CN103668355A - Copper plating method for surface of tungsten helical line of travelling wave tube - Google Patents
Copper plating method for surface of tungsten helical line of travelling wave tube Download PDFInfo
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- CN103668355A CN103668355A CN201310650260.9A CN201310650260A CN103668355A CN 103668355 A CN103668355 A CN 103668355A CN 201310650260 A CN201310650260 A CN 201310650260A CN 103668355 A CN103668355 A CN 103668355A
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Abstract
The invention discloses a copper plating method for the surface of a tungsten helical line of a travelling wave tube. The method comprises the following steps: cleaning with chromic acid; washing with water; etching with hydrochloric acid; washing with water; copper preplating; pulsed copper plating; washing with water; ethanol dehydration; drying; combustion of hydrogen; cleaning with chromic acid; washing with water; etching with hydrochloric acid; washing with water; pulsed copper plating; washing with water; ethanol dehydration; drying; combustion of hydrogen; etc. According to the invention, through considerable experiments, preparation technology is screened, and solutions for copper preplating and copper plating, concrete process conditions and processes like combustion of hydrogen are optimized; the whole copper plating method has strong operationality and high efficiency; the copper plating method can plate a compact and uniform copper layer which hardly undergoes peeling and foaming on the surface of the tungsten helical line, substantially improves thermal conductivity of the tungsten helical line and enables high frequency loss during microwave transmission to be substantially reduced compared with the prior art.
Description
Technical field
The present invention relates to a kind of working method of travelling-wave tubes tungsten helix, be specifically related to the copper electroplating method on a kind of travelling-wave tubes tungsten helix surface.
Background technology
The spiral-line of tungsten material is the vitals of assembling travelling-wave tubes, in order to increase the heat dispersion of tungsten helix, on tungsten helix surface, carry out copper plating treatment, existing spiral-line copper-plating technique is before copper facing, to need the thin Ni of first preplating one deck, then could electroplate the Cu layer that upper surface is smooth, bonding force is good.The plyability coating of this Ni and Cu is after pyroprocessing, can there is obvious variation in surface color, this is owing at high temperature plating Ni layer and plating Cu layer interaction formation Ni-Cu alloy, after forming Ni-Cu alloy, can cause tungsten helix thermal conductivity sharply to decline, compared with Cu coating, during microwave transmission, high-frequency loss meeting increases severely, and affect the performance of helix TWT, and address this problem method the most effectively, is exactly at the surperficial direct copper plating of tungsten helix.But prior art often ran into coating peeling at tungsten helix copper coating, bubble, the technical disadvantages such as binding force of cladding material is poor.
goal of the invention
The object of the invention is in order to solve the deficiencies in the prior art, by great many of experiments, screen, provide a kind of easy to operate, technological design is reasonable, can be fine and close on tungsten helix plated surface efficiently, the copper electroplating method of uniform copper layer, the method can effectively solve prior art copper layer peeling, the technical deficiency such as bubble and binding force of cladding material is poor.
Technical scheme: in order to realize above object, the technical solution used in the present invention is:
The copper electroplating method on travelling-wave tubes tungsten helix surface, it comprises the following steps:
(1), get tungsten helix and in the chromic acid solution of 1.5 ~ 2mol/L, clean 0.5 ~ 5 minute, after then taking out, water rinses, and then uses the hydrochloric acid etching 1 ~ 5 minute of 3 ~ 3.5mol/L, then water rinses surface acid;
(2), get the pretreated tungsten helix of step (1) and put into pre-plating solution, carry out pre-copper plating treatment;
(3), get the tungsten helix that the pre-copper plating treatment of step (2) crosses and put into plating solution, carry out pulse copper plating treatment, then take out after washing, with ethanol dehydration, dry;
(4), get the tungsten helix that step (3) copper plating treatment crosses and carry out annealing in hydrogen atmosphere processing;
(5), get the tungsten helix after step (4) annealing in hydrogen atmosphere is processed, use again the chromic acid solution of 1.5 ~ 2mol/L to clean 0.5 ~ 5 minute, then after taking out, water rinses, and then uses the hydrochloric acid etching 1 ~ 5 minute of 3 ~ 3.5mol/L, and then puts into plating solution, carry out pulse copper plating treatment, then take out after washing, with ethanol dehydration, dry, annealing in hydrogen atmosphere is processed, and obtains the travelling-wave tubes tungsten helix of copper coating.
As preferred version, the copper electroplating method on above-described travelling-wave tubes tungsten helix surface, comprising of the pre-plating solution that step (2) is described: 10g/L cupric pyrophosphate, 2mL/L ammoniacal liquor, 250g/L potassium pyrophosphate, 50g/L nitrilotriacetic acid(NTA), 50g/L Sodium phosphate dibasic, 2g/L ammonium nitrate, solvent is water; The pH of pre-plating solution is 8-9, and the temperature of preplating is 25 ℃ to 35 ℃, and current density is 1A/dm
2.
As preferred version, the copper electroplating method on above-described travelling-wave tubes tungsten helix surface, the described plating solution of described step (3) and step (5) comprises: 60g/L cupric pyrophosphate, 2mL/L ammoniacal liquor, 400g/L potassium pyrophosphate, 45g/L nitrilotriacetic acid(NTA), 45g/L Sodium phosphate dibasic, 2g/L ammonium nitrate, solvent is water; The pH of electroplate liquid is 7-8, and the temperature of plating is 55 ℃, and current density is 0.7A/dm
2.
As preferred version, the copper electroplating method on above-described travelling-wave tubes tungsten helix surface, the temperature that the described annealing in hydrogen atmosphere of step (4) is processed is 1050 ± 20 ℃, soaking time is 3 ~ 5 minutes.
As preferred version, the copper electroplating method on above-described travelling-wave tubes tungsten helix surface, the temperature that the described annealing in hydrogen atmosphere of step (5) is processed is 1000 ± 20 ℃, soaking time 15 ~ 20 minutes.
As preferred version, the copper electroplating method on above-described travelling-wave tubes tungsten helix surface carries out electrolysis treatment between step (3) copper plating treatment and the processing of step (4) annealing in hydrogen atmosphere, and the current density of electrolysis treatment is 0.3A/dm
2, the time is 1 ~ 2 minute.
Beneficial effect: the copper electroplating method on travelling-wave tubes tungsten helix provided by the invention surface compared with prior art has the following advantages:
The copper electroplating method on travelling-wave tubes tungsten helix provided by the invention surface, by great many of experiments, screen preparation technology, especially add after ammonium nitrate, coating obviously improves in the bonding force on tungsten basal body surface, and process through the annealing in hydrogen atmosphere of selection process, the techniques such as secondary copper facing, whole technique is workable, and efficiency is high.Experimental result shows: copper electroplating method provided by the invention is can be on tungsten helix plated surface fine and close, evenly, is difficult for peeling, and the copper layer of foaming can improve the thermal conductivity of tungsten helix greatly, and during microwave transmission, high-frequency loss obviously reduces compared with prior art.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention, should understand these embodiment is only not used in and limits the scope of the invention for the present invention is described, after having read the present invention, those skilled in the art all fall within the application's claims limited range to the modification of the various equivalent form of values of the present invention.
Embodiment 1
The copper electroplating method on travelling-wave tubes tungsten helix surface, it comprises the following steps:
(1), get tungsten helix and in the chromic acid solution of 1.5mol/L, clean 0.5 minute, after then taking out, water rinses, and then uses the hydrochloric acid etching 1 minute of 3mol/L, then water rinses surface acid;
(2), get the pretreated tungsten helix of step (1) and put into pre-plating solution, carry out pre-copper plating treatment;
(3), get the tungsten helix that the pre-copper plating treatment of step (2) crosses and put into plating solution, carry out pulse copper plating treatment, then take out after washing, with ethanol dehydration, dry;
(4), get the tungsten helix that step (3) copper plating treatment crosses and carry out annealing in hydrogen atmosphere processing;
(5), get the tungsten helix after step (4) annealing in hydrogen atmosphere is processed, with the chromic acid solution of 1.5mol/L, clean 0.5 minute, after then taking out, water rinses again, and then uses the hydrochloric acid etching 1 minute of 3mol/L, then water rinses surface acid, and then put into plating solution, and carry out pulse copper plating treatment, then take out after washing, with ethanol dehydration, dry, annealing in hydrogen atmosphere is processed, and obtains the travelling-wave tubes tungsten helix of copper coating.
As preferred version, the copper electroplating method on above-described travelling-wave tubes tungsten helix surface, comprising of the pre-plating solution that step (2) is described: 10g/L cupric pyrophosphate, 2mL/L ammoniacal liquor, 250g/L potassium pyrophosphate, 50g/L nitrilotriacetic acid(NTA), 50g/L Sodium phosphate dibasic, 2g/L ammonium nitrate, solvent is water; The pH of pre-plating solution is 8-9, and the temperature of preplating is 25 ℃, and current density is 1A/dm
2.
As preferred version, the copper electroplating method on above-described travelling-wave tubes tungsten helix surface, the described plating solution of described step (3) and step (5) comprises: 60g/L cupric pyrophosphate, 2mL/L ammoniacal liquor, 400g/L potassium pyrophosphate, 45g/L nitrilotriacetic acid(NTA), 45g/L Sodium phosphate dibasic; 2g/L ammonium nitrate; The pH of pre-plating solution is 7-8, and the temperature of preplating is 55 ℃, and current density is 0.7A/dm
2.
As preferred version, the copper electroplating method on above-described travelling-wave tubes tungsten helix surface, the temperature that the described annealing in hydrogen atmosphere of step (4) is processed is 1020 ℃, soaking time is 5 minutes.
As preferred version, the copper electroplating method on above-described travelling-wave tubes tungsten helix surface, the temperature that the described annealing in hydrogen atmosphere of step (5) is processed is 1020 ℃, soaking time 20 minutes.
As preferred version, the copper electroplating method on above-described travelling-wave tubes tungsten helix surface carries out electrolysis treatment between step (3) copper plating treatment and the processing of step (4) annealing in hydrogen atmosphere, and the current density of electrolysis treatment is 0.3A/dm
2, the time is 1 minute.
Embodiment 2
The copper electroplating method on travelling-wave tubes tungsten helix surface, it comprises the following steps:
(1), get tungsten helix and in the chromic acid solution of 2mol/L, clean 3 minutes, after then taking out, water rinses, and then uses the hydrochloric acid etching 5 minutes of 3.5mol/L, then water rinses surface acid;
(2), get the pretreated tungsten helix of step (1) and put into pre-plating solution, carry out pre-copper plating treatment;
(3), get the tungsten helix that the pre-copper plating treatment of step (2) crosses and put into plating solution, carry out pulse copper plating treatment, then take out after washing, with ethanol dehydration, dry;
(4), get the tungsten helix that step (3) copper plating treatment crosses and carry out annealing in hydrogen atmosphere processing;
(5), get the tungsten helix after step (4) annealing in hydrogen atmosphere is processed, with the chromic acid solution of 2mol/L, clean 3 minutes, after then taking out, water rinses again, and then uses the hydrochloric acid etching 5 minutes of 3.5mol/L, then water rinses surface acid, and then put into plating solution, and carry out pulse copper plating treatment, then take out after washing, with ethanol dehydration, dry, annealing in hydrogen atmosphere is processed, and obtains the travelling-wave tubes tungsten helix of copper coating.
As preferred version, the copper electroplating method on above-described travelling-wave tubes tungsten helix surface, comprising of the pre-plating solution that step (2) is described: 10g/L cupric pyrophosphate, 2mL/L ammoniacal liquor, 250g/L potassium pyrophosphate, 50g/L nitrilotriacetic acid(NTA), 50g/L Sodium phosphate dibasic, 2g/L ammonium nitrate, solvent is water; The pH of pre-plating solution is 8-9, and the temperature of preplating is 25 ℃, and current density is 1A/dm
2.
As preferred version, the copper electroplating method on above-described travelling-wave tubes tungsten helix surface, the described plating solution of described step (3) and step (5) comprises: 60g/L cupric pyrophosphate, 2mL/L ammoniacal liquor, 400g/L potassium pyrophosphate, 45g/L nitrilotriacetic acid(NTA), 45g/L Sodium phosphate dibasic; 2g/L ammonium nitrate; The pH of pre-plating solution is 7-8, and the temperature of preplating is 55 ℃, and current density is 0.7A/dm
2.
As preferred version, the copper electroplating method on above-described travelling-wave tubes tungsten helix surface, the temperature that the described annealing in hydrogen atmosphere of step (4) is processed is 1050 ℃, soaking time is 3 minutes.
As preferred version, the copper electroplating method on above-described travelling-wave tubes tungsten helix surface, the temperature that the described annealing in hydrogen atmosphere of step (5) is processed is 1000 ℃, soaking time 15 minutes.
As preferred version, the copper electroplating method on above-described travelling-wave tubes tungsten helix surface carries out electrolysis treatment between step (3) copper plating treatment and the processing of step (4) annealing in hydrogen atmosphere, and the current density of electrolysis treatment is 0.3A/dm
2, the time is 1 minute.
Embodiment 3
1, get the copper facing tungsten helix that embodiment 1 and embodiment 2 prepare, according to tectum (deposition layer and electroless plating layer) the adhesion strength test method > > on GB/T 5270-200X < < metallic matrix, detect, the diameter of copper facing tungsten helix of the present invention is 0.4mm, by it on the axle of 3 times, result shows that coating does not occur peeling, comes off, excellent property.
2, get the copper facing tungsten helix that the embodiment of the present invention 1 and 2 prepares, be assembled in travelling-wave tubes, performance test results shows, compare with prior art copper facing tungsten helix, the travelling-wave tubes that adopts copper facing tungsten helix assembling of the present invention to obtain, during microwave transmission, high-frequency loss has reduced respectively 23% and 25%, has obtained good technique effect.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (6)
1. the copper electroplating method on travelling-wave tubes tungsten helix surface, is characterized in that, it comprises the following steps:
(1), get tungsten helix and in the chromic acid solution of 1.5 ~ 2mol/L, clean 0.5 ~ 5 minute, after then taking out, water rinses, and then uses the hydrochloric acid etching 1 ~ 5 minute of 3 ~ 3.5mol/L, then water rinses surface acid;
(2), get the pretreated tungsten helix of step (1) and put into pre-plating solution, carry out pre-copper plating treatment;
(3), get the tungsten helix that the pre-copper plating treatment of step (2) crosses and put into plating solution, carry out pulse copper plating treatment, then take out after washing, with ethanol dehydration, dry;
(4), get the tungsten helix that step (3) copper plating treatment crosses and carry out annealing in hydrogen atmosphere processing;
(5), get the tungsten helix after step (4) annealing in hydrogen atmosphere is processed, use the chromic acid solution of 1.5 ~ 2mol/L to clean 0.5 ~ 5 minute, after then taking out, water rinses, and then uses 3 ~ 3.5mol/L hydrochloric acid etching 1 ~ 5 minute again, then water rinses surface acid, and then put into plating solution, and carry out pulse copper plating treatment, then take out after washing, with ethanol dehydration, dry, annealing in hydrogen atmosphere is processed, and obtains the travelling-wave tubes tungsten helix of copper coating.
2. the copper electroplating method on travelling-wave tubes tungsten helix according to claim 1 surface, it is characterized in that, comprising of the pre-plating solution that step (2) is described: 10g/L cupric pyrophosphate, 2mL/L ammoniacal liquor, 250g/L potassium pyrophosphate, 50g/L nitrilotriacetic acid(NTA), 50g/L Sodium phosphate dibasic, 2g/L ammonium nitrate, solvent is water; The pH of pre-plating solution is 8-9, and the temperature of preplating is 25 ℃ to 35 ℃, and current density is 1A/dm
2.
3. the copper electroplating method on travelling-wave tubes tungsten helix according to claim 1 surface, it is characterized in that, the described plating solution of described step (3) and step (5) comprises: 60g/L cupric pyrophosphate, 2mL/L ammoniacal liquor, 400g/L potassium pyrophosphate, 45g/L nitrilotriacetic acid(NTA), 45g/L Sodium phosphate dibasic, 2g/L ammonium nitrate, solvent is water; The pH of plating solution is 7-8, and the temperature of plating is 55 ℃, and current density is 0.7A/dm
2.
4. the copper electroplating method on travelling-wave tubes tungsten helix according to claim 1 surface, is characterized in that, the temperature that the described annealing in hydrogen atmosphere of step (4) is processed is 1050 ± 20 ℃, and soaking time is 3 ~ 5 minutes.
5. the copper electroplating method on travelling-wave tubes tungsten helix according to claim 1 surface, is characterized in that, the temperature that the described annealing in hydrogen atmosphere of step (5) is processed is 1000 ± 20 ℃, soaking time 15 ~ 20 minutes.
6. the copper electroplating method on travelling-wave tubes tungsten helix according to claim 1 surface, is characterized in that, between step (3) copper plating treatment and the processing of step (4) annealing in hydrogen atmosphere, carries out electrolysis treatment, and the current density of electrolysis treatment is 0.3A/dm
2, the time is 1 ~ 2 minute.
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| CN201310650260.9A CN103668355B (en) | 2013-12-06 | 2013-12-06 | The copper electroplating method on a kind of travelling-wave tubes tungsten helix surface |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110791792A (en) * | 2019-11-11 | 2020-02-14 | 中国科学院电子学研究所 | Method for composite copper plating of inner wall of coupler corrugated pipe and coupler corrugated pipe |
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| CN110791792A (en) * | 2019-11-11 | 2020-02-14 | 中国科学院电子学研究所 | Method for composite copper plating of inner wall of coupler corrugated pipe and coupler corrugated pipe |
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