CN114686719A - High-strength gold wire material and preparation method thereof - Google Patents
High-strength gold wire material and preparation method thereof Download PDFInfo
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- CN114686719A CN114686719A CN202210311658.9A CN202210311658A CN114686719A CN 114686719 A CN114686719 A CN 114686719A CN 202210311658 A CN202210311658 A CN 202210311658A CN 114686719 A CN114686719 A CN 114686719A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C5/02—Alloys based on gold
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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Abstract
The invention relates to a high-strength gold wire material and a preparation method thereof, wherein the material comprises the following components in percentage by weight: the strengthening elements are less than 0.5 percent, and the balance is gold, wherein the strengthening elements are at least three of zirconium, scandium, beryllium, nickel, aluminum and copper. The high-strength gold wire material has the advantages of high reliability, high strength, good plasticity, few defects, good processability and the like, and can be applied to the field of electronic packaging.
Description
Technical Field
The invention belongs to the field of metal preparation, and particularly relates to a high-strength gold wire material and a preparation method thereof.
Background
In the microelectronics industry, gold wire is mainly used as an electrical connection lead, and the reliability of the gold wire is one of the determining factors of the service life of the device, which is used for connecting the inner chip bonding area with the external lead frame in the primary electronic package of various semiconductor components, integrated circuits or large-scale integrated circuits and the like.
Gold is one of the most stable metals, it does not oxidize and adsorb gases, has good ductility, but ordinary gold wire cannot meet the performance requirements of modern bonding processes because of its softer texture. The alloying of the trace elements to the gold wire is one of the effective ways to improve the mechanical and bonding properties of the gold wire, but the influence of the trace alloy elements on the properties of the gold wire is beneficial and has disadvantages. For example: trace beryllium can strengthen the gold wire and improve the strength, but beryllium exceeding 0.05% can embrittle the gold wire and make the drawing process of the filament difficult. Therefore, the correct selection of the trace elements and the control of the appropriate addition amount are one of the keys for realizing the optimized combination of the mechanical properties of the gold bonding wire.
The preparation of the high-strength gold wire comprises the steps of adding multiple trace elements of zirconium, scandium, beryllium, nickel, aluminum and copper into pure gold, preparing a gold alloy rod by adopting a vacuum melting technology, and then removing internal stress of the gold wire, separating out a dispersed phase, and adjusting strength and elongation percentage through drawing deformation and continuous annealing. Compared with the prior art, the invention has the advantages of excellent strength, good plasticity and reliability, superior performance to common gold wires, and suitability for miniaturization, integration and modular development of electronic components.
Disclosure of Invention
The invention aims to provide a high-strength gold wire material and a preparation method thereof, wherein the material has the characteristics of high reliability, high strength, good plasticity, few defects and good processability.
The technical scheme of the invention is as follows:
a high-strength gold wire material comprises the following components in percentage by weight: the strengthening element is less than 0.5 percent, and the rest is gold.
The strengthening elements are selected from zirconium, scandium, beryllium, nickel, aluminum and copper.
The preparation method of the material comprises the following steps:
1) taking the raw materials according to the proportion, carrying out vacuum melting under the protection of argon, and fully stirring after the raw materials are completely melted;
2) leading the ingot into a gold alloy rod through a crystallizer;
3) and homogenizing the gold alloy rod for 1-5 h, performing cold machining deformation, and finally performing an annealing process to obtain the high-strength gold wire.
The vacuum degree in the step 1) is less than 10-2And Pa, introducing argon gas, and keeping the pressure at 1-10 Pa.
Step-type smelting current is adopted in the vacuum smelting in the step 1), and the interval time of current regulation is 1-2 min each time until the raw materials are completely melted.
And step 1), electromagnetically stirring the metal solution for 1-2 min.
In the step 3), a vacuum annealing furnace or an annealing furnace with protective atmosphere is adopted, and the vacuum degree is less than 10-1Pa, argon or nitrogen is adopted as inert protective gas, and the homogenization treatment temperature is 500-800 ℃.
And 3) performing cold working deformation by drawing deformation.
And 3) carrying out the annealing process, namely carrying out continuous annealing treatment in a continuous annealing furnace at the temperature of 200-500 ℃ to obtain the high-strength gold wire.
According to the method, a small amount of trace alloying elements are added into the gold, namely the mass percentage of the gold is not less than 99.5%, so that the strength and the processing performance of the gold wire material can be greatly improved. The vacuum melting technology is adopted in the melting process, the traditional induction melting mode is abandoned, low-melting-point impurity elements in the alloy can be removed, the solidification shrinkage cavity in the cast ingot is greatly reduced, and the oxidation volatilization of the elements is also reduced.
The method disclosed by the invention is based on a vacuum technology, and combines the modes of solid solution strengthening, fine grain strengthening and the like, so that the grain structure, the strength and the fine processing capacity of the gold wire material are greatly improved, and the mechanical property of the gold wire material is improved.
Light metal Be and hardware fittingThe alloy has larger atomic ratio and atomic size difference, trace beryllium can generate solid solution strengthening effect on gold, and excessive beryllium can cause gold embrittlement; the rare earth element scandium has solid solution strengthening effect and aging strengthening effect on the gold tool; the solid solubility of zirconium in gold changes with the temperature, and second-phase strengthening particles Au are formed with the temperature reduction5Solute atoms of the Zr and the gold wire prevent dislocation slippage in the stretching deformation process to generate a Coriolis gas cluster effect, so that the tensile strength is greatly improved; at high temperature, the solubility of nickel, aluminum and copper in gold is high, and the solution strengthening effect on gold is strong.
The invention has the beneficial effects that:
1) the ingot casting structure of the vacuum continuous casting smelting is fine and uniform, has few defects, and is the basis for ensuring the micronization processing;
2) the smelting process adopts stepped smelting, so that the smelting temperature is accurately controlled, and alloy elements are uniformly distributed;
3) partial alloying elements are dissolved in the gold matrix in a solid solution mode to form solid solution strengthening;
4) the addition of rare earth elements forms high-melting-point nucleation particles during solidification to promote nucleation and generate a dispersed precipitated phase, so that the grain refinement is facilitated, and the dispersed particles are pinned in a grain boundary to prevent the grains from growing;
drawings
Fig. 1 is a graph of room temperature tensile force-displacement curve of high strength gold wire in example 5 of the present invention, wherein lines 1-5 represent tensile force-displacement curves of 5 test samples (to ensure reliability of test data).
Detailed Description
Example 1
1) Ingredients
The content of the gold raw material is 99.99 percent, and the content of the gold raw material in the embodiment is 1000 grams.
2) Smelting of high-strength gold wire material
Putting gold raw material into a vacuum melting furnace, sealing the furnace door, vacuumizing to 1.3 multiplied by 10-3Pa, introducing argon gas for protection, and keeping the pressure at 3 Pa; starting the vacuum melting equipment, and gradually adjusting the melting current as follows: 0A → 3A → 6A → 9A → 12A → 15A → 18A → 21A, adjusting the current interval time to 2min, straightAfter the materials are completely melted, starting electromagnetic stirring for 2min, and then carrying out ingot guiding to form a ingot with a diameter of
The gold rod of (1).
3. Processing of high-strength gold wire material
Has a diameter of
Homogenizing the gold rod for 2h, performing cold drawing deformation to 0.02mm, and performing continuous annealing treatment at 200 ℃ to obtain the high-strength gold wire material.
Example 2
1) Ingredients
Taking the following components (raw materials) according to the weight percentage of the components: 0.01 percent of scandium, 0.1 percent of nickel, 0.2 percent of aluminum and the balance of gold.
2) Smelting of high-strength gold wire material
Placing the prepared raw materials into a vacuum melting furnace, sealing the furnace door, and vacuumizing to 5.1 × 10-3Pa, introducing argon gas for protection, and keeping the pressure at 3 Pa; starting the vacuum melting equipment, and gradually adjusting the melting current as follows: 0A → 3A → 6A → 9A → 12A → 15A → 18A → 21A, adjusting the current interval time to 2min, starting electromagnetic stirring for 2min after complete melting, and making the dummy ingot with diameter
The gold rod of (1).
3. Processing of high-strength gold wire material
Diameter of
Homogenizing the gold rod for 2h, performing cold drawing deformation to 0.02mm, and performing continuous annealing treatment at 200 ℃ to obtain the high-strength gold wire material.
Example 3
1) Ingredients
Taking the following components (raw materials) according to the weight percentage of the components: zirconium 0.05%, nickel 0.1%, copper 0.2%, and the balance gold.
2) Smelting of high-strength gold wire material
Placing the prepared raw materials into a vacuum melting furnace, sealing the furnace door, and vacuumizing to 1.1 × 10-3Pa, introducing argon for protection, and keeping the pressure at 5 Pa; starting the vacuum melting equipment, and gradually adjusting the melting current as follows: 0A → 3A → 6A → 9A → 12A → 15A → 18A → 21A, adjusting the current interval time to 2min, starting electromagnetic stirring for 2min after complete melting, and making the dummy ingot with diameter
The gold rod of (1).
3. Processing of high-strength gold wire material
Diameter of
Homogenizing the gold rod for 2h, performing cold drawing deformation to 0.02mm, and performing continuous annealing treatment at 250 ℃ to obtain the high-strength gold wire material.
Example 4
1) Ingredients
Taking the following components (raw materials) according to the weight percentage: 0.04% of scandium, 0.001% of beryllium, 0.1% of nickel, 0.2% of copper and the balance of gold.
2) Smelting of high-strength gold wire material
Placing the prepared raw materials into a vacuum melting furnace, sealing the furnace door, and vacuumizing to 3 × 10-3Pa, introducing argon gas for protection, and keeping the pressure at 7 Pa; starting the vacuum melting equipment, and gradually adjusting the melting current as follows: 0A → 3A → 6A → 9A → 12A → 15A → 18A → 21A, adjusting the current interval time to 2min, starting electromagnetic stirring for 2min after complete melting, and making the dummy ingot with diameter
The gold rod of (1).
3. Processing of high-strength gold wire material
Diameter of
Homogenizing the gold rod for 2h, performing cold drawing deformation to 0.02mm, and performing continuous annealing treatment at 300 ℃ to obtain the high-strength gold wire material.
Example 5
1) Ingredients
Taking the following components (raw materials) according to the weight percentage of the components: zirconium 0.01%, scandium 0.05%, nickel 0.1%, copper 0.2%, and the balance gold.
2) Smelting of high-strength gold wire material
Placing the prepared raw materials into a vacuum melting furnace, sealing the furnace door, and vacuumizing to 7 x 10-3Pa, introducing argon gas for protection, and keeping the pressure at 2 Pa; starting the vacuum melting equipment, and gradually adjusting the melting current as follows: 0A → 3A → 6A → 9A → 12A → 15A → 18A → 21A, adjust the current interval time to 2min, after complete melting, start the electromagnetic stirring for 2min, and then proceed the dummy ingot to diameter
The gold rod of (1).
3. Processing of high-strength gold wire material
Diameter of
Homogenizing the gold rod for 3h, performing cold drawing deformation to 0.02mm, and performing continuous annealing treatment at 300 ℃ to obtain the high-strength gold wire material.
Example 6
1) Ingredients
Taking the following components (raw materials) according to the weight percentage of the components: 0.1% of zirconium, 0.05% of scandium, 0.001% of beryllium, 0.1% of aluminum, 0.1% of copper and the balance of gold.
2) Smelting of high-strength gold wire material
Placing the prepared raw materials into a vacuum melting furnace, sealing the furnace door, and vacuumizing to 8 x 10-3Pa, introducing argon for protection, and keeping the pressure at 5 Pa; starting the vacuum melting equipment, and gradually adjusting the melting current as follows: 0A → 3A → 6A → 9A → 12A → 15A → 18A → 21A, adjusting the current interval time to 2min, starting electromagnetic stirring for 2min after complete meltingThen, the dummy ingot is formed into a diameter of
The gold rod of (1).
3. Processing of high-strength gold wire material
Diameter of
Homogenizing the gold rod for 3.5h, performing cold drawing deformation to 0.02mm, and performing continuous annealing treatment at 350 ℃ to obtain the high-strength gold wire material.
Example 7
1) Ingredients
Taking the following components (raw materials) according to the weight percentage of the components: 0.05% of zirconium, 0.05% of scandium, 0.001% of beryllium, 0.1% of nickel, 0.1% of aluminum, 0.1% of copper and the balance of gold.
2) Smelting of high-strength gold wire material
Placing the prepared raw materials into a vacuum melting furnace, sealing the furnace door, and vacuumizing to 3 × 10-3Pa, introducing argon gas for protection, and keeping the pressure at 7 Pa; starting the vacuum melting equipment, and gradually adjusting the melting current as follows: 0A → 3A → 6A → 9A → 12A → 15A → 18A → 21A, adjusting the current interval time to 2min, starting electromagnetic stirring for 2min after complete melting, and making the dummy ingot with diameter
The gold rod of (1).
3. Processing of high-strength gold wire material
Diameter of
Homogenizing the gold bar for 4h, performing cold drawing deformation to 0.02mm, and performing continuous annealing treatment at 350 ℃ to obtain the high-strength gold wire material.
The gold wire materials described in examples 1 to 7 were used for performance tests: 1) and (3) testing tensile mechanical properties: hard gold wire diameter of
The stretching speed is 2 mm/min; 2) the temperature cycle number test conditions are as follows: diameter of gold wire
The high temperature is 125 ℃, the low temperature is-55 ℃, the heating rate is 5 ℃/min, the exposure time is 10min, the test times are 500, each group tests 25, and the wire breakage condition after the test is judged. The experimental results are shown in table 1:
TABLE 1 series of gold wire Properties
In the process of preparing the high-strength gold wire material, strengthening modes such as solid solution strengthening, fine grain strengthening, dispersion strengthening and the like are adopted, so that the strength and the temperature cycle performance of the gold wire are improved, and the high-strength gold wire material can be applied to the fields of integrated circuits and semiconductor elements.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and those skilled in the art can make modifications without departing from the spirit of the present invention. The scope of the invention is to be determined by the claims.
Claims (9)
1. A high-strength gold wire material is characterized in that: the material comprises the following components in percentage by weight: the strengthening element is less than 0.5 percent, and the rest is gold.
2. The material of claim 1, wherein: the strengthening elements are at least three of zirconium, scandium, beryllium, nickel, aluminum and copper.
3. A method for the preparation of a material according to any of claims 1-2, characterized by the steps of:
1) taking raw materials according to the mixture ratio of any one of claims 1-2, carrying out stepped vacuum melting under the protection of argon, and fully stirring after the raw materials are completely melted;
2) leading the ingot into a gold alloy rod through a crystallizer;
3) and homogenizing the gold alloy rod for 1-5 h, and performing cold machining deformation to obtain the high-strength gold wire.
4. The method of claim 3, wherein: the vacuum degree in the step 1) is less than 10-2And Pa, introducing argon gas, and keeping the pressure at 1-10 Pa.
5. The method of claim 3, wherein: step 1) current of step-type vacuum melting is adjusted, the current interval time is 1-2 min each time, and the raw materials are completely melted.
6. The method of claim 3, wherein: and step 1), electromagnetically stirring the metal solution for 1-2 min.
7. The method of claim 3, wherein: homogenizing in step 3): vacuum annealing is adopted, and the vacuum degree is less than 10-1Pa, adopting argon or nitrogen as inert protective gas, and treating at 500-800 ℃.
8. The method of claim 3, wherein: and 3) performing cold working deformation by drawing deformation.
9. The method of claim 8, wherein: and 8) continuously annealing the high-strength gold wire subjected to the drawing deformation at 200-500 ℃ to obtain the high-strength gold wire.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114921678A (en) * | 2022-05-06 | 2022-08-19 | 紫金矿业集团黄金珠宝有限公司 | Ultrahigh-strength gold material, and preparation method and equipment thereof |
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| CN111254311A (en) * | 2020-03-27 | 2020-06-09 | 上杭县紫金佳博电子新材料科技有限公司 | 4N gold bonding wire capable of being processed into 6-micron diameter by drawing and preparation method thereof |
| CN111763844A (en) * | 2020-05-20 | 2020-10-13 | 上杭县紫金佳博电子新材料科技有限公司 | Bonding gold belt and preparation method thereof |
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| CN101689519A (en) * | 2007-12-03 | 2010-03-31 | 新日铁高新材料株式会社 | Bonding wire for semiconductor devices |
| CN102451893A (en) * | 2010-10-26 | 2012-05-16 | 苏州金江铜业有限公司 | Manufacturing method for alloy wire rod |
| CN102127663A (en) * | 2010-12-30 | 2011-07-20 | 宁波康强电子股份有限公司 | Gold bonding wire and preparation method thereof |
| US20140376352A1 (en) * | 2013-06-24 | 2014-12-25 | Seagate Technology Llc | Materials for near field transducers, near field tranducers containing same, and methods of forming |
| CN109003903A (en) * | 2018-07-02 | 2018-12-14 | 上杭县紫金佳博电子新材料科技有限公司 | A kind of bonding gold wire and preparation method thereof |
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| CN111763844A (en) * | 2020-05-20 | 2020-10-13 | 上杭县紫金佳博电子新材料科技有限公司 | Bonding gold belt and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114921678A (en) * | 2022-05-06 | 2022-08-19 | 紫金矿业集团黄金珠宝有限公司 | Ultrahigh-strength gold material, and preparation method and equipment thereof |
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