CN103540935A - Gold-plating method of high silicon-aluminum composite material - Google Patents
Gold-plating method of high silicon-aluminum composite material Download PDFInfo
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- CN103540935A CN103540935A CN201310553767.2A CN201310553767A CN103540935A CN 103540935 A CN103540935 A CN 103540935A CN 201310553767 A CN201310553767 A CN 201310553767A CN 103540935 A CN103540935 A CN 103540935A
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Abstract
The invention relates to a gold-plating method of a high silicon-aluminum composite material. According to a second zinc immersion treatment method of conventional aluminum alloy electroplating, pre-treatment of the method comprises the following six steps: cleaning and oil removing; alkaline etching; bright dipping; primary zinc immersion; zinc annealing; secondary zinc immersion. The gold-plating method subsequently comprises the following steps: I, preplating chemical nickel in a chemical nickel-plating liquid; II, plating nickel for the first time according to a conventional nickel-plating method, wherein the nickel layer is 2-3 microns thick; III, performing aging treatment; IV, performing activating treatment; V, plating nickel for the second time according to a conventional nickel-plating method, wherein the nickel layer is 2-3 microns thick; VI, taking a pure gold plate or a platinum titanium mesh as an anode and the high silicon-aluminum composite material as a cathode according to a conventional pure gold-plating method, wherein the gold layer is 2-3 microns thick; VII, detecting the binding force of the plating layer. The plating layer observed under tenfold amplifying glass is free from peeling and bubbling phenomena and good in binding force. The binding force of the gold-plating plating layer and a high silicon-aluminum base material adopted by the method provided by the invention is firm and reaches the standard of appendix A of GJB1420 General Specification of Semiconductor Integrated Circuit Shell.
Description
Technical field
The present invention relates to a kind of gold plating method, the gold plating method of the high aluminium silicon composite material Si-50Al that particularly a kind of silicone content is 50%, is mainly used in multi-chip T/R component package housing, belongs to electronic package material engineering Application Areas.
Background technology
Controllable (the Controlled Expansion of the coefficient of expansion, CE) serial high silicon content aluminum matrix composite, because possessing, density is low, thermal expansivity is little, heat conductivity is good, there is good machinability and welding property, be extremely suitable as airborne, missile-borne, the field T/R component package material such as spaceborne.But the specific physical due to this material, its electroplating surface difficulty is large, as unreasonable in technological process, and it is not high that coating is prone to bonding force, there are the quality problems such as bubbling, peeling in coating after welding or high cold cycle, has a strong impact on housing welding property and resistance to air loss.At present, what this material development technology was the most ripe is the Osprey company of Britain, the high sial of Osprey development is applied in many aerospace fields abroad as encapsulating housing material, its high sial craft of gilding adopts similar aluminium alloy craft of gilding, and it is qualified that binding force of cladding material reaches 350 ℃ of temperature baking 2 minutes.Premium properties in view of this kind of material, in recent years, domestic related scientific research unit carries out material preparation and through engineering approaches applied research always, wherein take the domestic enterprise that Jiangsu Hao Ran jet deposition company is representative possesses starting material through engineering approaches throughput, can mass production silicone content is 70%, 50%, 27% silumin; Aspect craft of gilding research, Harbin Institute of Technology, its Gold plated Layer and base material bonding force meet 250 ℃ of thermal shock tests, and high sial that China Electronics science and technology group company the 13rd develops is gold-plated, and to meet the lower 350 ℃ of bonding forces of atmosphere protection qualified.
Summary of the invention
For prior art, have the deficiency of coating and basal body binding force, problem to be solved by this invention is to provide a kind of gold plating method of high aluminium silicon composite material, and described high aluminium silicon composite material is Si-50Al matrix material.
The gold plating method of high aluminium silicon composite material comprises pre-treatment, and described pre-treatment routinely plating on aluminium alloy secondary soaking zinc treatment process is divided into cleaning oil removing, alkaline etching, bright dipping, once soaks zinc, moves back zinc and six steps of secondary soaking zinc.Concrete operation step after pre-treatment is as follows:
1) preplating chemical nickel: the part after pre-treatment is put into chemical nickel-plating liquid preplating, under 80 ± 2 ℃ of conditions of temperature, 20 minutes preplating time;
2) nickel plating for the first time: nickel plating process routinely, nickel plating in conventional nickel plating solution, 2 ~ 3 microns of nickel layer thickness, take out, and clean, dry;
3) ageing treatment: by step 2) part of Ni plated is put into vacuum oven and is carried out ageing treatment, and aging temperature is 360 ± 10 ℃, is incubated 1 hour, vacuum tightness 1.1 * 10
-3pa, heats up with stove, after furnace cooling, takes out;
4) activation: the part after step 3) is processed is put into activation solution, under 15 ~ 25 ℃ of conditions of temperature, soaks 20 ~ 30 seconds;
5) nickel plating for the second time: nickel plating process routinely, the part nickel plating in conventional nickel plating solution after step 4) is processed, 2 ~ 3 microns of nickel layer thickness, take out, and clean;
6) gold-plated: using proof gold plate or platinum titanium net as anode, high aluminium silicon composite material is negative electrode, plates routinely pure gold method, the part after step 5) is processed carries out gold-plated, 2 ~ 3 microns of golden layer thicknesses; Described high aluminium silicon composite material is Si-50Al matrix material;
7) binding force of cladding material detects: with stove, be warming up to 300 ℃, with being placed in 450 ℃ ± 10 ℃ retort furnaces, toast 2 minutes, take out, be cooled to room temperature, 10 times are amplified Microscopic observation coating without peeling bubbling phenomenon, binding force of cladding material is fine, and coating and high silica/aluminum-based material firm binding force reach GJB1420 < < semiconductor integrated circuit shell general specification > > appendix A specified standards.
Described chemical nickel plating liquid formula: nickelous chloride (NiCl
26H
2o) 20 ~ 22g/L, inferior sodium phosphate (NaH
2pO
2h
2o) 10 ~ 13 g/L, ammonium chloride (NH
4cl) 25～35g/L, ammonium citrate ((NH4)
3c
6h
5o
7) 45～55g/L, ammoniacal liquor 50mL/L, pH value 8 ~ 10.
Described activation solution formula: hydrochloric acid (HCl) 150 ~ 200ml/L, iron(ic) chloride (FeCl
36H
2o) 150 ~ 200g/L and water 1L.
Useful technique effect of the present invention embodies in the following areas:
1. the gold-plated coating structure of high aluminium silicon composite material in the present invention is mainly by nickel and two kinds of gold, binding force of cladding material is strong, through GJB1420 < < semiconductor integrated circuit shell general specification > > appendix A: through 450 ℃ of high bakes 2 minutes, do not occur that coating bubbles, comes off etc., it is visible under SEM400 doubly scans, between nickel dam and base material, nickel dam and gold layer all in conjunction with tight, transition interface is clear between layers, referring to Fig. 2;
2. the high aluminium silicon composite material of the present invention (Si-50Al matrix material) is middle because of the silicon containing 50%, referring to Fig. 1, silicon becomes irregular form to be dispersed in material structure with aluminium, silicon possesses and the equal nonreactive chemical property of nitric acid, hydrochloric acid and alkali, and aluminium all reacts with soda acid, when dip-galvanizing, nonmetallic silicon face is difficult to the heavy zinc of displacement, and it is very poor that the existence of a large amount of silicon in surface causes coating to be combined with base material, and even substrate surface cannot deposit coating.In the present invention, adopt the alkaline etching solution of low-concentration sodium hydroxide and the light-emitting solution of hydrofluoric acid containing, can be so that the reactive aluminum in base material weaken, and silicon can react with hydrofluoric acid, and silicon and aluminium are synchronously dissolved, and eliminates the too much accumulation of surface silicon, improves binding force of cladding material;
3. Si-50Al matrix material craft of gilding Process Design has adopted ageing treatment in the present invention, after nickel plating for the first time, by part process certain temperature and the ageing treatment of time, the internal stress of its coating is fully discharged like this, the tissue of chemical Ni-plating layer changes simultaneously, its plasticity and toughness improve, theoretical analysis is thought can there is certain interface mutual diffusion between chemical Ni-plating layer and base material at this temperature, in interface, form certain diffusion layer, the combination of electroless nickel layer and base material is improved greatly, even become one, subsequently due to consider chemical Ni-plating layer through ageing treatment rear surface due to oxidation and alloy characteristic, follow-up, be difficult to activation treatment before gold-plated, therefore increasing nickel layer after chemical nickel plating covers, activation is carried out on nickel layer surface like this, just can fully guarantee the combination between electronickelling and substrate nickel,
4. the high aluminium silicon composite material in the present invention is gold-plated, according to SEM enlargement ratio scale, directly perceived coating total thickness approximately 7～8 μ m that measure, nickel dam approximately 4.5～5.5 μ m wherein, golden layer thickness approximately 2.5 μ m, as seen from Figure 3, from section, see that transition is clear between layers, between coating and substrate in conjunction with closely, tight and break-off, scolder is sprawled infiltration at coating surface, without rosin joint or sealing-off.After simultaneously gold-plated by T/R shell product, carry out Laser seal welding test, housing resistance to air loss detects and reaches 2.175 * 10-3Pacm
3/ s.
Accompanying drawing explanation
Fig. 1 is the SEM microscopic appearance figure of Si-50Al matrix material in the present invention.
Fig. 2 is the gold-plated transverse section of Si-50Al matrix material SEM microscopic appearance figure in the present invention.
Fig. 3 is weldability sample transverse section SEM microscopic appearance figure in the present invention.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described.
Following examples are raw materials used: hydrofluoric acid (HF), concentrated nitric acid (HNO
3), sodium hydroxide NaOH, sodium carbonate Na
2cO
3, sodium phosphate Na
3pO
4, zinc oxide (ZnO) 100g/L, Seignette salt (KNaC
4h
4o
6), SODIUMNITRATE (NaNO
3), nickelous chloride (NiCl
26H
2o), inferior sodium phosphate (NaH
2pO
2h
2o), ammonium chloride (NH
4cl), ammonium citrate ((NH4)
3c
6h
5o
7), ammoniacal liquor, single nickel salt (NiSO
47H
2o), sodium-chlor (NaCl), boric acid (H
3bO
3), hydrochloric acid (HCl), iron(ic) chloride (FeCl
36H
2o), potassium auric cyanide (KAu (CN)
2), citric acid (H
3c
6h
5o
7), Tripotassium Citrate (K
3c
6h
5o
7), acetone, is market conventional chemical reagent on sale and commodity.
Embodiment 1:
The gold-plated concrete operation step of Si-50Al matrix material is as follows:
Preparation gold plating liquid: take potassium auric cyanide, citric acid according to formula, Tripotassium Citrate first injects 1/3rd deionized water in plating solution, adds the potassium auric cyanide taking and it is fully dissolved; By the citric acid taking and Tripotassium Citrate, separately with pouring into after deionized water dissolving in coating bath, supplementary deionized water is to the liquid level of working.The gold plating liquid composition and the content that are mixed with are: potassium auric cyanide 20 g/L, citric acid 12 g/L, Tripotassium Citrate 30g/L.
Preparation alkaline etching solution: according to formula weighing sodium hydroxide, sodium carbonate, sodium phosphate, be mixed with solution, the alkaline etching solution composition being mixed with and content are NaOH 5g/L, Na
2cO
330g/L, Na
3pO
440g/L and water 1L.
Preparation bright dipping solution: measure hydrofluoric acid and concentrated nitric acid by formula, hydrofluoric acid is added slowly in concentrated nitric acid and stirred be cooled to room temperature.
Prepare one time zincate solution: in coating bath, inject 1/3rd deionized water, add the sodium hydroxide taking and it is fully dissolved, add while hot the zinc oxide taking, be stirred well to completely and dissolve, again the Seignette salt taking and iron trichloride are added to coating bath after dissolving separately respectively, finally add the hydrofluoric acid measuring, supplementary deionized water is to the liquid level of working.The zincate solution composition and the content that are mixed with are: sodium hydroxide 500g/L, zinc oxide 100g/L, Seignette salt 10g/L, iron trichloride 2g/L, hydrofluoric acid 1mL/L.
Preparation secondary soaking zinc liquid: inject 1/3rd deionized water in coating bath, add the sodium hydroxide taking and make
It fully dissolves, and adds while hot the zinc oxide taking, and is stirred well to completely and dissolves, then the Seignette salt taking and iron trichloride are added to coating bath after dissolving separately respectively, finally adds the SODIUMNITRATE taking, and supplementary deionized water is to the liquid level of working.The secondary soaking zinc liquid composition and the content that are mixed with are: sodium hydroxide 100g/L, zinc oxide 20g/L, Seignette salt 20g/L, iron trichloride 2g/L, SODIUMNITRATE 1g/L.
Preparation chemical nickel-plating liquid: inject 1/3rd deionized water in coating bath, add the nickelous chloride taking and make it
Fully dissolve, add coating bath, then add coating bath after the inferior sodium phosphate taking is dissolved separately after the ammonium chloride taking, ammonium citrate are dissolved separately respectively, measure ammoniacal liquor add in coating bath by formula, supplementary deionized water is to the liquid level of working.The chemical nickel solution composition and the content that are mixed with are: nickelous chloride 21g/L, inferior sodium phosphate 12 g/L, ammonium chloride 35g/L, ammonium citrate 45g/L, ammoniacal liquor 50mL/L.
Preparation nickel plating solution: inject 1/3rd deionized water in coating bath, add the single nickel salt taking and it is fully dissolved, after being dissolved separately, the sodium-chlor taking adds coating bath, after again the boric acid taking fully being dissolved with hot deionized water boiling is lower separately, add coating bath, supplementary deionized water, to the liquid level of working, is adjusted pH value to the claimed range of filling a prescription with diluted sodium hydroxide solution.The nickel-plating liquid composition and the content that are mixed with are: single nickel salt 170g/L, and sodium-chlor 10g/L, boric acid 30g/L, under 20 ℃ of conditions of temperature, pH 5.0.
Preparation activation solution: toward coating bath in, inject 1/3rd deionized water, add the iron(ic) chloride taking and it is fully dissolved, measured hydrochloric acid is slowly added to coating bath, fully stirring, supplementary deionized water is to the liquid level of working, and is cooled to after room temperature stand-by.The activation solution composition and the content that are mixed with are: hydrochloric acid 170ml/L, iron(ic) chloride 180g/L.
First high aluminium silicon composite material is carried out to pre-treatment, pre-treatment routinely plating on aluminium alloy secondary soaking zinc treatment process is divided into six steps: clean oil removing, alkaline etching, bright dipping, once soak zinc, move back zinc and secondary soaking zinc; Concrete operations are as follows: with the high aluminium silicon composite material part of suitable copper conductor clamping, put into the acetone soln ultrasonic cleaning oil removing 15min of 20 ℃; In the alkaline etching solution of 62 ℃ of temperature, swing gently 10S again, take out, in flowing water, fully clean and be dried; Then put into 15 ℃ of light-emitting solution, swing fast part, after 4S, take out, fully washing, puts into subsequently a zincate solution and swings gently 45 seconds, 20 ℃ of temperature immediately, taking-up is put into cold water and is washed, then puts into and move back zinc liquid and move back zinc, 3 seconds time, taking-up is after flowing water cleans, put into immediately secondary soaking zinc liquid and swing gently 15 seconds, 15 ℃ of temperature, take out, running water wash, obtains pre-treatment part;
1) preplating chemical nickel: pre-treatment part is put into chemical nickel-plating liquid preplating immediately, under 80 ± 2 ℃ of conditions of temperature, preplating 20 minutes;
2) nickel plating for the first time: nickel plating process routinely, the part that step 1) was processed fully cleans in cold water, proceeds to nickel plating in nickel plating solution, under 20 ℃ of conditions of temperature, pH5.0, current density 0.7A/dm
2, 20 minutes time, take out, clean, dry;
3) ageing treatment: by step 2) vacuum oven of putting into of Ni plated carries out ageing treatment, and aging temperature is 360 ℃, is incubated 1 hour, vacuum tightness 1.1 * 10
-3pa, heats up with stove, after furnace cooling, takes out;
4) activation: the part after step 3) is processed is put into activation solution, under 15 ℃ of conditions of temperature, limit swings gently limit and soaks taking-up afterwards in 20 seconds, in flowing water, fully cleans;
5) nickel plating for the second time: nickel plating process routinely, the part after step 4) is processed is put into immediately nickel-plating liquid and is carried out nickel plating for the second time, and under 20 ℃ of conditions of temperature, pH 5.0, current density 0.7A/dm
2, 20 minutes time, take out, clean;
6) gold-plated: using proof gold plate or platinum titanium net as anode, high aluminium silicon composite material is negative electrode, plates routinely pure gold method, the part after step 5) is processed carries out gold-plated, plating condition: temperature 60 C, pH 4.8, current density 0.4/dm
2, 14 minutes time, golden layer thickness is 2.45 microns.
Experimental result: after the part that Si-50Al composite processing is made is gold-plated as stated above, the crystallization of outward appearance gold layer is careful, color even, after rising to 300 ℃ with stove, putting into 455～460 ℃ of retort furnaces dries 2 minutes, take out, cooling under room temperature after, be placed under 10 times of magnifying glasses, observe coating without peeling bubbling phenomenon, binding force of cladding material is fine.
Embodiment 2:
The gold-plated concrete operation step of Si-50Al matrix material is as follows:
Preparation gold plating liquid: take potassium auric cyanide, citric acid according to formula, Tripotassium Citrate first injects 1/3rd deionized water in plating solution, adds the potassium auric cyanide taking and it is fully dissolved; By the citric acid taking and Tripotassium Citrate, separately with pouring into after deionized water dissolving in coating bath, supplementary deionized water is to the liquid level of working.The gold plating liquid composition and the content that are mixed with are: potassium auric cyanide 22 g/L, citric acid 11 g/L, Tripotassium Citrate 32g/L.
Preparation alkaline etching solution: according to formula weighing sodium hydroxide, sodium carbonate, sodium phosphate, be mixed with solution, the alkaline etching solution composition being mixed with and content are NaOH 8g/L, Na
2cO
335g/L, Na
3pO
450g/L and water 1L.
Preparation bright dipping solution: measure hydrofluoric acid and concentrated nitric acid by formula, hydrofluoric acid is added slowly in concentrated nitric acid and stirred be cooled to room temperature.
Prepare one time zincate solution: in coating bath, inject 1/3rd deionized water, add the sodium hydroxide taking and it is fully dissolved, add while hot the zinc oxide taking, be stirred well to completely and dissolve, again the Seignette salt taking and iron trichloride are added to coating bath after dissolving separately respectively, finally add the hydrofluoric acid measuring, supplementary deionized water is to the liquid level of working.The zincate solution composition and the content that are mixed with are: sodium hydroxide 500g/L, zinc oxide 100g/L, Seignette salt 10g/L, iron trichloride 2g/L, hydrofluoric acid 1mL/L.
Preparation secondary soaking zinc liquid: inject 1/3rd deionized water in coating bath, add the sodium hydroxide taking and it is fully dissolved, add while hot the zinc oxide taking, be stirred well to completely and dissolve, again the Seignette salt taking and iron trichloride are added to coating bath after dissolving separately respectively, finally add the SODIUMNITRATE taking, supplementary deionized water is to the liquid level of working.The secondary soaking zinc liquid composition and the content that are mixed with are: sodium hydroxide 100g/L, zinc oxide 20g/L, Seignette salt 20g/L, iron trichloride 2g/L, SODIUMNITRATE 1g/L.
Preparation chemical nickel-plating liquid: inject 1/3rd deionized water in coating bath, add the nickelous chloride taking and it is fully dissolved, after being dissolved separately respectively, the ammonium chloride taking, ammonium citrate add coating bath, after again the inferior sodium phosphate taking being dissolved separately, add coating bath, by formula, measure ammoniacal liquor and add in coating bath, supplementary deionized water is to the liquid level of working.The chemical nickel solution composition and the content that are mixed with are: nickelous chloride 19g/L, inferior sodium phosphate 11 g/L, ammonium chloride 30g/L, ammonium citrate 45g/L, ammoniacal liquor 50mL/L.
Preparation nickel plating solution: inject 1/3rd deionized water in coating bath, add the single nickel salt taking and it is fully dissolved, after being dissolved separately, the sodium-chlor taking adds coating bath, after again the boric acid taking fully being dissolved with hot deionized water boiling is lower separately, add coating bath, supplementary deionized water, to the liquid level of working, is adjusted pH value to the claimed range of filling a prescription with diluted sodium hydroxide solution.The nickel-plating liquid composition and the content that are mixed with are: single nickel salt 190g/L, sodium-chlor 12g/L, boric acid 35g/L.
Preparation activation solution: toward coating bath in, inject 1/3rd deionized water, add the iron(ic) chloride taking and it is fully dissolved, measured hydrochloric acid is slowly added to coating bath, fully stirring, supplementary deionized water is to the liquid level of working, and is cooled to after room temperature stand-by.The activation solution composition and the content that are mixed with are: hydrochloric acid 150ml/L, iron(ic) chloride 158g/L.
First high aluminium silicon composite material is carried out to pre-treatment, pre-treatment routinely plating on aluminium alloy secondary soaking zinc treatment process is divided into six steps: clean oil removing, alkaline etching, bright dipping, once soak zinc, move back zinc and secondary soaking zinc; Concrete operations are as follows: with the high aluminium silicon composite material part of suitable copper conductor clamping, put into the acetone soln ultrasonic cleaning oil removing 15min of 20 ℃; Put into again 65 ℃ of alkaline etching solution and swing gently 11S, take out, in flowing water, fully clean and be dried.Then put into 15 ℃ of light-emitting solution, swing fast part, after 6S, take out, fully washing, puts into subsequently a zincate solution and swings gently 50 seconds, 20 ℃ of temperature immediately, taking-up is put into cold water and is washed, then puts into and move back zinc liquid and move back zinc, 3 seconds time, taking-up is after flowing water cleans, put into immediately secondary soaking zinc liquid and swing gently 14 seconds, 15 ℃ of temperature, take out, running water wash, obtains pre-treatment part;
1) preplating chemical nickel: pre-treatment part is put into chemical nickel-plating liquid preplating immediately, under 80 ± 2 ℃ of conditions of temperature, preplating 20 minutes;
2) nickel plating for the first time: nickel plating process routinely, after fully cleaning in cold water, the part after step 1) is processed proceeds to nickel plating in nickel plating solution, and under 20 ℃ of conditions of temperature, pH 4.9, current density 0.7A/dm
2, 20 minutes time, take out, clean, dry;
3) ageing treatment: by step 2) part after nickel plating is put into vacuum oven and is carried out ageing treatment, and aging temperature is 370 ℃, is incubated 1 hour, vacuum tightness 1.1 * 10
-3pa, heats up with stove, after furnace cooling, takes out;
4) activation: the part after step 3) is processed is put into activation solution, under 15 ℃ of conditions of temperature, limit swings gently limit and soaks taking-up afterwards in 24 seconds, in flowing water, fully cleans;
5) nickel plating for the second time: nickel plating process routinely, the part after step 4) is processed is put into immediately nickel-plating liquid and is carried out nickel plating for the second time, and under 20 ℃ of conditions of temperature, pH 4.9, current density 0.7A/dm
2, 20 minutes time, take out, clean;
6) gold-plated: using proof gold plate or platinum titanium net as anode, high aluminium silicon composite material is negative electrode, plates routinely pure gold method, the part after step 5) is processed carries out gold-plated, plating condition: 58 ℃ of temperature, pH 5.0, current density 0.5/dm
2, 12 minutes time, golden layer thickness is 2.67 microns.
Experimental result: after the part that Si-50Al composite processing is made is gold-plated as stated above, the crystallization of outward appearance gold layer is careful, color even, after rising to 300 ℃ with stove, putting into 455～460 ℃ of retort furnaces dries 2 minutes, take out, cooling under room temperature after, be placed under 10 times of magnifying glasses, observe coating without peeling bubbling phenomenon, binding force of cladding material is fine.
Embodiment 3:
The gold-plated concrete operation step of Si50% aluminium silicon composite material is as follows:
Preparation gold plating liquid: take potassium auric cyanide, citric acid according to formula, Tripotassium Citrate first injects 1/3rd deionized water in plating solution, adds the potassium auric cyanide taking and it is fully dissolved; By the citric acid taking and Tripotassium Citrate, separately with pouring into after deionized water dissolving in coating bath, supplementary deionized water is to the liquid level of working.The gold plating liquid composition and the content that are mixed with are: potassium auric cyanide 25 g/L, citric acid 10 g/L, Tripotassium Citrate 35g/L.
Preparation alkaline etching solution: according to formula weighing sodium hydroxide, sodium carbonate, sodium phosphate, be mixed with solution, the alkaline etching solution composition being mixed with and content are NaOH 6g/L, Na
2cO
340g/L, Na
3pO
448g/L and water 1L.
Preparation bright dipping solution: measure hydrofluoric acid and concentrated nitric acid by formula, hydrofluoric acid is added slowly in concentrated nitric acid and stirred be cooled to room temperature.
Prepare one time zincate solution: in coating bath, inject 1/3rd deionized water, add the sodium hydroxide taking and it is fully dissolved, add while hot the zinc oxide taking, be stirred well to completely and dissolve, again the Seignette salt taking and iron trichloride are added to coating bath after dissolving separately respectively, finally add the hydrofluoric acid measuring, supplementary deionized water is to the liquid level of working.The zincate solution composition and the content that are mixed with are: sodium hydroxide 500g/L, zinc oxide 100g/L, Seignette salt 10g/L, iron trichloride 2g/L, hydrofluoric acid 1mL/L.
Preparation secondary soaking zinc liquid: inject 1/3rd deionized water in coating bath, add the sodium hydroxide taking and it is fully dissolved, add while hot the zinc oxide taking, be stirred well to completely and dissolve, again the Seignette salt taking and iron trichloride are added to coating bath after dissolving separately respectively, finally add the SODIUMNITRATE taking, supplementary deionized water is to the liquid level of working.The secondary soaking zinc liquid composition and the content that are mixed with are: sodium hydroxide 100g/L, zinc oxide 20g/L, Seignette salt 20g/L, iron trichloride 2g/L, SODIUMNITRATE 1g/L.
Preparation chemical nickel-plating liquid: inject 1/3rd deionized water in coating bath, add the nickelous chloride taking and make it
Fully dissolve, add coating bath, then add coating bath after the inferior sodium phosphate taking is dissolved separately after the ammonium chloride taking, ammonium citrate are dissolved separately respectively, measure ammoniacal liquor add in coating bath by formula, supplementary deionized water is to the liquid level of working.The chemical nickel solution composition and the content that are mixed with are: nickelous chloride 21g/L, inferior sodium phosphate 11 g/L, ammonium chloride 30g/L, ammonium citrate 45g/L, ammoniacal liquor 50mL/L.
Preparation nickel plating solution: inject 1/3rd deionized water in coating bath, add the single nickel salt taking and it is fully dissolved, after being dissolved separately, the sodium-chlor taking adds coating bath, after again the boric acid taking fully being dissolved with hot deionized water boiling is lower separately, add coating bath, supplementary deionized water, to the liquid level of working, is adjusted pH value to the claimed range of filling a prescription with diluted sodium hydroxide solution.The nickel-plating liquid composition and the content that are mixed with are: single nickel salt 150g/L, sodium-chlor 10g/L, boric acid 30g/L.
Preparation activation solution: toward coating bath in, inject 1/3rd deionized water, add the iron(ic) chloride taking and it is fully dissolved, measured hydrochloric acid is slowly added to coating bath, fully stirring, supplementary deionized water is to the liquid level of working, and is cooled to after room temperature stand-by.The activation solution composition and the content that are mixed with are: hydrochloric acid 200ml/L, iron(ic) chloride 200g/L.
First high aluminium silicon composite material is carried out to pre-treatment, pre-treatment routinely plating on aluminium alloy secondary soaking zinc treatment process is divided into six steps: clean oil removing, alkaline etching, bright dipping, once soak zinc, move back zinc and secondary soaking zinc; Concrete operations are as follows: with the high aluminium silicon composite material part of suitable copper conductor clamping, put into the acetone soln ultrasonic cleaning oil removing 15min of 20 ℃; Put into again 64 ℃ of alkaline etching solution and swing gently 10S, take out, in flowing water, fully clean and be dried.Then put into 15 ℃ of light-emitting solution, swing fast part, after 5S, take out, fully washing, puts into subsequently a zincate solution and swings gently 35 seconds, 20 ℃ of temperature immediately, taking-up is put into cold water and is washed, then puts into and move back zinc liquid and move back zinc, 3 seconds time, taking-up is after flowing water cleans, put into immediately secondary soaking zinc liquid and swing gently 14 seconds, 15 ℃ of temperature, take out, running water wash, obtains pre-treatment part;
1) preplating chemical nickel: pre-treatment part is put into chemical nickel-plating liquid preplating, under 80 ± 2 ℃ of conditions of temperature, preplating 20 minutes;
2) nickel plating for the first time: nickel plating process routinely, after fully cleaning in cold water, the part after step 1) is processed proceeds to nickel plating in nickel plating solution, and under 20 ℃ of conditions of temperature, pH 4.8, current density 0.7A/dm
2, 20 minutes time, take out, clean, dry;
3) ageing treatment: by step 2) part after nickel plating is put into vacuum oven and is carried out ageing treatment, and aging temperature is 370 ℃, is incubated 1 hour, vacuum tightness 1.1 * 10
-3pa, heats up with stove, after furnace cooling, takes out;
4) activation: the part after step 3) is processed is put into activation solution, under 15 ℃ of conditions of temperature, limit swings gently limit and soaks taking-up afterwards in 24 seconds, in flowing water, fully cleans;
5) nickel plating for the second time: nickel plating process routinely, the part after step 4) is processed is put into immediately nickel-plating liquid and is carried out nickel plating for the second time, and under 20 ℃ of conditions of temperature, pH 4.8, current density 0.7A/dm
2, 20 minutes time, take out, clean;
6) gold-plated: using proof gold plate or platinum titanium net as anode, high aluminium silicon composite material is negative electrode, plates routinely pure gold method, the part after step 5) is processed carries out gold-plated, plating condition: 55 ℃ of temperature, pH 5.1, current density 0.3/dm
2, 15 minutes time, golden layer thickness is 2.15 microns.
Experimental result: after the part that Si-50Al composite processing is made is gold-plated as stated above, the crystallization of outward appearance gold layer is careful, color even, after rising to 300 ℃ with stove, putting into 455～460 ℃ of retort furnaces dries 2 minutes, take out, cooling under room temperature after, be placed under 10 times of magnifying glasses, observe coating without peeling bubbling phenomenon, binding force of cladding material is fine.
Claims (3)
1. the gold plating method of high aluminium silicon composite material, comprise pre-treatment, described pre-treatment routinely plating on aluminium alloy secondary soaking zinc treatment process is divided into six steps: clean oil removing, alkaline etching, bright dipping, once soak zinc, move back zinc and secondary soaking zinc, it is characterized in that: the concrete operation step after pre-treatment is as follows:
1) preplating chemical nickel: the part after pre-treatment is put into chemical nickel-plating liquid preplating, under 80 ± 2 ℃ of conditions of temperature, 20 minutes preplating time;
2) nickel plating for the first time: nickel plating process routinely, nickel plating in conventional nickel plating solution, 2 ~ 3 microns of nickel layer thickness, take out, and clean, dry;
3) ageing treatment: by step 2) part of Ni plated is put into vacuum oven and is carried out ageing treatment, and aging temperature is 360 ± 10 ℃, is incubated 1 hour, vacuum tightness 1.1 * 10
-3pa, heats up with stove, after furnace cooling, takes out;
4) activation: the part after step 3) is processed is put into activation solution, under 15 ~ 25 ℃ of conditions of temperature, soaks 20 ~ 30 seconds;
5) nickel plating for the second time: nickel plating process routinely, the part nickel plating in conventional nickel plating solution after step 4) is processed, 2 ~ 3 microns of nickel layer thickness, take out, and clean;
6) gold-plated: using proof gold plate or platinum titanium net as anode, high aluminium silicon composite material is negative electrode, plates routinely pure gold method, the part after step 5) is processed carries out gold-plated, 2 ~ 3 microns of golden layer thicknesses; Described high aluminium silicon composite material is Si-50Al matrix material;
7) binding force of cladding material detects: with stove, be warming up to 300 ℃, with being placed in 450 ℃ ± 10 ℃ retort furnaces, toast 2 minutes, take out, be cooled to room temperature, 10 times are amplified Microscopic observation coating without peeling bubbling phenomenon, binding force of cladding material is fine, and coating and high silica/aluminum-based material firm binding force reach GJB1420 < < semiconductor integrated circuit shell general specification > > appendix A specified standards.
2. the gold plating method of high aluminium silicon composite material according to claim 1, it is characterized in that: described chemical nickel plating liquid formula: nickelous chloride 20 ~ 22g/L, inferior sodium phosphate 10 ~ 13 g/L, ammonium chloride 25～35g/L, ammonium citrate 45～55g/L, ammoniacal liquor 50mL/L, pH value 8 ~ 10.
3. the gold plating method of high aluminium silicon composite material according to claim 1, is characterized in that: described activation solution formula: hydrochloric acid 150 ~ 200ml/L, iron(ic) chloride 150 ~ 200g/L and water 1L.
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