EuO 2 and EuF 3 to the conventional enamel glaze, which can improve the hardness of the glaze and the adhesion with the steel plate, and can effectively prevent the occurrence of fish scale explosion.
具体实施方式detailed description
以下具体实施例对本发明作进一步阐述，但不作为对本发明的限定。The following specific examples further illustrate the present invention, but are not intended to limit the present invention.
以下百分数为重量百分数。The following percentages are percentages by weight.
实施例1Example 1
配方：formula:
SiO2 50％、Al2O3 20％、B2O3 15％、Na2O 1.2％、K2O 1.3％、EuO2 10％、EuF32.5％。SiO 2 50%, Al 2 O 3 20%, B 2 O 3 15%, Na 2 O 1.2%, K 2 O 1.3%, EuO 2 10%, EuF 3 2.5%.
制备方法：Preparation:
1)称取配方量的SiO2、Al2O3和B2O3预先混合球磨，混合均匀度≥99.5％；1) Pre-mixed and ball-milled SiO 2 , Al 2 O 3 and B 2 O 3 in the formula amount, and the mixing uniformity is ≥99.5%;
2)将其他原料加入步骤1)的混合物料中，混合球磨，混合均匀度≥98％；2) Add other raw materials into the mixed material in step 1), mix and ball mill, and the mixing uniformity is ≥98%;
3)将步骤2)的混合物料送入转炉或池炉中熔制，温度控制在1250℃；3) The mixed material in step 2) is sent to a converter or a pool furnace for melting, and the temperature is controlled at 1250°C;
4)待物料完全熔融后打钎，将熔融的液态玻璃快速拉成1.2的玻璃丝进行检测，在玻璃丝的1m内有2个节即为熔制完成；4) Brazing is performed after the material is completely melted, and the molten liquid glass is quickly pulled into a 1.2-inch glass filament for detection. If there are 2 knots within 1m of the glass filament, the melting is completed;
5)将熔制好的玻璃液体快速倒入水中激淬，滤干后即得。5) Quickly pour the melted glass liquid into water to quench it, filter it dry and get it.
实施例2Example 2
配方：formula:
SiO2 65％、Al2O3 20％、B2O3 8.9％、Na2O 1.5％、K2O 1.6％、EuO2 1％、EuF3 2％。SiO 2 65%, Al 2 O 3 20%, B 2 O 3 8.9%, Na 2 O 1.5%, K 2 O 1.6%, EuO 2 1%, EuF 3 2%.
制备方法：Preparation:
1)称取配方量的SiO2、Al2O3和B2O3预先混合球磨，混合均匀度≥99.5％；1) Pre-mixed and ball-milled SiO 2 , Al 2 O 3 and B 2 O 3 in the formula amount, and the mixing uniformity is ≥99.5%;
2)将其他原料加入步骤1)的混合物料中，混合球磨，混合均匀度≥98％；2) Add other raw materials into the mixed material in step 1), mix and ball mill, and the mixing uniformity is ≥98%;
3)将步骤2)的混合物料送入转炉或池炉中熔制，温度控制在1280℃；3) The mixed material in step 2) is sent to a converter or a pool furnace for melting, and the temperature is controlled at 1280°C;
4)待物料完全熔融后打钎，将熔融的液态玻璃快速拉成1.5m的玻璃丝进行检测，在玻璃丝的1m内有3个节即为熔制完成；4) Brazing is performed after the material is completely melted, and the molten liquid glass is quickly drawn into a 1.5m glass filament for detection, and the melting is completed if there are 3 knots within 1m of the glass filament;
5)将熔制好的玻璃液体快速倒入水中激淬，滤干后即得。5) Quickly pour the melted glass liquid into water to quench it, filter it dry and get it.
实施例3Example 3
配方：formula:
SiO2 60％、Al2O3 25％、B2O3 7.2％、Na2O 1.3％、K2O 1.5％、EuO2 2％、EuF3 3％。SiO 2 60%, Al 2 O 3 25%, B 2 O 3 7.2%, Na 2 O 1.3%, K 2 O 1.5%, EuO 2 2%, EuF 3 3%.
制备方法：Preparation:
1)称取配方量的SiO2、Al2O3和B2O3预先混合球磨，混合均匀度≥99.5％；1) Pre-mixed and ball-milled SiO 2 , Al 2 O 3 and B 2 O 3 in the formula amount, and the mixing uniformity is ≥99.5%;
2)将其他原料加入步骤1)的混合物料中，混合球磨，混合均匀度≥98％；2) Add other raw materials into the mixed material in step 1), mix and ball mill, and the mixing uniformity is ≥98%;
3)将步骤2)的混合物料送入转炉或池炉中熔制，温度控制在1260℃；3) The mixed material in step 2) is sent to a converter or a pool furnace for melting, and the temperature is controlled at 1260°C;
4)待物料完全熔融后打钎，将熔融的液态玻璃快速拉成1.3m的玻璃丝进行检测，在玻璃丝的1m内有2个节即为熔制完成；4) Brazing is performed after the material is completely melted, and the molten liquid glass is quickly pulled into a 1.3m glass filament for detection, and the melting is completed if there are 2 knots within 1m of the glass filament;
5)将熔制好的玻璃液体快速倒入水中激淬，滤干后即得。5) Quickly pour the melted glass liquid into water to quench it, filter it dry and get it.
实施例4Example 4
配方：formula:
SiO2 55％、Al2O3 30％、B2O3 4％、Na2O 1.5％、K2O 1.5％、EuO2 3％、EuF3 5％。SiO 2 55%, Al 2 O 3 30%, B 2 O 3 4%, Na 2 O 1.5%, K 2 O 1.5%, EuO 2 3%, EuF 3 5%.
制备方法：Preparation:
1)称取配方量的SiO2、Al2O3和B2O3预先混合球磨，混合均匀度≥99.5％；1) Pre-mixed and ball-milled SiO 2 , Al 2 O 3 and B 2 O 3 in the formula amount, and the mixing uniformity is ≥99.5%;
2)将其他原料加入步骤1)的混合物料中，混合球磨，混合均匀度≥98％；2) Add other raw materials into the mixed material in step 1), mix and ball mill, and the mixing uniformity is ≥98%;
3)将步骤2)的混合物料送入转炉或池炉中熔制，温度控制在1280℃；3) The mixed material in step 2) is sent to a converter or a pool furnace for melting, and the temperature is controlled at 1280°C;
4)待物料完全熔融后打钎，将熔融的液态玻璃快速拉成1.2m的玻璃丝进行检测，在玻璃丝的1m内有3个节即为熔制完成；4) Brazing is performed after the material is completely melted, and the molten liquid glass is quickly drawn into a 1.2m glass filament for testing. If there are 3 knots within 1m of the glass filament, the melting is completed;
5)将熔制好的玻璃液体快速倒入水中激淬，滤干后即得。5) Quickly pour the melted glass liquid into water to quench it, filter it dry and get it.
对照例1Comparative example 1
配方：formula:
SiO2 60％、Al2O3 25％、B2O3 7.2％、Na2O 1.3％、K2O 1.5％、ZrO2 4％、CoO 1％。SiO 2 60%, Al 2 O 3 25%, B 2 O 3 7.2%, Na 2 O 1.3%, K 2 O 1.5%, ZrO 2 4%, CoO 1%.
制备方法：Preparation:
1)称取配方量的SiO2、Al2O3和B2O3预先混合球磨，混合均匀度≥99.5％；1) Pre-mixed and ball-milled SiO 2 , Al 2 O 3 and B 2 O 3 in the formula amount, and the mixing uniformity is ≥99.5%;
2)将其他原料加入步骤1)的混合物料中，混合球磨，混合均匀度≥98％；2) Add other raw materials into the mixed material in step 1), mix and ball mill, and the mixing uniformity is ≥98%;
3)将步骤2)的混合物料送入转炉或池炉中熔制，温度控制在1260℃；3) The mixed material in step 2) is sent to a converter or a pool furnace for melting, and the temperature is controlled at 1260°C;
4)待物料完全熔融后打钎，将熔融的液态玻璃快速拉成1.3m的玻璃丝进行检测，在玻璃丝的1m内有2个节即为熔制完成；4) Brazing is performed after the material is completely melted, and the molten liquid glass is quickly pulled into a 1.3m glass filament for detection, and the melting is completed if there are 2 knots within 1m of the glass filament;
5)将熔制好的玻璃液体快速倒入水中激淬，滤干后即得。5) Quickly pour the melted glass liquid into water to quench it, filter it dry and get it.
将上述实施例1～4和对照例1的搪瓷釉料以厚度为2.3mm的低碳钢Q235A(C0.2w％,S 0.05w％,P 0.04w％,Mn 0.8w％,Fe余量)为基体制成搪瓷钢板，进行附着性、耐磨性和耐腐蚀性检测。The enamel glaze of the above-mentioned Examples 1-4 and Comparative Example 1 was made of low-carbon steel Q235A (C0.2w%, S 0.05w%, P 0.04w%, Mn 0.8w%, Fe balance) with a thickness of 2.3mm Enamel steel plates are made for the substrate, and the adhesion, wear resistance and corrosion resistance tests are carried out.
1、附着力测试：1. Adhesion test:
在搪瓷钢板表面用锋利的刀刃划出100个大小均匀的间隔为1mm的小方格(划痕深度控制在保证膜下基体金属暴露)，搪瓷釉料脱落的小方格数N1，在膜上的画格区域贴上宽度为24mm的透明胶带，并保证胶带与方格的膜之间结合紧密。5min后，用一垂直膜面的立即将胶带揭开，并再次统计膜脱落的小方格数N2。评估方法如下：采用百分制，膜附着力分数＝100-(N1+N2)，附着力分数越大，说明附着力越好。On the surface of the enamel steel plate, use a sharp blade to scratch 100 small squares with uniform size and interval of 1mm (the depth of the scratch is controlled to ensure that the base metal under the film is exposed), and the number of small squares where the enamel glaze falls off is N1. Paste a transparent tape with a width of 24mm on the area of the grid, and ensure that the tape is tightly bonded to the film of the grid. After 5 minutes, immediately peel off the adhesive tape with a stick perpendicular to the film surface, and count the number N2 of the small squares where the film falls off again. The evaluation method is as follows: using a percentage system, the film adhesion score = 100-(N1+N2), the greater the adhesion score, the better the adhesion.
2、耐磨性测试：2. Wear resistance test:
将搪瓷钢板放入振动研磨机中连续振动研磨2h后取出，观察搪瓷钢板的棱角和表面的膜层是否有脱落。Put the enamel steel plate into the vibrating grinder for continuous vibration grinding for 2 hours, then take it out, and observe whether the edges and corners of the enamel steel plate and the film layer on the surface fall off.
3、耐腐蚀性测试：3. Corrosion resistance test:
将搪瓷钢板置于盐雾腐蚀箱内，在35℃下用5％的氯化钠水溶液喷溅2h后，取出再将其置于另一个温度为40度、相对湿度为80％的恒温恒湿箱中，观察其在多长时间后表面出现异常，时间越长，说明膜层的耐腐蚀性越好。Put the enamel steel plate in the salt spray corrosion box, spray it with 5% sodium chloride aqueous solution for 2 hours at 35°C, take it out and put it in another constant temperature and humidity chamber with a temperature of 40°C and a relative humidity of 80%. In the box, observe how long it takes for the surface to appear abnormal. The longer the time, the better the corrosion resistance of the film layer.
4、显微硬度测试4. Micro hardness test
用FM-700型显微硬度仪测量搪瓷层的硬度，荷载200g，负荷保持10s。The hardness of the enamel layer was measured with a FM-700 microhardness tester, with a load of 200g and a load of 10s.
试验结果见下表:The test results are shown in the table below:
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