CN109898074A - A kind of method of chemically coating nickel by magnesium-alloy-boron layer - Google Patents

A kind of method of chemically coating nickel by magnesium-alloy-boron layer Download PDF

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Publication number
CN109898074A
CN109898074A CN201910288849.6A CN201910288849A CN109898074A CN 109898074 A CN109898074 A CN 109898074A CN 201910288849 A CN201910288849 A CN 201910288849A CN 109898074 A CN109898074 A CN 109898074A
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China
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alloy
magnesium
nickel
treatment
boron layer
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CN201910288849.6A
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刘小珍
王新富
陈捷
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Shanghai Institute of Technology
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Shanghai Institute of Technology
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Abstract

The present invention provides a kind of methods of chemically coating nickel by magnesium-alloy-boron layer characterized by comprising step 1: being polished magnesium alloy and be rinsed with water;Step 2: by the magnesium alloy after polishing, be put into pre-treatment in pretreatment liquid, the process conditions of pre-treatment be pre-treatment temperature be room temperature~50 DEG C, the pre-treatment time is 5~15min, speed of agitator is 100~600rpm, after pre-treatment, is rinsed with water, dry;The pretreatment liquid be containing organic compound, rare-earth salts, alkali, phosphate and OP emulsifier aqueous solution;Step 3: the magnesium alloy after pre-treatment is put into chemical nickel plating-boron layer in plating solution.Oil removing, acid etching, activation step are combined into a step pre-treatment by the present invention, simplify the step of Mg alloy surface carries out chemical nickel plating-boron layer.

Description

A kind of method of chemically coating nickel by magnesium-alloy-boron layer
Technical field
The present invention relates to a kind of methods of chemically coating nickel by magnesium-alloy-boron layer.
Background technique
Magnesium alloy is structural metallic materials, has that density is low, specific strength is high, electromagnetic wave shielding bigger than elasticity modulus and leads The advantages that electrical conductivity can be good, there is very big application potential in fields such as space flight and aviation, auto industry, electronic communications.But it has There is very high chemical activity, is easy to corrode in the environment of application.Carrying out surface treatment appropriate to magnesium alloy can be improved it Corrosion resistance, carrying out chemical plating nickel-boron in Mg alloy surface is a kind of effective method.Chemical plating is carried out in Mg alloy surface at present The step of nickel-boron, is more, the steps include: mechanical grinding, oil removing, acid etching, activation, plating etc., and many middle layers are also wanted It is sensitized, activated, restored again.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of chemically coating nickel by magnesium-alloy-boron layer.
In order to achieve the above object, the present invention provides a kind of method of chemically coating nickel by magnesium-alloy-boron layer, feature exists In, comprising:
Step 1: being polished magnesium alloy and be rinsed with water;
Step 2: by the magnesium alloy after polishing, being put into pre-treatment in pretreatment liquid, the process conditions of pre-treatment are pre-treatment Temperature is room temperature~50 DEG C, the pre-treatment time is 5~15min, speed of agitator is 100~600rpm, after pre-treatment, uses water It rinses, it is dry;The pretreatment liquid be containing organic compound, rare-earth salts, alkali, phosphate and OP emulsifier aqueous solution;
Step 3: the magnesium alloy after pre-treatment is put into chemical nickel plating-boron layer in plating solution, the process conditions of plating are as follows: temperature It is 65~90 DEG C, speed of agitator is 100~600rpm, and plating time is 30~120min, and bath pH value is 11~14, and plating is complete Bi Hou, plating piece are rinsed with water, dry;The plating solution is the aqueous solution of the reducing agent containing nickel salt, organic matter, alkali and boracic.
Preferably, magnesium alloy is carried out to be polishing to silver with the silicon carbide waterproof abrasive paper that dehydrated alcohol soaks in the step 1 White.
Preferably, the organic compound in the step 2 is sodium lactate, potassium lactate, sodium citrate, potassium citrate, wine The mixture of one or more of stone acid sodium, potassium tartrate, natrium malicum and potassium malate composition.
Preferably, the rare-earth salts in the step 2 is rare earth sulfate, rare earth-iron-boron, one in rare earth nitrades The mixture of kind or two or more compositions;The rare earth be lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, One of lutetium, scandium and yttrium or more than one rare earth.
Preferably, the alkali in the step 2 is one of potassium hydroxide, sodium hydroxide, ammonium hydroxide and sodium carbonate or two The mixture of kind composition described above.
Preferably, the phosphate in the step 2 is one or more of potassium phosphate, sodium phosphate and ammonium phosphate The mixture of composition.
Preferably, the concentration difference of the organic compound in the step 2, rare-earth salts, alkali, phosphate and OP emulsifier Are as follows: 0.06~30g/L, 0.03~20g/L, 10~100g/L, 2~20g/L, 1~9g/L.
Preferably, the nickel salt in the step 3 is one of nickel chloride, nickel acetate, nickel sulfate and basic nickel carbonate Or the mixture of two or more compositions.
Preferably, the organic matter in the step 3 is disodium ethylene diamine tetraacetate, sodium citrate, lactic acid and ethylenediamine One or both of composition mixture.
Preferably, the alkali in the step 3 is one of sodium hydroxide, potassium hydroxide, ammonium hydroxide and sodium carbonate or two The mixture of kind composition described above.
Preferably, the reducing agent of the boracic in the step 3 be sodium borohydride, potassium borohydride, dimethylamino borine and The mixture of one or more of trimethylamine groups borine composition.
Preferably, the nickel salt in the step 3, organic matter, alkali, boracic the concentration of reducing agent be respectively as follows: 7~35g/ L, 10~100g/L, 0.04~100g/L, 0.15~15g/L.
Compared with prior art, the beneficial effects of the present invention are:
Oil removing, acid etching, activation step are combined into a step pre-treatment by the present invention, are simplified Mg alloy surface and are carried out chemistry The step of nickel plating-boron layer.Contained using nickel and boron in Bruker AXS Microanalysis GmbH energy disperse spectroscopy measurement coating Amount, is calculated by mass percentage respectively 96.75~88.11% and 3.25~11.89%.Using magnificent 660 electrochemical operations of occasion It stands, the corrosion potential of coating is measured in 5% sodium chloride solution, corrosion potential is -0.550~-0.071V.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited Range.
Used each raw material is commercial product in following embodiment.
Room temperature in following embodiment is 25 DEG C.
Embodiment 1
A kind of method of chemically coating nickel by magnesium-alloy-boron layer, specific steps are as follows:
In the beaker of 1L be added 700mL water, 0.06g sodium lactate, 0.03g lanthanum sulfate, 10g potassium hydroxide, 2g potassium phosphate, 1gOP-10 emulsifier dissolves to form sodium lactate-lanthanum sulfate-potassium hydroxide-potassium phosphate-OP-10 emulsifier mixed solution, moves into 1L In volumetric flask, it is diluted with water to scale, pretreatment liquid is made.
The silicon carbide waterproof abrasive paper soaked with dehydrated alcohol the WE43M magnesium alloy to be plated to 100mm × 100mm × 2mm carries out It is polishing to silvery white and is rinsed with water.
Above-mentioned pretreatment liquid is transferred in the beaker of 2L, the magnesium alloy after above-mentioned 100mm × 100mm × 2mm polishing is put Enter pre-treatment in pretreatment liquid, the temperature of pre-treatment is room temperature (25 DEG C), the pre-treatment time is 5min, speed of agitator is 100rpm, after pre-treatment, pre-treatment part is rinsed with water, and is air-dried.
In the beaker of 1L be added 900mL water, 7g nickel chloride, 10g disodium ethylene diamine tetraacetate, 0.04g sodium hydroxide, 0.15 sodium borohydride dissolves to form nickel chloride-disodium ethylene diamine tetraacetate-sodium hydroxide-sodium borohydride mixed solution, with 4% It is 11 that sodium hydroxide solution, which adjusts pH value, moves into 1L volumetric flask, is diluted with water to scale, and plating solution is made.
Above-mentioned plating solution is transferred in the beaker of 2L, the magnesium alloy after above-mentioned 100mm × 100mm × 2mm pre-treatment is put into Chemical nickel plating-boron layer in the plating solution that pH is 11, the temperature of plating is 65 DEG C, plating time 30min, speed of agitator 100rpm After plating, plating piece is taken out, is rinsed with water only, is air-dried, obtain with coated magnesium alloy.
Using the content of nickel and boron in Bruker AXS Microanalysis GmbH energy disperse spectroscopy measurement coating, by quality It is respectively 96.75% and 3.25% that percentages, which are calculated,.Using magnificent 660 electrochemical workstations of occasion, surveyed in 5% sodium chloride solution Determine the corrosion potential of coating, corrosion potential is -0.550V.
Embodiment 2
A kind of method of chemically coating nickel by magnesium-alloy-boron layer, specific steps are as follows:
In the beaker of 1L be added 700mL water, 15g potassium malate, 15g sodium citrate, 18g yttrium nitrate, 2g Dineodymium trisulfate, 50g sodium carbonate, 50g concentration are 34.35% ammonium hydroxide, 10g sodium phosphate, 10g ammonium phosphate, 9gOP-4 emulsifier dissolve to form malic acid Potassium-sodium citrate-yttrium nitrate-Dineodymium trisulfate-sodium carbonate-ammonium hydroxide-sodium phosphate-phosphoric acid ammonium-OP-4 emulsifier mixed solution moves into 1L In volumetric flask, it is diluted with water to scale, pretreatment liquid is made.
The silicon carbide waterproof abrasive paper soaked with dehydrated alcohol the AZ91D magnesium alloy to be plated to 100mm × 100mm × 2mm carries out It is polishing to silvery white and is rinsed with water.
Above-mentioned pretreatment liquid is transferred in the beaker of 2L, the magnesium alloy after above-mentioned 100mm × 100mm × 2mm polishing is put Enter pre-treatment in pretreatment liquid, the temperature of pre-treatment is 50 DEG C, the pre-treatment time is 15min, speed of agitator 600rpm, preceding place After reason, pre-treatment part is rinsed with water, and is air-dried.
900mL water, 25g basic nickel carbonate, 10g nickel acetate, 50g lactic acid, 50g ethylenediamine, 50g are added in the beaker of 1L Potassium hydroxide, 50g sodium carbonate, 0.5g potassium borohydride, 14.5g trimethylamine groups borine, dissolution form basic nickel carbonate-nickel acetate- Lactic acid-ethylenediamine-potassium hydroxide-sodium carbonate-potassium borohydride-trimethylamine groups borine mixed solution, it is molten with 40% sodium hydroxide It is 14 that liquid, which adjusts pH value, moves into 1L volumetric flask, is diluted with water to scale, and plating solution is made.
Above-mentioned plating solution is transferred in the beaker of 2L, the magnesium alloy after above-mentioned 100mm × 100mm × 2mm pre-treatment is put into Chemical nickel plating-boron layer in the plating solution that pH is 14, the temperature of plating is 90 DEG C, plating time 120min, speed of agitator are 600rpm after plating, takes out plating piece, is rinsed with water only, air-dries, obtain with coated magnesium alloy.
Using the content of nickel and boron in Bruker AXS Microanalysis GmbH energy disperse spectroscopy measurement coating, by quality It is respectively 88.11% and 11.89% that percentages, which are calculated,.Using magnificent 660 electrochemical workstations of occasion, in 5% sodium chloride solution The corrosion potential of coating is measured, corrosion potential is -0.100V.
Embodiment 3
A kind of method of chemically coating nickel by magnesium-alloy-boron layer, specific steps are as follows:
700mL water, 7g potassium tartrate, 8g potassium citrate, 5g cerous nitrate, 5g praseodymium chloride, 55g hydrogen are added in the beaker of 1L Sodium oxide molybdena, 10g sodium phosphate, 5gOP-30 emulsifier dissolve to form potassium tartrate-potassium citrate-cerous nitrate-praseodymium chloride-hydroxide Sodium-sodium phosphate-OP-30 emulsifier mixed solution moves into 1L volumetric flask, is diluted with water to scale, and pretreatment liquid is made.
The silicon carbide waterproof abrasive paper soaked with dehydrated alcohol the VW75M magnesium alloy to be plated to 100mm × 100mm × 2mm carries out It is polishing to silvery white and is rinsed with water.
Above-mentioned pretreatment liquid is transferred in the beaker of 2L, the magnesium alloy after above-mentioned 100mm × 100mm × 2mm polishing is put Enter pre-treatment in pretreatment liquid, the temperature of pre-treatment is 38 DEG C, the pre-treatment time is 10min, speed of agitator 350rpm, preceding place After reason, pre-treatment part is rinsed with water, and is air-dried.
900mL water, 21g nickel sulfate, 55g sodium citrate, 4g sodium hydroxide, 49g concentration are added in the beaker of 1L is 34.35% ammonium hydroxide, 8g dimethylamino borine dissolve that form nickel sulfate-sodium citrate-ammonium hydroxide-dimethylamino borine mixing molten Liquid, adjusting pH value with 4% sodium hydroxide solution is 13, moves into 1L volumetric flask, is diluted with water to scale, plating is made Liquid.
Above-mentioned plating solution is transferred in the beaker of 2L, the magnesium alloy after above-mentioned 100mm × 100mm × 2mm pre-treatment is put into PH is chemical nickel plating-boron layer in 13 plating solutions, and the temperature of plating is 75 DEG C, plating time 80min, speed of agitator 350rpm, After plating, plating piece is taken out, is rinsed with water only, is air-dried, obtain with coated magnesium alloy.
Using the content of nickel and boron in Bruker AXS Microanalysis GmbH energy disperse spectroscopy measurement coating, by quality It is respectively 91.65% and 8.35% that percentages, which are calculated,.Using magnificent 660 electrochemical workstations of occasion, surveyed in 5% sodium chloride solution Determine the corrosion potential of coating, corrosion potential is -0.071V.

Claims (10)

1. a kind of method of chemically coating nickel by magnesium-alloy-boron layer characterized by comprising
Step 1: being polished magnesium alloy and be rinsed with water;
Step 2: by the magnesium alloy after polishing, being put into pre-treatment in pretreatment liquid, the process conditions of pre-treatment are pre-treatment temperature For room temperature~50 DEG C, the pre-treatment time be 5~15min, speed of agitator is 100~600rpm, after pre-treatment, rushed with water It washes, it is dry;The pretreatment liquid be containing organic compound, rare-earth salts, alkali, phosphate and OP emulsifier aqueous solution;
Step 3: the magnesium alloy after pre-treatment being put into chemical nickel plating-boron layer in plating solution, the process conditions of plating are as follows: temperature 65 ~90 DEG C, speed of agitator is 100~600rpm, and plating time is 30~120min, and bath pH value is 11~14, and plating finishes Afterwards, plating piece is rinsed with water, dry.
2. the method for chemically coating nickel by magnesium-alloy-boron layer as described in claim 1, which is characterized in that use nothing in the step 1 The silicon carbide waterproof abrasive paper of water-ethanol wetting carries out magnesium alloy to be polishing to silvery white.
3. the method for chemically coating nickel by magnesium-alloy-boron layer as described in claim 1, which is characterized in that having in the step 2 Machine compound is sodium lactate, potassium lactate, sodium citrate, potassium citrate, sodium tartrate, potassium tartrate, natrium malicum and malic acid The mixture of one or more of potassium composition.
4. the method for chemically coating nickel by magnesium-alloy-boron layer as described in claim 1, which is characterized in that dilute in the step 2 Earth salt is the mixture of one or more of rare earth sulfate, rare earth-iron-boron, rare earth nitrades composition;Described is dilute Soil is one of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, scandium and yttrium or more than one rare earth.
5. the method for chemically coating nickel by magnesium-alloy-boron layer as described in claim 1, which is characterized in that the alkali in the step 2 For the mixture of one or more of potassium hydroxide, sodium hydroxide, ammonium hydroxide and sodium carbonate composition.
6. the method for chemically coating nickel by magnesium-alloy-boron layer as described in claim 1, which is characterized in that the phosphorus in the step 2 Hydrochlorate is the mixture of one or more of potassium phosphate, sodium phosphate and ammonium phosphate composition.
7. the method for chemically coating nickel by magnesium-alloy-boron layer as described in claim 1, which is characterized in that having in the step 2 Machine compound, rare-earth salts, alkali, phosphate and OP emulsifier concentration be respectively as follows: 0.06~30g/L, 0.03~20g/L, 10~ 100g/L, 2~20g/L, 1~9g/L.
8. the method for chemically coating nickel by magnesium-alloy-boron layer as described in claim 1, which is characterized in that the plating in the step 3 Liquid is the aqueous solution of the reducing agent containing nickel salt, organic matter, alkali and boracic.
9. the method for chemically coating nickel by magnesium-alloy-boron layer as claimed in claim 8, which is characterized in that the nickel in the step 3 Salt is the mixture of one or more of nickel chloride, nickel acetate, nickel sulfate and basic nickel carbonate composition;The step Organic matter in 3 is the mixing of one or both of disodium ethylene diamine tetraacetate, sodium citrate, lactic acid and ethylenediamine composition Object;Alkali in the step 3 is one or more of sodium hydroxide, potassium hydroxide, ammonium hydroxide and sodium carbonate composition Mixture;The reducing agent of boracic in the step 3 is sodium borohydride, potassium borohydride, dimethylamino borine and trimethylamine groups The mixture of one or more of borine composition.
10. the method for chemically coating nickel by magnesium-alloy-boron layer as claimed in claim 8, which is characterized in that in the step 3 Nickel salt, organic matter, alkali, boracic reducing agent concentration be respectively as follows: 7~35g/L, 10~100g/L, 5~100g/L, 0.15~ 15g/L。
CN201910288849.6A 2019-04-11 2019-04-11 A kind of method of chemically coating nickel by magnesium-alloy-boron layer Pending CN109898074A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3615733A (en) * 1968-08-13 1971-10-26 Shipley Co Electroless copper plating
CN1500910A (en) * 2002-11-15 2004-06-02 中国科学院金属研究所 Chemical nickel-plating method on magnesium alloy surface
CN1827851A (en) * 2006-03-15 2006-09-06 厦门大学 Method for chemical plating of nickel-boron alloy on magnesium alloy surface
CN101880872A (en) * 2010-06-10 2010-11-10 沈阳理工大学 Method for performing direct chemical Ni-P alloy plating on surface of magnesium alloy
CN108677178A (en) * 2018-06-21 2018-10-19 安徽金达节能材料发展有限公司 Aluminum alloy surface silane corrosion-resisting film and preparation method thereof under a kind of marine environment

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3615733A (en) * 1968-08-13 1971-10-26 Shipley Co Electroless copper plating
CN1500910A (en) * 2002-11-15 2004-06-02 中国科学院金属研究所 Chemical nickel-plating method on magnesium alloy surface
CN1827851A (en) * 2006-03-15 2006-09-06 厦门大学 Method for chemical plating of nickel-boron alloy on magnesium alloy surface
CN101880872A (en) * 2010-06-10 2010-11-10 沈阳理工大学 Method for performing direct chemical Ni-P alloy plating on surface of magnesium alloy
CN108677178A (en) * 2018-06-21 2018-10-19 安徽金达节能材料发展有限公司 Aluminum alloy surface silane corrosion-resisting film and preparation method thereof under a kind of marine environment

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
翟宗诚 等: "《汽车修理及再生技术》", 30 September 2009, 江西科学技术出版社 *

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Application publication date: 20190618