CN116988050A - Preparation process of nickel-phosphorus alloy coating on surface of alumina fiber - Google Patents

Preparation process of nickel-phosphorus alloy coating on surface of alumina fiber Download PDF

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Publication number
CN116988050A
CN116988050A CN202310984814.2A CN202310984814A CN116988050A CN 116988050 A CN116988050 A CN 116988050A CN 202310984814 A CN202310984814 A CN 202310984814A CN 116988050 A CN116988050 A CN 116988050A
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China
Prior art keywords
nickel
plating
solution
plating solution
concentration
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CN202310984814.2A
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Chinese (zh)
Inventor
张健
蒋世权
王迎春
马小民
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Molun Zhuhai Industrial Technology Co ltd
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Guozhuang New Material Technology Jiangsu Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
    • C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
    • C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
    • C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
    • C23C18/1875—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment only one step pretreatment
    • C23C18/1882—Use of organic or inorganic compounds other than metals, e.g. activation, sensitisation with polymers

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemically Coating (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The application belongs to the technical field of composite fiber material preparation, and relates to a preparation process of a nickel-phosphorus alloy coating on the surface of an alumina fiber. The method comprises the steps of dispersing, activating and preparing a plating solution, wherein the main salt in the plating solution is any one of nickel sulfate, nickel chloride and nickel acetate, the concentration of the main salt in the plating solution is 5-60g/L, the reducing agent is sodium hypophosphite solution, and the PH of the plating solution is 11; plating: and (3) placing the activated fibers in a plating solution, slowly stirring, heating in a water bath at 50-80 ℃ for plating until the plating solution is clarified and the plating is finished, taking out the plated fibers, and naturally airing to obtain the product. The application realizes the application of the nickel-phosphorus alloy coating on the surface of the alumina by a chemical liquid phase deposition mode, and has simple process operation flow and lower cost. The prepared product has excellent performance and stable product quality.

Description

Preparation process of nickel-phosphorus alloy coating on surface of alumina fiber
Technical Field
The application belongs to the technical field of composite fiber material preparation, and relates to a preparation process of a nickel-phosphorus alloy coating on the surface of an alumina fiber.
Background
Alumina fiber has excellent properties such as high specific modulus, specific strength, ablation resistance, high-temperature insulation and the like, and is one of the current commonly used Metal Matrix Composite (MMC) reinforcements, but wettability between the alumina fiber and metal is always a bottleneck problem restricting MMC preparation. Although the wettability of the matrix can be improved to a certain extent, the matrix alloying can affect the high heat conductivity of the matrix, and meanwhile, adverse reaction between fibers and metal can be caused, so that the fiber of the reinforcement is damaged, and the effect of the reinforcement on improving the performance of the composite material is weakened. The metallization of the fiber surface can effectively improve the wettability between the fiber reinforcement and the metal melt, and is a popular technical direction of current researches. However, in the prior art, the fiber is required to be subjected to degreasing, roughening, sensitization, activation and other processes before plating, the degreasing and roughening process easily causes the damage of the surface of the fiber, the unstable performance of the product is caused, and the defective rate is high; the palladium salt commonly used in the activation process is too expensive, and the production cost is high; in addition, due to the large difficulty of nickel plating, some processes adopt a high-pressure hydrogen reduction method, and the risk coefficient is high, so that the method is not suitable for industrial popularization and application.
Nickel-phosphorus alloys have excellent corrosion resistance compared with other alloys and are suitable for being used in some places with strong corrosiveness, but the existing technology at present cannot be used for plating the nickel-phosphorus alloy on the surface of aluminum oxide fibers.
Disclosure of Invention
The application provides a novel preparation process of a nickel-phosphorus alloy coating on the surface of an alumina fiber, aiming at the problems existing in the traditional alumina fiber nickel plating process.
In order to achieve the above purpose, the application is realized by adopting the following technical scheme:
the preparation process of the nickel-phosphorus alloy coating on the surface of the alumina fiber comprises the following steps:
(1) Dispersing: adding alumina fiber into the dispersion liquid, carrying out ultrasonic treatment, and then cleaning;
(2) Activating: mixing kh650 solution and silver nitrate solution to obtain an activating solution, and soaking the cleaned fiber in the activating solution for 10-20min at 30-50 ℃;
(3) Preparing a plating solution: sequentially adding main salt, a complexing agent, a reducing agent, a stabilizing agent and a 50% sodium hydroxide solution into deionized water, and uniformly mixing to obtain a plating solution, wherein the main salt is any one of nickel sulfate, nickel chloride and nickel acetate, the concentration of the main salt in the plating solution is 5-60g/L, the reducing agent is a sodium hypophosphite solution, and the PH of the plating solution is 11;
(4) Plating: and (3) placing the activated fibers in a plating solution, slowly stirring, heating in a water bath at 50-80 ℃ for plating until the plating solution is clarified and the plating is finished, taking out the plated fibers, and naturally airing to obtain the product.
Preferably, the dispersion liquid in the step (1) is any one of sodium acetate, hexadecanoic acid, octadecanoic acid, octadecenoic acid and boric acid.
Preferably, the kh650 concentration in the activating solution in the step (2) is 10-20g/L, and the silver nitrate concentration is 10-30g/L.
Preferably, the complexing agent in the step (3) is any one of sodium citrate, glycollic acid and lactic acid, and the stabilizer is any one of ammonium chloride, sodium iodate and thiourea; the concentration of the complexing agent in the plating solution is 10-60g/L, the concentration of the reducing agent is 4-40g/L, and the concentration of the stabilizing agent is 5-40g/L.
Preferably, in the step (4), the stirring speed is 50-100 rpm, and the plating time is 20-30min.
Compared with the prior art, the application has the advantages and positive effects that:
1. the application realizes the application of the nickel-phosphorus alloy coating on the surface of the alumina by a chemical liquid phase deposition mode, and has simple process operation flow and lower cost.
2. The prepared product has excellent performance and stable product quality.
Drawings
Fig. 1a is an SEM photograph of the coated alumina fiber of example 1, and fig. 1b is an SEM photograph of the coated alumina fiber after immersion in the etchant.
FIG. 2 is an EDS spectrum of the coated fiber of example 1.
FIG. 3 is a graph of elemental cross-section of the coated alumina fiber of example 1.
FIG. 4 is a graph of the axial elemental distribution of the coated alumina fiber of example 1.
Fig. 5 is an SEM photograph of the plated alumina fiber of comparative example 1.
Fig. 6 is an SEM photograph of the modified fiber of comparative example 2.
Fig. 7 is an EDS spectrum of the coated fiber of comparative example 2.
Fig. 8 is an SEM photograph of the modified fiber of comparative example 3.
Fig. 9 is an EDS spectrum of the coated fiber of comparative example 3.
Fig. 10 is an SEM photograph of the modified fiber of comparative example 4.
FIG. 11 is an EDS spectrum of the coated fiber of comparative example 4.
Detailed Description
In order that the above objects, features and advantages of the application will be more clearly understood, a further description of the application will be provided with reference to specific examples. It should be noted that, without conflict, the embodiments of the present application and features in the embodiments may be combined with each other.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application, however, the present application may be practiced otherwise than as described herein, and therefore the present application is not limited to the specific embodiments of the disclosure that follow.
Example 1
The embodiment provides a preparation process of a nickel-phosphorus alloy coating on the surface of an alumina fiber, which comprises the following specific steps.
2g of continuous alumina fiber (commercially available, produced by Jiangsu New Material technology, inc., trade mark ML 996); placing the fibers into ultrasonic cleaning for 6min, selecting sodium acetate dispersion liquid from the built-in solution to disperse the fibers (the fibers can be immersed), taking out and washing the fibers with deionized water for more than 10 seconds to clean the fibers; 100ml of the activating solution was prepared so that the kh650 concentration in the activating solution was 10g/L and the silver nitrate solution concentration was 15g/L. The fiber after the dispersion and cleaning is placed into an activating solution, soaked for 10min at the temperature of 40 ℃, and then taken out and cleaned by deionized water. The method comprises the steps of sequentially adding main salt nickel sulfate, complexing agent sodium citrate, reducer sodium hypophosphite, stabilizer ammonium chloride and 50% sodium hydroxide solution into deionized water to prepare plating solution. Wherein the concentration of main salt in the plating solution is 20g/L, the concentration of complexing agent is 30g/L, the concentration of reducing agent is 20g/L, and the concentration of stabilizing agent is 20g/L. Finally, the pH value of the plating solution is adjusted to 11 by using 50% sodium hydroxide solution by mass fraction. And then placing the fiber into a plating solution, heating in a water bath, controlling the temperature at 70 ℃, controlling the stirring speed in the reaction at 50 r/min, slowly stirring the plating solution, taking out the alumina fiber when the clarification reaction of the plating solution is stopped, and naturally airing to obtain the alumina fiber with the nickel-phosphorus alloy coating.
The resulting product was tested as shown in fig. 1 to 4. Fig. 1 is an SEM photograph of the fiber, and it can be seen from fig. 1 that the resulting coating is smooth, dense, and complete. Fig. 2 is an EDS spectrum of a fiber, showing that the coating deposited a large amount of nickel metal with a small amount of phosphorus. Fig. 3 is a fiber cross-section element profile. Fig. 4 is a fiber axial element distribution diagram. From fig. 3 and 4, it can be observed that the fiber forms a distinct sheath-core structure, and nickel-phosphorus elements are uniformly distributed on the surface layer of the fiber, at which time the fiber surface forms a desired nickel-phosphorus alloy coating.
Al with nickel-phosphorus alloy coating 2 O 3 The fiber was placed in a 6wt% NaCl solution and immersed for 48 hours and 96 hours, and the resistance value change was measured to detect the corrosion resistance. The results are shown in Table 1 below.
TABLE 1 resistance change before and after soaking Nickel-phosphorus alloy coated fiber
It can be observed from table 1 that the resistance value after the fiber is soaked is less in change and changes in a reasonable range, meanwhile, fig. 1a and fig. 1b are respectively the surface morphology of the nickel-plated fiber before soaking, as can be observed from fig. 1a, the plating layer before corrosion is compact and complete, as can be observed from fig. 1b, the plating layer surface after corrosion is still complete, and almost no change occurs, which indicates that the nickel-phosphorus alloy coating has excellent corrosion resistance.
Example 2
Taking 2g of continuous alumina fiber; placing the fiber into ultrasonic cleaning for 6min, selecting hexadecanoic acid dispersion liquid from the built-in solution to disperse the fiber, taking out, and washing with deionized water for more than 10 seconds until the fiber is cleaned; 100ml of an activating solution containing silver nitrate with a concentration of 10g/L kh650 and a concentration of 15g/L was taken. The fiber after the dispersion and cleaning is placed into an activating solution, soaked for 15min at the temperature of 30 ℃, and then taken out and cleaned by deionized water. The method comprises the steps of sequentially adding main salt nickel sulfate, complexing agent sodium citrate, reducer sodium hypophosphite, stabilizer ammonium chloride and 50% sodium hydroxide solution into deionized water to prepare plating solution. Wherein the concentration of main salt in the plating solution is 5g/L, the concentration of complexing agent is 20g/L, the concentration of reducing agent is 10g/L, and the concentration of stabilizer is 15g/L. Finally, the pH value of the plating solution is adjusted to 11 by using 50% sodium hydroxide solution by mass fraction. And then placing the fiber into a plating solution, heating in a water bath, controlling the temperature at 60 ℃, controlling the stirring speed in the reaction at 70 r/min, slowly stirring the plating solution, taking out the alumina fiber when the clarification reaction of the plating solution is stopped, and naturally airing to obtain the alumina fiber with the nickel-phosphorus alloy coating.
Example 3
Taking 2g of continuous alumina fiber; placing the fiber into ultrasonic cleaning for 6min, selecting boric acid dispersion liquid from the built-in solution to disperse the fiber, taking out, and washing with deionized water for more than 10 seconds until the fiber is cleaned; 100ml of an activating solution containing 20g/L kh650 and 30g/L silver nitrate is taken, the dispersed and washed fiber is placed into the activating solution, soaked for 20min at 50 ℃, and then taken out and washed by deionized water. The method comprises the steps of sequentially adding main salt nickel sulfate, complexing agent sodium citrate, reducer sodium hypophosphite, stabilizer ammonium chloride and 50% sodium hydroxide solution into deionized water to prepare plating solution. Wherein the concentration of main salt in the plating solution is 30g/L, the concentration of complexing agent is 60g/L, the concentration of reducing agent is 40g/L, and the concentration of stabilizing agent is 40g/L. Finally, the pH value of the plating solution is adjusted to 11 by using 50% sodium hydroxide solution by mass fraction. And then placing the fiber into a plating solution, heating in a water bath, controlling the temperature at 80 ℃, controlling the stirring speed in the reaction to be 100 revolutions per minute, slowly stirring the plating solution, taking out the alumina fiber when the clarification reaction of the plating solution is stopped, and naturally airing to obtain the alumina fiber with the nickel-phosphorus alloy coating.
Comparative example 1
The comparative example changes the component concentration and the proportion of the plating solution. The plating solution comprises the following components: the main salt nickel sulfate 40g/L, complexing agent sodium citrate 50g/L, reducing agent sodium hypophosphite 30g/L, stabilizer ammonium chloride 5g/L, then the pH value of the plating solution is adjusted to 11 by using 50% sodium hydroxide solution by mass fraction. The remaining steps remain the same as in example 1. The resulting nickel phosphorus alloy coated alumina fiber is shown in fig. 5. Fig. 5 is an SEM photograph of the modified fiber, and it can be seen from fig. 5 that the plating effect will be affected by changing the plating process, the coating particles are not uniform, and the surface is rough.
Comparative example 2
This comparative example did not sonicate the fibers and the remaining procedure was as in example 1. The results of the fiber detection obtained are shown in fig. 6 to 7. It can be seen from the figure that the plating effect is affected by changing the components of the dispersion liquid, the particle size of the coating is different, the surface is rough, the surface is incomplete, a complete coating cannot be formed, the nickel metal content is reduced, no phosphorus element exists, a nickel-phosphorus alloy coating cannot be formed, and the plating effect is poor.
Comparative example 3
The comparative example was conducted by changing the soaking temperature in the activation treatment, setting the soaking temperature to room temperature, and the remaining production process was identical to that of example 1. The product is shown in fig. 8 and 9. It can be seen from the figure that the coated particles also exhibit a phenomenon of varying size, incomplete surface, failure to form a complete coating, extremely low nickel metal content, and no phosphorus element.
Comparative example 4
The comparative example did not carry out a dispersion treatment of the fibers and the rest of the procedure was identical to example 1. The results of the product testing are shown in fig. 10 and 11. It can be seen from the figure that the dispersion treatment of the fiber will seriously affect the plating effect, almost no particles are deposited on the surface of the fiber, and the energy spectrum of fig. 11 shows that the nickel element content on the surface of the fiber only accounts for 1.41wt% and no phosphorus element appears, which indicates that the dispersion treatment step plays a critical role in the process.
According to the application, the continuous alumina fiber is subjected to dispersion treatment, so that the surface of the alumina fiber is contacted with noble metal ions as much as possible, the reaction activation point is increased, other pretreatment steps are changed, and the silane coupling agent is combined with metal silver ions to achieve effective deposition of activated metal so as to smoothly finish subsequent plating, so that the surface of the alumina fiber is provided with a nickel-phosphorus alloy coating, the preparation of the nickel-phosphorus alloy coating on the surface of the continuous alumina fiber can be effectively finished through a chemical liquid phase deposition process, the whole process flow is simple and convenient, the preparation cost is low, and the pretreatment idea is novel and unique, thereby being the first process for realizing nickel-phosphorus alloy deposition on the surface of the alumina fiber in China.
The present application is not limited to the above-mentioned embodiments, and any equivalent embodiments which can be changed or modified by the technical content disclosed above can be applied to other fields, but any simple modification, equivalent changes and modification made to the above-mentioned embodiments according to the technical substance of the present application without departing from the technical content of the present application still belong to the protection scope of the technical solution of the present application.

Claims (5)

1. The preparation process of the nickel-phosphorus alloy coating on the surface of the alumina fiber is characterized by comprising the following steps:
(1) Dispersing: adding alumina fiber into the dispersion liquid, carrying out ultrasonic treatment, and then cleaning;
(2) Activating: mixing kh650 solution and silver nitrate solution to obtain an activating solution, and soaking the cleaned fiber in the activating solution for 10-20min at 30-50 ℃;
(3) Preparing a plating solution: sequentially adding main salt, a complexing agent, a reducing agent, a stabilizing agent and a 50% sodium hydroxide solution into deionized water, and uniformly mixing to obtain a plating solution, wherein the main salt is any one of nickel sulfate, nickel chloride and nickel acetate, the concentration of the main salt in the plating solution is 5-60g/L, the reducing agent is a sodium hypophosphite solution, and the PH of the plating solution is 11;
(4) Plating: and (3) placing the activated fibers in a plating solution, slowly stirring, heating in a water bath at 50-80 ℃ for plating until the plating solution is clarified and the plating is finished, taking out the plated fibers, and naturally airing to obtain the product.
2. The process for preparing the nickel-phosphorus alloy coating on the surface of the alumina fiber according to claim 1, wherein the dispersion liquid in the step (1) is any one of sodium acetate, hexadecanoic acid, octadecanoic acid, octadecenoic acid and boric acid.
3. The process for preparing the nickel-phosphorus alloy coating on the surface of the alumina fiber according to claim 1, wherein the kh650 concentration in the activating solution in the step (2) is 10-20g/L and the silver nitrate concentration is 10-30g/L.
4. The process for preparing the nickel-phosphorus alloy coating on the surface of the alumina fiber according to claim 1, wherein the complexing agent in the step (3) is any one of sodium citrate, glycollic acid and lactic acid, and the stabilizer is any one of ammonium chloride, sodium iodate and thiourea; the concentration of the complexing agent in the plating solution is 10-60g/L, the concentration of the reducing agent is 4-40g/L, and the concentration of the stabilizing agent is 5-40g/L.
5. The process for preparing the nickel-phosphorus alloy coating on the surface of the alumina fiber according to claim 1, wherein the stirring speed in the step (4) is 50-100 rpm, and the plating time is 20-30min.
CN202310984814.2A 2023-08-07 2023-08-07 Preparation process of nickel-phosphorus alloy coating on surface of alumina fiber Pending CN116988050A (en)

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CN202310984814.2A CN116988050A (en) 2023-08-07 2023-08-07 Preparation process of nickel-phosphorus alloy coating on surface of alumina fiber

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