CN102168294B - Method for improving tungsten-base gold-plating bond strength - Google Patents
Method for improving tungsten-base gold-plating bond strength Download PDFInfo
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- CN102168294B CN102168294B CN2011101310872A CN201110131087A CN102168294B CN 102168294 B CN102168294 B CN 102168294B CN 2011101310872 A CN2011101310872 A CN 2011101310872A CN 201110131087 A CN201110131087 A CN 201110131087A CN 102168294 B CN102168294 B CN 102168294B
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Abstract
The invention relates to a method for improving the gold-plating bond strength of a tungsten metal surface, and belongs to the field of the surface modification of metal materials. In the method, the problems of dropping and delamination of plated gold on surfaces of tungsten materials are solved. The method comprises the following steps of: removing oxides on the surface of a tungsten spiral line before electroplating; electroplating copper at the temperature of between 20 and 60 DEG C and under a condition that the pH value is between 0.6 and 1.2 and a condition that the current density is between 0.1 and 0.3 A/dm<2> for 15 to 120 seconds, wherein copper layer electroplate liquid comprises 170 to 210 g/L of anhydrous cupric sulfate, 35 to 60 g/L of sulfuric acid and the balance of water, and the pH value is regulated by the sulfuric acid and sodium hydroxide; and electroplating the gold at the temperature of between 20 and 35 DEG C under a condition that the pH value is between 8 and 11 and a condition that the current density is between 0.4 and 0.6 A/dm<2> for 150 to 300 seconds, wherein gold-plating liquid comprises 5 to 8 g/L of gold sodium sulfite, 30 to 40 g/L of anhydrous sodium sulfite and the balance of water, and the pH value is regulated by the sulfuric acid and the sodium hydroxide. In the method, gold-plating samples are subjected to heat treatment in a hydrogen furnace at the temperature of between 950 and 1,000 DEG C for 30 minutes, and gold-plating layers are not dropped.
Description
Technical field
The invention belongs to the metal surface properties modification technical field, a kind of method that strengthens the gold-plated bonding strength in tungsten metallic surface is provided, gold-platedly come off to solve the tungsten material surface, the problem of peeling.
Background technology
Characteristics such as TWT spiral-line material requires to possess HMP, high conduction, high heat conduction, high firmness, main at present tungsten or the molybdenum of adopting.But because the resistivity of tungsten, molybdenum is higher, high-frequency loss is big, causes working temperature to raise, and has a strong impact on the stability and the safety of TWT.For reducing the high-frequency loss on spiral-line surface, generally adopt the spiral-line coating surface to have the method for high heat conduction, low-resistivity thin-film material, such as copper facing or gold-plated, but still existing problems.The high temperature evaporation phenomenon often takes place in copper facing, pollutes adjacent components; And directly gold-plated on the tungsten helix surface, Gold plated Layer voluntarily peeling, come off, influence the work-ing life and the safety of TWT.
Summary of the invention
In order to solve the bonding force problem on Gold plated Layer and spiral-line surface; The present invention starts with from electroplating technology; A kind of method that strengthens the gold-plated bonding force intensity in tungsten metallic surface is provided; Obtained in this way and the firm Gold plated Layer of tungsten helix surface bonding, and 950 ℃～1000 ℃ gold-plated sample carried out thermal treatment in 30 minutes in the hydrogen stove after, find that Gold plated Layer does not come off, skin effect phenomenon.
In order to realize the foregoing invention purpose, the present invention has adopted following process step:
(1) pre-treatment
Before the plating, place the hydrogen stove to carry out thermal treatment in 30 minutes tungsten helix, to remove the tungsten helix oxide on surface at 950 ℃;
(2) electro-coppering
The composition of transition copper layer electroplate liquid: cupric sulfate pentahydrate 170～210g/L, sulfuric acid 35～60g/L, all the other are water;
Processing parameter: pH value 0.6～1.2, current density 0.1～0.3A/dm
2, 20～60 ℃ of temperature, electroplating time 15s～120s, the pH value is regulated with sulfuric acid and sodium hydroxide;
(3) electrogilding
After obtaining copper electroplating layer, adopt gold plating liquid to carry out gold-plated;
The composition of gold plating liquid: gold sodium sulfide: 5～8g/L, sodium sulphite anhydrous 99.3: 30～40g/L, all the other are water;
Processing parameter: pH value 8～11, current density 0.4～0.6A/dm
2, 25～35 ℃ of temperature, electroplating time 150s～300s, the pH value is regulated when the electro-coppering time with sulfuric acid and sodium hydroxide and is less than 15s or during greater than 120s, the copper layer that is obtained is too thin or blocked up, and follow-up Gold plated Layer combination is poor.Gold-plated again after electro-coppering between 15～120s, the Gold plated Layer and the matrix bond that are obtained are firm.
The invention has the advantages that adopting copper plating process to obtain thickness earlier is the transition layer of 0.05～1 μ m, gold-plated again on transition layer.Adopt this method can obtain the Gold plated Layer firm with matrix bond.Method is simple, and processing parameter is regulated and control easily.
Description of drawings
Instance 1 electroplating effect figure.
Embodiment
Instance 1: press the composition preparation of electroplate liquid in the table 1, the adjusting electroplating time is 15s, then according to above-mentioned process step electro-coppering transition layer.
Table 1 practical implementation condition
Electroplating effect and Fig. 1 of instance 2 and instance 3 are similar.
Instance 2: press the composition preparation of electroplate liquid in the table 2, the adjusting electroplating time is 40s, then according to above-mentioned process step electro-coppering transition layer.
Table 2 practical implementation condition
Instance 3: press the composition preparation of electroplate liquid in the table 3, the adjusting electroplating time is 120s, presses then
According to above-mentioned process step electro-coppering transition layer.
Table 3 practical implementation condition
Claims (1)
1. method that improves the gold-plated bonding force intensity in tungsten metallic surface is characterized in that step is following:
(1) pre-treatment
Before the plating, place the hydrogen stove to carry out thermal treatment in 30 minutes tungsten helix, to remove the tungsten helix oxide on surface at 950 ℃;
(2) electro-coppering
The composition of transition copper layer electroplate liquid: cupric sulfate pentahydrate 170～210g/L, sulfuric acid 35～60g/L, all the other are water;
Processing parameter: pH value 0.6～1.2, current density 0.1～0.3A/dm
2, 20～60 ℃ of temperature, electroplating time 15s～120s, the pH value is regulated with sulfuric acid and sodium hydroxide;
(3) electrogilding
After obtaining copper electroplating layer, adopt gold plating liquid to carry out gold-plated;
The composition of gold plating liquid: gold sodium sulfide: 5～8g/L, sodium sulphite anhydrous 99.3: 30～40g/L, all the other are water;
Processing parameter: pH value 8～11, current density 0.4～0.6A/dm
2, 25～35 ℃ of temperature, electroplating time 150s～300s, the pH value is regulated with sulfuric acid and sodium hydroxide;
Gold-plated back is carried out thermal treatment in 30 minutes at 950 ℃～1000 ℃ to gold-plated sample in the hydrogen stove.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101310872A CN102168294B (en) | 2011-05-19 | 2011-05-19 | Method for improving tungsten-base gold-plating bond strength |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101310872A CN102168294B (en) | 2011-05-19 | 2011-05-19 | Method for improving tungsten-base gold-plating bond strength |
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| Publication Number | Publication Date |
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| CN102168294A CN102168294A (en) | 2011-08-31 |
| CN102168294B true CN102168294B (en) | 2012-07-04 |
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| CN2011101310872A Expired - Fee Related CN102168294B (en) | 2011-05-19 | 2011-05-19 | Method for improving tungsten-base gold-plating bond strength |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102758232A (en) * | 2012-07-02 | 2012-10-31 | 北京工业大学 | Method for improving gold-plating bonding strength on surface of molybdenum-based electrical contact |
| CN102925943A (en) * | 2012-10-18 | 2013-02-13 | 北京工业大学 | Method for preparing high-strength, high-electrical conductivity and high-thermal conductivity metallic composite material for high-frequency structural member of traveling wave tube |
| CN105401180A (en) * | 2015-12-23 | 2016-03-16 | 苏州市金星工艺镀饰有限公司 | Electroplating liquid of wear-resistant gold-plated film and electroplating method thereof |
| CN105803499A (en) * | 2016-04-10 | 2016-07-27 | 北京工业大学 | Low-resistivity composite rod of output window needle for millimeter-wave traveling wave pipe |
| CN107385481A (en) * | 2017-07-26 | 2017-11-24 | 苏州鑫旷新材料科技有限公司 | A kind of cyanide-free gold electroplating liquid |
| CN109903877B (en) * | 2019-03-26 | 2020-09-18 | 王飞 | Manufacturing method of X-ray diffraction optical focusing element |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87211969U (en) * | 1987-08-22 | 1988-07-20 | 北京高熔金属材料厂 | Continuous electroplating device for gold-plating tungsten filament |
| CN101383253A (en) * | 2007-09-05 | 2009-03-11 | 中国科学院电子学研究所 | Preparation for slow wave component of spiral line travelling-wave tube |
| CN101694825A (en) * | 2009-10-14 | 2010-04-14 | 安徽华东光电技术研究所 | Method for processing tungsten helical line of millimeter wave traveling-wave tube |
| CN101899692A (en) * | 2010-07-30 | 2010-12-01 | 安徽华东光电技术研究所 | Electroless copper plating method for helical line for travelling wave tube |
-
2011
- 2011-05-19 CN CN2011101310872A patent/CN102168294B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87211969U (en) * | 1987-08-22 | 1988-07-20 | 北京高熔金属材料厂 | Continuous electroplating device for gold-plating tungsten filament |
| CN101383253A (en) * | 2007-09-05 | 2009-03-11 | 中国科学院电子学研究所 | Preparation for slow wave component of spiral line travelling-wave tube |
| CN101694825A (en) * | 2009-10-14 | 2010-04-14 | 安徽华东光电技术研究所 | Method for processing tungsten helical line of millimeter wave traveling-wave tube |
| CN101899692A (en) * | 2010-07-30 | 2010-12-01 | 安徽华东光电技术研究所 | Electroless copper plating method for helical line for travelling wave tube |
Non-Patent Citations (2)
| Title |
|---|
| 费娜等.螺旋线型毫米行波管的散热问题.《真空电子技术》.2010,第71-73页. * |
| 韩勇等.螺旋线镀膜对慢波组件散热性能影响的研究.《电子与信息学报》.2008,第30卷(第8期),第2029-2032页. * |
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