CN109518140A - A kind of preparation method of ultra-pure, isometric fine grain aluminium target - Google Patents
A kind of preparation method of ultra-pure, isometric fine grain aluminium target Download PDFInfo
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- CN109518140A CN109518140A CN201811437850.2A CN201811437850A CN109518140A CN 109518140 A CN109518140 A CN 109518140A CN 201811437850 A CN201811437850 A CN 201811437850A CN 109518140 A CN109518140 A CN 109518140A
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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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B21/00—Obtaining aluminium
- C22B21/06—Obtaining aluminium refining
-
- 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
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
Abstract
The invention belongs to materials processing technology fields, and in particular to a kind of preparation method of ultra-pure, isometric fine grain aluminium target.Preparation method of the invention, it is combined using vacuum casting and forging rolling, semiconductor chip is prepared with ultra-pure, isometric fine grain sputtered aluminum target at room temperature with cold rolling and heat-treating methods in 99.9999% or more high-purity aluminium ingot progress remelting molding to purity in vacuum induction melting furnace.The preparation method further decreases the crystallite dimension of high-purity aluminium ingot to 1mm or less by carrying out remelting to high-purity aluminium ingot, greatly simplify later period plastic deformation process, raising is become a useful person efficiency, reduce production cost, it is finally obtained it is ultra-pure, its grain size of isometric fine grain aluminium target is uniform, and be maintained at 100 μm or less.
Description
Technical field
The invention belongs to materials processing technology fields, and in particular to a kind of preparation side of ultra-pure, isometric fine grain aluminium target
Method.
Background technique
Method one of of the magnetron sputtering plating as physical vapor deposition coating film, is widely used in Electronic Components Manufacturing
Manufacturing field, such as semiconductor integrated circuit, flat-panel screens and recording medium industry.Compared with other plated film modes,
High with institute's film plating layer hardness, film performance is stablized, the advantages such as wear-corrosion resistance height.Splash-proofing sputtering metal target is magnetron sputtering
One of main raw material(s) of plated film, maximum in the high-end production of electronic components field dosage such as semiconductor is ultra-pure aluminum target.
In the case where guaranteeing the identical situation of magnetron sputtering technique, the crystal grain of target is more tiny, is orientated more uniform, magnetron sputtering mistake
Cheng Zhong, sputter rate is faster, and the resulting film quality of sputtering sedimentation is higher.But by the special solidification property institute of superpure metal
Fixed, metal purity is higher, hinders the chicken extract of grain growth fewer, and the probability of heterogeneous forming core is lower in process of setting, leads to crystal grain
Overgrowth.Usual 99.999%~99.9999% ultra-pure aluminium ingot passes through impurity member in control aluminium ingot as obtained by segregation method
The segregation efficiency of element improves the purity of aluminium ingot.But it is excessively coarse by ultra-pure aluminium ingot crystallite dimension that the method obtains, it reaches
It is maximum up to 10cm or more to a centimetre rank.This grain size is far from satisfying the crystallite dimension of magnetic control spattering target
It is required that the standard lower than 200um.
Currently, being directed to the preparation method of the isometric fine grain sputtered aluminum target of ultra-pure aluminum, many researchs have been done both at home and abroad, wherein
Reaching rafifinal crystal grain refinement by plastic deformation process is more common and effective method, and such as: multiway forging method is delivered crowded
Platen press and accumulative folded hypodesmus etc., make annealing treatment material with after plastic deformation, then reach the crystalline substance of needs in a manner of crystallization
Grain size.Currently, being directed to the preparation of ultra-pure aluminum ultrafine grain sputtering target both at home and abroad, there is patent CN101638760A, uses
Ultra-pure aluminum plate is placed in after equal channel angular pressurization grinding tool carries out extrusion process and carried out cold treatment in a large amount of liquid nitrogen again；
Also there is CN 10200253A to be plastically deformed using the method for multidirectional open die forging to aluminium ingot, then carry out cold rolling at 0-5 DEG C, from
And reach the method for refinement crystal grain.Above method, which has complex process, high production cost and crystal grain refinement size, to protect
The problem of 100 μm of card or less is uniformly distributed.
Summary of the invention
Based on problem above, the object of the present invention is to provide a kind of preparation method of ultra-pure, isometric fine grain aluminium target, institutes
Target is stated suitable for semiconductor chip, preparation method can by ultra-pure aluminum crystal grain stability contorting at 100 μm hereinafter, and improving
Efficiency of becoming a useful person, reduces production cost.
The technical solution of the present invention is as follows:
The present invention provides a kind of preparation method of ultra-pure, isometric fine grain aluminium target, comprising the following steps:
(1) remelting: the rafifinal ingot surface that purity is 99.9999% or more is subjected to molten pre-treatment, it is ensured that described high-purity
Aluminium ingot surface oxide-free, impurity etc., are subsequently placed in vacuum refusion in the stove, and high-purity molten aluminum is obtained after being completely melt；
(2) double teeming: high-purity molten aluminum being cast in ingot mould and carries out double teeming, in cooling procedure to high-purity molten aluminum
Electromagnetic agitation is carried out, the high-purity aluminium ingot of new mint is obtained after double teeming；
(3) make annealing treatment: by the high-purity aluminium ingot of the new mint 200-400 DEG C heat preservation 20-50 hours, then make the new mint
High-purity aluminium ingot is cooling with room temperature, further refines crystal grain；
(4) it forges and presses: the new mint rafifinal ingot surface after annealing is handled, it is ensured that surface oxide-free,
Then free from admixture, any surface finish carry out forging and stamping processing；
(5) roll: will forging and stamping treated that the high-purity aluminium ingot of the new mint carries out rolling process；
(6) the high-purity aluminium ingot of the new mint after rolling process is subjected to heat preservation cooling treatment, crystallite dimension is made less than 100
μm equiax crystal ultra-pure aluminum.
The preparation method of ultra-pure, isometric fine grain aluminium target according to the present invention, in step (1), the temperature in vacuum furnace
It is 680-800 DEG C, vacuum degree 3.8x10-2~1.7x10-4, the vacuum degree and refusion in the stove temperature obtain founding new
The crystallite dimension control cast in high-purity aluminium ingot has a direct impact, and the in-furnace temperature and vacuum degree can guarantee in the high-purity aluminium ingot of new mint
Crystallite dimension in 1mm or less.
The preparation method of ultra-pure, isometric fine grain aluminium target according to the present invention, in step (2), high-purity molten aluminum
After pouring into aluminium ingot completely, processing is rapidly cooled to aluminium ingot and high-purity molten aluminum with cooling water, is also beneficial to reduce described new
The crystallite dimension of high-purity aluminium ingot is cast to 1mm or less.
The preparation method of ultra-pure, isometric fine grain aluminium target according to the present invention, in step (2), high-purity molten aluminum
It after temperature reaches 690-720 DEG C, pours into ingot mould, electromagnetic agitation is carried out to high-purity molten aluminum in cooling procedure, to described
Crystallite dimension control has direct contribution in 1mm or less in the high-purity aluminium ingot of new mint.
The preparation method of ultra-pure, isometric fine grain aluminium target according to the present invention, in step (4), first by the new mint
High-purity aluminium ingot is forged and pressed respectively along X, Y cross-sectional direction, then is forged and pressed along Z-direction；
The preparation method of ultra-pure, isometric fine grain aluminium target according to the present invention, in step (5), rolling temperature 23-
28 DEG C, rolling number is 5-30 times.Above step (4), forging and stamping sequence, direction and the rolling temperature of (5), number combine, and make crystalline substance
Grain more refines, and granularity is more uniform.
The preparation method of ultra-pure, isometric fine grain aluminium target according to the present invention, through step (4), (5) forging and stamping and rolling
The deformation total amount of the high-purity aluminium ingot of the new mint after reason is 25-70%, and the control parameter of total deformation is also and in final target
Crystal grain refinement Chengdu and homogeneity are directly related.
The preparation method of ultra-pure, isometric fine grain aluminium target according to the present invention, in step (6), holding temperature is
120-300 DEG C, soaking time 30-200min, the setting of the cooling heat treatment parameter of the above heat preservation guarantees the thin of manager's size
Change and homogeneous grain diameter.
The invention has the benefit that
The preparation method of ultra-pure, isometric fine grain aluminium target of the invention is combined using vacuum casting and forging rolling, in vacuum
Remelting molding is carried out in 99.9999% or more high-purity aluminium ingot to purity in induction melting furnace, at room temperature with cold rolling and Re Chu
The method of reason prepares semiconductor chip with ultra-pure, isometric fine grain sputtered aluminum target.The preparation method passes through to high-purity
Aluminium ingot carries out remelting and further decreases the crystallite dimension of high-purity aluminium ingot to 1mm hereinafter, greatly simplifying later period plastic deformation process, mentions
Height is become a useful person efficiency, reduces production cost, it is finally obtained it is ultra-pure, its grain size of isometric fine grain aluminium target is uniform, and keep
At 100 μm or less.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the polarisation tissue of ultra-pure, isometric fine grain aluminium target made from preparation method of the invention；
Fig. 2 is the forging and stamping schematic diagram of X described in step (4) and Y-direction in preparation method of the invention；
Fig. 3 is the forging and stamping schematic diagram of Z-direction described in step (4) in preparation method of the invention.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be carried out below
Detailed description.Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art are obtained all without making creative work
Other embodiment belongs to the range that the present invention is protected.
Embodiment 1
The present invention provides a kind of preparation method of ultra-pure, isometric fine grain aluminium target, comprising the following steps:
(1) remelting: the rafifinal ingot surface that purity is 99.9999% or more is subjected to molten pre-treatment, it is ensured that described high-purity
Aluminium ingot surface oxide-free, impurity etc. are subsequently placed in vacuum refusion in the stove, and in-furnace temperature is 680 DEG C, vacuum degree 1.7x10-4,
High-purity molten aluminum is obtained after being completely melt；
(2) double teeming: high-purity molten aluminum that the temperature reaches 690 DEG C being cast in ingot mould and carries out double teeming, the rafifinal
After liquid pours into aluminium ingot completely, processing is rapidly cooled to aluminium ingot and high-purity molten aluminum with cooling water, in cooling procedure to institute
It states high-purity molten aluminum and carries out electromagnetic agitation, the high-purity aluminium ingot of new mint is obtained after double teeming, the crystallite dimension of the high-purity aluminium ingot of new mint is in 1mm
Below；
(3) it makes annealing treatment: the high-purity aluminium ingot of the new mint being kept the temperature 20 hours at 400 DEG C, then makes the new mint rafifinal
Ingot is cooling with room temperature, further refines crystal grain；
(4) it forges and presses: the new mint rafifinal ingot surface after annealing is handled, it is ensured that surface oxide-free,
Then free from admixture, any surface finish carry out forging and stamping processing, specifically: first by the high-purity aluminium ingot of the new mint along X, Y cross-sectional direction point
It is not forged and pressed, then is forged and pressed along Z-direction, as shown in Figure 2,3；
(5) roll: will forging and stamping treated that the high-purity aluminium ingot of the new mint carries out rolling process, rolling temperature is 28 DEG C, is rolled
Number processed is 5 times；After the completion of rolling, the deformation total amount of the high-purity aluminium ingot of new mint is 25%；
(6) the high-purity aluminium ingot of the new mint after rolling process is subjected to heat preservation cooling treatment, holding temperature is 300 DEG C, is protected
The warm time is 30min, and equiax crystal ultra-pure aluminum of the crystallite dimension less than 100 μm is made.
Embodiment 2
The present invention provides a kind of preparation method of ultra-pure, isometric fine grain aluminium target, comprising the following steps:
(1) remelting: the rafifinal ingot surface that purity is 99.9999% or more is subjected to molten pre-treatment, it is ensured that described high-purity
Aluminium ingot surface oxide-free, impurity etc. are subsequently placed in vacuum refusion in the stove, and in-furnace temperature is 800 DEG C, vacuum degree 3.8x10-,
High-purity molten aluminum is obtained after being completely melt；
(2) double teeming: high-purity molten aluminum that the temperature reaches 720 DEG C being cast in ingot mould and carries out double teeming, the rafifinal
After liquid pours into aluminium ingot completely, processing is rapidly cooled to aluminium ingot and high-purity molten aluminum with cooling water, in cooling procedure to institute
It states high-purity molten aluminum and carries out electromagnetic agitation, the high-purity aluminium ingot of new mint is obtained after double teeming, the crystallite dimension of the high-purity aluminium ingot of new mint is in 1mm
Below；
(3) it makes annealing treatment: the high-purity aluminium ingot of the new mint being kept the temperature 50 hours at 200 DEG C, then makes the new mint rafifinal
Ingot is cooling with room temperature, further refines crystal grain；
(4) it forges and presses: the new mint rafifinal ingot surface after annealing is handled, it is ensured that surface oxide-free,
Then free from admixture, any surface finish carry out forging and stamping processing, specifically: first by the high-purity aluminium ingot of the new mint along X, Y cross-sectional direction point
It is not forged and pressed, then is forged and pressed along Z-direction, as shown in Figure 2,3；
(5) roll: will forging and stamping treated that the high-purity aluminium ingot of the new mint carries out rolling process, rolling temperature is 23 DEG C, is rolled
Number processed is 30 times；After the completion of rolling, the deformation total amount of the high-purity aluminium ingot of new mint is 70%；
(6) the high-purity aluminium ingot of the new mint after rolling process is subjected to heat preservation cooling treatment, holding temperature is 1200 DEG C, is protected
The warm time is 200min, and equiax crystal ultra-pure aluminum of the crystallite dimension less than 100 μm is made.
Embodiment 3
The present invention provides a kind of preparation method of ultra-pure, isometric fine grain aluminium target, comprising the following steps:
(1) remelting: the rafifinal ingot surface that purity is 99.9999% or more is subjected to molten pre-treatment, it is ensured that described high-purity
Aluminium ingot surface oxide-free, impurity etc. are subsequently placed in vacuum refusion in the stove, and in-furnace temperature is 750 DEG C, vacuum degree 3.5x10-3,
High-purity molten aluminum is obtained after being completely melt；
(2) double teeming: high-purity molten aluminum that the temperature reaches 710 DEG C being cast in ingot mould and carries out double teeming, the rafifinal
After liquid pours into aluminium ingot completely, processing is rapidly cooled to aluminium ingot and high-purity molten aluminum with cooling water, in cooling procedure to institute
It states high-purity molten aluminum and carries out electromagnetic agitation, the high-purity aluminium ingot of new mint is obtained after double teeming, the crystallite dimension of the high-purity aluminium ingot of new mint is in 1mm
Below；
(3) it makes annealing treatment: the high-purity aluminium ingot of the new mint being kept the temperature 40 hours at 300 DEG C, then makes the new mint rafifinal
Ingot is cooling with room temperature, further refines crystal grain；
(4) it forges and presses: the new mint rafifinal ingot surface after annealing is handled, it is ensured that surface oxide-free,
Then free from admixture, any surface finish carry out forging and stamping processing, specifically: first by the high-purity aluminium ingot of the new mint along X, Y cross-sectional direction point
It is not forged and pressed, then is forged and pressed along Z-direction, as shown in Figure 2,3；
(5) roll: will forging and stamping treated that the high-purity aluminium ingot of the new mint carries out rolling process, rolling temperature is 25 DEG C, is rolled
Number processed is 20 times；After the completion of rolling, the deformation total amount of the high-purity aluminium ingot of new mint is 40%；
(6) the high-purity aluminium ingot of the new mint after rolling process is subjected to heat preservation cooling treatment, holding temperature is 200 DEG C, is protected
The warm time is 100min, and equiax crystal ultra-pure aluminum of the crystallite dimension less than 100 μm is made.
Figure of description part, Fig. 1 show ultra-pure, isometric fine grain aluminium target made from preparation method of the invention
Polarisation tissue, it can be seen that crystallite dimension therein is respectively less than 100 μm, and epigranular.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (10)
1. a kind of preparation method of ultra-pure, isometric fine grain aluminium target, which comprises the following steps:
(1) remelting: high-purity aluminium ingot is placed in vacuum refusion in the stove, high-purity molten aluminum is obtained after being completely melt；
(2) double teeming: high-purity molten aluminum being cast in ingot mould and carries out double teeming, is carried out in cooling procedure to high-purity molten aluminum
Electromagnetic agitation obtains the high-purity aluminium ingot of new mint after double teeming；
(3) it makes annealing treatment: cooling with room temperature by the high-purity aluminium ingot of the new mint after 200-400 DEG C of heat preservation；
(4) it forges and presses: the high-purity aluminium ingot of the new mint after annealing is subjected to forging and stamping processing；
(5) roll: will forging and stamping treated that the high-purity aluminium ingot of the new mint carries out rolling process；
(6) the high-purity aluminium ingot of the new mint after rolling process is subjected to heat preservation cooling treatment, crystallite dimension is made less than 100 μm
Equiax crystal ultra-pure aluminum.
2. preparation method according to claim 1, which is characterized in that in step (1), the temperature in vacuum furnace 680-
800 DEG C, vacuum degree 3.8x10-2~1.7x10-4。
3. preparation method according to claim 1, which is characterized in that in step (2), high-purity molten aluminum pours into completely
After in aluminium ingot, processing is rapidly cooled to aluminium ingot and high-purity molten aluminum with cooling water.
4. preparation method according to claim 1, which is characterized in that in step (2), high-purity temperature of aluminum liquid reaches
It after 690-720 DEG C, pours into ingot mould, electromagnetic agitation is carried out to high-purity molten aluminum in cooling procedure.
5. preparation method according to claim 1, which is characterized in that is obtained after step (2) double teeming processing is described new
The crystallite dimension cast in high-purity aluminium ingot is less than 1mm.
6. preparation method according to claim 1, which is characterized in that in step (3), soaking time is 20-50 hours.
7. preparation method according to claim 1, which is characterized in that in step (4), first by the high-purity aluminium ingot of the new mint
It is forged and pressed along X, Y cross-sectional direction, then is forged and pressed along Z-direction respectively.
8. preparation method according to claim 1, which is characterized in that in step (5), rolling temperature is 23-28 DEG C, is rolled
Number processed is 5-30 times.
9. preparation method according to claim 1, which is characterized in that after step (4), (5) forging and stamping and rolling process
The deformation total amount of the high-purity aluminium ingot of new mint is 25-70%.
10. preparation method according to claim 1, which is characterized in that in step (6), holding temperature 120-300
DEG C, soaking time 30-200min.
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| CN110484874A (en) * | 2019-08-16 | 2019-11-22 | 韶关市欧莱高新材料有限公司 | A kind of preparation method of high-purity aluminum pipe sputtering target material |
| CN111318570A (en) * | 2020-03-05 | 2020-06-23 | 爱发科电子材料（苏州）有限公司 | Process for manufacturing micronized target material crystal grains |
| CN111590279A (en) * | 2020-06-03 | 2020-08-28 | 福建阿石创新材料股份有限公司 | High-purity metal rotary target material and preparation method thereof |
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| CN111590279A (en) * | 2020-06-03 | 2020-08-28 | 福建阿石创新材料股份有限公司 | High-purity metal rotary target material and preparation method thereof |
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