CN109628897A - A kind of high-purity alusil alloy sputtering target material blank and preparation method thereof - Google Patents
A kind of high-purity alusil alloy sputtering target material blank and preparation method thereof Download PDFInfo
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- CN109628897A CN109628897A CN201811484894.0A CN201811484894A CN109628897A CN 109628897 A CN109628897 A CN 109628897A CN 201811484894 A CN201811484894 A CN 201811484894A CN 109628897 A CN109628897 A CN 109628897A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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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
- C22C1/026—Alloys based on aluminium
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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
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/02—Alloys based on aluminium with silicon as the next major constituent
Abstract
The present invention is a kind of high-purity alusil alloy sputtering target material blank and preparation method thereof.A kind of preparation method of high-purity alusil alloy sputtering target material blank, comprising: (1) by high-purity aluminium and HIGH-PURITY SILICON vacuum fusion, be configured to the intermediate alloy melt that silicone content is 7-13wt%；(2) intermediate alloy melt is cast as intermediate alloy；(3) by high-purity aluminium and intermediate alloy vacuum fusion, it is configured to high-purity Al-Si alloy melt that silicone content is 0.9-1.1wt%；(4) high-purity Al-Si alloy melt is refined online, high-purity Al-Si alloy melt after must refining；(5) by high-purity Al-Si alloy melt on-line filtration after refining, molten aluminum is obtained；(6) molten aluminum is subjected to pieces of bar stock casting, obtains high-purity alusil alloy sputtering target material blank.A kind of high-purity alusil alloy sputtering target material blank of the present invention and preparation method thereof, using AL-1wt%Si alloy is prepared after vacuum melting furnace autogamy rafifinal silicon intermediate alloy, the alusil alloy target blank that high cleanliness, ingredient are uniform and surface quality is excellent is prepared by casting state modulator.
Description
Technical field
Present invention relates particularly to a kind of high-purity alusil alloy sputtering target material blanks and preparation method thereof.
Background technique
In recent years, with the fast development of microelectronic field, sputtering target material using more and more extensive.Sputtering is to utilize height
The ion beam current of speed energy, bombards the surface of solids, so that the atom of the surface of solids is left solid and be deposited on substrate surface, prepare thin
Membrane material.The solid bombarded is then referred to as sputtering target material, hereinafter referred to as target.
The fast development of semiconductor integrated circuit (IC) and the increase of integrated level make its quality requirement to metal interconnection wire
It further increases.Main supplementary material of the ultra-pure aluminum alloy target material as metal interconnection wire in IC manufacture, market scale day
Benefit expands.The quality of sputtering target material plays a crucial role the performance of metallic film material.
The deelectric transferred of pure aluminum metal interconnection line, stress migration and resistance to chemical attack are poor, add in rafifinal quantitative
Element silicon the deelectric transferred and stress migration ability of interconnection line can be improved, it is hard to promote interconnection line while improving recrystallization temperature
Degree.
A large number of experiments is studies have shown that ingredient, crystallite dimension and the crystal orientation of sputtering target material have spatter film forming quality
Extreme influence.(1) ingredient: sputtering target material is high to component requirements, and being primarily due to the alkali metal elements such as Na, K can spread to PN junction
Film is caused to be pierced；The heavy metal elements such as Fe, Ni are also easy to produce interface energy level leak resistance；Gaseous impurity C, O, N damage film
Stability；U, the radioactive elements such as Th, which may induce, delays work.Therefore circuit structure is finer, it is higher to aluminum substrate purity requirement.
(2) crystallite dimension: the sputtering target material of same ingredient, crystallite dimension is more tiny, and grain size is more uniform, and spatter film forming rate is got over
Fastly, film thickness distribution is also more uniform.(3) crystal grain is orientated: sputter rate increases with the increase of atom solid matter degree, overall steady
It is scheduled within the scope of one.(200) and the raising of (220) crystal face ratio is conducive to magnetron sputtering deposition.
But sputtering in the preparation of high-purity AL-1wt%Si target blank with being primarily present that target blank degree of purity is low, ingredient
The problems such as equal control is difficult and casting and forming is not easy.
Prior art CN105331856A (a kind of Al-Si alloy of microalloying and its preparation method of aluminium alloy rod) is mentioned
A kind of Al-Si alloy of microalloying, the micro alloyed aluminium alloy bar tensile strength 110MPa or more after annealing, elongation are supplied
29% or more rate is not easy fracture of wire during processing scale aluminium alloy welding wire, and welding wire surface is highly polished, and spatter is small, connects
Head tensile strength is good, is suitable for high-volume Virtual production aluminium-silicon alloy welding wire.Its ingredient is as follows: the silicon of 4.7~5.8wt%
Si；The iron Fe of 0~≤0.15wt%；The copper Cu of 0.01~0.1wt%；The manganese Mn of 0.005~0.03wt%；0.01~0.1%
Strontium Sr；Remaining is aluminium.But the invention prepares alusil alloy bar using melting and casting and rolling process, and through drawing process system
Standby aluminium alloy welding wire.Because the alusil alloy purity for sputtering target material is much higher than welding wire purity, the invention smelting technology can not be protected
Demonstrate,prove sputtering target material purity demand.
Prior art CN1718314A (aluminium silicon bonding line without mould continuous casting process) belong to alloy material metallurgy and
Processing, specifically design a kind of IC bonding wire Al-1%Si wire rod without mould continuous casting technology.In the process, it prepares first
AL- (10%-20%) Si aluminium silicon intermediate alloy ingot casting, then intermediate alloy ingot casting is added into fine aluminium solution, AL- is made
The unidirectional columanar structure's wire rod of alusil alloy is made with no mould continuous casting mode in (0.85%-1.15%) Si solution.The technology is maximum
Feature is to eliminate casting mold, is directly drawn using the performance tension of aluminium alloy solution and is cooled down rapidly, forms very thin solid-liquid
Two-phase section, substantially increases the temperature gradient of solid-liquid interface, accurately control in addition cooling water intensity of cooling and aluminium alloy it is quiet
Pressure surface guarantees to radiate along wire rod longitudinal direction, obtains unidirectional evenly distributed columanar structure's structure, and bar diameter is φ 5-
φ 8mm, it is ideal blank needed for production bonding aluminum steel.The best column crystal orientation that the finished product obtains, is subsequent drawing key
Zygonema extra fine filament has established good organization foundation.However, the invention use can produce diameter phi 5- φ 8mm without mould continuous casting technology
Bar, but produce the target blank of major diameter because lacking refining, in filter progress increase bar caused by impurity, hydrogen content height etc.
The risk of defect, and Surface of Rod Bar quality is bad.
Prior art CN105525149A (a kind of preparation method of aluminum alloy sputtering target material) discloses a kind of aluminium alloy and splashes
It shoots at the target the preparation method of material, comprising the following steps: (1) use cold mould magnetic agitation cast aluminium alloy gold ingot casting；(2) aluminium alloy is cast
Ingot carries out part homogenization heat treatment, and material internal is made to form 1-2 μm of diameter of precipitation；(3) ingot casting is subjected to multi-ram forging,
Refine crystal grain；(4) it carries out intermediate annealing process and eliminates forging stress；(5) cold rolling is carried out, crystal grain, enhancing sputtering are further refined
Face { 200 } is orientated content；(6) recrystallization annealing is carried out, obtains splashing with the aluminium alloy of uniform, refinement recrystallization microstructure
It shoots at the target material.The aluminium alloy target crystalline grains obtained by the method for the invention are tiny, and Microstructure Uniformity significantly improves.But it should
Cold mould magnetic agitation cast aluminium alloy gold ingot casting is used in invention, and crystal grain is refined using multi-ram forging, cold rolling and recrystallization annealing
Tissue.Because blank technical process for casting is not known in the invention, the comparison present invention is more advantageous to control molten aluminum using vacuum melting
Ingredient degree of purity and uniformity.
Prior art CN104451566A (a kind of preparation method of rafifinal target) discloses a kind of rafifinal silicon target
Preparation method, it includes the solution treatment of step 1, after rafifinal silicon materials are kept the temperature 2-6 hours at 520-550 DEG C, is taken
Water quenching after out；The rolling of step 2, rafifinal silicon materials cold rolling on milling train by solution treatment, thickness deformation amount are 75-
90%, it is water-cooled in the operation of rolling；The recrystallization annealing of step 3, the rafifinal silicon materials after rolling are in temperature 350-450
1-10 hours are kept the temperature at DEG C.Compared with prior art, the solution have the advantages that: the resulting warp for being higher by aluminium silicon sputtering target material
Size Control is gone through within 60 μm, crystal grain is oriented to random texture, and crystallite dimension and the texture distribution of the sputtering target material are entirely capable of
Meet technique production requirement, the processing is simple, and machined parameters control is reliable.But the invention is tied using solution treatment, rolling and again
Brilliant annealing process refines rafifinal silicon sputtering target material crystallite dimension, and crystal grain is made to be random texture.Not yet explicitly its rafifinal
The preparation method of silicon target blank.
Prior art CN102230098A (a kind of production method of AL-Si system alloy) is a kind of AL-Si system casting aluminium conjunction
Golden production method.Molten aluminum, aluminium ingot are added addition silicon or intermediate alloy melting, remove the gred, remove through 730-760 DEG C of melting in a furnace
Gas obtains the higher aluminum melt of clarity, casts after standing: at 640 ± 20 DEG C, casting rate is control for cast temperature control
Motor speed processed is in 500 ± 20rpm, and in the interior outside of crystallizing wheel, upper and lower sides four direction is passed through cooling water, using 12 on four sides
Region configures cooling water, cooling water temperature: 30 ± 10 DEG C, pressure: 0.3-0.7MPa；The outer cold water flow of cooling water: 40-56m3/
h；Interior cold-zone water flow: 26-35m3/h；Outside cold-zone water flow: 12-18m3/h；Inside cold-zone water flow 11-16m3/h；Casting
After aligned, rolling code, after shearing product.Its production cost is low, and stable product quality and lumber recovery are higher, grain size compared with
It is good, at 1-2 grades.But invention cast molding after Al-Si alloy melt is refined, slag hitting using tyre type Casting Equipment.
Tyre type Casting Equipment is only capable of casting section in 3200mm2Blank below.And target blank sectional area needed for the present invention is greater than
22000mm2, tyre type Casting Equipment cannot achieve the casting of the specification section blank.
Prior art CN104388769A (a kind of high-cleanness, high aluminium silicon intermediate alloy and its production method) provides one kind
High-cleanness, high aluminium silicon intermediate alloy and its production method, are related to contained aluminium-base intermediate alloy technical field.The described method includes: intermediate frequency sense
It answers furnace to melt rafifinal to form molten bath, HIGH-PURITY SILICON is added, form aluminium alloy, the proportion of rafifinal and HIGH-PURITY SILICON after melting completely
According to the mass ratio (5-9) of Al:Si: (1-5) determine: in refining furnace, by inert gas or be vacuum-treated to and tonight into
Row refining is removed the gred with degasification, after the completion of refining, is directly poured, is obtained high-cleanness, high aluminium silicon intermediate alloy product.Height of the invention
Cleanliness aluminium silicon intermediate alloy is by mass percentage containing the silicon of 10-50%, impurity F e≤0.05%, impurity Cu≤0.05%,
Impurity Mn≤0.05%, impurity Zn≤0.05, the content of other single impurity elements are respectively less than 0.03%, other content of impurities
≤ 0.15%, and content≤5ppm of impurities H.But invention configuration aluminium silicon intermediate alloy component is about 10%-50%, is melted
Refining temperature is 1100 ± 10 DEG C.And the high-purity aluminium ingot of melting and silicon select 4N purity.The eutectic point of alusil alloy is 12.5%
Si.When intermediate alloy compositions are higher than eutectic point, there are primary silicon phases in alloy.Primary silicon is acicular texture, is unfavorable for the later period
Ingredient and microstructure homogenization when alloy configures, therefore intermediate alloy component of the present invention is no more than eutectic composition 13%Si.And 4N is pure
It spends aluminium and silicon configuration intermediate alloy micro impurity element Fe, Cu, Mn, Zn equal size is excessively high, about 20-30ppm is not able to satisfy sputtering
The high cleanliness demand of target.
In view of this, the present invention proposes a kind of high-purity alusil alloy sputtering target material blank and preparation method thereof.
Summary of the invention
The purpose of the present invention is to provide a kind of high-purity alusil alloy sputtering target material blank and preparation method thereof, preparation processes
Stablize, by autogamy rafifinal silicon intermediate alloy and intermediate alloy gradation adding technology, control composition degree of purity and homogenization, leads to
Stringent casting parameter designing is crossed, control pieces of bar stock interior tissue is uniform and surface quality is excellent, solves and sputters with high-purity
AL-1wt%Si target blank high cleanliness, ingredient equal control and casting and forming problem.
To achieve the goals above, used technical solution are as follows:
A kind of preparation method of high-purity alusil alloy sputtering target material blank the following steps are included:
(1) by high-purity aluminium and HIGH-PURITY SILICON at 800-850 DEG C vacuum fusion, be configured to silicone content be 7-13wt% centre
Alloy melt；
(2) intermediate alloy melt is cast using semicontinuous casting machine, obtains intermediate alloy；
(3) by high-purity aluminium and intermediate alloy at 730-745 DEG C vacuum fusion, be configured to silicone content be 0.9-1.1wt%
High-purity Al-Si alloy melt；
(4) high-purity Al-Si alloy melt is refined online using high-purity argon gas, high-purity alusil alloy after must refining
Melt；
(5) high-purity Al-Si alloy melt after refining is subjected to on-line filtration, obtains molten aluminum；
(6) molten aluminum is subjected to pieces of bar stock casting using semicontinuous casting machine water cooling, obtains high-purity alusil alloy and splashes
Penetrate target blank.
Further, the purity of the high-purity aluminium is 99.9995wt% or more；
The purity of the HIGH-PURITY SILICON is 99.9999wt% or more.
Further, in the step (1), after the high-purity aluminium is melted and mixed completely with HIGH-PURITY SILICON, 13- is stirred
17min。
Further, in the step (1), after the high-purity aluminium is melted and is mixed completely with HIGH-PURITY SILICON, stirring
15min。
Further, in the step (3), the intermediate alloy of melting is added by several times in the high-purity aluminium of melting.
Further, in the step (3), silicone content is 1.0wt% in high-purity Al-Si alloy melt.
Further, in the step (4), the argon flow is 2-5m3/ min, refining time 20min.
Further, in the step (5), the on-line filtration is double-stage filtering, two pieces of filter plate porositys point
It Wei not 40PPI and 50PPI.
Further, in the step (6), in the blank casting process, temperature of aluminum liquid is 680- in crystallizer
690 DEG C, casting speed 100-120mm/min, cooling water flow 15-20m3/h。
Another object of the present invention is to provide a kind of high-purity alusil alloy sputtering target material blank, which splashes
It penetrates target blank to be prepared by above-mentioned preparation method, impurity content is low, and spatter film forming performance is good.
Compared with prior art, the beneficial effects of the present invention are:
1, the present invention prepares rafifinal silicon using gradation adding technology vacuum melting by autogamy rafifinal silicon intermediate alloy
Alloy is refined online and is solved and sputtered with high-purity using hot top formula semicontinuous casting machine casting pieces of bar stock with bipolar filtering
AL-1wt%Si target blank high cleanliness, ingredient equal control and casting and forming problem.
2, high-purity alusil alloy target blank is sputtered using semi-continuous casting method preparation in the present invention, by casting process
Technology controlling and process alloying component degree of purity and uniformity.Semicontinuous casting technique has excellent degasification, slagging-off effect, makes this technique
It is suitble to big batch metaplasia to produce.
3, autogamy rafifinal silicon intermediate alloy of the present invention and pieces of bar stock is cast into, it can be achieved that intermediate alloy ingredient degree of purity
Control and guarantee alloying component uniformity.Using vacuum melting, online refining and bipolar filtering technique process, it is ensured that casting bar
The defects of batch components are uniformly, impurity micronutrient levels is low and surface is smooth, nothing is mingled with, stomata, shrinkage cavity.
4, the present invention passes through technical flow design, control sputtering impurity content in high-purity alusil alloy target blank
In extremely low level, the wherein alkali metal elements such as Na, K content≤0.2ppm；Contents of heavy metal elements≤the 1ppm such as Fe, Ni；U,Th
Equal radioactive element contents≤0.005ppm；C, the gaseous impurities such as O, N content≤10ppm.The control of trace metal impurities content can
Improve target as sputter filming performance.
5, high-purity alusil alloy sputtering target material blank prepared by the present invention sputters high-purity AL-1wt%Si target blank
Middle micro impurity element content is extremely low, and spatter film forming performance is good.
6, high-purity alusil alloy sputtering target material blank prepared by the present invention, i.e., high-purity AL-1wt%Si target blank ingredient,
Interior tissue is uniform, and Surface of Rod Bar is smooth, without be mingled with, stomata, shrinkage cavity the defects of.
Detailed description of the invention
Fig. 1 is process flow chart of the invention；
Fig. 2 is the micro-organization chart for the intermediate alloy bar that embodiment 1 is cast；
Fig. 3 is the micro-organization chart for high-purity alusil alloy sputtering target material blank that embodiment 1 is cast.
Specific embodiment
In order to which the present invention is further explained, a kind of high-purity alusil alloy sputtering target material blank and preparation method thereof, reaches expected
Goal of the invention, in conjunction with the preferred embodiment, to a kind of high-purity alusil alloy sputtering target material blank proposed according to the present invention and
Preparation method, specific embodiment, structure, feature and its effect, detailed description is as follows.In the following description, different
What " embodiment " or " embodiment " referred to is not necessarily the same embodiment.In addition, special characteristic, knot in one or more embodiments
Structure or feature can be combined by any suitable form.
Before elaborating a kind of high-purity alusil alloy sputtering target material blank of the present invention and preparation method thereof, it is necessary to right
The raw material referred in the present invention and method etc. are described further, to reach better effect.
Major technique key point of the present invention is: 1. using 99.999-99.9995wt% or more purity rafifinal raw material and
99.9999wt% or more purity HIGH-PURITY SILICON prepares rafifinal silicon intermediate alloy through vacuum melting.
2. sputtering the preparation process flow of high-purity alusil alloy target blank.Autogamy rafifinal silicon intermediate alloy.It uses
High-purity alusil alloy is prepared in gradation adding technology vacuum melting, refined online with bipolar filtering, using the hot semicontinuous casting of top formula
Make machine casting pieces of bar stock.
Main protection point is the main preparation process flow and parameter of high-purity alusil alloy target blank:
(1) using the ultrapure aluminum feedstock of 99.999-99.9995wt% purity and 99.9999wt% purity HIGH-PURITY SILICON, vacuum is molten
Refining (800-850 DEG C) prepares the intermediate alloy melt of 7-13wt%Si, i.e. aluminum melt；After high-purity aluminium and HIGH-PURITY SILICON melt completely,
15min or so is stirred, rafifinal silicon intermediate alloy stick is cast using hot top formula semicontinuous casting machine.
(2) using above-mentioned autogamy intermediate alloy and ultrapure aluminum feedstock, (730-745 DEG C) preparation 0.9- of vacuum melting
The high-purity Al-Si alloy melt of 1.1wt%Si.Wherein intermediate alloy uses gradation adding technology, i.e., once addition alloy melting is complete
Heat preservation stands 20min afterwards, uniform by function composite by electromagnetic stirring control composition, carries out secondary intermediate alloy after sampling composition detection and adds
Add.Micro impurity element is in extremely low level in control melt: the alkali metal elements such as Na, K content≤0.2ppm；The huge sum of money such as Fe, Ni
Belong to constituent content≤1ppm；U, the radioactive element contents such as Th≤0.005ppm；C, the gaseous impurities such as O, N content≤10ppm.
(3) it is refined online using high-purity argon gas, refining time 20min, argon flow 2-5m3/min.
(4) molten aluminum on-line filtration is carried out using the bipolar filter device of one piece of 40PPI and one piece of 50PPI porosity.
(5) pieces of bar stock casting is carried out using hot top formula semicontinuous casting machine, obtains high-purity alusil alloy sputtering target
Material blank.Control 680-690 DEG C of mould casting temperature, casting speed 80-100mm/min, cooling water flow 15-20m3/h。
After having understood above method etc., below in conjunction with Fig. 1 and specific embodiment to a kind of rafifinal silicon of the present invention
Alloy sputtering target blank and preparation method thereof is further described in detail:
The technical solution of the present invention is as follows:
(1) 99.9995wt% or more purity rafifinal raw material and 99.9999% or more purity polycrystalline ultrapure raw material: are used
Silicon is alloy raw material.
(2) it configures intermediate alloy: rafifinal and HIGH-PURITY SILICON is melted in vacuum melting furnace, being configured to silicone content is 7-
The intermediate alloy of 13wt%.Control temperature of aluminum liquid is at 800-850 DEG C to ensure that it is complete that polysilicon melts.Molten aluminum makes after melting completely
Molten aluminum 15min is stirred with graphite rotator, controls molten aluminum homogeneity of ingredients, and use semicontinuous casting machine casting alloy stick.
(3) it configures alloy: high-purity aluminium and rafifinal silicon intermediate alloy being melted in vacuum melting furnace, and is configured to silicon and contains
Amount is high-purity alusil alloy of 0.9-1.1wt%.Rafifinal silicon intermediate alloy using twice or repeatedly adding technology, with guarantee at
Divide uniformity.Controlling molten aluminum smelting temperature is 730-745 DEG C.
By autogamy rafifinal silicon intermediate alloy, high-purity alusil alloy is prepared using gradation adding technology vacuum melting, it can
To reduce size of microcrystal, and in alloy the mixing of each ingredient it is more uniform.
(4) it online refining: is refined online using high-purity argon gas, argon flow 2-5m3/ min, refining time 20min.
(5) on-line filtration bipolar filtering: is carried out using one piece of 40PPI and one piece of 50PPI porosity filter plate.
(6) pieces of bar stock is cast: carrying out the casting of φ 120-164mm pieces of bar stock, control using semicontinuous casting machine water cooling
Temperature of aluminum liquid is 680-690 DEG C, casting speed 100-120mm/min, cooling water flow 15-20m in crystallizer3/h。
Specific embodiment is as follows:
Embodiment 1.
Process flow chart as shown in Figure 1, specific steps are as follows:
(1) the ultrapure aluminum feedstock of 99.9995wt% or more purity and 99.9999% or more purity ultrapure raw material: are used
Polysilicon is alloy raw material.
Configuration intermediate alloy: high-purity aluminium and HIGH-PURITY SILICON are put into vacuum melting furnace according to the mass ratio of 88:12 and melted.It is high
Pure silicon feedstock is broken into the addition of powder agglomates shape, to accelerate silicon to melt.
Heat up melting after vacuum melting stove evacuation, and it is 830 DEG C that temperature of aluminum liquid is controlled after aluminium ingot melts completely, heat preservation 1
Hour.Homogenization of composition is carried out using graphite rotator stirring molten aluminum 15min again, obtains intermediate alloy melt.
(2) then intermediate alloy melt is cast using hot top formula casting machine, obtains intermediate alloy bar (its of rafifinal silicon
Microstructure is as shown in Figure 2).
(3) it configures alloy: above-mentioned intermediate alloy bar material is sawn to small bulk.Vacuum melting is added with certain proportion first
Furnace, heat up melting after vacuumizing.
730-745 DEG C of temperature of aluminum liquid is controlled after aluminium ingot melts completely using the static 20min of heat preservation.Sampling carries out 4460 light
Spectrum detection, measuring Si content in molten aluminum is 0.6wt%.Secondary addition intermediate alloy, is repeated once smelting technology, and be measured by sampling
Si content is 0.98wt% in molten aluminum, obtains high-purity Al-Si alloy melt.
(4) online refining: controlling high-purity alusil alloy melt temperature is 735 DEG C, carries out filling aluminium online, uses high-purity argon gas
Online refining, refining time 20min, argon flow 2-5m3/ min, high-purity Al-Si alloy melt after must refining.
(5) bipolar filtering: high-purity Al-Si alloy melt after refining is subjected to on-line filtration, obtains molten aluminum.
On-line filtration uses bipolar plate-type filtering, and two pieces of filter plate porositys are respectively 40PPI and 50PPI.
(6) pieces of bar stock is cast: molten aluminum carries out the casting of φ 120-164mm pieces of bar stock using semicontinuous casting machine water cooling,
Casting process controls in casting machine mold 680-685 DEG C of temperature of aluminum liquid, casting speed 100mm/min, cooling water flow 18-
20m3/ h obtains high-purity alusil alloy sputtering target material blank (its microstructure is as shown in Figure 3).Rafifinal silicon obtained closes
Golden sputtering target material blank surface is smooth, without be mingled with, stomata, shrinkage cavity the defects of.
It is carried out soaking, forging, rolling and recrystallization annealing is passed through behind this high-purity alusil alloy sputtering target material blank milling face
Microcosmic grain structure refines (mean grain size≤60 μm).
Fig. 2 show the intermediate alloy bar of casting, i.e. AL-12%Si rafifinal silicon intermediate alloy microstructure (50X),
White Primary α-Al Phase is evenly distributed in al-si eutectic tissue.
Fig. 3 show high-purity alusil alloy sputtering target material blank of casting, i.e. AL-1%Si target blank microstructure
(25X), casting ingot mean grain size 1.5-2.5mm.
High-purity alusil alloy sputtering target material blank sampling of preparation is subjected to impurity content detection (GDMS), testing number
According to as shown in table 1.
1 part of impurity elements content of table counts (GDMS detection)
| Element | Content/ppm | Element | Content/ppm | Element | Content/ppm | Element | Content/ppm |
| Na | 0.072 | K | < 0.05 | Mg | 0.066 | Fe | 0.72 |
| Ni | 0.19 | Cu | 0.62 | U | <0.005 | Th | <0.005 |
As shown in Table 1, impurity content is extremely low.
Embodiment 2.
Process flow chart as shown in Figure 1, specific steps are as follows:
(1) the ultrapure aluminum feedstock of 99.9995wt% or more purity and 99.9999% or more purity ultrapure raw material: are used
Polysilicon is alloy raw material.
Configuration intermediate alloy: high-purity aluminium and HIGH-PURITY SILICON are put into vacuum melting furnace according to the mass ratio of 93:7.HIGH-PURITY SILICON
Raw material is broken into powder agglomates shape and is added to accelerate silicon to melt.
Heat up melting after vacuum melting stove evacuation, and it is 800 DEG C that temperature of aluminum liquid is controlled after aluminium ingot melts completely, heat preservation 1
Hour.Homogenization of composition is carried out using graphite rotator stirring molten aluminum 13min again, obtains intermediate alloy melt.
(2) then intermediate alloy melt is cast using hot top formula casting machine, obtains rafifinal silicon and obtains intermediate alloy bar.
(3) it configures alloy: above-mentioned intermediate alloy bar material is sawn to small bulk.Vacuum melting is added with certain proportion first
Furnace, heat up melting after vacuumizing.
730-745 DEG C of temperature of aluminum liquid is controlled after aluminium ingot melts completely using the static 20min of heat preservation.Sampling carries out 4460 light
Spectrum detection, measuring Si content in molten aluminum is 0.4wt%.Secondary addition intermediate alloy, is repeated once smelting technology, and be measured by sampling
Si content is 0.91wt% in molten aluminum, obtains high-purity Al-Si alloy melt.
(4) online refining: controlling high-purity alusil alloy melt temperature is 730 DEG C, carries out filling aluminium online, uses high-purity argon gas
Online refining, refining time 20min, argon flow 2-5m3/ min, high-purity Al-Si alloy melt after must refining.
(5) bipolar filtering: high-purity Al-Si alloy melt after refining is subjected to on-line filtration, obtains molten aluminum.
On-line filtration uses bipolar plate-type filtering, and two pieces of filter plate porositys are respectively 40PPI and 50PPI.
(6) pieces of bar stock is cast: molten aluminum carries out the casting of φ 120-164mm pieces of bar stock using semicontinuous casting machine water cooling,
Casting process controls in casting machine mold 685-690 DEG C of temperature of aluminum liquid, casting speed 120mm/min, cooling water flow 15-
18m3/ h obtains high-purity alusil alloy sputtering target material blank.High-purity alusil alloy sputtering target material blank surface light obtained
It is sliding, without be mingled with, stomata, shrinkage cavity the defects of.
It is carried out soaking, forging, rolling and recrystallization annealing is passed through behind this high-purity alusil alloy sputtering target material blank milling face
Microcosmic grain structure refines (mean grain size≤60 μm).
Embodiment 3.
Process flow chart as shown in Figure 1, specific steps are as follows:
(1) the ultrapure aluminum feedstock of 99.9995wt% or more purity and 99.9999% or more purity ultrapure raw material: are used
Polysilicon is alloy raw material.
Configuration intermediate alloy: high-purity aluminium and HIGH-PURITY SILICON are put into vacuum melting furnace according to the mass ratio of 87:13.HIGH-PURITY SILICON
Raw material is broken into powder agglomates shape and is added to accelerate silicon to melt.
Heat up melting after vacuum melting stove evacuation, and it is 850 DEG C that temperature of aluminum liquid is controlled after aluminium ingot melts completely, heat preservation 1
Hour.Homogenization of composition is carried out using graphite rotator stirring molten aluminum 17min again, obtains intermediate alloy melt.
(2) then intermediate alloy melt is cast using hot top formula casting machine, obtains the intermediate alloy bar of rafifinal silicon.
(3) it configures alloy: above-mentioned intermediate alloy bar material is sawn to small bulk.Vacuum melting is added with certain proportion first
Furnace, heat up melting after vacuumizing.
730-745 DEG C of temperature of aluminum liquid is controlled after aluminium ingot melts completely using the static 20min of heat preservation.Sampling carries out 4460 light
Spectrum detection, measuring Si content in molten aluminum is 0.7wt%.Secondary addition intermediate alloy, is repeated once smelting technology, and be measured by sampling
Si content is 0.94wt% in molten aluminum.A small amount of intermediate alloy is added three times, is repeated once smelting technology, and molten aluminum is measured by sampling
Middle Si content is that 1.1wt%. obtains high-purity Al-Si alloy melt.
(4) online refining: controlling high-purity alusil alloy melt temperature is 732 DEG C, carries out filling aluminium online, uses high-purity argon gas
Online refining, refining time 20min, argon flow 2-5m3/ min, high-purity Al-Si alloy melt after must refining.
(5) bipolar filtering: high-purity Al-Si alloy melt after refining is subjected to on-line filtration, obtains molten aluminum.
On-line filtration uses bipolar plate-type filtering, and two pieces of filter plate porositys are respectively 40PPI and 50PPI.
(6) pieces of bar stock is cast: molten aluminum carries out the casting of φ 120-164mm pieces of bar stock using semicontinuous casting machine water cooling,
Casting process controls in casting machine mold 680-685 DEG C of temperature of aluminum liquid, casting speed 110mm/min, cooling water flow 18-
20m3/ h obtains high-purity alusil alloy sputtering target material blank.High-purity alusil alloy sputtering target material blank surface light obtained
It is sliding, without be mingled with, stomata, shrinkage cavity the defects of.
It is carried out soaking, forging, rolling and recrystallization annealing is passed through behind this high-purity alusil alloy sputtering target material blank milling face
Microcosmic grain structure refines (mean grain size≤60 μm).
A kind of high-purity alusil alloy sputtering target material blank of the present invention and preparation method thereof, using the raw material of high-purity
Prepare rafifinal silicon intermediate alloy；Cooperate function composite by electromagnetic stirring using vacuum melting furnace, using intermediate alloy gradation adding technology
Alloying component uniformity is controlled, and prepares high-purity AL-1wt%Si alloy target material blank using semicontinuous casting technique, makes product
Micro impurity element content it is extremely low, spatter film forming performance is good, and ingredient, interior tissue are uniform, and Surface of Rod Bar is smooth, no folder
The defects of miscellaneous, stomata, shrinkage cavity.
The above is only the preferred embodiment of the embodiment of the present invention, not makees any shape to the embodiment of the present invention
Limitation in formula, any simple modification to the above embodiments of technical spirit according to an embodiment of the present invention, equivalent variations
With modification, in the range of still falling within technical solution of the embodiment of the present invention.
Claims (10)
1. a kind of preparation method of high-purity alusil alloy sputtering target material blank, which comprises the following steps:
(1) by high-purity aluminium and HIGH-PURITY SILICON at 800-850 DEG C vacuum fusion, be configured to silicone content be 7-13wt% intermediate alloy
Melt；
(2) intermediate alloy melt is cast using semicontinuous casting machine, obtains intermediate alloy；
(3) by high-purity aluminium and intermediate alloy at 730-745 DEG C vacuum fusion, be configured to silicone content be 0.9-1.1wt% height
Pure Al-Si alloy melt；
(4) high-purity Al-Si alloy melt is refined online using high-purity argon gas, high-purity Al-Si alloy melt after must refining；
(5) high-purity Al-Si alloy melt after refining is subjected to on-line filtration, obtains molten aluminum；
(6) molten aluminum is subjected to pieces of bar stock casting using semicontinuous casting machine water cooling, obtains high-purity alusil alloy sputtering target
Material blank.
2. preparation method according to claim 1, which is characterized in that
The purity of the high-purity aluminium is 99.9995wt% or more；
The purity of the HIGH-PURITY SILICON is 99.9999wt% or more.
3. preparation method according to claim 1, which is characterized in that
In the step (1), after the high-purity aluminium is melted and mixed completely with HIGH-PURITY SILICON, 13-17min is stirred.
4. preparation method according to claim 3, which is characterized in that
In the step (1), after the high-purity aluminium is melted and mixed completely with HIGH-PURITY SILICON, 15min is stirred.
5. preparation method according to claim 1, which is characterized in that
In the step (3), the intermediate alloy of melting is added by several times in the high-purity aluminium of melting.
6. preparation method according to claim 1, which is characterized in that
In the step (3), silicone content is 1.0wt% in high-purity Al-Si alloy melt.
7. preparation method according to claim 1, which is characterized in that
In the step (4), the argon flow is 2-5m3/ min, refining time 20min.
8. preparation method according to claim 1, which is characterized in that
In the step (5), the on-line filtration is double-stage filtering, two pieces of filter plate porositys be respectively 40PPI with
50PPI。
9. preparation method according to claim 1, which is characterized in that
In the step (6), in the blank casting process, temperature of aluminum liquid is 680-690 DEG C in crystallizer, casting speed
100-120mm/min, cooling water flow 15-20m3/h。
10. a kind of high-purity alusil alloy sputtering target material blank, which is characterized in that high-purity alusil alloy sputtering target material blank is adopted
It is prepared with any one of claim 1-9 preparation method.
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