CN106381410A - Method, smelting furnace and system for preparing phosphor-copper anode for integrated circuit - Google Patents
Method, smelting furnace and system for preparing phosphor-copper anode for integrated circuit Download PDFInfo
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- CN106381410A CN106381410A CN201611070135.0A CN201611070135A CN106381410A CN 106381410 A CN106381410 A CN 106381410A CN 201611070135 A CN201611070135 A CN 201611070135A CN 106381410 A CN106381410 A CN 106381410A
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- copper
- integrated circuit
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- phosphor
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- RIRXDDRGHVUXNJ-UHFFFAOYSA-N [Cu].[P] Chemical compound [Cu].[P] RIRXDDRGHVUXNJ-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000003723 Smelting Methods 0.000 title claims abstract description 33
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000010949 copper Substances 0.000 claims abstract description 44
- 229910052802 copper Inorganic materials 0.000 claims abstract description 43
- 238000012545 processing Methods 0.000 claims abstract description 20
- 238000009749 continuous casting Methods 0.000 claims abstract description 18
- 229910000881 Cu alloy Inorganic materials 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 238000002844 melting Methods 0.000 claims description 31
- 230000008018 melting Effects 0.000 claims description 31
- 238000002360 preparation method Methods 0.000 claims description 29
- 238000005266 casting Methods 0.000 claims description 24
- 238000009413 insulation Methods 0.000 claims description 19
- 238000001953 recrystallisation Methods 0.000 claims description 15
- 238000009461 vacuum packaging Methods 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- 239000003610 charcoal Substances 0.000 claims description 9
- 239000013078 crystal Substances 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 8
- 229910052698 phosphorus Inorganic materials 0.000 claims description 8
- 239000011574 phosphorus Substances 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000012544 monitoring process Methods 0.000 claims description 6
- 238000007493 shaping process Methods 0.000 claims description 5
- PTVDYARBVCBHSL-UHFFFAOYSA-N copper;hydrate Chemical compound O.[Cu] PTVDYARBVCBHSL-UHFFFAOYSA-N 0.000 claims description 4
- 238000004806 packaging method and process Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 3
- 238000003780 insertion Methods 0.000 claims description 2
- 230000037431 insertion Effects 0.000 claims description 2
- 238000009434 installation Methods 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000011049 filling Methods 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 239000013081 microcrystal Substances 0.000 abstract 4
- 238000001816 cooling Methods 0.000 description 14
- 229910052760 oxygen Inorganic materials 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 11
- 239000001301 oxygen Substances 0.000 description 11
- 230000007423 decrease Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 238000007747 plating Methods 0.000 description 5
- 238000005253 cladding Methods 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002826 coolant Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229910000906 Bronze Inorganic materials 0.000 description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910000431 copper oxide Inorganic materials 0.000 description 2
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 2
- LBJNMUFDOHXDFG-UHFFFAOYSA-N copper;hydrate Chemical compound O.[Cu].[Cu] LBJNMUFDOHXDFG-UHFFFAOYSA-N 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 241000208140 Acer Species 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 229920000914 Metallic fiber Polymers 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 241000219000 Populus Species 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
Classifications
-
- 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
- C22C1/03—Making non-ferrous alloys by melting using master alloys
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/001—Continuous casting of metals, i.e. casting in indefinite lengths of specific alloys
- B22D11/004—Copper alloys
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/14—Plants for continuous casting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
-
- 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
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method, smelting furnace and system for preparing a phosphor-copper anode for an integrated circuit. The method comprises the steps that A-grade electrolytic copper with the copper content reaching 99.99% or above and a high-phosphor-copper alloy with the content of each single impurity not greater than 0.003% are adopted as raw materials; vacuum smelting and continuous casting are conducted, wherein the vacuum smelting furnace is selected for conducting copper-phosphor synthesis and traction on the A-grade electrolytic copper and the high-phosphor-copper alloy, so that a phosphor-copper alloy ingot is obtained; microcrystal treatment is conducted, wherein microcrystal treatment is conducted on the phosphor-copper alloy ingot in the vacuum state; and cold-state processing for formation is conducted, wherein processing for formation is conducted on the phosphor-copper alloy ingot obtained after microcrystal treatment at the normal temperature, so that the phosphor-copper anode for the integrated circuit is obtained. According to the method, smelting furnace and system for preparing the phosphor-copper anode for the integrated circuit, vacuum smelting and continuous casting are conducted on the raw materials; microcrystal treatment is conducted in the vacuum state; processing for formation is conducted at the normal temperature; the production process is simple; the prepared phosphor-copper anode for the integrated circuit has higher filling capacity and higher ductility; and copper is high in purity and small and uniform in grain size.
Description
Technical field
The present invention relates to the preparation method of phosphorus-copper anode, more specifically refer to a kind of system of phosphorus-copper anode for integrated circuit
Preparation Method and smelting furnace and its system.
Background technology
In large-scale integrated circuit produces, the etching of copper is extremely difficult, adopts copper plating process to prepare aborning
The copper interconnection line developing direction following by becoming integrated circuit, this technique mainly plates last layer by plating mode in groove
Copper facing that is fine and close, being evenly distributed, due to groove, children is thin, therefore it is required that the phosphorus-copper anode of plating has very high filling capacity,
And there is higher ductility, higher to the purity of copper and the requirement of grain size, and, in integrated circuits, to copper-plated oxygen
Content requirement is higher, when being because that oxygen content is high, easily produces copper oxide and Red copper oxide, and is distributed in grain boundaries, impact electricity
Plating effect, this is an important index.
Chinese patent 201010581922.8 discloses a kind of preparation method of phosphorus-copper anode for integrated circuit, using high-purity
As crucible and mold materials, in fine vacuum medium frequency induction melting furnace, fusing purity is 99.99% and above height to degree graphite
Fine copper ingot casting, adds the phosphor bronze alloy of phosphorous 6～16wt.% in 1150～1300 DEG C, add phosphor bronze alloy with
The weight of high purity copper ingot casting ratio for 1: 50～600, is incubated 20～30min at 1150～1300 DEG C, then after standing 20 minutes, pours
Enter graphite jig, obtain phosphor copper ingot casting；After the phosphor copper ingot casting excision ingot casting rising head obtaining, through multiway forging with roll
System, and after 0.5～12 hour recrystallization of 300～600 DEG C of insulations is processed, through surface treatment, it is machined into integrated electricity
Road phosphorus-copper anode, but this manufacturing process is still complicated.
Therefore, it is necessary to design a kind of preparation method of phosphorus-copper anode for integrated circuit, realize manufacturing process simply, preparation
Phosphorus-copper anode for integrated circuit there is very high filling capacity, and there is higher ductility, the purity of copper is high and grain size
Little and uniform.
Content of the invention
It is an object of the invention to overcoming the defect of prior art, provide a kind of preparation side of phosphorus-copper anode for integrated circuit
Method and smelting furnace and its system.
For achieving the above object, the present invention employs the following technical solutions：A kind of preparation side of phosphorus-copper anode for integrated circuit
Method, described preparation method includes：
Raw material reaches more than 99.99% A level cathode copper using copper content and individual event impurity is not more than 0.003%
High phosphor copper alloy；
Vacuum melting and continuous casting：Smelting furnace from vacuum carries out copper, phosphorus to described A level cathode copper and high phosphor copper alloy
Synthesis and traction, obtain phosphor copper ingot casting；
Crystallite is processed：Under vacuum conditions crystallite process is carried out to described phosphor copper ingot casting；
Cool grinding shapes：At normal temperatures the described phosphor copper ingot casting after crystallite process is processed shaping, obtains
Phosphorus-copper anode for integrated circuit.
Its further technical scheme is：After the step that described cool grinding shapes, also include
Cleaning and packaging：Described phosphorus-copper anode for integrated circuit is carried out with moistureproof temperature control cleaning treatment and vacuum packaging.
Its further technical scheme is：In the step of described vacuum melting and continuous casting, need to described A level cathode copper with
And high phosphor copper alloy carries out mixing, purify and fully mixing, and purifying and needing during fully mixing periodically with also
In log scale insertion copper water.
Its further technical scheme is：In the step with continuous casting for the described vacuum melting, drawn using Serve Motor Control
Speed, monitoring traction copper bar surface temperature is at 40 DEG C to 50 DEG C.
Its further technical scheme is：In described crystallite process step, need the crystal grain to described phosphor copper ingot casting
Multi-faceted broken, recrystallize in 450 DEG C to 550 DEG C crystallization operating rooms.
Its further technical scheme is：In described crystallite process step, need using Serve Motor Control recrystallization
Speed, the temperature of the described phosphor copper ingot casting of the monitoring port of export is at 40 DEG C to 50 DEG C.
Its further technical scheme is：Described cool grinding shape step in, need described phosphor copper ingot casting with
And mould needs to be cooled down with high pressure cooling medium, and use Serve Motor Control process velocity, the temperature of supervision molding
70 DEG C to 100 DEG C.
Present invention also offers smelting furnace, including the melting storehouse, intermediate bin and the thermal insulation barn that are connected successively, described intermediate bin
And it is provided with graphite flakes in described thermal insulation barn, it is provided with Linesless charcoal and feeding tank in described melting storehouse.
Its further technical scheme is：It is additionally provided with aerofluxuss rod in described intermediate bin, in described thermal insulation barn, be provided with temperature sensing
Device.
Present invention also offers a kind of preparation system of phosphorus-copper anode for integrated circuit, including above-mentioned smelting furnace, tie again
Crystal structure, processing mold and vacuum packing machine, described smelting furnace, recrystallization texture, processing mold and vacuum packing machine according to
Secondary be connected, raw material, after smelting furnace vacuum melting and continuous casting, carries out crystallite process through recrystallization texture, through processing mould
Tool forms processing at normal temperatures, is vacuum-packed using vacuum packing machine.
Compared with the prior art, the invention has the advantages that：A kind of preparation of the phosphorus-copper anode for integrated circuit of the present invention
Method, is used as raw material by the low high phosphor copper alloy of the A level cathode copper high using copper content and individual event impurity, using vacuum
Smelting furnace vacuum melting and continuous casting are carried out to raw material, also carry out under vacuum conditions being processed under crystallite process, room temperature
Shape, strictly control oxygen content, realize manufacturing process simply, the phosphorus-copper anode for integrated circuit of preparation has very high filling energy
Power, and there is higher ductility, the purity of copper is high little with grain size and uniform.
The invention will be further described with specific embodiment below in conjunction with the accompanying drawings.
Brief description
A kind of flow chart of the preparation method of phosphorus-copper anode for integrated circuit that Fig. 1 provides for the specific embodiment of the invention；
The main structure diagram of the smelting furnace that Fig. 2 provides for the specific embodiment of the invention；
The side structure schematic view of the smelting furnace that Fig. 3 provides for the specific embodiment of the invention；
The main structure diagram of the recrystallization texture that Fig. 4 provides for the specific embodiment of the invention；
The main structure diagram of the processing mold that Fig. 5 provides for the specific embodiment of the invention；
The main structure diagram of the vacuum packing machine that Fig. 6 provides for the specific embodiment of the invention；
The main structure diagram of the finished product after the packaging that Fig. 7 provides for the specific embodiment of the invention.
Specific embodiment
In order to more fully understand the technology contents of the present invention, with reference to specific embodiment, technical scheme is entered
One step introduction and explanation, but it is not limited to this.
Specific embodiment as shown in Fig. 1～7, a kind of preparation side of phosphorus-copper anode for integrated circuit that the present embodiment provides
Method, goes for integrated circuit electro-coppering, high-end PCB electro-coppering, during high-end plating surface treatment copper, realizes manufacturing
Process is simple, the phosphorus-copper anode for integrated circuit of preparation has very high filling capacity, and has higher ductility, copper pure
Degree is high little with grain size and uniform.
As shown in figure 1, a kind of preparation method of phosphorus-copper anode for integrated circuit, including：
Raw material reaches more than 99.99% A level cathode copper using copper content and individual event impurity is not more than 0.003%
High phosphor copper alloy；
S1, vacuum melting and continuous casting：Smelting furnace from vacuum is carried out to described A level cathode copper and high phosphor copper alloy
Copper, the synthesis of phosphorus and traction, obtain phosphor copper ingot casting；
S2, crystallite are processed：Under vacuum conditions crystallite process is carried out to described phosphor copper ingot casting；
S3, cool grinding shape：At normal temperatures the described phosphor copper ingot casting after crystallite process is processed shaping, obtains
Obtain phosphorus-copper anode for integrated circuit.
For the employing of raw material, need to meet the technical specification of phosphorus-copper anode for integrated circuit, because integrated circuit is used
The requirement of the constituent of phosphorus-copper anode：Cu >=99.95%, 0.025%≤P≤0.05%, Ag≤0.0025%, O≤
0.0003%, other individual event impurity≤0.001%, therefore need the high-purity A level cathode copper using high copper content, select high-purity simultaneously
The high phosphor copper alloy of degree, individual event impurity≤0.003% is it is ensured that the purity of raw material.
Further, above-mentioned S1 step, in vacuum melting and continuous casting step, first to raw material and carry out synthesis mixing,
Purify and abundant mix, fully mixing is in order to uniform further, then needs in whole process to ensure copper water temperature.
Specifically, represent that because temperature is too high crystallization cooling effect declines, crystal grain can the decline of thick, dense structure, work as copper
When bar surface temperature is high, the stepless decline of motor control hauling speed, when copper bar surface temperature is low, motor control hauling speed is no
Level lifting, in described S1 step, in the step of vacuum melting and continuous casting, using Serve Motor Control hauling speed, monitoring is led
Draw copper bar surface temperature at 40 DEG C to 50 DEG C.
In addition, above-mentioned S1 step, in vacuum melting and the step of continuous casting, and the smelting furnace from vacuum is it is ensured that copper phosphorus
Fully mix, and complete the process of whole melting continuous casting shaping under vacuum anaerobic it is ensured that oxygen content conforms to quality requirements.
This smelting furnace includes melting storehouse 10, intermediate bin 20 and thermal insulation barn 30, and intermediate bin 20 and thermal insulation barn 30 are all with pure
Graphite flakes 40 cladding thickness be 5cm to 15cm, play insulation with separate air effect, make warehouse be under vacuum state
Work.
Preferably, graphite flakes 40 cladding thickness is 10cm.
In addition, melting storehouse 10 cladding thickness be 15cm to 25cm Linesless charcoal 60 be totally dried, on the one hand ensure charging smoothly,
On the other hand ensure during charging, have Linesless charcoal 60 to have combustion height separated material air enough to enter, make warehouse be in work under vacuum state
Make.
Preferably, the cladding thickness of Linesless charcoal 60 is 20cm.
Above-mentioned S2 step, in described crystallite process step, needs multi-faceted to the crystal grain of described phosphor copper ingot casting
Broken, recrystallize in 450 DEG C to 550 DEG C crystallization operating rooms, organizational structure crystal grain children is thin, dense structure, metallic fiber are strong；
Recrystallized in the state of sealing and vacuum it is ensured that copper surface phosphorus content normal, this process is for raw in electroplating process
Become phosphorus film extremely important, vacuum anaerobic processing ensure that the oxygen content of phosphorus-copper anode reaches requirement.
Preferably, recrystallize in 500 DEG C of crystallization operating rooms it is ensured that copper crushes at this temperature and again ties rapidly
Brilliant, rapid cooling.
Further, the stepless decline of the speed due to recrystallizing when temperature is high, the speed recrystallizing when temperature is low is stepless
Lifting；In described S2 step, in crystallite process step, need the speed using Serve Motor Control recrystallization, monitor the port of export
Described phosphor copper ingot casting temperature at 40 DEG C to 50 DEG C.
For above-mentioned S3 step, in the step that described cool grinding shapes, need described phosphor copper ingot casting and
Mould needs to be cooled down with high pressure cooling medium.
Due to process velocity stepless decline when temperature is high, process velocity stepless lifting when temperature is low, using servomotor control
Process velocity processed, the temperature 70 C of supervision molding is to 100 DEG C.
At normal temperatures be processed shape it is ensured that the phosphorus content on copper surface non-volatile, ensure occur without because machine heat energy
Make copper surface oxidation.
After the step that described S3 step, cool grinding shape, also include
S4, cleaning and packaging：Described phosphorus-copper anode for integrated circuit is carried out with moistureproof temperature control cleaning treatment and vacuum packet
Dress.
For above-mentioned S3 step, specifically need after cleaning to complete drying under moistureproof controlled temperature space, reach quick,
The purpose being completely dried, ensures and will not form moisture or other moist medium on the surface of described phosphorus-copper anode for integrated circuit,
Make generation electrochemical reaction and variable color oxidation etc..
After described phosphorus-copper anode for integrated circuit cools down completely, using vacuum packaging, it is to avoid produce oxidation with air contact
Thing and because difference variation produces moist and oxide in product surface.
Due to integrated circuit to copper-plated oxygen content require higher, when being because that oxygen content is high, easily produce copper oxide and
Red copper oxide, and it is distributed in grain boundaries, affect electroplating effect, this is an important index, therefore, is preparing described integrated electricity
Road phosphorus-copper anode, needs strict control oxygen content.
A kind of preparation method of above-mentioned phosphorus-copper anode for integrated circuit, by adopt the high A level cathode copper of copper content with
And the low high phosphor copper alloy of individual event impurity is as raw material, the smelting furnace using vacuum carries out vacuum melting and company to raw material
Casting, also carries out under vacuum conditions being processed under crystallite process, room temperature shaping, strictly controls oxygen content, realize manufacturing process
Simply, the phosphorus-copper anode for integrated circuit of preparation has very high filling capacity, and has higher ductility, and the purity of copper is high
Little with grain size and uniform.
As shown in Figures 2 and 3, the present embodiment also proposed smelting furnace, for vacuum melting with continuous casting to prepare integrated electricity
Road phosphorus-copper anode.
Above-mentioned smelting furnace, including the melting storehouse 10 being connected successively, intermediate bin 20 and thermal insulation barn 30, described intermediate bin 20
And it is provided with graphite flakes 40 in described thermal insulation barn 30, it is provided with Linesless charcoal 60 and feeding tank 50 in described melting storehouse 10.
Above-mentioned smelting furnace, by and separating all with pure 40 insulations of graphite flakes in intermediate bin 20, thermal insulation barn 30
The effect of air, makes warehouse be in and works under vacuum state, covers Linesless charcoal 60 in melting storehouse 10, on the one hand ensures that charging is suitable
Profit, on the other hand ensures there are enough Linesless charcoals 60 as fuel during charging, and the entrance of air-isolation, makes warehouse be in vacuum
Work under state, improve the vacuum of whole smelting furnace.
The thickness of above-mentioned graphite flakes 40 is 5cm to 15cm it is preferred that the thickness of graphite flakes 40 is 10cm.
The thickness of above-mentioned Linesless charcoal 60 is 15cm to 25cm it is preferred that the thickness of Linesless charcoal 60 is 20cm.
Further, it is additionally provided with aerofluxuss rod 70 in intermediate bin 20, described aerofluxuss rod 70 can drain residual oxygen in copper water
Content, reduces the degree of oxidation of the phosphorus-copper anode for integrated circuit of preparation.
In the present embodiment, aerofluxuss rod 70 is batten.
Certainly, in other embodiment, above-mentioned aerofluxuss rod 70 can also be compound bar, the material of compound bar is poplar,
Maple is formed with bamboo chip polymeric compressing.
In addition, being provided with temperature sensor 80 in thermal insulation barn 30, specifically in order to monitor traction copper bar surface temperature 40
DEG C to 50 DEG C.
It is respectively equipped with channel structure 11 it is ensured that homogeneous heating in above-mentioned melting storehouse 10, intermediate bin 20 and thermal insulation barn 30
And copper phosphorus fully mixes.
Above-mentioned described channel structure 11 is included located at middle calandria, and is located on double channels skies of calandria surrounding
Chamber, is provided with flame retardant coating and cooling layer between described channel cavity and calandria.Can high current compared with single channel of homalographic
Density, makes the electric current density of channel can reach 9～12A/mm2, coil current density reaches 2～2.5A/mm2, can improve and add
The electrothermal efficiency of hot body is high.
The section of channel cavity (being also called sensing channel) is circular or oval, improves the transmission capacity of heat energy and has
Imitate pre- anti-blocking ditch phenomenon.
Described thermal insulation barn 30 is provided with the phosphor-copper crystalline texture 90 being connected with power source, for lengthening cooling stroke, reaches
Both meet crystal demand, meet production efficiency, the copper end of crystallizer needs to make encapsulation process, prevents air from entering from gap again
Enter.
Specifically, described phosphor-copper crystalline texture 90 is crystallizer, and above-mentioned power source is motor.
Temperature is too high to represent that crystallization cooling effect declines, and crystal grain can thick, dense structure decline, when copper bar surface temperature height
When, the stepless decline of motor control hauling speed, when copper bar surface temperature is low, the stepless lifting of motor control hauling speed.
In the present embodiment, described melting storehouse 10, intermediate bin 20 and the square-shaped arrangement of thermal insulation barn 30.
Certainly, in other embodiment, described melting storehouse 10, intermediate bin 20 and thermal insulation barn 30 can be in other irregular shapes
Shape is arranged.
The present embodiment also proposed a kind of preparation system of phosphorus-copper anode for integrated circuit, including above-mentioned smelting furnace, again
Crystalline texture, processing mold 95 and vacuum packing machine 97, described smelting furnace, recrystallization texture, processing mold 95 and vacuum
Packer 97 is connected successively, and raw material, after smelting furnace vacuum melting with continuous casting, carries out crystallite process through recrystallization texture,
Form processing at normal temperatures through processing mold 95, be vacuum-packed using vacuum packing machine 97.
Specifically, the crystallite that above-mentioned recrystallization texture includes being sequentially connected processes structure and cooling structure 93, described
Crystallite processes structure and described cooling structure 93 is used for broken recrystallization multi-faceted to crystal grain, is tied in sealed states again
Brilliant it is ensured that copper surface phosphorus content normal, vacuum anaerobic processing ensure that the oxygen content of phosphorus-copper anode reaches requirement.
The outlet of described cooling structure 93 is provided with thermometer, for monitoring the copper bar temperature of the port of export at 40 DEG C to 50 DEG C.
Above-mentioned crystallite processes in structure and is provided with mould 92.This mould 92 processes for crystallite and provides a sealing and vacuum
Environment.Charging copper rod 91, after the entrance of mould 92 enters, through the process of mould 92, then through overcooling structure cooling, obtains
To discharging copper rod 94.
The outer end of above-mentioned processing mold 95 is provided with cooling container 96, has high pressure cooling to be situated between in described cooling container 96
Matter, the cooling medium in cooling container 96 carries out high pressure cooling to worked copper bar and mould, controls processing temperature.
The above-mentioned technology contents only to be further illustrated the present invention with embodiment, are easier to understand in order to reader, but not
Represent embodiments of the present invention and be only limitted to this, any technology done according to the present invention extends or recreates, all by the present invention's
Protection.Protection scope of the present invention is defined by claims.
Claims (10)
1. a kind of preparation method of phosphorus-copper anode for integrated circuit is it is characterised in that described preparation method includes：
Raw material reaches more than 99.99% A level cathode copper and the high phosphorus of individual event impurity no more than 0.003% using copper content
Copper alloy；
Vacuum melting and continuous casting：Smelting furnace from vacuum carries out the conjunction of copper, phosphorus to described A level cathode copper and high phosphor copper alloy
Become and draw, obtain phosphor copper ingot casting；
Crystallite is processed：Under vacuum conditions crystallite process is carried out to described phosphor copper ingot casting；
Cool grinding shapes：At normal temperatures the described phosphor copper ingot casting after crystallite process is processed shaping, obtains integrated
Circuit phosphorus-copper anode.
2. a kind of preparation method of phosphorus-copper anode for integrated circuit according to claim 1 is it is characterised in that described cold
After the step that state shapes, also include
Cleaning and packaging：Described phosphorus-copper anode for integrated circuit is carried out with moistureproof temperature control cleaning treatment and vacuum packaging.
3. a kind of preparation method of phosphorus-copper anode for integrated circuit according to claim 1 is it is characterised in that described true
In the step of empty melting and continuous casting, need described A level cathode copper and high phosphor copper alloy are carried out mixing, purify and fully mixed
With, and purifying and needing during fully mixing periodically with going back in log scale insertion copper water.
4. a kind of preparation method of phosphorus-copper anode for integrated circuit according to claim 3 is it is characterised in that described true
In the step of empty melting and continuous casting, using Serve Motor Control hauling speed, monitoring traction copper bar surface temperature is at 40 DEG C extremely
50℃.
5. a kind of preparation method of phosphorus-copper anode for integrated circuit according to claim 1 is it is characterised in that described micro-
In brilliant process step, need the crystal grain to described phosphor copper ingot casting multi-faceted broken, crystallize operating room at 450 DEG C to 550 DEG C
Middle recrystallization.
6. a kind of preparation method of phosphorus-copper anode for integrated circuit according to claim 5 is it is characterised in that described micro-
In brilliant process step, need the speed using Serve Motor Control recrystallization, the described phosphor copper ingot casting of the monitoring port of export
Temperature is at 40 DEG C to 50 DEG C.
7. the preparation method of a kind of phosphorus-copper anode for integrated circuit according to any one of claim 1 to 6, its feature exists
In, in the step that described cool grinding shapes, the described phosphor copper ingot casting of needs and mould need to be cooled down with high pressure and be situated between
Matter is cooled down, and uses Serve Motor Control process velocity, and the temperature 70 C of supervision molding is to 100 DEG C.
8. smelting furnace is it is characterised in that include the melting storehouse, intermediate bin and the thermal insulation barn that are connected successively, described intermediate bin and
It is provided with graphite flakes in described thermal insulation barn, in described melting storehouse, be provided with Linesless charcoal and feeding tank.
9. smelting furnace according to claim 8 is it is characterised in that be additionally provided with batten in described intermediate bin, described thermal insulation barn
Inside it is provided with temperature sensor.
10. a kind of preparation system of phosphorus-copper anode for integrated circuit is it is characterised in that include the melting described in claim 8 or 9
Stove, recrystallization texture, processing mold and vacuum packing machine, described smelting furnace, recrystallization texture, processing mold and vacuum packet
Installation is connected successively, and raw material, after smelting furnace vacuum melting with continuous casting, carries out crystallite process through recrystallization texture, passes through
Processing mold forms processing at normal temperatures, is vacuum-packed using vacuum packing machine.
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| CN106381410B (en) | 2019-01-22 |
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Denomination of invention: Method and system for preparing phosphor-copper anode for integrated circuit Effective date of registration: 20200220 Granted publication date: 20190122 Pledgee: Shunde Guangdong rural commercial bank Nanhai Branch of Limited by Share Ltd. Pledgor: Cheon Western (China) Copper Ltd. Registration number: Y2020440000025 |
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Denomination of invention: A preparation method and system of phosphor copper anode for integrated circuits Granted publication date: 20190122 Pledgee: Shunde Guangdong rural commercial bank Nanhai Branch of Limited by Share Ltd. Pledgor: Foshan Cheng'an Group Co.,Ltd. Registration number: Y2024440000003 |