CN109536770B - Gold-beryllium alloy material for semiconductor device and preparation method thereof - Google Patents
Gold-beryllium alloy material for semiconductor device and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a gold beryllium alloy material for a semiconductor device and a preparation method thereof, wherein the method comprises the following steps: 1) taking gold and beryllium metals as raw materials, completely melting the gold on a vacuum induction melting furnace, adding the metal beryllium, and carrying out melting casting to obtain a gold-beryllium alloy ingot; wherein, the beryllium content in the alloy ingot is 0.5-2 wt.% of the nominal component of the alloy, and a certain proportion is added, and the balance is gold; 2) carrying out heat treatment on the alloy ingot obtained in the step 1 by using a heating furnace; 3) performing thermoplastic processing on the cast ingot along the thickness direction by using plastic processing equipment; 4) carrying out tempering heat treatment on the blank in a heating furnace every 1-2 times of processing; 5) repeating the steps 3) and 4) until the required thickness size of the plate is reached; 6) and (4) processing the alloy into the required gold-beryllium alloy material by adopting a stamping die. The gold-beryllium alloy material obtained by the method has uniform components, stable alloy and regular shape, and can meet the performance requirements of ohmic contact electrodes of semiconductor devices.
Description
Technical Field
The invention belongs to the technical field of evaporation film materials required by semiconductor devices in the microelectronic industry, and particularly relates to a gold-beryllium alloy material for the semiconductor devices and a preparation method thereof.
Background
The gold beryllium alloy material is used for preparing ohmic contact electrodes of semiconductor devices such as GaP, GaAs, GaN and the like. With the rapid development of the semiconductor industry in China in recent years, the demand for the gold-beryllium alloy is gradually increased, and meanwhile, the requirement for the quality of the product is higher and higher. Firstly, the alloy components of the product are uniform and stable, and the requirement on purity is high. Most of the existing gold beryllium material preparation methods in China firstly synthesize gold beryllium intermediate alloy with high beryllium content, and then smelt and synthesize the gold beryllium alloy again by taking the gold beryllium intermediate alloy and gold as raw materials. By adopting the secondary smelting method, impurities are easily introduced, so that the product purity is reduced; meanwhile, in the process of synthesizing the intermediate alloy, because the content of Be is high, and Be has special chemical properties, is easy to oxidize and has high toxicity, the requirement on the sealing property of equipment is extremely high, an operator is required to strictly do safety protection work, and otherwise, the operator can cause great damage to the human body. The invention provides a method for directly preparing gold-beryllium alloy, which can not only uniformly add beryllium into gold, but also has no toxicity and pollution.
On the other hand, the more regular the size of the gold beryllium alloy particles is, the closer the single weight of the gold beryllium alloy particles is, and the thickness of the evaporation coating can be more accurately controlled by strictly setting the single weight according to the requirements of a semiconductor device user on an evaporation process. The preparation method can realize any requirement of a user on single weight by adjusting the thickness, length, width (square) or diameter (circular) and other dimensions of the gold-beryllium alloy material
Disclosure of Invention
The invention aims to provide a gold-beryllium alloy material for a semiconductor device and a preparation method thereof.
In order to achieve the purpose, the invention provides the following technical scheme:
a gold beryllium alloy material for a semiconductor device comprises the following components: the beryllium content is 0.5 wt.% to 2 wt.%, and the balance is gold.
A preparation method of a gold beryllium alloy material for a semiconductor device comprises the following steps:
(1) taking gold and beryllium metals as raw materials, and then adding a certain proportion of metallic beryllium according to 0.5-2 wt.% of nominal component Be of the alloy, wherein the rest is gold; the purity of gold is not lower than 4N, and the purity of beryllium is not lower than 3N; after proportioning according to a certain proportion, rolling 5-10% of gold blocks by weight in each heat into 0.2-0.5 mm thin slices; wrapping the weighed metal beryllium by a gold sheet, and placing the metal beryllium into a feeding hopper above a vacuum induction melting furnace; putting the rest of gold materials into a graphite crucible;
(2) vacuumizing until the vacuum degree reaches × 10-1～×10-2After Pa, opening an inflation valve, and inflating high-purity argon into the furnace to 0.03-0.08 MPa;
(3) slowly feeding electricity, and carrying out induction heating to melt the gold in the crucible;
(4) after the gold is completely melted, opening the feeding hopper to add the gold sheet and the beryllium material wrapped by the gold sheet into the molten gold in the crucible;
(5) continuously heating for refining to melt the beryllium and fully mixing the beryllium with the gold;
(6) reducing the temperature after refining, and pouring when the temperature is 1100-1200 ℃ to obtain a gold-beryllium alloy ingot;
(7) carrying out heat treatment on the alloy ingot obtained in the step (6) by using a heating furnace; the heat treatment temperature is 400-550 ℃, and the time is 20-40 min;
(8) performing multi-pass hot rolling processing on the gold beryllium alloy cast ingot along the thickness direction by using plastic processing equipment to realize thickness reduction;
(9) carrying out tempering heat treatment on the blank in a heating furnace every 1-2 times of processing, wherein the tempering heat treatment temperature is 400-550 ℃, and the time is 3-10 min;
(10) repeating the steps (8) and (9) until the required thickness of the plate is reached;
(11) and (4) processing the plate obtained in the step (10) into regular particles by adopting a stamping die.
The preparation method of the gold beryllium alloy material for the semiconductor device is characterized in that 0.05-0.3 wt.% of metal beryllium is added according to the nominal composition of the alloy during the step (1).
The preparation method of the gold-beryllium alloy material for the semiconductor device is characterized in that the refining temperature is 1200-1300 ℃, and the refining time is 3-10 min.
The preparation method of the gold beryllium alloy material for the semiconductor device is characterized in that the deformation rate of the hot rolling pass in the step (8) is 2-8%, and the total deformation rate after the step (10) is finished is 25-75%.
The preparation method of the gold beryllium alloy material for the semiconductor device is characterized in that the sizes of the gold beryllium alloy material prepared by the method are as follows: the thickness is 0.5-3 mm, and the shape is square, round or special.
In another aspect, the invention provides a gold beryllium alloy material for a semiconductor device, which is prepared by the method.
The preparation method of the invention is to prepare the gold-beryllium alloy ingot by a vacuum induction melting secondary feeding method and then prepare the gold-beryllium alloy material by combining heat treatment and a hot rolling process. The beneficial effects are as follows:
1. in order to control the alloy components and prevent the beryllium content in the final gold-beryllium alloy from being low due to excessive volatilization of the metallic beryllium in an overheating smelting state, 0.05-0.3 wt.% of beryllium is added according to the nominal components of the alloy during the material mixing.
2. When in charging, the beryllium is wrapped by the gold sheet and placed in the charging hopper, and after the gold in the crucible is completely melted, the beryllium is charged for the second time and added into the crucible to be melted. Compared with the method of directly charging gold and beryllium into a crucible, the charging method can shorten the heating time of beryllium at high temperature, thereby effectively reducing volatilization and oxidation of beryllium. Because the metal beryllium is easy to combine with oxygen, the generated refractory oxide floats on the liquid level, and is easy to be involved in the cast ingot or left on the surface of the cast ingot during casting, thereby forming the defect of the cast ingot and influencing the quality of the cast ingot.
3. In the smelting process, in order to reduce the oxidation and volatilization of the metallic beryllium, the vacuum degree is firstly pumped to × 10-1～×10-2And after Pa, filling high-purity argon for atmosphere protection.
4. The ingot is processed by heat, so that the problem of large brittleness of the gold-beryllium alloy material is solved, and the processing performance of the material is improved. The temperature is controlled within the range of 400-550 ℃, and when the temperature is lower than 400 ℃, the cogging temperature of hot rolling cannot be reached enough, so that the blank is easy to crack along the rolling direction or the transverse direction during repeated rolling, and the control of the technological process is not facilitated.
5. The thickness of the plate can be controlled to reach any specific value through multi-pass hot rolling and stress relief annealing, so that the single weight of the final gold-beryllium alloy material is convenient to control, and the coating uniformity can be accurately controlled by a user of a semiconductor device.
Drawings
FIG. 1 is a flow chart of a method for preparing a gold-beryllium alloy material for a semiconductor device according to the invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1
The preparation method of the gold beryllium alloy material with nominal components of AuBe0.5 (the beryllium content is 0.5 percent, and the remainder is gold) comprises the following steps:
(1) gold and beryllium are used as raw materials, the purity of gold is not lower than 4N, and the purity of beryllium is not lower than 3N; proportioning according to 0.55 percent of Be, and making gold as the rest material. Wrapping beryllium with a gold sheet, and placing the gold sheet in a feeding hopper above a vacuum induction melting furnace; putting the rest of gold materials into a graphite crucible;
(2) vacuumizing to the vacuum degree of 5 × 10-2After Pa, opening an inflation valve, and inflating high-purity argon into the furnace to 0.05 MPa;
(3) slowly feeding electricity, and carrying out induction heating to melt the gold in the crucible;
(4) after the gold is completely melted, opening the feeding hopper to add the gold sheet and the beryllium material wrapped by the gold sheet into the molten gold in the crucible;
(5) continuously heating for refining at 1200-1300 ℃ for 5min to melt the beryllium and fully mix the beryllium with the gold;
(6) reducing the temperature after refining, and pouring when the temperature is 1100-1200 ℃ to obtain a gold-beryllium alloy ingot;
(7) carrying out heat treatment on the alloy ingot obtained in the step (6) by using a heating furnace; the heat treatment temperature is 420 ℃, and the time is 20 min;
(8) performing thermoplastic processing on the gold-beryllium alloy cast ingot by using plastic processing equipment, wherein the pass deformation is 10 percent, and the thickness reduction is realized;
(9) carrying out tempering heat treatment on the blank in a heating furnace at the temperature of 420 ℃ for 3min every time of finishing 1-2 times of processing;
(10) repeating the steps (8) and (9) until the thickness of the thin plate is 0.5 mm;
(11) and (4) processing the plate obtained in the step (10) into regular particles by adopting a stamping die.
Example 2
The preparation method of the gold beryllium alloy material with the components of AuBe0.7 (the beryllium content is 0.7 percent, and the rest is gold) comprises the following steps:
(1) gold and beryllium are used as raw materials, the purity of gold is not lower than 4N, and the purity of beryllium is not lower than 3N; proportioning according to 0.8 percent of Be, and making gold as the rest material. Wrapping beryllium with a gold sheet, and placing the gold sheet in a feeding hopper above a vacuum induction melting furnace; putting the rest of gold materials into a graphite crucible;
(2) vacuumizing, filling argon, smelting, refining and pouring according to the method of the embodiment 1 to obtain a gold-beryllium alloy ingot;
(3) carrying out heat treatment on the alloy ingot obtained in the step (2) by using a heating furnace, wherein the heat treatment temperature is 480 ℃ and the time is 35 min;
(4) performing thermoplastic processing on the gold-beryllium alloy cast ingot by using plastic processing equipment, wherein the pass deformation is 5 percent, and the thickness reduction is realized;
(5) carrying out tempering heat treatment on the blank in a heating furnace at 480 ℃ for 5min every 1-2 times of processing;
(6) repeating the steps (4) and (5) until the thickness of the thin plate is 0.5 mm;
(7) and (4) processing the plate obtained in the step (6) into regular particles by adopting a stamping die.
Example 3
The preparation method of the gold-beryllium alloy material with the components of AuBe1 (the beryllium content is 1 percent, and the rest is gold) comprises the following steps:
(1) gold and beryllium are used as raw materials, the purity of gold is not lower than 4N, and the purity of beryllium is not lower than 3N; proportioning according to 1.1 percent of Be, and making gold as the rest material. Wrapping beryllium with a gold sheet, and placing the gold sheet in a feeding hopper above a vacuum induction melting furnace; putting the rest of gold materials into a graphite crucible;
(2) vacuumizing, filling argon, smelting, refining and pouring according to the method of the embodiment 1 to obtain a gold-beryllium alloy ingot;
(3) carrying out heat treatment on the alloy ingot obtained in the step (2) by using a heating furnace, wherein the heat treatment temperature is 500 ℃, and the time is 30 min;
(4) performing thermoplastic processing on the gold-beryllium alloy cast ingot by using plastic processing equipment, wherein the pass deformation is 5 percent, and the thickness reduction is realized;
(5) carrying out tempering heat treatment on the blank in a heating furnace at the temperature of 500 ℃ for 5min every time of finishing 1-2 times of processing;
(6) repeating the steps (4) and (5) until the thickness of the thin plate is 1 mm;
(7) and (4) processing the plate obtained in the step (6) into regular particles by adopting a stamping die.
Example 4
The preparation method of the gold beryllium alloy material with the components of AuBe1.5 (the beryllium content is 1.5 percent, and the rest is gold) comprises the following steps:
(1) gold and beryllium are used as raw materials, the purity of gold is not lower than 4N, and the purity of beryllium is not lower than 3N; proportioning according to 1.7 percent of Be, and making gold as the rest material. Wrapping beryllium with a gold sheet, and placing the gold sheet in a feeding hopper above a vacuum induction melting furnace; putting the rest of gold materials into a graphite crucible;
(2) vacuumizing, filling argon, smelting, refining and pouring according to the method of the embodiment 1 to obtain a gold-beryllium alloy ingot;
(3) carrying out heat treatment on the alloy ingot obtained in the step (2) by using a heating furnace, wherein the heat treatment temperature is 530 ℃, and the time is 30 min;
(4) performing thermoplastic processing on the gold-beryllium alloy cast ingot by using plastic processing equipment, wherein the pass deformation is 5 percent, and the thickness reduction is realized;
(5) carrying out tempering heat treatment on the blank in a heating furnace at 530 ℃ for 8min every 1-2 times of processing;
(6) repeating the steps (4) and (5) until the thickness of the thin plate is 2 mm;
(7) and (4) processing the plate obtained in the step (6) into regular particles by adopting a stamping die.
Table 1 shows the composition and plastic working conditions of the gold-beryllium alloy material in the examples
The above embodiments describe the technical solutions of the present invention in detail. It will be clear that the invention is not limited to the described embodiments. Based on the embodiments of the present invention, those skilled in the art can make various changes, but any changes equivalent or similar to the present invention are within the protection scope of the present invention.
Claims (8)
1. A preparation method of a gold beryllium alloy material for a semiconductor device is characterized by comprising the following steps:
(1) taking gold and beryllium as raw material ingredients, adding 0.05-0.3 wt.% of metal beryllium according to 0.5-2 wt.% of nominal component Be of the alloy, and taking gold as the rest; the purity of gold is not lower than 4N, and the purity of beryllium is not lower than 3N; wrapping metal beryllium with a part of gold thin sheet, and putting the rest gold material into a graphite crucible;
(2) vacuumizing until the vacuum degree reaches × 10-1～×10-2After Pa, filling argon into the smelting furnace to 0.03-0.08 MPa;
(3) induction heating to melt the gold in the graphite crucible;
(4) after the gold is completely melted, adding the gold sheet and the metal beryllium wrapped by the gold sheet into the molten gold in the crucible;
(5) continuously heating for refining to melt the beryllium and fully mixing the beryllium with the gold;
(6) after refining, reducing the temperature, and pouring to obtain a gold-beryllium alloy ingot;
(7) carrying out heat treatment on the alloy ingot obtained in the step (6) by using a heating furnace; the heat treatment temperature is 400-550 ℃, and the time is 20-40 min;
(8) carrying out multi-pass hot rolling processing on the gold-beryllium alloy cast ingot to realize thickness reduction;
(9) carrying out tempering heat treatment on the blank in a heating furnace every 1-2 times of processing;
(10) repeating the steps (8) and (9) until the plate with the required thickness dimension is achieved;
(11) and (4) processing the plate obtained in the step (10) into a regular particle shape.
2. The method of claim 1, wherein the gold flakes in step (1) are prepared by rolling 5-10 wt% of gold per heat to 0.2-0.5 mm gold flakes.
3. The method according to claim 1, wherein the temperature of the refining in the step (5) is 1200 to 1300 ℃ and the refining time is 3 to 10 min.
4. The method of claim 1, wherein the casting is performed while the temperature is reduced to 1100 to 1200 ℃ in step (6).
5. The method of claim 1, wherein the hot rolling pass deformation in step (8) is between 2% and 8% and the total deformation after completion of step (10) is between 25% and 75%.
6. The method according to claim 1, wherein the tempering heat treatment in the step (9) is performed at a temperature of 400 to 550 ℃ for 3 to 10 min.
7. A gold-beryllium alloy material for semiconductor devices, prepared by the method of any one of claims 1 to 6, wherein the alloy material comprises the following components: the beryllium content is 0.5 wt.% to 2 wt.%, and the balance is gold.
8. The alloy material according to claim 7, wherein the alloy material has a thickness of 0.5 to 3mm and is square, circular or irregular in shape.
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| US4251621A (en) * | 1979-11-13 | 1981-02-17 | Bell Telephone Laboratories, Incorporated | Selective metal etching of two gold alloys on common surface for semiconductor contacts |
| CN102115833A (en) * | 2009-12-30 | 2011-07-06 | 北京有色金属与稀土应用研究所 | Gold beryllium alloy material for semiconductor devices and preparation method and application thereof |
| 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 |
| CN103122421A (en) * | 2011-11-21 | 2013-05-29 | 北京达博有色金属焊料有限责任公司 | Preparation method of high-performance gold bonding wire for package |
| CN105132873A (en) * | 2015-09-08 | 2015-12-09 | 有研亿金新材料有限公司 | Au-Sn alloy sputtering target material and preparation method thereof |
| CN106636722A (en) * | 2016-10-12 | 2017-05-10 | 洛阳鼎威材料科技有限公司 | Alloy material and preparation method thereof |
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| US4251621A (en) * | 1979-11-13 | 1981-02-17 | Bell Telephone Laboratories, Incorporated | Selective metal etching of two gold alloys on common surface for semiconductor contacts |
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| 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 |
| CN103122421A (en) * | 2011-11-21 | 2013-05-29 | 北京达博有色金属焊料有限责任公司 | Preparation method of high-performance gold bonding wire for package |
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