A PROCESS FOR SEALING AN ALUMINUM SUBSTRATE TO IMPROVE ITS RESISTANCE PROPERTIES

Abstract

A process is described for sealing an aluminum or aluminum alloy substrate and improving its alkali resistance properties while providing a satisfactory appearance. A multi-bath sealing system and kit is included, comprising at least one low-temperature bath with a primary sealing compound containing at least one nickel ion source and at least one fluoride ion source, and at least one high-temperature bath with a secondary sealing compound containing at least one silicate.

Description

AN ALUMINUM SUBSTRATE TO IMPROVE RESISTANCE PROPERTIES A PROCESS FOR SEALING THE LAYER TECHNICAL FIELD The present invention generally involves an aluminum substrate. a process for ensuring leak tightness and its use here It relates to a multi-bath sealing system. BACKGROUND OF THE INVENTION Aluminum substrates, under suitable processing conditions and corrosion resistance. Due to its durability properties, it is used in automotive, home and architectural applications. It is used in various industries. Aluminum substrates, various to develop desirable features for industries It can undergo several different processes. For example, aluminum substrates The layers can be cleaned and then treated with an alkaline substance. It can be etched. After etching, the aluminum substrate, To form an anodized aluminum oxide (“AAO”) layer an anodizing process that oxidizes the aluminum substrate It is held in place. The AAO layer is porous and subsequent processes It can be colored accordingly. The anodizing process, for example, depends on the voltage. current, pH, temperature, acid concentration, shaking, aluminum concentration and the amount and types of additives, etc. a controlled acidic environment under various variable parameters It is taking place in that environment. After anodizing, a porous and colorable AAO layer is formed. Optionally, an anodized aluminum substrate for heavy metals. in salt solutions a specific voltage and current (usually a condition that occurs when exposed to alternating current) electrolytic coloring process with electro- 1 It can be colored. In this process, heavy metal pigment is used. AAO layer during the first half-cycle of alternating current It is deposited into its pores. The AAO layer, alternating current further by anodic oxidation in the second half of the cycle It is being thickened. At the base of the pores in the AAO layer The accumulated heavy metals are discoloring the aluminum substrate. Kuhm et al., the holder of patent number US5587063A, subject herein as a reference describing an electro coloring process It is fully included. However, Kuhm uses electrocoloring. subsequently sealing the porous aluminum substrate It does not describe a method for achieving this. The aluminum substrate is subjected to an electro-coloring process. Regardless of whether it is captured or not, the AAO layer still It is porous. Therefore, anodizing and / or electrolytic After the coloring processes, the pores of the AAO layer typically for low, medium and high temperature sealing. a which may include one or more of its bathrooms It is sealed during the sealing process. Sealing processes corrosion, acid and / or alkaline resistance of aluminum substrate. It provides enhanced resistance properties, including those mentioned above. However, in certain industries, such as the automotive industry, Current sealing processes meet stringent industry standards. to develop the necessary resistance properties to meet is inadequate. For example, such sealing processes are insufficient. aluminum substrate with an alkaline bath at approximately pH 13 alkali resistance properties and scratch resistance when in contact insufficient to improve its resistance properties (aluminum substrate) layers exposed to the environment and / or real-world conditions (when left behind, it should be exposed to similar conditions). 2 Schoener et al., patent holder number EP0193964B1, the subject matter of which is in its entirety. Zirconium is included as a reference, as a key component. and / or titanium, fluoride ions and thiourea, SiO-based 2 containing an additive that is a silicate or a mixture thereof an acidic sealing compound with an aqueous low temperature This describes the bath (not exceeding 40°C). together, among others, aqueous low-temperature bath aluminum substrate with sufficient alkali resistance properties It does not provide. Lawlor, the patent holder under patent number US7851025B2, has made the subject matter entirely referenced. Included is a fully sealed anodized aluminum base. It relates to a method for processing the layers. Lawlor is a an aqueous silicate solution containing alkali metal silicate It explains. Aluminum substrate, but the substrate is a previous one. after being completely sealed by this method, treatment with silicate solution. Lawlor sees, among other things, that he is low. It does not adequately describe a bath at that temperature and the aluminum bottom It does not provide sufficient alkali resistance properties to the layer. The subject of Hecht's document US20120244280A1 is entirely referenced. Included as such, acid and alkali resistant, high gloss. a multi-stage method for producing anodized aluminum surfaces Hecht explains that the first one contained water-soluble alkali silicate. sealing compound and inorganic compounds and fluoride It describes the second sealing compound containing ions. However, Hecht, among other things, pointed out that inorganic compounds It is suggested that it should be zirconium, titanium and / or silicate based. It continues. Patent holder Jang et al., patent no. WO2023115366, the subject matter of which is in whole in a medium-temperature bath, included as a reference 3 first sealing compound and high for use second seal for use in a bath at a certain temperature It describes a sealant kit containing the compound. The primary sealing compound consists of fluoride ions, nickel, cobalt, chromium, cadmium and their mixture, the first ion, and zirconium, titanium, silicon, and a second ion that is a mixture of these. It requires. The second sealing compound is poly(met)acrylic. acids and derivatives, polyethers and derivatives, polyamides and derivatives, poly(sulfonic acid) and its derivatives and mixtures thereof. It contains a water-soluble polymer. However, Jang also all sealing baths at a high temperature It requires work. Mangano, the patent holder under patent number EP3245317, designs an aluminum substrate. the sealing process of the layer and then a silicate It describes an additional processing step involving the sealing compound. However, among other things, manganese is only found in nickel. a low-temperature bath containing fluoride or higher It describes a heated sealing bath. Current technologies initially perform an alkali resistance test. It can pass through, but is scratch-resistant after a scratch test. They cannot pass the test because they are not. Also, the automotive industry a suitable surface appearance, corrosion resistance and alkali resistance are desired Therefore, the sealing of aluminum substrates is crucial. for at least high alkali resistance, high scratch resistance and the desire is to provide a process that provides a satisfactory surface appearance is being done. A BRIEF DESCRIPTION OF THE INVENTION The aim of the present invention is to develop solutions for aluminum substrates. The goal is to provide a sealing process. 4 Another objective of the present invention is to apply aluminum to substrates. a product that provides improved alkali resistance properties The goal is to provide a sealing process. Another aim of the present invention is to make aluminum substrates resistant to scratching. a sealing process that improves resistance properties to provide. Another aim of the present invention is to be suitable for aluminum substrates. a sealing process that provides a surface appearance to provide. Another objective of the present invention is to create at least one low-temperature bath. and a multi-bath system containing at least one high-temperature bath The goal is to provide a sealing process. For this purpose, in one application, the present invention generally includes the following: a sealing of an aluminum substrate involving steps It is related to the process: a) a primary seal of the aluminum substrate contact with an aqueous low-temperature bath containing its composition to be made to happen; Here, the primary sealant compound contains at least one nickel ion source and at least one fluoride ion source includes; b) second sealing compound of aluminum substrate contact with an aqueous high-temperature bath containing to be made to happen; Here, the second sealant compound has at least one It contains silicate and c) optionally, at least one of the aluminum substrates an aqueous aging bath containing an aging component being brought into contact with. In another application, the present invention also includes the following: For sealing an anodized aluminum substrate It relates to a bath-type sealing system: a) at least one nickel ion source and at least one fluoride ion source containing the primary sealing compound containing the source first bathroom; b) a second sealing compound containing at least one silicate including a second bathroom and c) optionally containing at least one aging component a third bathroom. In another application, the present invention generally refers to an anodized finish. a sealing layer on an aluminum substrate to create it, with a multi-part kit to be processed here. It is related to the kit, which includes the following: a) at least one nickel-ion source and at least one fluoride source primary sealing compound containing; b) a second sealing composition containing at least one silicate and c) an aging process that includes at least one aging component composition. DETAILED DESCRIPTION OF PREFERRED APPLICATIONS The present invention generally applies to aluminum substrates. a process for ensuring leak tightness and this process It relates to an improved aluminum substrate. Natural (i.e., not electro-colored) or electro-colored colored aluminum substrates in a low-temperature bath and is brought into contact with a high-temperature bath. Low 6 the temperature bath must include at least one nickel-ion source and at least one fluoride source. It includes a primary sealing compound containing an ion source. The high-temperature bath should contain at least one metal, preferably a metasilicate. It contains a secondary sealing compound that includes silicate. The multi-step process provides at least resistance to strong corrosion, alkali, and scratching. It exhibits resistance properties. The many described here The step-by-step process, system, and kit all contribute to a positive outlook. It can provide. The use of the words "one" and "this" here does not mean that the context explicitly states otherwise. Unless otherwise specified, it expresses both singular and plural references. is doing. As used here, the term "approximate" refers to a parameter, a quantity, a measurable value such as a period of time, and so on. This indicates that the realization of the invention described herein is... to the extent that it is suitable for type variations, especially as specified a value of + / - 15% or less, preferably + / - 10% or less, more preferably + / - 5% or less, even more preferably + / - 1% or less and even more preferably to include + / - 0.1% or less It should be understood that the modifier "approximately" refers to... its value is specifically explained here. It should be understood. As used here, “below”, “lower”, “below”, Spatial relative terms such as "on top of," "over," and the like, one element or feature of another element(s) or feature(s) to provide ease of explanation in order to define its relationship It is used for this purpose. Also, the terms "front" and "back" where not restrictive and appropriate, each other It appears that it can be used in that place. 7 The terms “contains” and / or “contains” as used herein. specified properties, integers, steps, operations, indicates the presence of elements and / or components, but one or more more other properties, integers, steps, operations, elements, the existence or addition of the component and / or groups thereof It does not prevent. The term "largely non-exclusive," as used here, refers to... Unless otherwise defined for a particular element or compound, metal plating for bath analysis of a specific element or compound Ordinary analytics, well-known by experts in the field. This means it cannot be detected by these methods. Methods typically include atomic absorption spectrometry, titration, UV-Vis analysis, secondary ion mass spectrometry and It includes other commonly available analytical methods. As used here, “aluminum substrate” and “aluminum The terms "alloyed substrate" and "alloyed substrate" are used interchangeably and a substrate containing aluminum and / or aluminum alloy It is coming. The term “low temperature,” as used here, refers to a temperature of approximately 15 to a solution kept at a temperature of approximately 45°C, bath, system, electrolyte, composition and / or apparatus It is coming. The term “moderate temperature,” as used here, refers to approximately 45 to a solution kept at a temperature of approximately 70°C, bath, system, electrolyte, composition and / or apparatus It is coming. 8 The term “high temperature,” as used here, refers to approximately 70 to a solution kept at a temperature of approximately 100°C, bath, system, electrolyte, composition and / or apparatus It is coming. In an application, the existing invention generally follows these steps: a process for sealing an aluminum substrate containing It is related to: a) primary sealing composition of aluminum substrate contact with an aqueous low-temperature bath containing; Here, the primary sealant compound contains at least one nickel ion source and at least one fluoride ion source includes; b) second sealing compound of aluminum substrate contact with an aqueous high-temperature bath containing to be made to happen; Here, the second sealant compound has at least one It contains silicate and c) optionally, at least one of the aluminum substrates with an aqueous aging bath containing an aging component making contact. Contact of the aluminum substrate with any aqueous bath the process step, for example spraying, dipping, coating, washing and / or aluminum substrate in other ways with aqueous baths involving contact, by technically skilled personnel This can be accomplished in various known ways. In applications, the aluminum substrate is an anodized aluminum substrate. It is a substrate. Anodized aluminum substrate has at least low... processing in a heat bath and / or high temperature bath Upon inspection, the substrate is a sealed aluminum substrate. 9 In a preferred application, the process described above The steps are carried out in sequence. That is, (anodized) aluminum base The layer is first brought into contact with a low-temperature bath and then It is brought into contact with a high-temperature bath. Leakproof. aluminum substrate optional high temperature contact with aging bath after bath It can be done. Aluminum substrate aluminum metal and / or an aluminum It may contain an alloy. When an aluminum alloy is present, Aluminum content at least approximately 70% by weight, preferably by weight. at least 80%, preferably at least 90% by weight, even more preferably at least 95% by weight, preferably at least 98% by weight, and even more Preferably at least 99% by weight. Processed alloys. Reference to the ANSI / AA identification system for the Aluminum Association (2022) with, aluminum alloy compositions shown in Table 1 below. It may include, but is not limited to: TABLE 1 Series Al First Second Alloy Contents: Alloy Elements (weight %) Element (if available) 1000 >99 - 2000 >86 Cu 3000 >94 Mn Li, Be, B, O, 4000 >70 Si Mg, Si, Sc, 5000 >88 Mg Ti, V, Cr, Mn, 6000 >91 Mg and Si Fe, Ni, Cu, 7000 >82 Zn Zn, Ga, Sr, Zr, Ag, Sn, Pb, Bi Specific examples of aluminum alloys are limited to these. not including, AA2024, AA5754, AA6060, AA6061, AA6063, AA6082, It includes AA6463 and AA7075. Looking at the primary sealing compound, at least one nickel ion is present. Sources include nickel sulfate, nickel sulfamate, nickel acetate, nickel nitrate, nickel carbonate, nickel fluoride and one or more of the above It can be selected from a group consisting of combinations of more than one. In an application, at least one source of nickel ions is nickel sulfate. It includes. In a preferred application, a nickel-ion source. It is supplied as a nickel-based aqueous solution. Nickel-based The concentration of nickel ions in the aqueous solution is approximately 0.5 to approximately 5.0 g / L, preferably approximately 0.8 to approximately 2.5 g / L, more Ideally, it should be in the range of approximately 1 to approximately 2 g / L. Total nickel ions in the primary sealing compound concentration approximately 0.3 to approximately 4.0 g / L, preferably approximately 0.5 to approximately 2.0 g / L, preferably around 0.8 It is in the range of approximately 1.8 g / L. At least one source of fluoride ions, such as potassium fluoride or potassium bifluoride, hydrogen fluoride, sodium fluoride, sodium bifluoride, ammonium fluoride, ammonium bifluoride, nickel fluoride, heavy metal fluoride complex and one or more of the above It can be selected from a group consisting of combinations. Preference In an application where at least one fluoride ion source is nickel fluoride and contains at least one additional source of fluoride ions. In practice, at least one fluoride ion source is potassium fluoride. It includes. In a preferred application, a fluoride ion source. 11 It is supplied as a fluoride-based aqueous solution. Fluoride-based aqueous The concentration of fluoride ions in the solution is approximately 100 to approximately 1500 ppm, preferably approximately 150 to approximately 1000 ppm, more preferably in the range of approximately 400 to approximately 800 ppm It is possible. Total fluoride in the primary sealing compound. ion concentration approximately 200 to approximately 1000 ppm, preferably approximately 400 to approximately 800 ppm, preferably around 500 It is in the range of approximately 700 ppm. Fluorine-based aqueous solution, optionally a carbonate salt. It may contain the following components: Carbonate salt, calcium carbonate. potassium carbonate, magnesium carbonate, sodium carbonate, lithium carbonate, barium carbonate, and one or more of the above. from a group consisting of combinations of more It can be selected. In one application, the carbonate salt is calcium carbonate. It contains carbonate salt in a fluorine-based aqueous solution. concentration approximately 0 to approximately 3.0 g / L, preferably approximately 0.5 to approximately 2.5 g / L, preferably approximately 1 to approximately It can be in the range of 2 g / L. As explained here, at least one nickel-ion source and at least one Separate addition of the fluoride ion source (i.e., separate components) unexpectedly, nickel and fluoride as a single component. Better results from an ion source (i.e., nickel fluoride) It provides. In an application, at least one nickel-ion source and at least a fluoride ion source separates the bath from different component sources are added separately. Accordingly, a preferred one In practice, the primary sealing compound is nickel ion welding and Fluoride ion source separate additions to the primary sealing compound. It contains at least one fluoride ion source to form and It contains at least a significant amount of nickel. In applications, at least 12 a nickel-ion source contains nickel fluoride and at least one The fluoride ion source contains a different fluoride compound. As explained here, the low-temperature bath is approximately 5.0 to approximately 7.0, preferably approximately 5.5 to approximately 6.5, more preferably at a pH value between approximately 5.7 and approximately 6.3. is maintained. The low-temperature bath is also approximately 15 to around 45°C, preferably around 20 to around 35°C, more preferably at a temperature between approximately 25 and approximately 30°C. is maintained. In applications, the low-temperature bath is the first step. Apply the sealing compound to the aluminum substrate at a pressure of approximately 0.5 to approximately 1.6 min / µm, preferably approximately 0.75 to approximately 1.4 minutes / µm, preferably around 0.9 to around 1.3 It is applied at a rate in the range of minutes / µm. At low temperatures. The leakage thickness should be approximately 3 to approximately 30 µm, preferably around 9 µm. to approximately 20 µm, more preferably approximately 12 to approximately 18 It has a thickness in the µm range. After the first sealing compound is applied, the aluminum bottom The layer is brought into contact with a high-temperature bath. The high-temperature bath is a second bath containing at least one silicate. It contains a sealing compound. Silicate, sodium silicate, potassium silicate, magnesium silicate, calcium silicate and above combinations of one or more of the specified It can be selected from the group formed. In one application, sodium silicate It is silicate and / or potassium silicate. Silicate is preferably the one mentioned above. It is a metasilicate of the listed compounds. In one application, The preferred choice is sodium metasilicate and / or potassium metasilicate. In one application, the silicate concentration is approximately 0.2 to approximately 3.0 g / L, preferably. approximately 0.37 to approximately 1.5 g / L, more preferably approximately 0.49 to silicate (Si₂O₃) concentration in the range of approximately 0.74 g / L 2 added to the high-temperature bath as an aqueous solution 13 Total silicate found in the high-temperature bath is being processed. concentration approximately 0.2 to approximately 3.5 g / L, preferably approximately 0.3 to approximately 1.5 g / L, preferably around 0.5 It is in the range of approximately 1.0 g / L. As explained here, the high-temperature bath is approximately 7.0 to approximately 12.0, preferably approximately 8.0 to approximately 11.0, more preferably at a pH value between approximately 8.5 and approximately 10.0 is maintained. The high-temperature bath is also approximately 70 to around 100°C, preferably around 75 to around 95°C, more preferably at a temperature between approximately 80 and approximately 90°C. is being held. In one application, the high-temperature bath is used for the second sealant compound approximately 1.5 to approximately 4 minutes / µm, preferably approximately 2 to approximately 3.5 minutes / µm, more preferably at a rate of approximately 2.5 to approximately 3 minutes / µm It is applied. High-temperature sealing is approximately 3 to approximately 30 µm, preferably approximately 9 to approximately 20 µm, more preferably a thickness of approximately 12 to approximately 18 µm has. The aluminum substrate is applied before or during any step in the process. It can then be rinsed off. Example process steps: cleaning, etching, anodizing, electro-coloring, low temperature sealing, high-temperature sealing and / or aging It includes. That is, the aluminum substrate is processed through the above processes. before or after any of them and / or all of them It can be rinsed off. Optionally, aluminum substrate sealing baths. After contact with the aluminum substrate, it is optional. contact with a third sealing bath It can be made. The third sealing bath, aluminum bottom 14 at least one aging process to improve the surface appearance of the layer. It is an aging bath containing a component. In one application, The aging component propenoic acid is a polycarboxylate. copolymer, phosphinocarboxylic acid and one or more of the above It is selected from a group consisting of combinations of more than one. In one application, the aging component in the aging bath concentration approximately 0.01 to approximately 4 g / L, preferably approximately 0.5 to approximately 3 g / L, preferably approximately 1 to approximately It is in the range of 2 g / L. Aluminum substrate, if desired, can be reduced. and / or contact with high-temperature sealing baths It can also be exposed to an aging bath first. As explained here, the aging bath is approximately 5.0 to approximately 7.0, preferably approximately 5.4 to approximately 6.4, more preferably at a pH value between approximately 5.7 and approximately 6.1 It is kept. The aging bath is also approximately 60 to approximately 100°C, preferably around 70 to around 100°C, more preferably around 80 to around 100°C, or even better around 90°C It is kept at a temperature ranging from approximately 100°C. In applications, the aluminum substrate is approximately 2 to approximately 10 minutes, preferably about 3 to about 8 minutes, more preferably a period of approximately 4 to approximately 6 minutes It is exposed to an aging bath throughout. The required favorable surface appearance of the aluminum substrate, Energy It can be measured using dispersed X-ray (EDX) analysis. A suitable EDX spectroscopy microscope, Thermo Fisher Axia ChemiSEM is available from Scientific (Waltham, MA). EDX analysis measures the chemical composition of the AAO layer. In practice, EDX analysis detects the presence of fluorine, oxygen, silicon, and nickel. a positive surface appearance of the aluminum substrate based on It has been evaluated. Fluoride on the surface of the aluminum substrate. The oxygen ratio is approximately in the range of 0.03:1 to approximately 2:1, The amount of silicon by weight on the surface of the aluminum substrate. approximately between 0.3% and approximately 2.0% of aluminum. The ratio of nickel to silicon on its surface is approximately 0.7:1 to approximately 3:1. It is within this range. Aluminum substrate before the sealing process of the AAO layer It can undergo multiple pre-processing steps. This process processes, including but not limited to cleaning, alkalizing It includes etching, anodizing, and electro-coloring. Electro coloring is derived from the anodizing process of the AAO layer. heavy metals to fill the resulting exposed pores and involves the use of electrical currents. Heavy metals typically include chromium, manganese, iron, cobalt, and nickel. first transition series which includes copper and especially tin They are elements. Heavy metal salts generally have a pH value of approximately They are used as sulfates, with concentrations ranging from 0.1 to approximately 2.0. The pH value of electrocoloring baths is adjusted with sulfuric acid. It is being adjusted and maintained. The coloring process takes approximately 10 to at a voltage of approximately 25 V and the resulting current density It occurs in this way. The aluminum substrate acts as the cathode. and the counter electrode is made of graphite or stainless steel or electro from the same material that dissolves in the coloring electrolyte It can occur. An example of a series of multiple preprocessing options is clearly shown here. Afsin, Pinar et al., Electro-Coloring, cited as a reference. Mechanism of Aluminum Anodic Oxides in Tin-Based Electrolytes, 14 This is described in the document Coatings 616 (2024). Aluminum an alloy substrate in an alkaline sodium hydroxide solution (2.5 M NaOH solution, 60°C, 3 minutes) is etched and then 3 minutes Neutralization is applied throughout with a 2M nitric acid base. Neutralization 16 subsequently aluminum substrate, aluminum counter electrode in a conventional two-electrode cell in 1.7 MH SO4 aqueous solution 2 4 It is anoded by applying 16 V DC at 19°C. The resulting... The thickness of the aluminum anodic oxide (AAO) layers is 11 ± 1 µm. When anodized, the aluminum substrate is rated at 17 V (alternating current) at 24°C. (current - 50 Hz) 0.1 M SnSO₄, 0.2 MH SO₄ and 0.05 M as stabilizers 4 2 4 electro in a bath containing sulfosalicylic acid It is colored. After the aluminum substrate is colored, the surface appearance is determined. To improve existing acid, alkali and / or corrosion resistance pores using the invention's sealing process It is being closed. The present invention now refers to the following non-limiting examples. This will be shown by finding it: Pre-treatment of aluminum substrate: For all examples and comparative examples, see aluminum substrate. The substrate is Aluminum Alloy 6063. That is, the aluminum substrate. 98.9% Al by weight, 0.7% Mg by weight, 0.4% Si by weight and small It has a general composition consisting of impurities. Aluminum substrate The layer undergoes the following steps: 1) A solution containing 50 g / L Alumal Clean at 65°C for 10 minutes. Pre-treatment with cleaner; 2) Alumal Etch 235 and 65 g / L NaOH for 6 minutes at 65°C alkaline etching; 3) 24 g / L Alumal Elox 557 and 170 g / LH SO for 15 µm 2 4 annotation and 4) 70 g / L Alumal Color 890, 25 g / L for 7 minutes at 25°C Electro-coloring in Alumal Color 891 and 16 g / LH SO. 2 4 17 All of the above alumal compounds are derived from MacDermid Enthone (West (Haven, CT) is available. Other pretreatment processes and the order of processing options is outside the scope of the present invention by a person skilled in the technique that can be used without separation can be evaluated. Sealing compounds and conditions according to Examples 1 and 2 are as follows: This is given in Table 2: TABLE 2 Leakproof Leakproof Leakproof Condition Condition Condition ik ik ik ar ar ar Composition 1 Composition 2 Composition 3 Aqueous 7 g / L NiSO 4 Solution 25°C Aqueous 1 g / L 85°C Example: Aqueous 4 g / L 1 Na or K 3 - - k 1 KF and min / µm silicate min / µm CaCO3 solution pH 6.1 pH 8.9 3 based solution Aqueous 7 g / L Aqueous 1.5 25°C Aqueous 1 g / L 85°C NiSO₄ g / L 98°C 4 Example 1 Na or K 3 propenoic acid solution 5 min k 2 min / µm silicate min / µm Aqueous 4 g / L acid pH 5.9 pH 6.1 solution pH 8.9 KF and its solution 18 CaCO 3 based solution To make the first sealant compound for Samples 1 and 2, 18 g Ni-based aqueous stock solution and 5 g KF and calcium carbonate-based aqueous stock solution in 1 L of deionized water It is being resolved. The available samples were mixed with a carbonate containing at least one fluoride ion source. Despite containing salt, experts in the field can cold seal it. aluminum substrate without carbonate salt component It can be applied. The first one does not contain a carbonate component. To make the sealant compound, 18 g of Ni-based aqueous stock solution and 3.5 g ammonium bifluoride based aqueous stock solution 1 It is dissolved in liters of deionized water. Then, at pH 6.1 is being held. To make the second sealing compound for Examples 1 and 2, use 25 g. sodium silicone-based hot sealing stock solution 1 liter It is dissolved in deionized water and then maintained at pH 8.9. Although the available samples contain sodium silicate, the technique is expert. 25 g of potassium per person in 1 liter of Si-based hot gasket stock solution a silicone-based hot melt produced by dissolving it in deionized water It can use a leak-proof seal. To prepare the aging bath for Sample 2, use 1.5 g of propenoic acid. The stock solution is dissolved in 1 L of deionized water. Then the pH is... It is held at 5.9. After aqueous bathing with sealing compounds, Aluminum substrate in contact with bath containing Sealing Composition 1. 19 is done. After a desired period of time, the aluminum substrate It is brought into contact with a bath containing Sealing Composition 2. Finally, according to Example 2, aluminum substrate sealing. It is brought into contact with an aging bath containing component 3. According to Comparative Examples 1-4, sealing compounds and The conditions are given in Table 3 below: TABLE 3 Sealing Requirements Sealing Requirements Composition 1 Composition 2 Aqueous 0.2 g / L Comparative dissolved F 30°C Example 1 based on H ZrF5 min - - 2 6 solution pH 6.0 Aqueous 0.1 g / L dissolved Si SiO based 2 solution Aqueous 2 g / L thiourea solution Comparative 65-80°C Aqueous 1 g / L 90°C Example 2: NiF 2-15 min, Na SiO 3 min 2 3 pH 4.5 solution pH 6.0 Aqueous 0.5 g / L Aqueous 0.1 g / L Comparative NiF solution at 60°C, polyacrylic at 90°C. 2 Example 3 Aqueous 1 g / L 1-3 acid 1-3 dissolved F min / µm solution min / µm H₂ZrF₂ based pH 4.0 pH 8.0 2 6 solution Wet weight 0.25% SLS solution Comparative 60°C Wet weight 25°C Example 4 Aqueous weight. 3.5% 5 min 3.0% H ZrF 5 min 2 6 SiO2 solution pH 4.5 solution pH 6.0 2 Each sealing bath according to Comparative Examples After it is formed, the aluminum substrate sealing compound It was brought into contact with a bath containing 1. Then, as desired. At the end of the period, aluminum substrate Sealing Composition 2 (available It is brought into contact with a bath containing (if applicable). Test Conditions: Examples and Comparative Examples of Aluminum Substrates According to the procedure, after ensuring a watertight seal, aluminum substrates It has been subjected to an alkali resistance test. The test was performed on an aluminum substrate. the sheet is in contact with a bath with a pH of 13 for 10 minutes. It is produced by this process. The amount of resistance is determined by the aluminum substrate. by evaluating the change in the color of the layers is being measured. The degree of color change is clearly shown here. The AATCC Assessment 1 Procedure (ISO105-) is given as a reference. Measured according to test standard A02 (Edition 4, 2005). Two The aluminum substrate set was tested for color change: (1) after alkali resistance test and (2) aluminum substrates subjected to a scratch test and then an alkali resistance test. after being caught. As shown in Fig. 1A and 1B (1), the sealing according to Example 1. the process resulted in a scratch and alkali resistant product in both tests. It provides an aluminum substrate. Under ISO105-A02 standard. There has been no change in color, which is due to the aluminum base. 21 This indicates that the plate passed the test. As shown in Fig. 2. such as, contact of the aluminum substrate with an aging bath (2) The additional step of having it done did not affect the color or surface appearance. While improving, it still passed the test. On the contrary, Comparative Examples 1-4 show the opposite in both tests. It has failed. Every comparative test shows that the previous systems... Sufficient alkali and scratch resistance on aluminum substrate. to show that it could not provide it, previous sealing procedures It is based on the following systems:  Comparative Example 1: EP0193964  Comparative Example 2: US7851025  Comparative Example 3: WO2023115366  Comparative Example 4: US20120244280 In each example, as shown in Figs. 1A and 1B (2)-(4), A visible color change occurred in the aluminum substrate. This is a break from previous methods of aluminum substrates in the current invention. sufficient scratch resistance or alkali resistance This means it does not meet the specifications. From the scratch test. The color change that occurs before and after indicates this sealing. processes in real-world conditions and in various industries It has been shown to be ineffective when subjected to rigorous testing. Finally, the present invention makes reference to a specific application. Although explained and demonstrated, the claims here all the general and specific features of the described invention and the invention In terms of scope, there is a linguistic gap between these two. It should be understood that this encompasses all possible expressions. 22

Claims

1. Ensuring the sealing of an aluminum substrate. It is a process aimed at and characterized by the following steps: It includes: a) the primary sealing compound of the aluminum substrate contact with an aqueous low-temperature bath containing to be made to happen; Here, at least one of the primary sealing compounds nickel ion source and at least one fluoride ion source including; b) second sealing compound of aluminum substrate contact with an aqueous high-temperature bath containing to be made to happen; Here, at least one of the second sealing compounds because it contains silicate and c) optionally, at least one of the aluminum substrates an aqueous aging bath containing an aging component being brought into contact with.

2. It is a process according to claim 1, and its characteristic is that steps a)-c) are sequential. It is the occurrence of this.

3. The process is according to claim 1 or 2, and its characteristic is; aluminum substrate. The substrate is an anodized aluminum substrate.

4. It is a process according to any of the previous requirements, and its characteristic is; contact of aluminum substrate with aqueous low-temperature bath It is electro-coloring before processing.

5. It is a process according to any of the previous requirements, and its characteristic is; The aluminum substrate contains an aluminum alloy, aluminum the alloy has at least approximately 90% aluminum content by weight 23 preferably with an aluminum content of at least approximately 95% by weight. It is the fact that.

6. It is a process according to any of the previous requirements, and its characteristic is; at least one nickel ion source is nickel sulfate, nickel sulfamate, nickel acetate, nickel nitrate, nickel carbonate, nickel fluoride and a combination of one or more of the above It is the selection from the group.

7. It is a process according to any of the previous requirements, and its characteristic is; at least one nickel-ion source in a nickel-based aqueous solution its inclusion, optionally nickel in nickel-based aqueous solution the concentration of ions is approximately 0.5 to approximately 5.0 g / L It is within the range.

8. A process according to any of the previous requirements, and its characteristic is: at least one fluoride ion source, potassium fluoride, potassium bifluoride, hydrogen fluoride, sodium fluoride, sodium bifluoride, ammonium fluoride, ammonium bifluoride, nickel fluoride, heavy metal fluoride complex and combinations of one or more of the above It is the selection from the group that is formed.

9. A process according to claim 8, characterized by having at least one fluoride ion. The source containing a fluoride-based aqueous solution is optional. as here, fluoride ions in a fluoride-based aqueous solution concentration in the range of approximately 100 to approximately 1500 ppm It is the fact that.

10. The process according to claim 9, its characteristic is; a fluorine-based aqueous solution. It must also contain at least one carbonate salt, optionally here. at least carbonate salts such as calcium carbonate, potassium carbonate, magnesium carbonate, sodium carbonate, lithium carbonate, barium 24 carbonate and one or more of the above-mentioned It is the selection of a group consisting of combinations.

11. It is a process according to any of the previous requirements, and its characteristic is; at least one nickel-ion source and at least one fluoride-ion source Separate sealing compound components for low-temperature bath to be added separately, optionally at least one The fluoride ion source should be nickel-free, at least to a large extent. thus at least one nickel ion source and at least one fluoride ion source separate additions to the aqueous low-temperature bath of the source It is the creation of.

12. It is a process according to any of the previous requirements, and its characteristic is; aqueous low temperature bath approximately 15 to approximately 45°C stored at a temperature within the range and / or low water content the temperature bath on the aluminum substrate is approximately 0.5 to Sealing at a rate of approximately 1.6 minutes / µm formation and / or low temperature bath of aluminum substrate a thickness ranging from approximately 3 to approximately 30 µm has a leak-proof seal and / or low-temperature water seal. the bath has a pH value of approximately 5 to approximately 7 It is about preservation.

13. It is a process according to any of the previous requirements, and its characteristic is; at least one silicate: sodium silicate, potassium silicate, magnesium silicate, calcium silicate and optionally the above consisting of a combination of one or more of the specified elements The selection from the group requires that at least one silicate be a metasilicate.

14. It is a process according to any of the previous requirements, and its characteristic is; at least one silicate, optionally in a silicone-based aqueous solution. the presence of a solution, silicate in a silicone-based aqueous solution concentration in the range of approximately 0.2 to approximately 3.0 g / L It is the fact that.

15. It is a process according to any of the previous requirements, and its characteristic is; aqueous high-temperature bath approximately 70 to approximately 100°C stored at a temperature within the range and / or high water content the temperature bath on the aluminum substrate is approximately 1.5 to sealing at a rate of approximately 4 minutes / µm and / or high temperature bath on aluminum substrate a thickness ranging from approximately 3 to approximately 30 µm sealing and / or high-temperature aqueous bath maintained at a pH value between approximately 7 and approximately 12. It is done.

16. It is a process according to any of the previous requirements, and its characteristic is; the aging component propenoic acid, polycarboxylate copolymer, phosphinocarboxylic acid and one or more of the above It is the selection of a group consisting of combinations of more than one.

17. It is a process according to any of the previous requirements, and its characteristic is; concentration of the aging component in the aging bath should be in the range of approximately 0.01 to approximately 4 g / L and / or the aging bath temperature is approximately between 60 and 100°C. storage at a certain temperature and / or aluminum substrate for a period of approximately 2 to approximately 10 minutes contact with aging bath and / or aging the bath has a pH value of approximately 5 to approximately 7 It is about preservation.

18. For sealing an anodized aluminum substrate. It is a multi-bathroom system and its features include the following: 26 a) at least one nickel ion source and at least one fluoride ion source containing the primary sealing compound containing the source first bathroom; b) a second sealing compound containing at least one silicate including a second bathroom and c) optionally containing at least one aging component third bathroom.

19. System according to claim 18, characterized by having at least one nickel ion. the source and at least one fluoride ion source separately sealed The composition's components are added separately to the first bath. It is done.

20. A system according to claim 18 or 19, characterized by having at least one nickel. ion source nickel sulfate, nickel sulfamate, nickel acetate, nickel nitrate, nickel carbonate, nickel fluoride and one or more of the above It is the selection of a group consisting of combinations of more than one.

21. The system is defined according to either of claims 18-20, and its characteristic is: the first bath should be at a temperature between approximately 15 and approximately 45°C. kept at temperature and / or here the second bath approximately 70 to It is kept at a temperature of approximately 100°C.

22. Anodized to create a sealing layer. a multi-part for processing an aluminum substrate It is a kit, and its features include the following: a) at least one nickel-ion source and at least one fluoride source primary sealing compound containing; b) a second sealing composition containing at least one silicate and c) an aging process that includes at least one aging component composition. 27 23. According to claim 22, it is a multiple part, characterized by having at least one nickel. ion source and separate components of at least one fluoride ion source These are added separately to the primary sealant compound. 28