CN109536770A - A kind of semiconductor device gold beryllium alloy material and preparation method - Google Patents
A kind of semiconductor device gold beryllium alloy material and preparation method Download PDFInfo
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- CN109536770A CN109536770A CN201811471664.0A CN201811471664A CN109536770A CN 109536770 A CN109536770 A CN 109536770A CN 201811471664 A CN201811471664 A CN 201811471664A CN 109536770 A CN109536770 A CN 109536770A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/02—Alloys based on gold
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
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Abstract
The invention discloses a kind of semiconductor device gold beryllium alloy material and preparation methods, this method comprises the following steps: 1) using gold, beryllium metal as raw material, on vacuum induction melting furnace, after being first completely melt gold, metallic beryllium is added again, and melting and casting obtains golden beryllium alloy ingot casting；Wherein, beryllium content is 0.5~2wt.% of alloy nominal composition polygamy certain proportion again in alloy cast ingot, and surplus is gold；2) it is heat-treated using the alloy cast ingot that heating furnace obtains step 1；3) ingot casting through-thickness is thermoformed using plastic processing equipment；4) blank is carried out tempering heat treatment in heating furnace by the processing of 1~2 passage of every completion；5) step 3) and 4) is repeated, until required plate thickness size；6) stamping die is used, golden beryllium alloy material needed for being processed into.The golden beryllium alloy material composition obtained by this method is uniform, and alloy is stablized, and regular shape can meet the performance requirement of semiconductor device ohmic contact electrode.
Description
Technical field
The invention belongs to membrane material technical field is evaporated needed for semiconductor devices in microelectronics industry, and in particular to one kind is partly led
Body device golden beryllium alloy material and preparation method thereof.
Background technique
Golden beryllium alloy material is used for the Ohm contact electrode preparation of the semiconductor devices such as GaP, GaAs and GaN.With me
The rapid development of state's semicon industry in recent years, the demand to golden beryllium alloy increasingly increase, and simultaneously, want to the quality of product
Ask higher and higher.Be first product alloying component uniformly, stablize, and it is higher for purity requirement.Domestic existing golden beryllium
Material preparation method is first to synthesize the higher golden beryllium intermediate alloy of beryllium content mostly, then again with golden beryllium intermediate alloy and Jin Weiyuan
Melting synthesizes golden beryllium alloy to material again.Using the method for this secondary smelting, impurity introducing is tended to have, so that it is pure to reduce product
Degree；Meanwhile during synthesizing intermediate alloy, since the content of Be is higher, and the chemical property of Be is special, oxidizable and have
Biggish toxicity, thus it is high to the sealing requirements of equipment, it is also desirable to and operator strictly carries out security protection work, otherwise can be right
The person causes greatly to injure.The present invention provides a kind of method for directly preparing golden beryllium alloy, can not only be homogeneously added into beryllium
Into gold, and it is nontoxic, pollution-free.
On the other hand, the size of golden beryllium alloy particle is more regular, and single weight is more close, semiconductor devices user's root
According to the demand to evaporation process, the thickness of vapor plating more can be accurately controlled by strictly setting single weight.This hair
Bright preparation method, by adjusting the thickness of golden beryllium alloy material, length and width (rectangular) or diameter (circle) equidimension, it can be achieved that with
Any requirement of the family to single weight
Summary of the invention
The object of the present invention is to provide a kind of semiconductor device gold beryllium alloy materials and preparation method thereof.
To achieve the above object, the invention provides the following technical scheme:
A kind of semiconductor device gold beryllium alloy material, ingredient are as follows: beryllium content 0.5wt.%~2wt.%, remaining is
Gold.
A kind of semiconductor device gold beryllium alloy material, preparation method, this method comprises the following steps:
(1) using gold, beryllium metal as raw material, according to 0.5~2wt.% of alloy nominal composition Be a certain proportion of gold of polygamy again
Belong to beryllium, clout is gold；The purity of gold is not less than 4N, and the purity of beryllium is not less than 3N；It, will be in every heat according to a certain percentage after ingredient
The gold bullion of 5%~10% weight is rolled into the thin slice of 0.2~0.5mm；Metallic beryllium after weighing is wrapped up with gold plaque, is placed in true
In loading hopper above empty induction melting furnace；Remaining gold material is put in graphite crucible；
(2) it is evacuated to vacuum degree and reaches × 10-1~× 10-2After Pa, charge valve is opened, high-purity argon is filled with into furnace
Gas, until 0.03~0.08MPa；
(3) start slow power transmission, induction heating makes the gold in crucible start to melt；
(4) after gold is completely melt, loading hopper is opened, makes the beryllium material of gold plaque and its package that the gold into crucible be added together molten
In liquid；
(5) continue heating to be refined, so that beryllium melts, while be sufficiently mixed with gold；
(6) temperature is reduced after refining, when temperature is at 1100~1200 DEG C, is poured, golden beryllium alloy ingot casting is obtained；
(7) it is heat-treated using the alloy cast ingot that heating furnace obtains step (6)；Heat treatment temperature is 400~550
DEG C, the time is 20~40min；
(8) golden beryllium alloy ingot casting through-thickness is subjected to multistage hot deformation processing using plastic processing equipment, realized thick
Degree is thinned；
(9) blank is carried out tempering heat treatment in heating furnace by the processing of 1~2 passage of every completion, and tempering heat treatment temperature is 400
~550 DEG C, the time is 3~10min；
(10) (8), (9) step are repeated, until required plate thickness size；
(11) step (10) resulting plate is processed into rule particle shape using stamping die.
The preparation method of semiconductor device gold beryllium alloy material as described above, which is characterized in that the step (1) is matched
By the metallic beryllium of 0.05~0.3wt.% of alloy nominal composition polygamy when material.
The preparation method of semiconductor device gold beryllium alloy material as described above, which is characterized in that refining temperature 1200
~1300 DEG C, 3~10min of refining time.
The preparation method of semiconductor device gold beryllium alloy material as described above, which is characterized in that step (8) heat
Pass deformation rate 2%~8% is rolled, the total deformation rate after completing step (10) is 25%~75%.
The preparation method of semiconductor device gold beryllium alloy material as described above, which is characterized in that this method preparation
The size of golden beryllium alloy material are as follows: 0.5~3mm of thickness, shape are rectangular, round or special-shaped.
On the other hand, the present invention provides a kind of semiconductor device gold beryllium alloy material, is using side as described above
Method preparation.
The preparation method is that preparing golden beryllium alloy ingot casting by vacuum induction melting secondary charging method, then pass through
Heat treatment combines hot rolling technology to prepare golden beryllium alloy material.The beneficial effect is that the following aspects:
1. preventing metallic beryllium from volatilizing excessive in the case where crossing hot smelting state and leading to final golden beryllium alloy for control alloying component
Middle beryllium content is relatively low, therefore, by the beryllium of 0.05~0.3wt.% of alloy nominal composition polygamy when ingredient.
2. when charging, beryllium gold plaque package is placed in loading hopper, after the gold in crucible is completely melt, secondary batching,
Beryllium, which is added in crucible, makes its fusing.This charging method, compared with just gold and beryllium are fully enclosed in crucible when direct charging,
Heated time of the beryllium in high temperature can be shortened, the volatilization and oxidation of beryllium can be effectively reduced in this way.Because metallic beryllium easily with oxygen knot
It closes, the refractory oxides of generation swim on liquid level, and when casting is easily involved in inside ingot or stays in ingot casting surface, form ingot casting and lack
It falls into, influences ingot quality.
3. in fusion process, in order to reduce the oxidation and volatilization of metallic beryllium, being first evacuated to vacuum degree and reaching × 10-1~×
10-2After Pa, it is re-filled with high-purity argon gas and carries out atmosphere protection.
4. pair ingot casting uses hot-working, the big problem of golden beryllium alloy material brittleness itself is overcome, the processing of material is improved
Performance.Temperature control is not enough to reach the cogging temperature of hot rolling, causes in 400~550 DEG C of ranges when temperature is lower than 400 DEG C
Blank is easy to be unfavorable for technical process control along rolling direction or lateral embrittlement when repeat-rolling.
5. it can control plate thickness by multistage hot deformation and stress relief annealing and reach any particular value, consequently facilitating
The single weight of the final golden beryllium alloy material of control, is conducive to semiconductor devices user and accurately controls plating film uniformity.
Detailed description of the invention
Fig. 1 is the flow chart of the preparation method of semiconductor device gold beryllium alloy material of the present invention.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples.
Embodiment 1
Prepare the golden beryllium alloy material that nominal composition is AuBe0.5 (beryllium content is 0.5%, and clout is gold), preparation side
Method are as follows:
(1) using gold, beryllium metal as raw material, golden purity is not less than 4N, and the purity of beryllium is not less than 3N；According to Be 0.55%
Ingredient, clout are gold.Beryllium is wrapped up with gold plaque, is placed in the loading hopper above vacuum induction melting furnace；Remaining gold material is put in stone
In black crucible；
(2) it is evacuated to vacuum degree and reaches 5 × 10-2After Pa, charge valve is opened, high-purity argon gas is filled with into furnace, until
0.05MPa；
(3) start slow power transmission, induction heating makes the gold in crucible start to melt；
(4) after gold is completely melt, loading hopper is opened, makes the beryllium material of gold plaque and its package that the gold to crucible be added together molten
In liquid；
(5) continue heating to be refined, 1200 DEG C~1300 DEG C of temperature, refine 5min, so that beryllium melts, while being filled with gold
Divide mixing；
(6) temperature is reduced after refining, when temperature is at 1100~1200 DEG C, is poured, golden beryllium alloy ingot casting is obtained；
(7) it is heat-treated using the alloy cast ingot that heating furnace obtains step (6)；Heat treatment temperature is 420 DEG C, the time
For 20min；
(8) golden beryllium alloy ingot casting is thermoformed using plastic processing equipment, pass deformation 10%, is realized thick
Degree is thinned；
(9) blank is carried out tempering heat treatment in heating furnace by the processing of 1~2 passage of every completion, and tempering heat treatment temperature is 420
DEG C, time 3min；
(10) (8), (9) step are repeated, until with a thickness of the light sheet of 0.5mm；
(11) step (10) resulting plate is processed into rule particle shape using stamping die.
Embodiment 2
Prepared composition is the golden beryllium alloy material of AuBe0.7 (beryllium content is 0.7%, and clout is gold), preparation method are as follows:
(1) using gold, beryllium metal as raw material, golden purity is not less than 4N, and the purity of beryllium is not less than 3N；Match according to Be 0.8%
Material, clout are gold.Beryllium is wrapped up with gold plaque, is placed in the loading hopper above vacuum induction melting furnace；Remaining gold material is put in graphite
In crucible；
(2) it is vacuumized according to the method for embodiment 1, applying argon gas, melting, refining, casting, obtains golden beryllium alloy casting
Ingot；
(3) it is heat-treated using the alloy cast ingot that heating furnace obtains step (2), heat treatment temperature is 480 DEG C, the time
For 35min；
(4) golden beryllium alloy ingot casting is thermoformed using plastic processing equipment, pass deformation 5%, is realized thick
Degree is thinned；
(5) blank is carried out tempering heat treatment in heating furnace by the processing of 1~2 passage of every completion, and tempering heat treatment temperature is 480
DEG C, time 5min；
(6) (4), (5) step are repeated, until with a thickness of the light sheet of 0.5mm；
(7) step (6) resulting plate is processed into rule particle shape using stamping die.
Embodiment 3
Prepared composition is the golden beryllium alloy material of AuBe1 (beryllium content is 1%, and clout is gold), preparation method are as follows:
(1) using gold, beryllium metal as raw material, golden purity is not less than 4N, and the purity of beryllium is not less than 3N；Match according to Be 1.1%
Material, clout are gold.Beryllium is wrapped up with gold plaque, is placed in the loading hopper above vacuum induction melting furnace；Remaining gold material is put in graphite
In crucible；
(2) it is vacuumized according to the method for embodiment 1, applying argon gas, melting, refining, casting, obtains golden beryllium alloy casting
Ingot；
(3) it is heat-treated using the alloy cast ingot that heating furnace obtains step (2), heat treatment temperature is 500 DEG C, the time
For 30min；
(4) golden beryllium alloy ingot casting is thermoformed using plastic processing equipment, pass deformation 5%, is realized thick
Degree is thinned；
(5) blank is carried out tempering heat treatment in heating furnace by the processing of 1~2 passage of every completion, and tempering heat treatment temperature is 500
DEG C, time 5min；
(6) (4), (5) step are repeated, until with a thickness of the light sheet of 1mm；
(7) step (6) resulting plate is processed into rule particle shape using stamping die.
Embodiment 4
Prepared composition is the golden beryllium alloy material of AuBe1.5 (beryllium content is 1.5%, and clout is gold), preparation method are as follows:
(1) using gold, beryllium metal as raw material, golden purity is not less than 4N, and the purity of beryllium is not less than 3N；Match according to Be 1.7%
Material, clout are gold.Beryllium is wrapped up with gold plaque, is placed in the loading hopper above vacuum induction melting furnace；Remaining gold material is put in graphite
In crucible；
(2) it is vacuumized according to the method for embodiment 1, applying argon gas, melting, refining, casting, obtains golden beryllium alloy casting
Ingot；
(3) it is heat-treated using the alloy cast ingot that heating furnace obtains step (2), heat treatment temperature is 530 DEG C, the time
For 30min；
(4) golden beryllium alloy ingot casting is thermoformed using plastic processing equipment, pass deformation 5%, is realized thick
Degree is thinned；
(5) blank is carried out tempering heat treatment in heating furnace by the processing of 1~2 passage of every completion, and tempering heat treatment temperature is 530
DEG C, time 8min；
(6) (4), (5) step are repeated, until with a thickness of the light sheet of 2mm；
(7) step (6) resulting plate is processed into rule particle shape using stamping die.
The ingredient and plastic processing condition of golden beryllium alloy material in 1 embodiment of table
Technical solution of the present invention is described in detail in above-described embodiment.It is apparent that the present invention is not limited being retouched
The embodiment stated.Based on the embodiments of the present invention, those skilled in the art can also make a variety of variations accordingly, but appoint
What is equal with the present invention or similar variation shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of semiconductor device gold beryllium alloy material, which comprises the steps of:
(1) using gold, beryllium metal as raw material, according to 0.5~2wt.% of alloy nominal composition Be a certain proportion of metal of polygamy again
Beryllium, clout are gold；The purity of gold is not less than 4N, and the purity of beryllium is not less than 3N；The metallic beryllium golden thin slice of a part is wrapped up, remaining
Gold material is put in graphite crucible；
(2) it is evacuated to vacuum degree and reaches × 10-1~× 10-2After Pa, argon gas is filled with into smelting furnace, until 0.03~
0.08MPa；
(3) induction heating makes the gold fusing in graphite crucible；
(4) after gold is completely melt, the metallic beryllium of gold plaque and its package is added together in the golden melt to crucible；
(5) continue heating to be refined, so that beryllium melts, while be sufficiently mixed with gold；
(6) temperature is reduced after refining, is poured, golden beryllium alloy ingot casting is obtained；
(7) it is heat-treated using the alloy cast ingot that heating furnace obtains step (6)；
(8) golden beryllium alloy ingot casting is subjected to multistage hot deformation processing, realizes that thickness is thinned；
(9) blank is carried out tempering heat treatment in heating furnace by the processing of 1~2 passage of every completion；
(10) (8), (9) step are repeated, until reaching the plate of required thickness size；
(11) by plate obtained by step (10), it is processed into rule particle shape.
2. the method as described in claim 1, which is characterized in that press alloy nominal composition polygamy when ingredient described in step (1)
The metallic beryllium of 0.05~0.3wt.%.
3. the method as described in claim 1, which is characterized in that gold thin slice described in step (1) be by 5% in every heat~
The gold of 10% weight is rolled into the golden thin slice of 0.2~0.5mm.
4. the method as described in claim 1, which is characterized in that 1200~1300 DEG C of the temperature of refining described in step (5), essence
Refine 3~10min of time.
5. the method as described in claim 1, which is characterized in that when temperature described in step (6) is reduced to 1100~1200 DEG C,
It is poured.
6. the method as described in claim 1, which is characterized in that heat treatment temperature described in step (7) is 400~550 DEG C, when
Between be 20~40min.
7. the method as described in claim 1, which is characterized in that hot rolling pass deformation rate 2%~8% described in step (8), it is complete
It is 25%~75% at the total deformation rate after step (10).
8. the method as described in claim 1, which is characterized in that tempering heat treatment temperature described in step (9) is 400~550
DEG C, the time is 3~10min.
9. the semiconductor device gold beryllium alloy material of any one of claim 1-8 method preparation, which is characterized in that the alloy
The ingredient of material are as follows: beryllium content 0.5wt.%~2wt.%, remaining is gold.
10. alloy material as claimed in claim 9, which is characterized in that 0.5~3mm of thickness of the alloy material, shape are
It is rectangular, round or special-shaped.
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Cited By (1)
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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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