WO2022041785A1 - Glaçure de revêtement de sol de plaque d'émail sur acier inoxydable, procédé de préparation associé et application associée - Google Patents

Glaçure de revêtement de sol de plaque d'émail sur acier inoxydable, procédé de préparation associé et application associée Download PDF

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Publication number
WO2022041785A1
WO2022041785A1 PCT/CN2021/087687 CN2021087687W WO2022041785A1 WO 2022041785 A1 WO2022041785 A1 WO 2022041785A1 CN 2021087687 W CN2021087687 W CN 2021087687W WO 2022041785 A1 WO2022041785 A1 WO 2022041785A1
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Prior art keywords
glaze
stainless steel
temperature
enamel
time
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PCT/CN2021/087687
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English (en)
Chinese (zh)
Inventor
邢翰学
曹益亭
傅昂挺
张军
黄新亮
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浙江开尔新材料股份有限公司
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Publication of WO2022041785A1 publication Critical patent/WO2022041785A1/fr

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Classifications

    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23D—ENAMELLING OF, OR APPLYING A VITREOUS LAYER TO, METALS
    • C23D5/00—Coating with enamels or vitreous layers
    • C23D5/02—Coating with enamels or vitreous layers by wet methods
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/19—Iron or steel

Definitions

  • the invention relates to the field of enamel material preparation, in particular to a bottom glaze glaze of a stainless steel enamel plate and a preparation method and application thereof.
  • Enamel plate refers to a composite material in which inorganic vitreous materials are condensed on the base steel plate by melting and firmly combined with the steel plate. Enamel coating on the surface of the steel plate can prevent the steel plate from rusting, so that the steel plate will not form an oxide layer on the surface when it is heated and can resist the erosion of various liquids. Enamel products have excellent properties such as high hardness, high temperature resistance, wear resistance, insulation, safety and non-toxicity, and easy washing and cleaning, and the enamel layer can also give the products a beautiful appearance. Inner and outer walls, decorative wall panels for tunnels, sterile operating room walls, pedestrian underpass wall panels and heat exchangers, etc.
  • the enamel plate is generally made of low carbon steel plate, but once the edge and corner of the low carbon steel enamel plate explodes, the bottom plate exposed to the external environment will be rusted. Furthermore, when it is used as an outer curtain wall, due to the The larger perforation rate pursued by the exterior curtain wall decoration will also cause the problem of plate deformation.
  • These problems have been the main reasons for limiting the application of mild steel enamel panels in exterior curtain wall decoration.
  • stainless steel has the properties of corrosion resistance, high strength, steel deformation is not easy to break, and environmental protection, and stainless steel has good ductility and toughness, suitable for harsh environments (humidity, acid and alkali and other indoor and outdoor environments) use. Therefore, replacing low carbon steel with stainless steel base material will be able to solve some problems existing in the current exterior curtain wall decoration.
  • the present invention achieves the goals of good enamel adhesion and high quality of the porcelain surface by improving the formulation and preparation process of the enamel layer bottom glaze glaze.
  • a base glaze for a stainless steel enamel plate comprising the following components: in terms of mass percentage, including the following components: SiO 2 30-38%; B 2 O 3 15-19%; Al 2 O 3 6-10%; TiO2 1-2 %; BaO 1-4%; Na2O 14-19%; K2O 5-10 %; MgO 0.1-0.6%; P2O5 2-4 %; ZnO 0.2-0.8%; Cr2O3 0.1-0.3%; CuO 0.4-0.8%; CoO 0.3-0.9%; NiO 0.7-1.2% and MnO2 0.8-1.3%.
  • bottom glaze There are two types of stainless steel enamel glaze: bottom glaze and top glaze.
  • the bottom glaze needs to be combined with stainless steel. How to make the bottom glaze and stainless steel achieve high adhesion is the technical difficulty of stainless steel enamel plates.
  • SiO 2 is the main component and is the main glass network forming body.
  • Increasing the content of SiO 2 in the range of 30-38% can improve the mechanical strength and hardness of the glaze, as well as the gloss, chemical stability and thermal stability of the glaze.
  • the B 2 O 3 in the glaze provided by the present invention is not only a solvent for the enamel but also a network former of the enamel, which can promote the formation of a glass phase at a low temperature stage.
  • the increase of B 2 O 3 content will increase the mechanical strength and abrasion resistance of the enamel.
  • B 2 O 3 has a good fluxing effect, which can reduce the softening temperature, viscosity, surface tension and expansion coefficient of the enamel, which is beneficial to the melting of metal oxides and the formation of adhesion.
  • Al 2 O 3 in the glaze provided by the present invention is an intermediate oxide, which can not only combine with silicon dioxide, but also combine with alkaline oxides. It can not only improve the vitrification ability of the enamel, but also inhibit the crystallization, and can significantly improve the elasticity, hardness and chemical stability of the glaze, and improve the resistance to chemical corrosion.
  • the TiO2 in the glaze provided by the present invention is to increase the opacity, acid resistance and luster of the enamel. Due to the good opacity, the enamel only needs to be coated with a thin layer, so this porcelain layer has high thermal stability, impact resistance and flexural strength, and has good chemical stability; at the same time, TiO 2 improves the luster of the enamel. , make the surface of enamel products more smooth and delicate.
  • BaO in the glaze provided by the invention is a fluxing agent, barium has the largest ionic radius among alkali metals, the strongest alkalinity is also the best fluxing effect among alkali metal oxidations, and can also improve the anti-organic resistance of the glaze. Acid corrosion ability.
  • K 2 O and Na 2 O in the glaze provided by the invention are strong fluxes of the glaze, which can significantly reduce the melting temperature and high temperature viscosity of the glaze, increase the refractive index of the glaze, and thereby improve the gloss of the glaze.
  • K 2 O and Na 2 O have low melting points. During the melting process of enamel, they are prone to chemical reaction with SiO 2 , and the reaction will release a lot of heat, thereby reducing the external heating temperature and reducing the viscosity at high temperature.
  • MgO is also a fluxing agent of the glaze, which can not only reduce the melt viscosity, but also reduce the expansion coefficient of the glaze, reduce the cracking of the glaze surface, and improve the quality of the porcelain surface.
  • the P 2 O 5 in the glaze provided by the invention can increase the opacity of the glaze, increase the reflection coefficient of the porcelain layer, and cooperate with titanium dioxide to jointly improve the chemical stability of the glaze.
  • the ZnO in the glaze provided by the invention can play a good fluxing effect in a large range, reduce the expansion coefficient of the glaze, and improve the gloss.
  • the mass fraction of zinc oxide is selected to be 0.2-0.8%.
  • the Cr 2 O 3 in the glaze provided by the invention can improve the chemical stability and high temperature resistance performance of the enamel, and at the same time can also be beneficial to the formation of the stainless steel enamel adhesion in the invention.
  • CuO, CoO, NiO and MnO 2 in the glaze provided by the present invention are adhesives, and the four adhesives have an interaction relationship, and their interaction can react with iron, so that the enamel penetrates into the surface layer of the steel plate and promotes the enamel glaze Infiltrating the stainless steel surface at high temperature promotes the dissolution of iron and iron oxide, and controls the oxidation conditions of the interface, which is conducive to the formation of a more uniform bubble structure in the porcelain layer and a good adhesion between the bottom glaze and the stainless steel.
  • the bottom glaze of the above-mentioned stainless steel enamel plate in terms of mass percentage, includes the following components: SiO 2 36.39%; B 2 O 3 17.87%; Al 2 O 3 7.06%; TiO 2 1.15%; BaO 2.79% ; Na 2 O 17.59%; K 2 O 9.96%; MgO 0.18%; P 2 O 5 2.95%; ZnO 0.57%; Cr 2 O 3 0.15% ; %.
  • the invention also discloses a method for preparing the base glaze of the above-mentioned stainless steel enamel plate, comprising the following steps: (1) mixing the components according to the proportion;
  • the enamel frit is turned into a ball mill and ground to form a glaze.
  • the melting temperature is 1000-1200° C.
  • the enamel frit is ground and passed through a 70-90 mesh sieve.
  • a stainless steel enamel plate comprising a stainless steel substrate, a bottom glaze and a top glaze; the bottom glaze and the top glaze are sequentially attached to the stainless steel substrate; and the raw material of the bottom glaze is any one of claims 1-2 The bottom glaze glaze.
  • the surface glaze formula in the present invention has no particularity, and the general surface glaze formula can realize enamel coating.
  • the components of the surface glaze are: SiO 2 : 30%-50%, B 2 O 3 : 15%-25%, Al 2 O 3 : 5%-10%, CaO: 3%-5% %, TiO 2 : 15% to 18%, BaO: 7% to 10%, Na 2 O: 10% to 16%, K 2 O: 3% to 5%, MgO: 0.5% to 0.8%, P 2 O 5 : 2% to 4%, ZnO: 2% to 5%.
  • the thickness of the bottom glaze is controlled at 90-140um; the thickness of the top glaze is controlled at 80-120um.
  • the thickness of the porcelain layer has a great influence on the porcelain surface and the adhesion.
  • the thickness of the bottom glaze is between 90-140um to obtain a better porcelain surface and a better adhesion level.
  • the problem of chromatic aberration if the thickness of the surface glaze exceeds 120um, it is easy to have insufficient surface uniformity, and the problem of chromatic aberration will also occur.
  • the firing temperature of the bottom glaze is 800-840°C, and the firing time is 4 minutes; the firing temperature of the top glaze is 800-840°C, and the firing time is 4-5 minutes.
  • the stainless steel substrate is austenitic stainless steel, and the content of some chemical elements in it is as follows: carbon ⁇ 0.030%, silicon ⁇ 1.00%, manganese ⁇ 2.00%, phosphorus ⁇ 0.035%, sulfur ⁇ 0.030%, nickel 8.00- 20.00%, chromium 18.00-20.00%.
  • the commonly used stainless steel is austenitic stainless steel, so the present invention focuses on the enamelling on austenitic stainless steel.
  • the bottom glaze glaze provided by the present invention has the best enamel coating effect on the austenitic stainless steel with the above chemical element content.
  • the invention also discloses the preparation method of the above-mentioned stainless steel enamel plate, comprising the following steps:
  • S1 stainless steel substrate preparation stainless steel plate is obtained after laser nitrogen cutting, corner bending, laser welding, grinding and surface treatment;
  • S2 glaze spraying glaze spraying by wet spraying process
  • the bottom glaze firing temperature is 800-840 °C, and the firing time is 4 minutes; the surface glaze firing temperature is 800-840 °C, and the firing time is 4-5 minutes.
  • the invention uses laser cutting to complete the cutting of the stainless steel plate, which can ensure the accuracy of the cutting size and facilitate the installation of the plate; and nitrogen cutting is used to protect the cutting surface from being oxidized, reduce the probability of the knife edge bursting, and the laser automatically cuts, reducing labor operation, to maximize the production capacity, the used stainless steel laser cutting process is consistent with the existing process, and the present invention will not describe it in detail. Corner bending is formed according to the existing production process. Due to the special material of stainless steel, the deformation of manual welding is large, and the process test is changed to laser welding. Since the oxidation of the laser welding seam is less, the welding seam can be slightly polished. In addition, the present invention achieves the purpose of good enamel adhesion and high quality of the enamel surface at a firing temperature of 800° C. at a low temperature.
  • the thickness of the stainless steel plate during laser welding in S1 is 1.5mm, the welding power is 800W, the welding speed is 0.8m/min, and the focal length is the positive focus point.
  • the welding parameters of the normal production steel plate are the welding power of 2400W, the welding speed of 1m/min, and the focal length of the positive focus point.
  • the present invention reduces the power to reduce the amount of deformation, and then reduces the welding speed by reducing the welding speed. In order to achieve the effect of full welding seam, but the power is too low, the plate cannot be fully welded, and the laser light output is unstable.
  • the welding effect of stainless steel plate is the best under the above parameters.
  • the surface treatment in the S1 is specifically:
  • the first course degreasing, sodium carbonate concentration: 8-10%, temperature: 60-70 °C, time: 7-8min;
  • Second pass degreasing, sodium carbonate concentration: 8-10%, temperature: 60-70°C, time: 7-8min;
  • the third course hot water rinse, temperature: 50-60 °C, time: 3-4min;
  • the fourth course rinse with cold water, normal temperature, time: 2-3min;
  • the fifth step drying, temperature: 300-350 °C, time: 8-10min.
  • the method to increase the adhesion of stainless steel in the industry is surface sandblasting, which forms a certain roughness on the surface of the stainless steel plate, but the sandblasting of the large plate is difficult for the site, equipment and uniformity.
  • the invention adopts the chemical immersion method to treat the surface of the stainless steel, which has the advantages of small treatment difficulty and good effect.
  • the present invention obtains a smooth and delicate porcelain surface through the overall ratio of the above-mentioned components, using titanium dioxide and phosphorus pentoxide with good turbidity, and cooperates with CuO, CoO, NiO, MnO 2 to promote adhesion, and then combine with
  • the bottom glaze of the stainless steel enamel plate provided by the present invention has the characteristics of high adhesion, high weather resistance and high corrosion resistance;
  • the stainless steel enamel plate prepared by using the glaze provided by the present invention at a relatively low firing temperature has good adhesion, and the obtained enamel porcelain surface is smooth and delicate;
  • Table 1 List of mass fractions (%) of each component in Examples 1-3
  • a preparation method of bottom glaze glaze of stainless steel enamel plate comprising the following steps:
  • Examples 4-6 were prepared by using the glaze formulations of Examples 1-3 respectively.
  • a preparation method of a stainless steel enamel plate comprising the following steps:
  • S1 stainless steel substrate preparation 304 stainless steel plate is obtained after laser nitrogen cutting, corner bending, laser welding, grinding and surface treatment;
  • the thickness of the stainless steel plate is 1.5mm, the welding power is 800W, the welding speed is 0.8m/min, and the focal length is the positive focus point;
  • the surface treatment is as follows:
  • the first course degreasing, concentration: 8%, temperature: 70°C, time: 8min;
  • Second pass degreasing, concentration: 8%, temperature: 70°C, time: 8min;
  • the third course hot water rinse, temperature: 50-60 °C, time: 3min;
  • the fourth course rinse with cold water, normal temperature, time: 2min;
  • the fifth step drying, temperature: 300°C, time: 8min;
  • S2 glaze spraying use the base glaze glaze of Example 4 to carry out glaze spraying by wet spraying process; the base glaze thickness is controlled at 90-140um; the top glaze thickness is controlled at 80-120um;
  • Examples 7-9 all adopt the above-mentioned preparation method, the difference is that the firing temperature of the bottom glaze is 800°C, 820°C and 840°C, respectively.
  • Example 7-9 The base glaze in Example 7-9 was changed to the base glaze glaze prepared in Example 5, and the rest was the same as that of Example 7-9.
  • Example 4-6 The bottom glaze in Example 4-6 was changed to the bottom glaze glaze prepared in Example 6 and fired, and the rest were the same as those in Example 7-9.
  • the stainless steel enamel glaze is obtained according to the components and mass fractions of Example 1 to Example 3. After firing at different temperatures, the porcelain surfaces fired by the glaze formula of Example 1 are all smooth and delicate. , the lowest temperature required to form a level 1 bond. Therefore, the base glaze glaze formula of Example 1 is the best formula, and the obtained stainless steel enamel glaze has good porcelain surface quality while ensuring good adhesion.
  • the spraying thickness of the bottom glaze was modified to 90-120um and 120-140um respectively, and the rest were the same as those in Example 7.
  • the spraying thickness of the bottom glaze was modified to 30-50um, 50-70um, 70-90um, and 140-160um respectively, and the rest were the same as those in Example 7.
  • the thickness of the underglaze porcelain layer has a great influence on the porcelain surface and the adhesion.
  • the porcelain layer thickness between 90-140um can obtain better porcelain surface and better adhesion.
  • the 304 stainless steel plate was welded by laser welding, and the welding power and welding speed were changed.
  • the welding effect is shown in Table 4.
  • Table 4 Stainless steel welding process test record table: using laser welding process.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Life Sciences & Earth Sciences (AREA)
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Abstract

L'invention concerne une glaçure de revêtement de sol d'une plaque d'émail sur acier inoxydable, comprenant les composants suivants en pourcentage en masse : 30 à 38% de SiO2 ; 15 à 19% de B2O3 ; 6 à 10% de Al2O3 ; 1 à 2% de TiO2 ; 1 à 4% de BaO ; 14 à 19% de Na2O ; 5 à 10% de K2O ; 0,1 à 0,6% de MgO ; 2 à 4% de P2O5 ; 0,2 à 0,8% de ZnO ; 0,1 à 0,3% de Cr2O3 ; 0,4 à 0,8% de CuO ; 0,3 à 0,9% de CoO ; 0,7 à 1,2% de NiO ; et 0,8 à 1,3% de MnO2. La plaque d'émail sur acier inoxydable préparée à partir de la glaçure à une température de frittage basse présente une bonne adhérence, et la surface d'émail obtenue est lisse et fine.
PCT/CN2021/087687 2020-08-28 2021-04-16 Glaçure de revêtement de sol de plaque d'émail sur acier inoxydable, procédé de préparation associé et application associée WO2022041785A1 (fr)

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CN202010889270.8 2020-08-28
CN202010889270.8A CN112062469B (zh) 2020-08-28 2020-08-28 一种不锈钢搪瓷板的底釉釉料及其制备方法和应用

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CN113789514A (zh) * 2021-08-23 2021-12-14 江阴硅普搪瓷股份有限公司 一种耐高温、耐磨、耐强冲击的防腐微晶釉的制备方法
CN114873915A (zh) * 2022-04-26 2022-08-09 九牧厨卫股份有限公司 一种用于不锈钢卫浴产品的陶瓷釉及其应用
CN115386875A (zh) * 2022-08-26 2022-11-25 湖南星城壹品装饰工程有限公司 一种净水滤芯套筒内外表面上瓷工艺
CN115817061A (zh) * 2022-12-02 2023-03-21 浙江开尔新材料股份有限公司 一种板面镂空艺术图案搪瓷板的生产方法

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CN112062469B (zh) * 2020-08-28 2022-06-03 浙江开尔新材料股份有限公司 一种不锈钢搪瓷板的底釉釉料及其制备方法和应用
CN114368245A (zh) * 2021-12-23 2022-04-19 张柳松 一种不锈钢瓷画的制作方法
CN115818962A (zh) * 2022-12-16 2023-03-21 江阴硅普搪瓷股份有限公司 基于纳米材料的耐酸搪瓷预磨粉及其制备方法
KR102546576B1 (ko) * 2023-03-07 2023-06-23 주식회사 디디글로벌 동박제조용 서스플레이트의 제조방법

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CN113789514A (zh) * 2021-08-23 2021-12-14 江阴硅普搪瓷股份有限公司 一种耐高温、耐磨、耐强冲击的防腐微晶釉的制备方法
CN113789514B (zh) * 2021-08-23 2023-07-28 江阴硅普搪瓷股份有限公司 一种耐高温、耐磨、耐强冲击的防腐微晶釉的制备方法
CN114873915A (zh) * 2022-04-26 2022-08-09 九牧厨卫股份有限公司 一种用于不锈钢卫浴产品的陶瓷釉及其应用
CN115386875A (zh) * 2022-08-26 2022-11-25 湖南星城壹品装饰工程有限公司 一种净水滤芯套筒内外表面上瓷工艺
CN115386875B (zh) * 2022-08-26 2024-04-23 湖南星城壹品装饰工程有限公司 一种净水滤芯套筒内外表面上瓷工艺
CN115817061A (zh) * 2022-12-02 2023-03-21 浙江开尔新材料股份有限公司 一种板面镂空艺术图案搪瓷板的生产方法

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