CN113549963B - Additive for plating rhenium coating on tungsten and tungsten alloy matrix and preparation method thereof - Google Patents
Additive for plating rhenium coating on tungsten and tungsten alloy matrix and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an additive for plating a rhenium coating on a tungsten and tungsten alloy substrate and a preparation method thereof, relating to the technical field of plating solution additives, wherein each liter of plating additive comprises the following raw materials by weight: 10-25 mg of 3-methoxy-4-hydroxybenzaldehyde, 2-18 mg of benzoic acid, 56-70 mg of p-benzoquinone, 5-15 mg of tetraethylenepentamine, 34-50 mg of sodium benzoylyellow imide, 45-75 mg of polyacrylamide, 5-10 mg of diethanolamine, 15-35 mg of polyaluminum chloride and 5-10 mg of ascorbic acid; adding the raw materials into deionized water, sealing, heating to 75-85 ℃, and keeping the temperature for 10-30 min to fully dissolve the raw materials to obtain the composite material. The invention has the beneficial effects that the flatness and the glossiness of the surface of the plating layer can be improved, and particularly, the generation of cracks of the rhenium coating can be inhibited, so that the obtained plating layer is compact and has no cracks.
Description
Technical Field
The invention relates to the technical field of an additive for plating a rhenium coating, in particular to a plating additive for plating the rhenium coating in an acid environment and a preparation method thereof.
Background
Electroplating is a process of depositing a thin layer of metal, alloy or composite material on a conductive solid surface by an electrochemical route, and is a special electrolytic process. Rhenium (Rhenium) is a rare high-melting metal (3180 ℃), and has excellent high modulus, high-temperature mechanical properties and thermal shock resistance, and the properties make Rhenium especially suitable for being used in ultrahigh-temperature and strong thermal shock working environments. Currently rhenium coatings can be obtained by MOCVD and electroplating methods.
The rhenium coating is a commonly used method for obtaining the rhenium coating, but the rhenium obtained by electrochemical deposition has poor coating quality, a large amount of microcracks are generated on the surface, the coating is easy to fall off, and the coating is high in brittleness. The use of rhenium as a plating additive is commonly achieved to achieve good performance of the coating. At present, research on rhenium electroplating additives is less in China, for example, CN 101899693A provides a method for locally plating rhenium on an oxygen-free copper substrate, the electroplating additives are not added except main salt and other additional salt, the bonding force of the obtained plating layer is not strong, and the density can not meet the requirements. For example, CN 104846408A provides a plating solution formula and an electroplating method for plating a compact rhenium film on a copper substrate, and a certain mass fraction of gelatin, vanillin, sodium dodecyl sulfate, citric acid and other substances are added as additives, so that a uniform and compact coating with good adhesion can be obtained on the copper substrate. Based on the above problems, there is a need to provide an electroplating additive and a preparation method thereof, which are suitable for use in the rhenium coating electroplating of tungsten and tungsten alloy substrates, so as to effectively solve the above problems.
Disclosure of Invention
The invention aims to solve at least one of the technical problems in the prior art: an electroplating additive used on tungsten and tungsten alloy matrix and a preparation method thereof are provided. The electroplating additive prepared by the invention is suitable for various electroplating current processes (direct current electroplating and pulse electroplating), and the flatness and the glossiness of a plating layer can be improved by a small amount required by each electroplating; the corrosion resistance and the coating hardness can be obviously improved. Meanwhile, the plating solution can be kept clear and can be reused.
The technical solution of the invention is as follows:
an additive for plating rhenium coating on tungsten and its alloy substrate,
each liter of the electroplating additive comprises the following raw materials by weight: 10-25 mg of 3-methoxy-4-hydroxybenzaldehyde, 2-18 mg of benzoic acid, 56-70 mg of p-benzoquinone, 5-15 mg of tetraethylenepentamine, 34-50 mg of sodium benzoylyellow imide, 5-10 mg of diethanolamine and 5-10 mg of ascorbic acid.
As a preferred technical scheme of the invention, each liter of electroplating additive comprises the following raw materials by weight: 45-75 mg of polyacrylamide and 15-35 mg of polyaluminium chloride.
As a preferred technical scheme of the invention, each liter of electroplating additive comprises the following raw materials by weight: 10-18 mg of 3-methoxy-4-hydroxybenzaldehyde, 5-12 mg of benzoic acid, 60-65 mg of p-benzoquinone, 8-13 mg of tetraethylenepentamine, 40-45 mg of sodium benzoylyellow imide, 50-60 mg of polyacrylamide, 8-10 mg of diethanolamine, 20-30 mg of polyaluminium chloride and 6-9 mg of ascorbic acid.
As a preferred technical scheme of the invention, each liter of electroplating additive comprises the following raw materials by weight: 12mg of 3-methoxy-4-hydroxybenzaldehyde, 6mg of benzoic acid, 63mg of p-benzoquinone, 9mg of tetraethylenepentamine, 43mg of sodium phthalimide, 57mg of polyacrylamide, 9mg of diethanolamine, 24mg of polyaluminum chloride and 7mg of ascorbic acid.
As a preferred technical scheme of the invention, each liter of electroplating additive comprises the following raw materials by weight: 15mg of 3-methoxy-4-hydroxybenzene, 10mg of benzoic acid, 65mg of p-benzoquinone, 12mg of tetraethylenepentamine, 45mg of sodium o-benzoylxanthimide, 60mg of polyacrylamide, 10mg of diethanolamine, 30mg of polyaluminum chloride and 9mg of ascorbic acid.
A method for preparing rhenium coating additive electroplated on tungsten and tungsten alloy matrix comprises the following steps: weighing raw materials of each additive, adding the raw materials of each additive into deionized water, sealing, heating to 70-90 ℃ by using a magnetic stirrer, and preserving heat for 10-30 min to fully dissolve the raw materials to obtain the additive for plating the rhenium coating on the tungsten and the alloy matrix thereof.
As a preferred technical scheme of the invention, the mixture is heated to 80 ℃ by a magnetic stirrer and is kept for 20min.
The holes and cracks existing in the rhenium coating prepared by the electroplating method are the main obstacles for preventing the application of the rhenium coating, and the main reasons for generating the defects are as follows: firstly, the surface impurity treatment is not thorough, and the influence of impurities can be eliminated through strict control pretreatment flow; secondly, the surface stress is large, the common method is to anneal after plating, and the influence of the stress on the plating layer is reduced by adding electroplating additives; thirdly, gas is generated in the electroplating process, so that the defects of air holes and the like appear on the coating. In order to solve the problems, the additive disclosed by the invention can release surface stress by adding benzoic acid, ascorbic acid and the like, improve the flatness and glossiness of the surface of a coating, particularly inhibit the generation of rhenium coating cracks, and meanwhile, under an acidic environment, benzoquinone has good affinity with hydrogen generated during electroplating, and the following reactions occur:
therefore, the additive provided by the invention is beneficial to improving the flatness and the glossiness of the surface of the plating layer and inhibiting the generation of cracks of the rhenium coating, so that the obtained plating layer is compact and has no cracks. Meanwhile, the addition of the polyaluminium chloride and the polyacrylamide can settle impurities, so that the clarification of the plating solution can be kept, the times of the repeated use of the plating solution are increased, and the production cost is saved.
The invention has at least one of the following beneficial effects:
the additive for plating the rhenium coating on the tungsten and the alloy matrix thereof can be suitable for plating the rhenium coating on a pure tungsten matrix and other tungsten alloy matrixes. According to the invention, by adding 3-methoxy-4-hydroxybenzaldehyde, benzoic acid, p-benzoquinone, tetraethylenepentamine, sodium o-benzoylsuccinimide, diethanolamine, ascorbic acid and the like, surface stress can be released, the flatness and glossiness of the surface of the coating can be improved, and particularly, the generation of cracks of a rhenium coating can be inhibited; meanwhile, the addition of the polyaluminium chloride and the polyacrylamide can settle impurities, so that the clarification of the plating solution can be kept, the times of the repeated use of the plating solution are increased, and the production cost is saved. Therefore, the additive disclosed by the invention is beneficial to improving the flatness and glossiness of the surface of the plating layer and inhibiting the generation of cracks of the rhenium coating by the combined action of a plurality of components, so that the obtained plating layer is compact and has no cracks, and the quality of the plated rhenium layer can be improved.
Drawings
FIG. 1 is a surface scanning electron microscope image of a tungsten alloy plate plated with a rhenium coating, as shown in example 1, at 5000 times magnification.
FIG. 2 is a scanning electron microscope photomicrograph of a surface of a tungsten alloy sheet electroplated with a rhenium coating, magnified 5000 times as large as that of example 2.
FIG. 3 is a scanning electron microscope photomicrograph of a surface of a tungsten alloy sheet electroplated with a rhenium coating, magnified 5000 times as large as that of example 3.
FIG. 4 is a scanning electron microscope photomicrograph of a surface of a tungsten alloy sheet electroplated with a rhenium coating, magnified 5000 times as large as that of example 4.
FIG. 5 is a scanning electron microscope photomicrograph of a surface of a rhenium electroplated coating of a tungsten alloy sheet of the mode of comparative example 1, taken at 5000 Xmagnification.
FIG. 6 is a scanning electron microscope photomicrograph of a surface of a rhenium electroplated coating of a tungsten alloy sheet according to the mode of comparative example 2, at a magnification of 5000.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
An additive for plating rhenium coating on tungsten and tungsten alloy matrix, wherein each liter of the plating additive contains the following raw materials by weight: 12mg of 3-methoxy-4-hydroxybenzaldehyde, 6mg of benzoic acid, 63mg of p-benzoquinone, 9mg of tetraethylenepentamine, 43mg of sodium o-benzoylxanthylimide, 57mg of polyacrylamide, 9mg of diethanolamine, 24mg of polyaluminum chloride and 7mg of ascorbic acid.
The preparation method comprises the following steps:
weighing the raw materials and deionized water, adding the weighed raw materials of the rhenium coating electroplating additive on the tungsten alloy substrate into the deionized water, sealing, preparing into 1L solution, heating to 80 ℃ by using a magnetic stirrer, and preserving heat for 20min to fully dissolve the raw materials, thereby obtaining the rhenium coating electroplating additive.
The prepared additive solution is added into the rhenium electroplating solution according to the proportion (6 ml of prepared electroplating additive is added into each liter of electroplating solution), the shape of the rhenium coating obtained on the W-Re5 alloy sheet is shown in figure 1, and as can be seen from figure 1, the tungsten alloy substrate obtained in the example 1 has good flatness and glossiness and has no cracks; therefore, the additive in example 1 can help to improve the flatness and glossiness of the rhenium coating surface, and particularly can inhibit the generation of cracks on the rhenium coating, so that the obtained coating is compact and has no cracks.
Example 2
An additive for plating rhenium coating on tungsten and tungsten alloy matrix, wherein each liter of the plating additive comprises the following raw materials by weight: 15mg of 3-methoxy-4-hydroxybenzene, 10mg of benzoic acid, 65mg of p-benzoquinone, 12mg of tetraethylenepentamine, 45mg of sodium o-benzoylxanthimide, 60mg of polyacrylamide, 10mg of diethanolamine, 30mg of polyaluminum chloride and 9mg of ascorbic acid.
The preparation method comprises the following steps:
weighing the raw materials and deionized water, adding the weighed raw materials of the rhenium coating electroplating additive on the tungsten alloy substrate into the deionized water, sealing, preparing into 1L solution, heating to 80 ℃ by using a magnetic stirrer, and preserving heat for 20min to fully dissolve the raw materials, thereby obtaining the rhenium coating electroplating additive.
The prepared additive solution is added into the plating rhenium solution according to the proportion (6 ml of prepared plating additive is added into each liter of plating solution), the shape and the appearance of the rhenium coating obtained on the W-Re5 alloy sheet are shown in figure 2, and as can be seen from figure 2, the flatness and the glossiness obtained on the tungsten alloy substrate in the example 2 are good, and no crack exists; therefore, the additive in example 1 can help to improve the flatness and glossiness of the rhenium coating surface, and especially can inhibit the generation of cracks on the rhenium coating, so that the obtained coating is compact and has no cracks.
Example 3
An additive for plating rhenium coating on tungsten and its alloy substrate,
each liter of the electroplating additive comprises the following raw materials by weight: 10mg of 3-methoxy-4-hydroxybenzaldehyde, 2mg of benzoic acid, 56mg of p-benzoquinone, 5mg of tetraethylenepentamine, 34mg of sodium o-benzoylyellow imide, 45mg of polyacrylamide, 5mg of diethanolamine, 15mg of polyaluminum chloride and 5mg of ascorbic acid.
The preparation method comprises the following steps:
weighing the raw materials and deionized water, adding the weighed raw materials of the rhenium coating electroplating additive on the tungsten and tungsten alloy matrix into the deionized water, sealing, preparing into 1L solution, heating to 85 ℃ by using a magnetic stirrer, and keeping the temperature for 10min to fully dissolve the raw materials to obtain the rhenium coating electroplating additive.
The prepared additive solution is added into the rhenium electroplating solution according to the proportion (6 ml of prepared electroplating additive is added into each liter of electroplating solution), the shape of the rhenium coating obtained on the W-Re5 alloy sheet is shown in figure 3, and as can be seen from figure 3, the tungsten alloy substrate obtained in the example 3 has good flatness and glossiness and has no cracks; therefore, the additive in example 3 can help to improve the flatness and glossiness of the rhenium coating surface, and particularly can inhibit the generation of cracks on the rhenium coating, so that the obtained coating is compact and has no cracks.
Example 4
An additive for plating rhenium coating on tungsten and its alloy substrate,
each liter of the electroplating additive comprises the following raw materials by weight: 25mg of 3-methoxy-4-hydroxybenzaldehyde, 18mg of benzoic acid, 70mg of p-benzoquinone, 15mg of tetraethylenepentamine, 50mg of sodium o-benzoylyellow imide, 75mg of polyacrylamide, 10mg of diethanolamine, 35mg of polyaluminum chloride and 10mg of ascorbic acid.
The preparation method comprises the following steps:
weighing the raw materials and deionized water, adding the weighed raw materials of the rhenium plating coating additive on the tungsten and the alloy matrix thereof into the deionized water, sealing, preparing into 1L solution, heating to 75 ℃ by using a magnetic stirrer, and preserving heat for 30min to fully dissolve the raw materials, thus obtaining the rhenium plating coating additive.
The additive solution prepared in the above way is added into the rhenium electroplating solution according to the proportion (6 ml of prepared electroplating additive is added into each liter of electroplating solution), the rhenium coating on the W-Re5 alloy sheet is in the shape of a graph shown in FIG. 4, as can be seen from FIG. 4, the rhenium coating obtained on the tungsten alloy substrate in the example 4 is good in quality and free of cracks, and the bonding force between the coating and the tungsten alloy substrate is strong, so that the rhenium coating is not easy to fall off, therefore, the additive in the example 4 can help to improve the flatness and the glossiness of the rhenium coating surface, especially can inhibit the generation of cracks of the rhenium coating, and enables the obtained coating to be compact and free of cracks.
Comparative example 1
The additive of the invention is not added into the electroplating solution, and the electroplating is directly carried out.
The morphology of the rhenium coating obtained on the W-Re5 alloy sheet is shown in FIG. 5, and therefore, the rhenium coating obtained on the tungsten alloy substrate in example 5 has poor quality, pores and cracks exist in the whole range, and the surface flatness and the glossiness are poor.
Comparative example 2
The difference from example 1 is that: the additive does not contain benzoic acid and ascorbic acid, namely, each liter of electroplating additive contains the following raw materials by weight: 12mg of 3-methoxy-4-hydroxybenzaldehyde, 63mg of p-benzoquinone, 9mg of tetraethylenepentamine, 43mg of sodium o-benzoylsuccinimide, 57mg of polyacrylamide, 9mg of diethanolamine and 24mg of polyaluminium chloride.
The additive solution prepared above is added into the rhenium electroplating solution according to the proportion (6 ml of prepared electroplating additive is added into each liter of electroplating solution), the shape of the rhenium coating obtained on the W-Re5 alloy sheet is shown in figure 6, and as can be seen from figure 6, the rhenium coating obtained on the tungsten alloy substrate in the example 6 is poor in quality, and pores and cracks exist on the surface.
Comparing examples 1-4 with comparative examples 1-2, it can be seen that the rhenium coatings obtained in examples 1-4 have good quality, no cracks, good surface flatness and good glossiness; the rhenium coating obtained in the comparative example 1 has poor quality, pores and cracks exist in the whole range, and the surface evenness and the glossiness are poor; the rhenium coating obtained in comparative example 2 had pores and cracks on the surface. The rhenium coating layers obtained in the examples 1-4 are obviously superior to those obtained in the comparative example 1 (no additive of the invention is added in the electroplating solution) and those obtained in the comparative example 2 (the additive lacks of the components of benzoic acid and ascorbic acid), so that the additive of the invention is beneficial to improving the quality of the rhenium coating layer, and the additive of the invention is beneficial to improving the flatness and glossiness of the coating layer surface and inhibiting the generation of cracks of the rhenium coating layer through the combined action of the benzoic acid and the ascorbic acid and other components, so that the obtained coating layer is compact and has no cracks.
The above are merely characteristic embodiments of the present invention, and do not limit the scope of the present invention in any way. All technical solutions formed by adopting the equivalent exchange or the equivalent substitution fall within the protection scope of the present invention.
Claims (7)
1. An additive for plating rhenium coating on tungsten and tungsten alloy substrates is characterized in that each liter of the plating additive comprises the following raw materials by weight: 10-25 mg of 3-methoxy-4-hydroxybenzaldehyde, 2-18 mg of benzoic acid, 56-70 mg of p-benzoquinone, 5-15 mg of tetraethylenepentamine, 34-50 mg of sodium benzoylyellow imide, 5-10 mg of diethanolamine and 5-10 mg of ascorbic acid; each liter of the electroplating additive also comprises the following raw materials by weight: 45-75 mg of polyacrylamide and 15-35 mg of polyaluminium chloride.
2. The additive for plating rhenium coating on tungsten and tungsten alloy substrates as claimed in claim 1, wherein each liter of the plating additive comprises the following raw materials by weight: 10-18 mg of 3-methoxy-4-hydroxybenzaldehyde, 5-12 mg of benzoic acid, 60-65 mg of p-benzoquinone, 8-13 mg of tetraethylenepentamine, 40-45 mg of sodium benzoylyellow imide, 8-10 mg of diethanolamine and 6-9 mg of ascorbic acid.
3. The additive for plating rhenium coating on tungsten and tungsten alloy substrates as claimed in claim 2, wherein each liter of the plating additive comprises the following raw materials by weight: 50-60 mg of polyacrylamide and 20-30 mg of polyaluminium chloride.
4. The additive for plating rhenium coating on tungsten and tungsten alloy substrates as claimed in claim 3, wherein each liter of the plating additive comprises the following raw materials by weight: 12mg of 3-methoxy-4-hydroxybenzaldehyde, 6mg of benzoic acid, 63mg of p-benzoquinone, 9mg of tetraethylenepentamine, 43mg of sodium phthalimide, 57mg of polyacrylamide, 9mg of diethanolamine, 24mg of polyaluminum chloride and 7mg of ascorbic acid.
5. The additive for plating rhenium coating on tungsten and tungsten alloy substrates as claimed in claim 3, wherein each liter of the plating additive comprises the following raw materials by weight: 15mg of 3-methoxy-4-hydroxybenzene, 10mg of benzoic acid, 65mg of p-benzoquinone, 12mg of tetraethylenepentamine, 45mg of sodium o-benzoylxanthimide, 60mg of polyacrylamide, 10mg of diethanolamine, 30mg of polyaluminum chloride and 9mg of ascorbic acid.
6. A method for preparing an additive for plating rhenium coating on tungsten and tungsten alloy substrates as claimed in claim 1, which comprises the following steps: weighing raw materials of each additive, adding the raw materials of each additive into deionized water, sealing, heating to 75-85 ℃ by using a magnetic stirrer, and preserving heat for 10-30 min to fully dissolve the raw materials to obtain the additive.
7. The method for preparing the additive for plating the rhenium coating on the tungsten and the tungsten alloy substrate according to the claim 6 is characterized by comprising the following steps: heating to 80 deg.C with a magnetic stirrer and holding for 20min.
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