CN112030147A - Electromagnetic pure iron chemical nickel and phosphorus alloy plating process - Google Patents
Electromagnetic pure iron chemical nickel and phosphorus alloy plating process Download PDFInfo
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- CN112030147A CN112030147A CN202010689924.2A CN202010689924A CN112030147A CN 112030147 A CN112030147 A CN 112030147A CN 202010689924 A CN202010689924 A CN 202010689924A CN 112030147 A CN112030147 A CN 112030147A
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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
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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
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1837—Multistep pretreatment
- C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
Abstract
The invention relates to a process for chemically plating nickel-phosphorus alloy on electromagnetic pure iron, which aims at solving the problems that the plating layer of the electromagnetic pure iron chemically plated nickel-phosphorus alloy is not firmly combined with a base metal, the plating layer is peeled, rusty spots or rusty spots are easy to generate and the like. On the other hand, in order to improve the corrosion resistance of the electromagnetic pure iron chemical nickel-phosphorus alloy plating layer, cold water washing is not carried out after chemical nickel-phosphorus alloy plating, the situation that the density of the plating layer is severely influenced by cold and hot changes is prevented, and hot water washing is directly carried out. In addition, after the oil-free compressed air is used for drying, the electromagnetic pure iron is placed into the drying box for drying, the bonding strength of the electromagnetic pure iron chemical nickel-phosphorus alloy is increased, the density of a coating layer is improved, and the corrosion resistance of the electromagnetic pure iron is further improved.
Description
Technical Field
The invention belongs to the technical field of manufacturing of an electromagnetic pure iron surface chemical nickel-phosphorus alloy for aerospace, and particularly relates to a process for chemically plating nickel-phosphorus alloy on electromagnetic pure iron.
Background
The electromagnetic pure iron is high-quality steel with the iron content of more than 99.5 percent, and is a low-carbon, low-sulfur and low-phosphorus iron material. The electromagnetic pure iron is a widely used soft magnetic material, has higher magnetic induction intensity, and is very suitable for manufacturing magnetic parts working in a strong magnetic field. In the fields of aerospace and aviation, electromagnetic pure iron is an important metal material. However, the surface of the electromagnetic pure iron material exposed in the air is easy to oxidize, and the electromagnetic pure iron produced by general machining has oil stains and oxides on the surface, cannot be directly used on aerospace and aviation product equipment, and needs to be subjected to certain surface treatment to obtain corrosion resistance or weldability. The prior electromagnetic pure iron nickel-phosphorus plating alloy layer mainly has the problems of weak combination of a plating layer and a base metal, peeling of the plating layer, easy generation of rusty spots or rusty spots and the like, thereby limiting the popularization and application of the electromagnetic pure iron chemical nickel-phosphorus plating alloy.
Disclosure of Invention
In order to solve the problems, the invention provides a process for chemically plating nickel-phosphorus alloy on electromagnetic pure iron, which solves the problems of infirm combination of a plating layer and a base metal, peeling of the plating layer, easy generation of rusty spots or rusty spots and the like.
The technical scheme adopted by the invention is as follows: the process is characterized in that chemical oxidation treatment is added to the electromagnetic pure iron before chemical nickel-phosphorus alloy plating, a chemical oxidation film layer is removed by dilute hydrochloric acid after the chemical oxidation treatment, and the treated electromagnetic pure iron can further activate the surface of the electromagnetic pure iron and increase the surface roughness of the electromagnetic pure iron to play a role in increasing the bonding strength of a plating layer.
On the other hand, in order to improve the anti-corrosion capability of the electromagnetic pure iron chemical nickel-phosphorus alloy plating layer, after chemical nickel-phosphorus alloy plating, cold water washing is not carried out, the density of the plating layer is prevented from being severely influenced by cold and hot changes, hot water washing is directly carried out, and the anti-corrosion capability of the electromagnetic pure iron is further improved. In addition, after the pure electromagnetic iron is dried by oilless compressed air, the pure electromagnetic iron is placed into a drying box and is subjected to heat preservation for 15-25 min at the temperature of 90-100 ℃, and then is heated to 190-220 ℃ and is subjected to heat preservation for 2-3 h, so that the bonding strength of the pure electromagnetic iron chemical nickel-phosphorus plating alloy can be further increased, the density of a plating layer is improved, and the corrosion resistance of the pure electromagnetic iron is improved.
The method specifically comprises the following steps:
step 1, deoiling, namely putting electromagnetic pure iron in NaOH 20-50 g/L, Na2CO3 30～50g/L、Na3PO4 20～30g/L、Na2SiO33-5 g/L, and the balance of water, wherein the mixed solution is subjected to oil removal at the temperature of 60-90 ℃ for 5-15 min;
step 2, washing with hot water, namely washing with hot water at the temperature of 70-90 ℃;
step 3, washing with cold water until the water film is not broken within 30 seconds;
step 4, carrying out weak corrosion, namely using 50-100 g/L aqueous solution containing HCl to corrode for 3-5 s at room temperature;
step 5, washing with cold water, and cleaning with cold water;
step 6, hot water washing, namely washing with hot water at the temperature of 70-90 ℃;
step 7, chemical oxidation, namely putting the electromagnetic pure iron in NaOH 550-650 g/L, NaNO2180-250 g/L, and the balance of water, and oxidizing in a mixed solution at the temperature of 135-145 ℃ for 20-30 min;
step 8, washing with hot water, namely washing with hot water at the temperature of 70-90 ℃;
step 9, washing with cold water, and cleaning with cold water;
step 10, activating for 3-5 seconds at room temperature by using a solution containing 150-200 g/L of HCl and 3-5 g/L of corydalis tuber with the balance of water;
step 11, washing with cold water, and cleaning with cold water;
step 12, hot water washing, namely washing with hot water at the temperature of 70-90 ℃;
step 13, chemically plating nickel-phosphorus alloy, and putting the electromagnetic pure iron in NiSO4·6H2O 25～50g/L，NaH2PO2·H2O 10～20g/L，Na3C6H5O7·2H2O 8～12g/L，CH3COONa·3H2O13-16 g/L, lactic acid 18-23 mL/L, saccharin 0.2-0.5 g/L and the balance of water, wherein the pH value is 4.5-4.9, the temperature is 82-90 ℃, and the time is 30-50 min;
step 14, hot water washing, namely washing with hot water at the temperature of 70-90 ℃;
step 15, drying, namely drying by using oilless compressed air;
step 16, hot water washing, namely washing with hot water at the temperature of 70-90 ℃;
and 17, drying, namely putting the parts into a drying box for drying at the temperature of 90-100 ℃ for 20-30 min.
Further optimizing, drying again after drying in the step 17, preserving heat for 15-25 min at the temperature of 90-100 ℃, and then increasing the temperature to 190-220 ℃ and preserving heat for 2-3 h.
The invention has the beneficial effects that:
1. aiming at the problems that the electromagnetic pure iron chemical nickel-phosphorus plating alloy plating layer is not firmly combined with a base metal, the plating layer is skinned, rusty spots or rusty spots are easily generated and the like, chemical oxidation treatment is added to the electromagnetic pure iron before the chemical nickel-phosphorus plating alloy, a chemical oxidation film layer is removed by dilute hydrochloric acid after the chemical oxidation treatment, and the treatment can further activate the surface of the electromagnetic pure iron and increase the surface roughness of the electromagnetic pure iron to play a role in increasing the bonding strength of the plating layer;
2. aiming at the problems that the plating layer of the electromagnetic pure iron chemical nickel-phosphorus plating alloy is not firmly combined with the base metal, the plating layer peels, rusty spots or rusty spots are easy to generate and the like, after the electromagnetic pure iron chemical nickel-phosphorus plating alloy is dried, the electromagnetic pure iron is placed into a drying box and is subjected to heat preservation for 15-25 min at the temperature of 90-100 ℃, and then is heated to 190-220 ℃ and is subjected to heat preservation for 2-3 h, so that the bonding strength of the electromagnetic pure iron chemical nickel-phosphorus plating alloy can be further increased, the density of the plating layer is improved, and the corrosion resistance of the electromagnetic pure iron is improved;
3. in order to improve the corrosion resistance of the electromagnetic pure iron chemical nickel-phosphorus alloy plating layer, the cold water washing is not carried out after the chemical nickel-phosphorus alloy plating, the density of the plating layer is prevented from being severely influenced by cold and hot changes, and the hot water washing is directly carried out, so that the corrosion resistance of the electromagnetic pure iron chemical nickel-phosphorus alloy plating layer is improved.
Detailed Description
The first embodiment,
Step 1, deoiling, namely putting electromagnetic pure iron with the NaOH content of 20g/L, Na2CO3 50g/L、Na3PO4 20g/L、Na2SiO35g/L, and the balance of water, wherein the mixed solution is subjected to oil removal at the temperature of 60 ℃ for 15 min;
step 2, washing with hot water, namely washing with hot water at the temperature of 90 ℃;
step 3, washing with cold water until the water film is not broken within 30 seconds;
step 4, carrying out weak corrosion, namely corroding for 3-5 s at room temperature by using a 50g/L aqueous solution containing HCl;
step 5, washing with cold water, and cleaning with cold water;
step 6, washing with hot water, namely washing with hot water at the temperature of 90 ℃;
step 7, chemical oxidation, namely putting the electromagnetic pure iron in NaOH 550g/L, NaNO2250g/L, and the balance of water, and oxidizing in a mixed solution at the temperature of 135 ℃ for 30 min;
step 8, washing with hot water, namely washing with hot water at the temperature of 90 ℃;
step 9, washing with cold water, and cleaning with cold water;
step 10, activating for 3-5 seconds at room temperature by using a solution containing 150g/L of HCl and 3g/L of other water;
step 11, washing with cold water, and cleaning with cold water;
step 12, washing with hot water, namely washing with hot water at the temperature of 90 ℃;
step 13, chemically plating nickel-phosphorus alloy, and putting the electromagnetic pure iron in NiSO4·6H2O 25g/L，NaH2PO2·H2O 20g/L，Na3C6H5O7·2H2O 8g/L，CH3COONa·3H2O16 g/L, lactic acid 18mL/L, saccharin 0.5g/L and the balance of water, wherein the pH value is 4.9, the temperature is 82 ℃, and the time is 50 min;
step 14, washing with hot water, namely washing with hot water at the temperature of 90 ℃;
step 15, drying, namely drying by using oilless compressed air;
step 16, washing with hot water, namely washing with hot water at the temperature of 90 ℃;
and step 17, drying, namely, putting the parts into a drying box for drying at the temperature of 90 ℃ for 30 min.
And step 18, drying again, keeping the temperature for 15min at 100 ℃, and then keeping the temperature for 3h when the temperature is raised to 190 ℃.
Example II,
Step 1, deoiling, namely putting electromagnetic pure iron with the NaOH content of 50g/L, Na2CO3 30g/L、Na3PO4 30g/L、Na2SiO33g/L, and the balance of water, wherein the mixed solution is subjected to oil removal at the temperature of 80 ℃ for 10 min;
step 2, washing with hot water, namely washing with hot water at the temperature of 80 ℃;
step 3, washing with cold water until the water film is not broken within 30 seconds;
step 4, carrying out weak corrosion, namely corroding for 3-5 s at room temperature by using 100g/L aqueous solution containing HCl;
step 5, washing with cold water, and cleaning with cold water;
step 6, washing with hot water, namely washing with hot water at the temperature of 80 ℃;
step 7, chemical oxidation, namely putting the electromagnetic pure iron in NaOH 650g/L, NaNO2180g/L and the balance of water, and oxidizing in a mixed solution at the temperature of 140 ℃ for 25 min;
step 8, washing with hot water, namely washing with hot water at the temperature of 80 ℃;
step 9, washing with cold water, and cleaning with cold water;
step 10, activating for 3-5 seconds at room temperature by using a solution of HCl 200g/L, 5g/L and the balance of water;
step 11, washing with cold water, and cleaning with cold water;
step 12, washing with hot water, namely washing with hot water at the temperature of 80 ℃;
step 13, chemically plating nickel-phosphorus alloy, and putting the electromagnetic pure iron in NiSO4·6H2O 50g/L，NaH2PO2·H2O 10g/L，Na3C6H5O7·2H2O 12g/L，CH3COONa·3H2O13 g/L, lactic acid 23mL/L, saccharin0.2g/L, and the balance of water, wherein the pH value is 4.5, the temperature is 85 ℃, and the time is 40 min;
step 14, washing with hot water, namely washing with hot water at the temperature of 80 ℃;
step 15, drying, namely drying by using oilless compressed air;
step 16, washing with hot water, namely washing with hot water at the temperature of 80 ℃;
and step 17, drying, namely, putting the parts into a drying box for drying at the temperature of 90 ℃ for 25 min.
And step 18, drying again, preserving the heat for 20min at the temperature of 100 ℃, and then increasing the temperature to 200 ℃ and preserving the heat for 2.5 h.
Example III,
Step 1, deoiling, namely putting electromagnetic pure iron with the NaOH content of 35g/L, Na2CO3 40g/L、Na3PO4 25g/L、Na2SiO34g/L, and the balance of water, wherein the mixed solution is subjected to oil removal at the temperature of 90 ℃ for 5 min;
step 2, washing with hot water, namely washing with hot water at the temperature of 70 ℃;
step 3, washing with cold water until the water film is not broken within 30 seconds;
step 4, carrying out weak corrosion, namely corroding for 3-5 s at room temperature by using 75g/L aqueous solution containing HCl;
step 5, washing with cold water, and cleaning with cold water;
step 6, washing with hot water, namely washing with hot water at the temperature of 70 ℃;
step 7, chemical oxidation, namely placing the electromagnetic pure iron in NaOH 600g/L, NaNO2Oxidizing 200g/L in a mixed solution with the balance being water at the temperature of 145 ℃ for 20 min;
step 8, washing with hot water, namely washing with hot water at the temperature of 70 ℃;
step 9, washing with cold water, and cleaning with cold water;
step 10, activating for 3-5 seconds at room temperature by using HCl 175g/L, if the amount of HCl 4g/L and the balance of water solution;
step 11, washing with cold water, and cleaning with cold water;
step 12, washing with hot water, namely washing with hot water at the temperature of 70 ℃;
step 13, chemically plating nickel-phosphorus alloy, and putting the electromagnetic pure iron in NiSO4·6H2O 35g/L，NaH2PO2·H2O 15g/L，Na3C6H5O7·2H2O 10g/L，CH3COONa·3H2O15 g/L, lactic acid 20mL/L, saccharin 0.3g/L, and the balance of water, wherein the pH value is 4.7, the temperature is 90 ℃, and the time is 45 min;
step 14, washing with hot water, namely washing with hot water at the temperature of 70 ℃;
step 15, drying, namely drying by using oilless compressed air;
step 16, washing with hot water, namely washing with hot water at the temperature of 70 ℃;
and step 17, drying, namely, putting the parts into a drying box for drying at the temperature of 100 ℃ for 20 min.
And step 18, drying again, keeping the temperature at 90 ℃ for 25min, and then raising the temperature to 220 ℃ for 2 h.
The above description is only for the best mode of the present invention, but the scope of the present invention is not limited thereto, and any alternatives and modifications that can be easily conceived by those skilled in the art within the technical scope of the present invention are also included in the scope of the present invention.
Those skilled in the art will appreciate that the invention may be practiced without these specific details.
Claims (2)
1. The process for chemically plating the nickel-phosphorus alloy on the electromagnetic pure iron is characterized by comprising the following steps of:
step 1, deoiling, namely putting electromagnetic pure iron in NaOH 20-50 g/L, Na2CO3 30～50g/L、Na3PO4 20～30g/L、Na2SiO33-5 g/L, and the balance of water, wherein the mixed solution is subjected to oil removal at the temperature of 60-90 ℃ for 5-15 min;
step 2, washing with hot water, namely washing with hot water at the temperature of 70-90 ℃;
step 3, washing with cold water until the water film is not broken within 30 seconds;
step 4, carrying out weak corrosion, namely using 50-100 g/L aqueous solution containing HCl to corrode for 3-5 s at room temperature;
step 5, washing with cold water, and cleaning with cold water;
step 6, hot water washing, namely washing with hot water at the temperature of 70-90 ℃;
step 7, chemical oxidation, namely putting the electromagnetic pure iron in NaOH 550-650 g/L, NaNO2180-250 g/L, and the balance of water, and oxidizing in a mixed solution at the temperature of 135-145 ℃ for 20-30 min;
step 8, washing with hot water, namely washing with hot water at the temperature of 70-90 ℃;
step 9, washing with cold water, and cleaning with cold water;
step 10, activating for 3-5 seconds at room temperature by using a solution containing 150-200 g/L of HCl and 3-5 g/L of corydalis tuber with the balance of water;
step 11, washing with cold water, and cleaning with cold water;
step 12, hot water washing, namely washing with hot water at the temperature of 70-90 ℃;
step 13, chemically plating nickel-phosphorus alloy, and putting the electromagnetic pure iron in NiSO4·6H2O 25～50g/L，NaH2PO2·H2O 10～20g/L，Na3C6H5O7·2H2O 8～12g/L，CH3COONa·3H2O13-16 g/L, lactic acid 18-23 mL/L, saccharin 0.2-0.5 g/L and the balance of water, wherein the pH value is 4.5-4.9, the temperature is 82-90 ℃, and the time is 30-50 min;
step 14, hot water washing, namely washing with hot water at the temperature of 70-90 ℃;
step 15, drying, namely drying by using oilless compressed air;
step 16, hot water washing, namely washing with hot water at the temperature of 70-90 ℃;
and 17, drying, namely putting the parts into a drying box for drying at the temperature of 90-100 ℃ for 20-30 min.
2. The electromagnetic pure iron chemical nickel-phosphorus alloy plating process according to claim 1, wherein the step 17 of drying is followed by drying again, the temperature is kept at 90-100 ℃ for 15-25 min, and then the temperature is raised to 190-220 ℃ for 2-3 h.
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