Composition for degreasing, polishing and passivating copper alloy, preparation method and treatment method

Abstract

The embodiment of the invention discloses a composition for degreasing, polishing and passivating copper alloy. The composition can be used for degreasing, polishing and passivating the copper alloy at the same time. The composition comprises: a surfactant including an active agent component, isomeric alcohol polyoxyethylene ether and fatty alcohol polyoxyethylene ether, the active agent component being selected from one or more of polyether siloxane and tetramethyl decynediol; the chemical polishing agent comprises an acid component, hydrogen peroxide and polyethylene glycol, wherein the acid components comprise phosphoric acid and sulfuric acid; the passivation protective agent comprises phosphotungstic acid and a passivation component, and the passivation component is selected from at least one of sodium tungstate, benzotriazole and sodium benzoate; and water. The embodiment of the invention further provides a preparation method of the composition for degreasing, polishing and passivating the copper alloy and a treatment method for degreasing, polishing and passivating the copper alloy.

Description

Technical Field

[0001] The invention relates to the technical field of copper alloy degreasing, polishing and passivation, and in particular to a composition, a preparation method and a treatment method for copper alloy degreasing, polishing and passivation. Background Art

[0002] Degreasing, chemical polishing and passivation protection of copper alloys are common processing and storage protection processes for copper alloys. The degreasing process is to clean the oil stains on the surface of the copper alloy to prepare for the subsequent chemical polishing and passivation; the chemical polishing process is to remove the oxide layer on the surface of the copper alloy, and at the same time micro-etch the surface to make the surface smoother and brighter, and even make the surface produce a mirror reflection effect; the passivation process is to form a dense protective film on the surface of the copper alloy, so that the workpiece will not be oxidized and cause discoloration even if it is exposed to the air for a long time, and the original color of the copper alloy is maintained.

[0003] At present, copper alloy degreasing, chemical polishing and passivation are usually three independent process steps, the order is first degreasing, then chemical polishing, and finally passivation. The three independent process steps inevitably require three types of treatment agents, which increases the difficulty of use for users. Summary of the invention

[0004] One purpose of the embodiments of the present application is to solve at least one problem in the above background and provide corresponding beneficial effects.

[0005] Another object of an embodiment of the present application is to provide a composition for degreasing, polishing and passivation of copper alloys, which can be used for degreasing, polishing and passivation of copper alloys at the same time.

[0006] Another purpose of the embodiments of the present application is to provide a method for preparing a composition for degreasing, polishing and passivation of copper alloys, which can be used to prepare a composition for degreasing, polishing and passivation of copper alloys.

[0007] Another purpose of the embodiment of the present application is to provide a method for degreasing, polishing and passivating a copper alloy based on the composition for degreasing, polishing and passivating a copper alloy, so as to reduce the difficulty of use for users.

[0008] The embodiments of the present application mainly achieve the above objectives through the following technical solutions.

[0009] In one aspect, the present application embodiment provides a composition for degreasing, polishing and passivation of a copper alloy, comprising:

[0010] A surfactant, comprising an active agent component, isomeric alcohol polyoxyethylene ether, and fatty alcohol polyoxyethylene ether, wherein the active agent component is selected from any one of polyether siloxane and tetramethyldecynediol;

[0011] A chemical polishing agent, comprising an acid component, hydrogen peroxide, and polyethylene glycol; wherein the acid component comprises phosphoric acid and sulfuric acid;

[0012] A passivation protective agent, comprising phosphotungstic acid and a passivation component, wherein the passivation component is selected from at least one of sodium tungstate, benzotriazole and sodium benzoate; and

[0013] water.

[0014] In some technical solutions, the mass ratio of the surfactant, the chemical polishing agent and the passivation protective agent is 12-13:45-55:7-8.

[0015] In some technical schemes, the mass ratio of the active agent component, the isomeric alcohol polyoxyethylene ether, and the fatty alcohol polyoxyethylene ether is 2-3:5:5-6.

[0016] In some technical schemes, the mass ratio of the phosphoric acid, the sulfuric acid, the hydrogen peroxide, and the polyethylene glycol is 15:15:10 to 15:5.

[0017] In some technical solutions, the mass ratio of the phosphotungstic acid to the passivation component is 3-5:3-5.

[0018] In some technical schemes, the acid component of the chemical polishing agent also includes hydroxyethylidene diphosphoric acid, and the mass ratio of the phosphoric acid to the hydroxyethylidene diphosphoric acid is 15:5.

[0019] In some technical solutions, the mass ratio of the surfactant, the chemical polishing agent, the passivation protective agent and the water is 12-13:45-55:7-8:25-34.

[0020] In some technical solutions, based on 100 parts by weight of the composition, the water content is the balance.

[0021] In some technical solutions, the active agent component is selected from tetramethyldecynediol, the mass fraction of the isomeric alcohol polyoxyethylene ether is 5%, the mass fraction of the fatty alcohol polyoxyethylene ether is 5%, and the mass fraction of the tetramethyldecynediol is 2%;

[0022] The mass fraction of the phosphoric acid is 15%, the mass fraction of the sulfuric acid is 15%, the mass fraction of the hydrogen peroxide is 15%, and the mass fraction of the polyethylene glycol is 5%;

[0023] The passivation component is selected from benzotriazole, the mass fraction of the phosphotungstic acid is 5%, and the mass fraction of the benzotriazole is 3%.

[0024] In some technical solutions, the active agent component is selected from polyether siloxane, the mass fraction of the polyether siloxane is 3%, the mass fraction of the isomeric alcohol polyoxyethylene ether is 5%, and the mass fraction of the fatty alcohol polyoxyethylene ether is 5%;

[0025] The mass fraction of the phosphoric acid is 15%, the mass fraction of the sulfuric acid is 15%, the mass fraction of the hydrogen peroxide is 10%, and the mass fraction of polyethylene glycol is 5%;

[0026] The passivation component is selected from sodium tungstate, the mass fraction of the sodium tungstate is 3%, and the mass fraction of the phosphotungstic acid is 5%.

[0027] In some technical solutions, the active agent component is selected from polyether siloxane, the mass fraction of polyether siloxane is 2%, the mass fraction of isomeric alcohol polyoxyethylene ether is 5%, and the mass fraction of fatty alcohol polyoxyethylene ether is 6%;

[0028] The acid component also includes hydroxyethylidene diphosphoric acid, wherein the mass fraction of the phosphoric acid is 15%, the mass fraction of the sulfuric acid is 15%, the mass fraction of the hydroxyethylidene diphosphoric acid is 5%, the mass fraction of the hydrogen peroxide is 15%, and the mass fraction of the polyethylene glycol is 5%;

[0029] The passivation component is selected from sodium tungstate and sodium benzoate, the mass fraction of the sodium tungstate is 3%, the mass fraction of the phosphotungstic acid is 3%, and the mass fraction of the sodium benzoate is 1%.

[0030] In one aspect, the present application provides a method for preparing a composition for degreasing, polishing and passivation of a copper alloy, which is used to prepare the composition for degreasing, polishing and passivation of a copper alloy as claimed in claim 1, and the preparation method comprises the following steps:

[0031] The acid component of the chemical polishing agent is added into water and stirred evenly, and then hydrogen peroxide, polyethylene glycol, a surfactant and a passivation protective agent are added and stirred evenly to obtain a copper alloy degreasing, polishing and passivation composition.

[0032] In one aspect, the present application embodiment provides a method for degreasing, polishing and passivation of a copper alloy, comprising:

[0033] A composition for degreasing, polishing and passivation of a copper alloy is prepared into a first treatment liquid with a first use concentration and a second treatment liquid with a second use concentration; wherein the first use concentration is greater than the second use concentration;

[0034] Performing a degreasing and polishing treatment on the copper alloy workpiece using a first treatment liquid;

[0035] After the degreasing and polishing treatment, the copper alloy workpiece is passivated using a second treatment liquid.

[0036] In some technical solutions,

[0037] The first use concentration is between 30-60%;

[0038] The second use concentration is between 5-15%.

[0039] The beneficial effects of the embodiments of the present invention include:

[0040] 1. In some embodiments, the embodiments of the present application provide a composition for degreasing, polishing and passivation of copper alloys, which can be used for degreasing, polishing and passivation of copper alloys at the same time.

[0041] 2. In some embodiments, the embodiments of the present application provide a method for preparing a composition for degreasing, polishing and passivation of a copper alloy, which can be used to prepare a composition for degreasing, polishing and passivation of a copper alloy.

[0042] 3. In some embodiments, the embodiments of the present application provide a method for degreasing, polishing and passivation of copper alloy to reduce the difficulty of use for users. DETAILED DESCRIPTION

[0043] The present invention is described in further detail below so that those skilled in the art can implement it according to the description.

[0044] The terms "first", "second", "third", etc. in the embodiments of the present application are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first", "second", etc. may explicitly or implicitly include at least one of the features.

[0045] Furthermore, the terms "comprises", "includes", "contains" and any variations thereof are intended to cover non-exclusive inclusions. For example, a process, method, system, product or device comprising a series of steps or units is not limited to the listed steps or units, but may optionally include steps or units not listed, or may optionally include other steps or units inherent to these processes, methods, products or devices.

[0046] It should also be noted that, unless otherwise clearly specified and limited, the terms "connected" and "connected" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium.

[0047] In addition to the above, it is still necessary to emphasize that the reference to "embodiment" in this article means that the specific features, structures or characteristics described in conjunction with the embodiment may be included in at least one embodiment of the present application. The appearance of this phrase in various places in the specification does not necessarily refer to the same embodiment, nor is it an independent or alternative embodiment that is mutually exclusive with other embodiments. It is explicitly and implicitly understood by those skilled in the art that the embodiments described herein can be combined with other embodiments.

[0048] In a first aspect, the present application provides a composition for degreasing, polishing and passivation of a copper alloy, comprising:

[0049] A surfactant, including an active agent component, isomeric alcohol polyoxyethylene ether, and fatty alcohol polyoxyethylene ether, wherein the active agent component is selected from one or more of polyether siloxane and tetramethyldecynediol;

[0050] A chemical polishing agent, comprising an acid component, hydrogen peroxide, and polyethylene glycol, wherein the acid component comprises phosphoric acid and sulfuric acid;

[0051] A passivation protective agent, comprising phosphotungstic acid and a passivation component, wherein the passivation component is selected from one or more of sodium tungstate, benzotriazole and sodium benzoate; and

[0052] water.

[0053] The composition provided in the examples of the present application mainly includes three parts: a surfactant chemical polishing agent and a passivation protective agent, and can be used for degreasing, polishing and passivation of copper alloys at the same time.

[0054] Surfactants have strong wettability, strong permeability, and strong emulsification. The compound can achieve excellent degreasing effect. Under the micro-corrosion of chemical polishing components, it can more thoroughly clean the surface of the workpiece. On the other hand, it can provide very low surface tension, allowing the chemical polishing components to better wet and flatten the workpiece surface, thereby helping to achieve better flattening and brightening effects.

[0055] Chemical polishing agents mainly include acid components, hydrogen peroxide, and polyethylene glycol. The acid components combined with the oxidant hydrogen peroxide can effectively remove the oxide scale on the surface of the copper alloy, and micro-corrode the surface of the workpiece to produce a polishing and brightening effect. Polyethylene glycol fills the surface micropores during the polishing process, hindering the agent from further corrosive reaction with the substrate, thereby playing a role in peak cutting and smoothing.

[0056] The passivation protective agent mainly includes two or more of sodium tungstate, phosphotungstic acid, benzotriazole and sodium benzoate, which forms a dense protective layer by adsorption on the surface of the copper alloy, thereby playing a passivation protective role and preventing oxidation discoloration during storage.

[0057] In some embodiments, the mass ratio of the active agent component, the isomeric alcohol polyoxyethylene ether, and the fatty alcohol polyoxyethylene ether is 2-3:5:5-6.

[0058] In some embodiments, the mass ratio of the phosphoric acid, the sulfuric acid, the hydrogen peroxide, and the polyethylene glycol is 15:15:10 to 15:5.

[0059] In some embodiments, the mass ratio of the phosphotungstic acid to the passivation component is 3-5:3-5.

[0060] In some embodiments, the mass ratio of the surfactant, the chemical polishing agent, and the passivation protective agent is 12-13:45-55:7-8.

[0061] In some embodiments, the acid component of the chemical polishing agent further includes hydroxyethylidene diphosphoric acid, and the mass ratio of the phosphoric acid to the hydroxyethylidene diphosphoric acid is 15:5.

[0062] In some embodiments, the mass ratio of the surfactant, the chemical polishing agent, the passivation protective agent and the water is 12-13:45-55:7-8:25-34.

[0063] In some embodiments, based on 100 parts by weight of the composition, the water content is the balance.

[0064] In some embodiments, the mass fraction of the surfactant is 12-13%.

[0065] In some embodiments, the mass fraction of the chemical polishing agent is 45-55%.

[0066] In some embodiments, the mass fraction of the passivation protective agent is 7-8%.

[0067] In some embodiments, the active agent component is selected from tetramethyldecynediol, the mass fraction of the isomeric alcohol polyoxyethylene ether is 5%, the mass fraction of the fatty alcohol polyoxyethylene ether is 5%, and the mass fraction of the tetramethyldecynediol is 2%;

[0068] The mass fraction of the phosphoric acid is 15%, the mass fraction of the sulfuric acid is 15%, the mass fraction of the hydrogen peroxide is 15%, and the mass fraction of the polyethylene glycol is 5%;

[0069] The passivation component is selected from benzotriazole, the mass fraction of the phosphotungstic acid is 5%, and the mass fraction of the benzotriazole is 3%.

[0070] In some embodiments, the active agent component is selected from polyether siloxane, the mass fraction of the polyether siloxane is 3%, the mass fraction of the isomeric alcohol polyoxyethylene ether is 5%, and the mass fraction of the fatty alcohol polyoxyethylene ether is 5%;

[0071] The mass fraction of the phosphoric acid is 15%, the mass fraction of the sulfuric acid is 15%, the mass fraction of the hydrogen peroxide is 10%, and the mass fraction of polyethylene glycol is 5%;

[0072] The passivation component is selected from sodium tungstate, the mass fraction of the sodium tungstate is 3%, and the mass fraction of the phosphotungstic acid is 5%.

[0073] In some embodiments, the active agent component is selected from polyether siloxane, the mass fraction of polyether siloxane is 2%, the mass fraction of isomeric alcohol polyoxyethylene ether is 5%, and the mass fraction of fatty alcohol polyoxyethylene ether is 6%;

[0074] The acid component also includes hydroxyethylidene diphosphoric acid, wherein the mass fraction of the phosphoric acid is 15%, the mass fraction of the sulfuric acid is 15%, the mass fraction of the hydroxyethylidene diphosphoric acid is 5%, the mass fraction of the hydrogen peroxide is 15%, and the mass fraction of the polyethylene glycol is 5%;

[0075] The passivation component is selected from sodium tungstate and sodium benzoate, the mass fraction of the sodium tungstate is 3%, the mass fraction of the phosphotungstic acid is 3%, and the mass fraction of the sodium benzoate is 1%.

[0076] In a second aspect, the present application also provides a method for preparing a copper alloy degreasing, polishing and passivation composition, which can be used to prepare the copper alloy degreasing, polishing and passivation composition described in the first aspect, and the preparation method comprises the following steps:

[0077] The acid component of the chemical polishing agent is added into water and stirred evenly, and then hydrogen peroxide, polyethylene glycol, a surfactant and a passivation protective agent are added and stirred evenly to obtain a copper alloy degreasing, polishing and passivation composition.

[0078] In a third aspect, the present application also provides a method for degreasing, polishing and passivation of a copper alloy, comprising the following steps:

[0079] Step S101, taking a first treatment liquid with a first working concentration and a second treatment liquid with a second working concentration;

[0080] The first treatment liquid is configured according to the composition for degreasing, polishing and passivation of copper alloys described in the first aspect of the embodiment; specifically, water and the composition for degreasing, polishing and passivation of copper alloys are mixed to obtain the first treatment liquid, wherein the first usage concentration is the mass ratio of the composition for degreasing, polishing and passivation of copper alloys to the first treatment liquid.

[0081] The second treatment liquid is configured according to the composition for degreasing, polishing and passivation of copper alloys described in the embodiment of the first aspect; specifically, water and the composition for degreasing, polishing and passivation of copper alloys are mixed to obtain the second treatment liquid, wherein the second usage concentration is the mass ratio of the composition for degreasing, polishing and passivation of copper alloys to the second treatment liquid.

[0082] Step S102: Degreasing and polishing the copper alloy workpiece to be processed using the first processing liquid.

[0083] Step S103: After the degreasing and polishing treatment, the copper alloy workpiece is first rinsed with pure water.

[0084] Step S104: After the first rinsing, the copper alloy workpiece is passivated using a second treatment liquid.

[0085] Step S105: After the passivation treatment, the copper alloy workpiece is rinsed with pure water for a second time.

[0086] Step S106: After the second rinsing, the copper alloy workpiece is dried.

[0087] In some embodiments, the first concentration is greater than the second concentration. Thus, the treatment method of the embodiment of the present application achieves the effects of degreasing, polishing and passivation by adjusting the concentration of the composition. Specifically, when the concentration is high or low, the competition between the chemical polishing component and the passivation component leads to different effects: when the concentration is high, such as 30-60% (mass ratio), the working liquid contains more chemical polishing components, and the micro-corrosion ability of the copper alloy workpiece is stronger than the passivation protection component, so that the agent reflects the characteristics of chemical polishing, and a specific surfactant is added to the formula, which plays a role in degreasing and assisting in leveling the bright copper alloy during the chemical polishing process; when the concentration is low, such as 5-15% (mass ratio), the passivation component contained in the working liquid is stronger than the chemical polishing ability, so that the agent reflects the characteristics of passivation protection. In some embodiments, the first concentration is between 30-60%.

[0088] In some embodiments, the second use concentration is between 5-15%.

[0089] In some embodiments, the degreasing and polishing treatment of the copper alloy workpiece with the first treatment liquid includes:

[0090] The copper alloy sample is degreased and chemically polished using the first treatment solution at a first use concentration, according to a first treatment temperature and a first treatment time.

[0091] In some embodiments, the first treatment temperature is between 25-45°C.

[0092] In some embodiments, the second treatment time is between 0.5-3 minutes.

[0093] In some embodiments, the passivation treatment of the copper alloy workpiece with the second treatment solution includes:

[0094] The copper alloy sample is subjected to passivation protection treatment using the second treatment solution at the second use concentration, according to the second treatment temperature and the second treatment time, and finally rinsed with pure water and dried to obtain a treated copper alloy part.

[0095] In some embodiments, the second processing temperature is between 25-45°C.

[0096] In some embodiments, the second treatment time is between 5-8 minutes.

[0097] In some embodiments, the first rinse time is between 1-3 minutes and the temperature is 25°C.

[0098] In some embodiments, the second rinse time is between 1-3 minutes and the temperature is 25°C.

[0099] In some embodiments, the second rinse is performed 2-3 times.

[0100] In some embodiments, the drying temperature is 80-100°C.

[0101] In some embodiments, the drying time is between 10-15 minutes.

[0102] In some embodiments, the first concentration is equal to or less than the second concentration, and the first treatment temperature is greater than or equal to 55°C. That is, in addition to adjusting the concentration of the reagent to achieve degreasing, polishing and passivation, the degreasing and chemical polishing functions can also be achieved by increasing the first treatment temperature (such as a temperature greater than 55°C) under the condition that the first concentration is low (e.g., 10-15%). The principle is that increasing the temperature will increase the micro-corrosion ability of the polishing component to the copper alloy, and the chemical polishing ability is greater than the passivation protection ability, thereby reflecting the ability of chemical polishing.

[0103] <Preparation Example of Composition for Copper Alloy Processing>

[0104] According to the preparation method shown in S200 below, according to the formulations of Examples 1-3 and Comparative Examples 1-6, corresponding compositions for copper alloy processing are prepared.

[0105] S200, taking a container, adding water to the container; then adding the acid component of the chemical polishing agent into the water and stirring, after stirring evenly, adding other components in the formula of the copper alloy processing composition and stirring evenly, that is, obtaining the corresponding copper alloy processing composition.

[0106] Embodiment 1:

[0107] The formula of Example 1 is as follows:

[0108] A composition for processing copper alloys, comprising:

[0109] Pure water 30%;

[0110] Surfactants, including 5% of isomeric alcohol polyoxyethylene ether, 5% of fatty alcohol polyoxyethylene ether, and 2% of tetramethyldecynediol;

[0111] A chemical polishing agent, comprising an acid component, 15% hydrogen peroxide, and 5% polyethylene glycol, wherein the acid component comprises 15% phosphoric acid and 15% sulfuric acid;

[0112] The passivation protective agent includes 5% of phosphotungstic acid and 3% of benzotriazole.

[0113] Embodiment 2:

[0114] The formula of Example 2 is as follows:

[0115] A composition for processing copper alloys, comprising:

[0116] Pure water 34%;

[0117] Surfactants, including 3% polyether siloxane, 5% isomeric alcohol polyoxyethylene ether, and 5% fatty alcohol polyoxyethylene ether;

[0118] A chemical polishing agent, comprising an acid component, 10% hydrogen peroxide, and 5% polyethylene glycol, wherein the acid component comprises 15% phosphoric acid and 15% sulfuric acid;

[0119] The passivation protective agent includes 3% sodium tungstate and 5% phosphotungstic acid.

[0120] Embodiment 3:

[0121] The formula of Example 3 is as follows:

[0122] A composition for processing copper alloys, comprising:

[0123] Pure water 25%;

[0124] Surfactants, including 2% polyether siloxane, 5% isomeric alcohol polyoxyethylene ether, and 6% fatty alcohol polyoxyethylene ether;

[0125] A chemical polishing agent, comprising an acid component, 15% hydrogen peroxide, and 5% polyethylene glycol, wherein the acid component comprises 15% phosphoric acid, 15% sulfuric acid, and 5% hydroxyethylidene diphosphonic acid;

[0126] The passivation protective agent includes 3% sodium tungstate, 3% phosphotungstic acid and 1% sodium benzoate.

[0127] Comparative Example 1:

[0128] The formula of Comparative Example 1 is as follows:

[0129] A composition for processing copper alloys, comprising:

[0130] Pure water 42%;

[0131] A chemical polishing agent, comprising an acid component, 15% hydrogen peroxide, and 5% polyethylene glycol, wherein the acid component comprises 15% phosphoric acid and 15% sulfuric acid;

[0132] The passivation protective agent includes 5% of phosphotungstic acid and 3% of benzotriazole.

[0133] Comparative Example 2:

[0134] The formula of Comparative Example 2 is as follows:

[0135] A composition for processing copper alloys, comprising:

[0136] Pure water 45%;

[0137] Surfactants, including 5% of isomeric alcohol polyoxyethylene ether, 5% of fatty alcohol polyoxyethylene ether, and 2% of tetramethyldecynediol;

[0138] A chemical polishing agent, comprising an acid component and 5% polyethylene glycol, wherein the acid component comprises 15% phosphoric acid and 15% sulfuric acid;

[0139] The passivation protective agent includes 5% of phosphotungstic acid and 3% of benzotriazole.

[0140] Comparative Example 3:

[0141] The formula of Comparative Example 3 is as follows:

[0142] A composition for processing copper alloys, comprising:

[0143] Pure water 35%;

[0144] Surfactants, including 5% of isomeric alcohol polyoxyethylene ether, 5% of fatty alcohol polyoxyethylene ether, and 2% of tetramethyldecynediol;

[0145] A chemical polishing agent, comprising an acid component and 15% hydrogen peroxide, wherein the acid component comprises 15% phosphoric acid and 15% sulfuric acid;

[0146] The passivation protective agent includes 5% of phosphotungstic acid and 3% of benzotriazole.

[0147] Comparative Example 4:

[0148] The formula of Comparative Example 4 is as follows:

[0149] A composition for processing copper alloys, comprising:

[0150] Pure water 38%;

[0151] Surfactants, including 5% of isomeric alcohol polyoxyethylene ether, 5% of fatty alcohol polyoxyethylene ether, and 2% of tetramethyldecynediol;

[0152] The chemical polishing agent comprises an acid component, 15% hydrogen peroxide and 5% polyethylene glycol, wherein the acid component comprises 15% phosphoric acid and 15% sulfuric acid.

[0153] Comparative Example 5:

[0154] The formula of Comparative Example 5 is as follows:

[0155] A composition for processing copper alloys, comprising:

[0156] Pure water 45%;

[0157] Surfactants, including 5% of isomeric alcohol polyoxyethylene ether, 5% of fatty alcohol polyoxyethylene ether, and 2% of tetramethyldecynediol;

[0158] A chemical polishing agent, comprising an acid component, 15% hydrogen peroxide, and 5% polyethylene glycol, wherein the acid component comprises 15% phosphoric acid;

[0159] The passivation protective agent includes 5% of phosphotungstic acid and 3% of benzotriazole.

[0160] Comparative Example 6:

[0161] The formula of Comparative Example 6 is as follows:

[0162] A composition for processing copper alloys, comprising:

[0163] Pure water 45%;

[0164] Surfactants, including 5% of isomeric alcohol polyoxyethylene ether, 5% of fatty alcohol polyoxyethylene ether, and 2% of tetramethyldecynediol;

[0165] A chemical polishing agent, comprising an acid component, 15% hydrogen peroxide, and 5% polyethylene glycol, wherein the acid component comprises 15% sulfuric acid;

[0166] The passivation protective agent includes 5% of phosphotungstic acid and 3% of benzotriazole.

[0167] <Experimental example>

[0168] Take copper alloy material, process the copper alloy material into 10cm×5cm×0.3cm thin slices as copper alloy samples; set up 18 experimental groups 1-18, take 18 thin slices with the same size and the same surface processing state as copper alloy samples of experimental groups 1-18 respectively; experimental groups 1 and 10-17 all select the composition of Example 1 as an integrated test liquid to degrease, chemically polish and passivate the copper alloy samples for testing; experimental groups 2-9 respectively select the composition of Examples 2-3 and Comparative Examples 1-6 as an integrated test liquid to degrease, chemically polish and passivate the copper alloy samples for testing; experimental group 18 selects the composition of Comparative Examples 7-9 as the test liquid, degrease, chemically polish and passivate the copper alloy samples for testing. Record the corresponding treatment concentration, temperature and time of each group.

[0169] (I) The specific test treatment of each group in experimental groups 1-17 includes the following steps:

[0170] Before treatment, the surface reflectivity at the center point of each group of copper alloy specimens was measured and recorded;

[0171] The test liquid of each group is configured into a first treatment liquid of a first use concentration (higher concentration) and a second treatment liquid of a second use concentration (lower concentration);

[0172] Degreasing and polishing step: at a first use concentration (i.e., the use concentration of degreasing and polishing corresponding to Table 1), according to a first treatment temperature (i.e., the treatment time of degreasing and polishing corresponding to Table 1) and a first treatment time (i.e., the treatment temperature of degreasing and polishing corresponding to Table 1), the copper alloy sample is degreased and chemically polished using a first treatment liquid;

[0173] After degreasing and polishing, the copper alloy specimens were rinsed with pure water;

[0174] Passivation protection step: at a second use concentration (i.e., the use concentration of the passivation protection corresponding to Table 1), according to a second treatment temperature (i.e., the treatment time of the passivation protection corresponding to Table 1) and a second treatment time (i.e., the treatment temperature of the passivation protection corresponding to Table 1), the copper alloy sample is subjected to passivation protection treatment using a second treatment solution;

[0175] After passivation protection treatment, rinse with pure water and dry after rinsing;

[0176] Observe the appearance of the dried copper alloy samples (including cleanliness and color uniformity);

[0177] For copper alloy samples with qualified appearance, the surface reflectivity (surface reflectivity of the center point after degreasing, chemical polishing and passivation protection treatment) was tested again. For copper alloy samples with surface reflectivity greater than 80%, they were placed in a constant temperature oven at 60°C for high-temperature discoloration resistance test. The time when oxidation discoloration occurs on the surface of the copper alloy samples was observed to compare the effect of passivation protection.

[0178] The test conditions of each group are shown in Table 1 below.

[0179] Table 1. Test conditions of experimental groups 1-17

[0180]

[0181]

[0182] (II) The specific test process of experimental group 18 includes the following steps:

[0183] The existing degreasing composition (commercially available product) is configured into a third treatment liquid with a third use concentration, the existing polishing composition (commercially available product) is configured into a fourth treatment liquid with a fourth use concentration, and the existing passivation composition (commercially available product) is configured into a fifth treatment liquid with a fifth use concentration;

[0184] Degreasing step: degreasing the copper alloy sample using a first treatment liquid at a first use concentration (i.e., the degreasing use concentration corresponding to Table 2), according to a first treatment temperature (i.e., the degreasing treatment time corresponding to Table 2) and a first treatment time (i.e., the degreasing treatment temperature corresponding to Table 2);

[0185] Chemical polishing step: after the degreasing treatment, the copper alloy sample is degreased using a second treatment liquid at a second use concentration (i.e., the use concentration of the chemical polishing corresponding to Table 2), according to a second treatment temperature (i.e., the treatment time of the chemical polishing corresponding to Table 2) and a second treatment time (i.e., the treatment temperature of the chemical polishing corresponding to Table 2);

[0186] Passivation protection step: after chemical polishing, at a third use concentration (i.e., the use concentration of the passivation protection corresponding to Table 2), according to a third treatment temperature (i.e., the treatment time of the passivation protection corresponding to Table 2) and a third treatment time (i.e., the treatment temperature of the passivation protection corresponding to Table 2), the copper alloy sample is subjected to passivation protection treatment using the second treatment solution, and finally rinsed with pure water and dried;

[0187] Observe the appearance of the dried copper alloy samples (including cleanliness and color uniformity);

[0188] For copper alloy samples with qualified appearance, the surface reflectivity (surface reflectivity of the center point after degreasing, chemical polishing and passivation protection treatment) was tested again. For copper alloy samples with surface reflectivity greater than 80%, they were placed in a constant temperature oven at 60°C for high-temperature discoloration resistance test. The time when oxidation discoloration occurs on the surface of the copper alloy samples was observed to compare the effect of passivation protection.

[0189] The test conditions of experimental group 18 are specifically shown in Table 2.

[0190] Table 2. Test conditions of experimental group 18

[0191]

[0192] Experimental results and analysis :

[0193] The experimental results are shown in Table 3.

[0194] Table 3. Results

[0195]

[0196]

[0197] From the above results, we can see that:

[0198] 1. The copper alloy specimens of experimental groups 1-3 (compositions of embodiments 1-3) have good degreasing and polishing effects under the standard process conditions of degreasing and polishing (40% mass ratio concentration, 30°C, 180 seconds). After treatment, the surfaces are clean, flat, uniform in color, high in brightness, and the reflectivity is 97-98.2%. In addition, the experimental groups 1-3 have good high temperature oxidation discoloration resistance under the standard process conditions of passivation protection (10% mass ratio concentration, 30°C, 240 seconds).

[0199] 2. The composition of comparative example 1 selected in experimental group 4 lacks the surfactant component compared to example 1. After testing, the surface oil residue position has different colors and uneven gloss. It can be concluded that the surfactant component can effectively remove oil stains and prevent the oil stains from covering the surface and affecting the reaction between the chemical polishing component and the surface, resulting in different colors and uneven gloss.

[0200] 3. The composition of Comparative Example 2 selected in Experimental Group 5 lacks hydrogen peroxide compared to Example 1, and the brightness is average after testing; thus, it can be concluded that under the same process conditions, hydrogen peroxide is beneficial to improving the light emission speed and increasing the brightness.

[0201] 4. The composition of comparative example 3 selected in experimental group 6 lacks polyethylene glycol compared to example 1. Testing shows that polyethylene glycol has the function of leveling the surface. When polyethylene glycol is not added, the surface will be uneven, which in turn affects the brightness and reflectivity.

[0202] 5. The composition of comparative example 4 selected in experimental group 7 lacks the passivation protective agent component compared to example 1. After testing, the appearance and reflectivity are basically the same as those of experimental group 1, but lacks the adsorption protective layer formed on the surface by the passivation protective component. When placed at high temperature, oxidation discoloration quickly occurs.

[0203] 6. The compositions of Comparative Examples 5 and 6 selected in Experimental Groups 8-9 respectively lack sulfuric acid or phosphoric acid compared to Example 1. The surface brightness is average and the reflectivity is low after testing. It can be concluded that sulfuric acid and phosphoric acid increase the corrosive power and help to accelerate the light emission effect.

[0204] 7. Experimental groups 10-12, compared with experimental group 1, use concentrations of the composition in the passivation protection step are different; this affects the high-temperature oxidation resistance discoloration effect. From the high-temperature oxidation resistance discoloration results, it can be seen that within the range of 5-15% (mass ratio) use concentration, the effect of passivation protection will be enhanced with the increase of use concentration. The effect reaches a maximum at a use concentration of 15%, and increasing the concentration thereafter will deteriorate the passivation effect.

[0205] 8. Experimental groups 13-15, compared with experimental group 1, used different concentrations of the composition in degreasing and polishing, which affected the surface reflectivity (polishing effect). From the reflectivity results, it can be seen that in the use concentration range of 20-40% (mass ratio), the polishing effect is enhanced as the use concentration increases. When the use concentration reaches 40%, the effect is maximized. Continuing to increase the use concentration to 50%, the polishing effect is not greatly improved.

[0206] 9. Compared with experimental groups 14 and 16, the main difference is that the processing temperature of the composition in the degreasing and polishing step is different. From the reflectivity results, it can be seen that the increase in processing temperature can effectively increase the light output effect.

[0207] 10. Compared with experimental groups 14 and 17, the processing time of the composition in the degreasing and polishing steps and the passivation and protection steps was increased. From the results, it can be seen that the extension of the processing time can improve the polishing effect and the high-temperature oxidation resistance discoloration effect.

[0208] 11. Compared with Experimental Group 1, Experimental Group 18 uses a non-integrated test liquid. Under the premise of achieving the same polishing effect (reflectivity) and passivation effect, Experimental Group 18 is divided into three steps: degreasing, chemical polishing, and passivation protection. The reagents (test liquids) used in the three steps are different compositions, the total processing time is 800s, and the total amount of reagents used in the three steps is 100%; while Experimental Group 1 is divided into two steps: degreasing polishing and passivation protection, and the reagents are the same, the total reagent processing time is 420s, and the total amount of reagents used in the two steps is 50%. In addition, during the chemical polishing process, yellow smoke (nitrogen oxides) appeared in the commercially available products, while no yellow smoke appeared in Experimental Group 1. The comparison results show that the integrated reagent of the present invention can significantly and effectively reduce the user's use cost and difficulty, effectively improve production safety, and protect the health of operators.

[0209] The above specific embodiments have been described in detail for the present invention, but these do not constitute limitations on the present invention. The protection scope of the present invention is not limited to the above embodiments, and any equivalent modifications or changes made by ordinary technicians in the field based on the content disclosed by the present invention should be included in the protection scope recorded in the claims.

Claims

1. A composition for degreasing, polishing and passivation of copper alloy, characterized in that: include: A surfactant, comprising an active agent component, isomeric alcohol polyoxyethylene ether, and fatty alcohol polyoxyethylene ether, wherein the active agent component is selected from one or more of polyether siloxane and tetramethyldecynediol, A chemical polishing agent, comprising an acid component, hydrogen peroxide, and polyethylene glycol, wherein the acid component comprises phosphoric acid and sulfuric acid; A passivation protective agent, comprising phosphotungstic acid and a passivation component, wherein the passivation component is selected from one or more of sodium tungstate, benzotriazole and sodium benzoate; as well as water.

2. The composition for degreasing, polishing and passivation of copper alloy according to claim 1, characterized in that: The acid component of the chemical polishing agent also includes hydroxyethylidene diphosphoric acid, and the mass ratio of the phosphoric acid to the hydroxyethylidene diphosphoric acid is 15:

5.

3. The composition for degreasing, polishing and passivation of copper alloy according to claim 1, characterized in that: The mass ratio of the surfactant, the chemical polishing agent, the passivation protective agent and the water is 12-13:45-55:7-8:25-34.

4. The composition for degreasing, polishing and passivation of copper alloy according to claim 1, characterized in that: Based on 100 parts by weight of the composition, the water content is the balance; The mass ratio of the active agent component, the isomeric alcohol polyoxyethylene ether, and the fatty alcohol polyoxyethylene ether is 2-3:5:5-6; The mass ratio of the phosphoric acid, the sulfuric acid, the hydrogen peroxide, and the polyethylene glycol is 15:15:10 to 15:5; The mass ratio of the phosphotungstic acid to the passivation component is 3 to 5: The mass ratio of the surfactant, the chemical polishing agent and the passivation protective agent is 12-13:45-55:7-8.

5. The composition for degreasing, polishing and passivation of copper alloy according to claim 1, characterized in that: The active agent component is selected from tetramethyldecynediol, the mass fraction of the isomeric alcohol polyoxyethylene ether is 5%, the mass fraction of the fatty alcohol polyoxyethylene ether is 5%, and the mass fraction of the tetramethyldecynediol is 2%; The mass fraction of the phosphoric acid is 15%, the mass fraction of the sulfuric acid is 15%, the mass fraction of the hydrogen peroxide is 15%, and the mass fraction of the polyethylene glycol is 5%; The passivation component is selected from benzotriazole, the mass fraction of the phosphotungstic acid is 5%, and the mass fraction of the benzotriazole is 3%.

6. The composition for degreasing, polishing and passivation of copper alloy according to claim 1, characterized in that: The active agent component is selected from polyether siloxane, the mass fraction of the polyether siloxane is 3%, the mass fraction of the isomeric alcohol polyoxyethylene ether is 5%, and the mass fraction of the fatty alcohol polyoxyethylene ether is 5%; The mass fraction of the phosphoric acid is 15%, the mass fraction of the sulfuric acid is 15%, the mass fraction of the hydrogen peroxide is 10%, and the mass fraction of polyethylene glycol is 5%; The passivation component is selected from sodium tungstate, the mass fraction of the sodium tungstate is 3%, and the mass fraction of the phosphotungstic acid is 5%.

7. The composition for degreasing, polishing and passivation of copper alloy according to claim 1, characterized in that: The active agent component is selected from polyether siloxane, the mass fraction of polyether siloxane is 2%, the mass fraction of isomeric alcohol polyoxyethylene ether is 5%, and the mass fraction of fatty alcohol polyoxyethylene ether is 6%; The acid component also includes hydroxyethylidene diphosphoric acid, wherein the mass fraction of the phosphoric acid is 15%, the mass fraction of the sulfuric acid is 15%, the mass fraction of the hydroxyethylidene diphosphoric acid is 5%, the mass fraction of the hydrogen peroxide is 15%, and the mass fraction of the polyethylene glycol is 5%; The passivation component is selected from sodium tungstate and sodium benzoate, the mass fraction of the sodium tungstate is 3%, the mass fraction of the phosphotungstic acid is 3%, and the mass fraction of the sodium benzoate is 1%.

8. A method for preparing a composition for degreasing, polishing and passivating a copper alloy, which is used to prepare the composition for degreasing, polishing and passivating a copper alloy according to any one of claims 1 to 7, the preparation method comprising the following steps: The acid component of the chemical polishing agent is added into water and stirred evenly, and then hydrogen peroxide, polyethylene glycol, a surfactant and a passivation protective agent are added and stirred evenly to obtain a copper alloy degreasing, polishing and passivation composition.

9. A method for degreasing, polishing and passivation of copper alloy, characterized in that: include: A composition for degreasing, polishing and passivation of a copper alloy is prepared into a first treatment liquid with a first use concentration and a second treatment liquid with a second use concentration; wherein the first use concentration is greater than the second use concentration; Performing a degreasing and polishing treatment on the copper alloy workpiece using a first treatment liquid; After the degreasing and polishing treatment, the copper alloy workpiece is passivated using a second treatment liquid.

10. The method for degreasing, polishing and passivation of copper alloy according to claim 9, characterized in that: The first use concentration is between 30-60%; The second use concentration is between 5-15%.

Images