CN102286763A - Process method for electroplating copper on TC4 titanium alloy surface - Google Patents
Process method for electroplating copper on TC4 titanium alloy surface Download PDFInfo
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- CN102286763A CN102286763A CN201110246564XA CN201110246564A CN102286763A CN 102286763 A CN102286763 A CN 102286763A CN 201110246564X A CN201110246564X A CN 201110246564XA CN 201110246564 A CN201110246564 A CN 201110246564A CN 102286763 A CN102286763 A CN 102286763A
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Abstract
The invention discloses a process method for electroplating copper on a TC4 titanium alloy surface. The process method comprises the following steps: sequentially carrying out alkali-washing, deoiling and degreasing of a test sample or a workpiece, washing by using water, washing by acid and corroding, washing by using water, activating, washing by using water, electroplating, cleaning, passivating surface, cleaning and drying. The invention solves the technical problem that copper is difficultly plated on the TC4 titanium alloy surface, preplating treatment is not needed, and the copper is directly electroplated on the TC4 titanium alloy surface under the condition of room temperature. The process method has the advantages of simplicity, stability and reliability in process, convenience for operation, high efficiency, low cost, easiness for realization and the like, and can be used for obtaining a copper plating layer with favourable binding force, uniformity, compactness and smooth surface. The binding force is detected by using methods, such as an edge trimming method, a scratching method, a rubbing method, a polishing method and the like, and the plating layer and a substrate show an excellent binding force.
Description
Technical field
What the present invention relates to is a kind of TC4 titanium alloy surface copper electroplating technological process, belongs to the metal surface properties modification technical field.
Background technology
Copper has fusing point height, characteristics that plasticity is good, be applied in metal material surface and can reduce frictional coefficient greatly, reduce friction, the friction and wear behavior that improves metal material surface had good effect, especially for thread surface, have good anti-stick button effect, at present, the screw thread of petroleum pipeline mostly is to adopt copper facing to improve its wear resistance and anti-stick button performance.Titanium alloy is as the selection preferably of high-strength corrosion-resistant erosion oil pipe, but titanium alloy material viscosity is big, wears no resistance, and screw thread easily produces thread gluing, because titanium alloy surface copper facing technology is difficult to realization, becomes the technical bottleneck of titanium alloy as the petroleum pipeline material.
In recent years, the research that relates to titanium alloy surface copper facing technological method is very few, and not seeing has reliable and stable technology and application example thereof, mainly has following problem: (1) titanium elements chemically reactive is big, therefore surperficial easily generation oxidation electroplates or the very difficult realization of electroless plating at titanium alloy surface; (2) the surface bonding power of coating and matrix is poor, and quality of coating is difficult to satisfy the technical requirements of using; (3) the TC4 titanium alloy copper-plating technique research of publishing is very not complete, and some method need be carried out the preplating processing, and exploitativeness is poor.
At present, there is the research of a spot of titanium alloy copper-plating technique mainly to concentrate on to plate pre-treating process and simply compares, or the simple comparative analysis of quality of coating, but not seeing has the complete technical study and the report of production application thereof, and some investigators utilize cyanide copper plating at titanium alloy surface, and prussiate is huge poisonous substance matter on the one hand, big to human body harm, not environmental protection of cyanide copper plating on the other hand easily causes serious environmental to pollute, and nontoxic copper facing technology of TC4 titanium alloy surface and application thereof still belong to blank.Therefore research and realization TC4 titanium alloy surface copper facing Technique on T C4 titanium alloy are significant in the application of petroleum pipeline industrial circle.
Summary of the invention
In order to overcome the deficiency that prior art can't realize nontoxic copper facing and coating and basal body binding force difference, the invention provides the processing method of a kind of TC4 titanium alloy surface electro-coppering, need not preplating handle, directly copper facing on the TC4 titanium alloy surface, it is good to obtain bonding force, evenly, the coating of fine and close, any surface finish, and have technology simple, easy to operate, with low cost, be easy to realize, the efficient advantages of higher, be suitable for producing and using.
The present invention solves the process program that its technical problem adopts and may further comprise the steps:
1. alkali cleaning: it is 65～80 ℃ of alkaline washs that sample or workpiece are placed temperature, soaks 10～15 minutes;
2. washing: use the flowing water flushing to the no alkaline wash in surface on sample after the alkali cleaning or workpiece;
3. pickling: sample after will washing or workpiece place the pickle solution of room temperature to soak 1～2 minute, carry out surface corrosion and handle;
4. washing: use the flowing water flushing to the no pickle solution in surface on sample after the pickling or workpiece;
5. activation treatment: it is that 80～90 ℃ activation solution soaked 20～25 minutes that sample after will washing or workpiece place temperature, carries out surface activation process;
6. washing: sample after will activating or workpiece use the flowing water flushing to the no activation solution in surface;
7. electroplate: sample after will washing or workpiece place the electroplate liquid of room temperature to electroplate, and are electroplated to satisfy till the requirement of workpiece thickness of coating, and current density is 1.5～7.8A/dm
2
8. clean: sample after will electroplating or workpiece use the flowing water flushing to surperficial electroless plating liquid;
9. passivation: the sample or the workpiece passivating solution that places room temperature of oven dry were soaked 3～5 minutes, carry out the coating surface Passivation Treatment;
10. cleaning, drying: use the flowing water flushing to the no passivating solution in surface on sample after the passivation or workpiece, and then dry to surface drying end.
Described alkaline wash is with NaOH and Na
3PO
4Be dissolved in the distilled water, content is respectively: NaOH 75～100g/L, Na
3PO
420～25g/L.
Described pickle solution comprises HF, HNO
3And H
2O, content is respectively: HF 100～200ml/L, HNO
3300～400ml/L, H
2O 400～600ml/L, HF, HNO
3And H
2The component summation of O is 100%.
Described activation solution is with K
2Cr
2O
7Be dissolved in the distilled water with HF, content is respectively: K
2Cr
2O
7180～250g/L, HF 50～80ml/L.
Described electroplate liquid is with CuSO
45H
2O and H
2SO
4Be dissolved in the distilled water, content is respectively: CuSO
45H
2O150～200g/L, H
2SO
460～80ml/L.
Described passivating solution is with CrO
3, NaCl and H
2SO
4Be dissolved in the distilled water, content is respectively: CrO
380～90g/L; NaCl 1～2g/L; H
2SO
425～30ml/L.
The invention has the beneficial effects as follows: the invention solves the technical barrier that the copper facing of TC4 titanium alloy surface is difficult to realize, need not preplating handle, TC4 titanium alloy surface Direct Electroplating copper at ambient temperature, process stabilizing is reliable, can obtain that bonding force is good, even, fine and close, the copper coating of any surface finish, and have that technology is simple, easy to operate, efficient is high, with low cost, be easy to advantages such as realization.Adopt methods such as file limit method, scratch method, rubbing manipulation and polishing method that bonding force is detected, coating and matrix show extraordinary bonding force.
The present invention is further described below in conjunction with drawings and Examples.
Description of drawings
Fig. 1 is for adopting the coating cross section microstructure figure under the different electroplating time conditions that the present invention obtained, and wherein Fig. 1 (a) is for electroplating 20 minutes, and Fig. 1 (b) is for electroplating 30 minutes, and Fig. 1 (c) is for electroplating 40 minutes;
Fig. 2 is for adopting the coating surface macro morphology figure under the different electroplating time conditions that the present invention obtained, and wherein Fig. 2 (a) is for electroplating 20 minutes, and Fig. 2 (b) is for electroplating 30 minutes, and Fig. 2 (c) is for electroplating 40 minutes;
Fig. 3 is for adopting the coating surface microscopic appearance figure under the different electroplating time conditions that the present invention obtained, and wherein Fig. 3 (a) is for electroplating 20 minutes, and Fig. 3 (b) is for electroplating 30 minutes, and Fig. 3 (c) is for electroplating 40 minutes;
Fig. 4 distributes for adopting the coating cross section element under the different electroplating time conditions that the present invention obtained, and wherein Fig. 4 (a) is for electroplating figure a 20 minutes
IBe line scanning direction, figure a
IIFor the line sweep element distributes; Fig. 4 (b) is for electroplating figure b 30 minutes
IBe line scanning direction, figure b
IIFor the line sweep element distributes; Fig. 4 (c) is for electroplating figure c 40 minutes
IBe line scanning direction, figure c
IIFor the line sweep element distributes;
Fig. 5 is a method flow diagram of the present invention.
Embodiment
Embodiment 1
To TC4 titanium alloy specification is the specimen surface copper facing of 25 * 20 * 5mm
Solution formula: 1. soda-wash solution: NaOH 75g/L; Na
3PO
420g/L is Acidwash solution 2.: HF 100ml/L; HNO
3300ml/L; Distilled water 600ml/L is activated solution 3.: K
2Cr
2O
7180g/L; HF 50ml/L is electroplating solution 4.: CuSO
45H
2O 150g/L; H
2SO
460ml/L is passivating dip 5.: CrO
380g/L; NaCl 1.0g/L; H
2SO
425ml/L.
Implementation and operation: 1. alkali cleaning: it is 65 ℃ of alkaline washs that sample is placed temperature, soaks 15 minutes; 2. washing: the sample after the alkali cleaning is used the flowing water flushing; 3. pickling: the sample after will washing places the pickle solution of room temperature to soak 2 minutes, carries out surface corrosion and handles; 4. washing: the sample after the pickling is used the flowing water flushing; 5. activation treatment: it is that 80 ℃ activation solution soaked 25 minutes that the sample after will washing places temperature, carries out surface activation process; 6. washing: the sample after will activating uses the flowing water flushing; 7. electroplate: the sample after will washing places the electroplate liquid of room temperature to electroplate, and current density is 1.5A/dm
2, electroplating time is 30 minutes; 8. clean: the sample after will electroplating uses the flowing water flushing; 9. passivation: place the passivating solution of room temperature to soak 5 minutes on the sample of oven dry, carry out the coating surface Passivation Treatment; 10. cleaning, drying: the sample after the passivation is used distilled water flushing, dry again, finish.
Implementation result: TC4 titanium alloy specimen surface has obtained that bonding force is good, even, fine and close, the copper coating of any surface finish, adopt methods such as file limit method, scratch method, rubbing manipulation and polishing method that bonding force is detected, coating and matrix show extraordinary bonding force.
To TC4 titanium alloy specification is the specimen surface copper facing of 25 * 20 * 5mm
Solution formula: 1. soda-wash solution: NaOH 85g/L; Na
3PO
422.5g/L 2. Acidwash solution: HF 150ml/L; HNO
3350ml/L; Distilled water 500ml/L is activated solution 3.: K
2Cr
2O
7210g/L; HF 65ml/L is electroplating solution 4.: CuSO
45H
2O 180g/L; H
2SO
470ml/L is passivating dip 5.: CrO
385g/L; NaCl 1.5g/L; H
2SO
427.5ml/L.
Implementation and operation: 1. alkali cleaning: it is 70 ℃ of alkaline washs that sample is placed temperature, soaks 12 minutes; 2. washing: the sample after the alkali cleaning is used the flowing water flushing; 3. pickling: the sample after will washing places the pickle solution of room temperature to soak 1.5 minutes, carries out surface corrosion and handles; 4. washing: the sample after the pickling is used the flowing water flushing; 5. activation treatment: it is that 85 ℃ activation solution soaked 22 minutes that the sample after will washing places temperature, carries out surface activation process; 6. washing: the sample after will activating uses the flowing water flushing; 7. electroplate: the sample after will washing places the electroplate liquid of room temperature to electroplate, and current density is 3.5A/dm
2, electroplating time is 30 minutes; 8. clean: the sample after will electroplating uses the flowing water flushing; 9. passivation: place the passivating solution of room temperature to soak 4 minutes on the sample of oven dry, carry out the coating surface Passivation Treatment; 10. cleaning, drying: the sample after the passivation is used distilled water flushing, dry again, finish.
Implementation result: TC4 titanium alloy specimen surface has obtained that bonding force is good, even, fine and close, the copper coating of any surface finish, adopt methods such as file limit method, scratch method, rubbing manipulation and polishing method that bonding force is detected, coating and matrix show extraordinary bonding force.
To TC4 titanium alloy specification is the specimen surface copper facing of 25 * 20 * 5mm
Solution formula: 1. soda-wash solution: NaOH 100g/L; Na
3PO
425g/L is Acidwash solution 2.: HF 200ml/L; HNO
3400ml/L; Distilled water 400ml/L is activated solution 3.: K
2Cr
2O
7250g/L; HF 80ml/L is electroplating solution 4.: CuSO
45H
2O 200g/L; H
2SO
480ml/L is passivating dip 5.: CrO
390g/L; NaCl 2.0g/L; H
2SO
430ml/L.
Implementation and operation: 1. alkali cleaning: it is 80 ℃ of alkaline washs that sample is placed temperature, soaks 10 minutes; 2. washing: the sample after the alkali cleaning is used the flowing water flushing; 3. pickling: the sample after will washing places the pickle solution of room temperature to soak 1 minute, carries out surface corrosion and handles; 4. washing: the sample after the pickling is used the flowing water flushing; 5. activation treatment: it is that 90 ℃ activation solution soaked 20 minutes that the sample after will washing places temperature, carries out surface activation process; 6. washing: the sample after will activating uses the flowing water flushing; 7. electroplate: the sample after will washing places the electroplate liquid of room temperature to electroplate, and current density is 7.8A/dm
2, electroplating time is 30 minutes; 8. clean: the sample after will electroplating uses the flowing water flushing; 9. passivation: place the passivating solution of room temperature to soak 3 minutes on the sample of oven dry, carry out the coating surface Passivation Treatment; 10. cleaning, drying: the sample after the passivation is used distilled water flushing, dry again, finish.
Implementation result: TC4 titanium alloy specimen surface has obtained that bonding force is good, even, fine and close, the copper coating of any surface finish, adopt methods such as file limit method, scratch method, rubbing manipulation and polishing method that bonding force is detected, coating and matrix show extraordinary bonding force.
Embodiment 4
" the oil pipe box cupling interior threaded surface copper facing to TC4 titanium alloy 3 1/2
Solution formula: 1. soda-wash solution: NaOH 100g/L; Na
3PO
425g/L is Acidwash solution 2.: HF 100ml/L; HNO
3300ml/L; Distilled water 600ml/L is activated solution 3.: K
2Cr
2O
7250g/L; HF 50ml/L is electroplating solution 4.: CuSO
45H
2O 150g/L; H
2SO
480ml/L is passivating dip 5.: CrO
385g/L; NaCl 1.5g/L; H
2SO
430ml/L.
Implementation and operation: 1. alkali cleaning: it is 65 ℃ of alkaline washs that sample is placed temperature, soaks 10 minutes; 2. washing: the sample after the alkali cleaning is used the flowing water flushing; 3. pickling: the sample after will washing places the pickle solution of room temperature to soak 1 minute, carries out surface corrosion and handles; 4. washing: the sample after the pickling is used the flowing water flushing; 5. activation treatment: it is that 85 ℃ activation solution soaked 20 minutes that the sample after will washing places temperature, carries out surface activation process; 6. washing: the sample after will activating uses the flowing water flushing; 7. electroplate: the sample after will washing places the electroplate liquid of room temperature to electroplate, and current density is 3.5A/dm
2, electroplating time is 30 minutes; 8. clean: the sample after will electroplating uses the flowing water flushing; 9. passivation: place the passivating solution of room temperature to soak 5 minutes on the sample of oven dry, carry out the coating surface Passivation Treatment; 10. cleaning, drying: the sample after the passivation is used distilled water flushing, dry again, finish.
" oil pipe has obtained with the box cupling interior threaded surface that bonding force is good, even, fine and close, the copper coating of any surface finish to implementation result: TC4 titanium alloy 3 1/2; adopt method such as screw thread make-and-break test that bonding force is detected, coating and matrix show extraordinary bonding force.
Claims (6)
1. a TC4 titanium alloy surface copper electroplating technological process is characterized in that comprising the steps:
1. alkali cleaning: it is 65～80 ℃ of alkaline washs that sample or workpiece are placed temperature, soaks 10～15 minutes;
2. washing: use the flowing water flushing to the no alkaline wash in surface on sample after the alkali cleaning or workpiece;
3. pickling: sample after will washing or workpiece place the pickle solution of room temperature to soak 1～2 minute, carry out surface corrosion and handle;
4. washing: use the flowing water flushing to the no pickle solution in surface on sample after the pickling or workpiece;
5. activation treatment: it is that 80～90 ℃ activation solution soaked 20～25 minutes that sample after will washing or workpiece place temperature, carries out surface activation process;
6. washing: sample after will activating or workpiece use the flowing water flushing to the no activation solution in surface;
7. electroplate: sample after will washing or workpiece place the electroplate liquid of room temperature to electroplate, and are electroplated to satisfy till the requirement of workpiece thickness of coating, and current density is 1.5～7.8A/dm
2
8. clean: sample after will electroplating or workpiece use the flowing water flushing to surperficial electroless plating liquid;
9. passivation: the sample or the workpiece passivating solution that places room temperature of oven dry were soaked 3～5 minutes, carry out the coating surface Passivation Treatment;
10. cleaning, drying: use the flowing water flushing to the no passivating solution in surface on sample after the passivation or workpiece, and then dry to surface drying end.
2. TC4 titanium alloy surface copper electroplating technological process according to claim 1 is characterized in that: described alkaline wash is with NaOH and Na
3PO
4Be dissolved in the distilled water, content is respectively: NaOH 75～100g/L, Na
3PO
420～25g/L.
3. TC4 titanium alloy surface copper electroplating technological process according to claim 1, it is characterized in that: described pickle solution comprises HF, HNO
3And H
2O, content is respectively: HF 100～200ml/L, HNO
3300～400ml/L, H
2O 400～600ml/L, HF, HNO
3And H
2The component summation of O is 100%.
4. TC4 titanium alloy surface copper electroplating technological process according to claim 1, it is characterized in that: described activation solution is with K
2Cr
2O
7Be dissolved in the distilled water with HF, content is respectively: K
2Cr
2O
7180～250g/L, HF50～80ml/L.
5. TC4 titanium alloy surface copper electroplating technological process according to claim 1, it is characterized in that: described electroplate liquid is with CuSO
45H
2O and H
2SO
4Be dissolved in the distilled water, content is respectively: CuSO
45H
2O 150～200g/L, H
2SO
460～80ml/L.
6. TC4 titanium alloy surface copper electroplating technological process according to claim 1, it is characterized in that: described passivating solution is with CrO
3, NaCl and H
2SO
4Be dissolved in the distilled water, content is respectively: CrO
380～90g/L; NaCl 1～2g/L; H
2SO
425～30ml/L.
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|---|---|---|---|
| CN201110246564XA CN102286763A (en) | 2011-08-25 | 2011-08-25 | Process method for electroplating copper on TC4 titanium alloy surface |
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| CN103757676A (en) * | 2013-12-11 | 2014-04-30 | 中国航空工业标准件制造有限责任公司 | Pyrophosphate electrocoppering method of titanium alloy |
| CN103849914A (en) * | 2014-03-26 | 2014-06-11 | 西安石油大学 | Method for plating copper on titanium alloy coupling |
| CN104005059A (en) * | 2014-06-11 | 2014-08-27 | 沈阳飞机工业（集团）有限公司 | Method for electroplating chromium on TC1 titanium alloy and TC2 titanium alloy |
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