CN104419901B - A kind of manufacture method of tantalum target - Google Patents
A kind of manufacture method of tantalum target Download PDFInfo
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- CN104419901B CN104419901B CN201310379942.0A CN201310379942A CN104419901B CN 104419901 B CN104419901 B CN 104419901B CN 201310379942 A CN201310379942 A CN 201310379942A CN 104419901 B CN104419901 B CN 104419901B
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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
- 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
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- 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
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
-
- 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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
Abstract
The invention provides a kind of manufacture method of tantalum target.Including, hot forging treatment first is carried out to tantalum ingot, the tantalum ingot after processing the hot forging afterwards carries out an annealing process, forms the first tantalum target blank；Rolling process is carried out to the first tantalum target blank, the second tantalum target blank is formed；Double annealing technique is carried out to the second tantalum target blank, tantalum target is obtained.Tiny, the tantalum target consistent internal structure using above-mentioned technical proposal formation tantalum target internal grain, is prevented effectively from tantalum target inside and the defects such as layering occurs, so that during improving follow-up use, the sputter rate of tantalum target, and the tantalum films quality for being formed.
Description
Technical field
The present invention relates to semiconductor sputtering field, more particularly to a kind of manufacture method of tantalum target.
Background technology
Tantalum, is a kind of metallic element, and its quality is hard, be rich in ductility, and thermal coefficient of expansion very little, is resisted with high
Corrosivity and toughness.Based on above-mentioned advantage, tantalum is widely used the industrial circle such as chemical industry, microelectronics, electric.
Such as in microelectronic, tantalum is often used to prepare the membrane electrode and interconnection line of semiconductor devices.
Specifically, tantalum is applied to semiconductor devices preparation by magnetron sputtering mode.Its principle is heavy using physical vapor
Product technology（PVD）, gas ion bombardment tantalum target is accelerated with high pressure, it is sputtered out the tantalum atom on tantalum target, with film
Form is deposited on silicon chip, forms interconnecting construction or electrode on semiconductor chip.Wherein, the quality of tantalum target is directly affected
The film quality that magnetron sputtering is formed.
Traditional tantalum target preparation process includes：First pass through high vacuum electron beam smelting furnace and obtain High-purity Tantalum ingot, it is then right
Tantalum ingot is repeated plastic deformation, so as to obtain the tantalum target of specific dimensions.
However, being limited to tantalum bcc metals structure in itself, the solid matter face of tantalum crystal grain is 111 type cell configurations,
In plastic history, 111 type cell configurations of tantalum crystal grain can cause that sliding, tantalum crystal grain prototype structure preferentially occurs in tantalum intercrystalline
It is difficult to by double teeming, deformation ratio is relatively low, so that the crystal grain orientation inside the tantalum target for ultimately forming still is with 111 forms
It is main.This kind of structure belongs to " intrinsic " taeniae telarum of tantalum metal.Thus after the operation of rolling of plasticity, the tantalum target of acquisition is along thickness
Direction has serious texture lamination defect.And drawbacks described above is based on, and in magnetron sputtering process, the sputter rate of tantalum target
It is relatively low and extremely unstable, can change with the change of tantalum target inside texture, so that the tantalum for seriously reducing follow-up acquisition is thin
The uniformity of film.
With developing rapidly for semiconductor devices, the requirement for tantalum plated film is strict all the more.In order to solve inside tantalum target
Lamination defect, industry personnel are attempted that tantalum is realized plastic deformation under recrystallization temperature conditions above, are reduced in tantalum ingot with this
Portion's resistance of deformation.But the recrystallization temperature based on tantalum reaches 800 DEG C, above-mentioned technique for the requirement of the process equipments such as equipment of hot rolling
Height, and operation difficulty is big, the yield rate of tantalum target is low.
Therefore, how to reduce the resistance of deformation inside when tantalum ingot is plastically deformed, the deformation rate of its internal material is increased, so that
While eliminating tantalum target interior laminate layer phenomenon, technology difficulty and process costs are reduced, improve the yield rate of tantalum target, be ability
The problem of field technique personnel's urgent need to resolve.
The content of the invention
To solve the above problems, the invention provides a kind of manufacture method of tantalum target, so as to overcome existing tantalum target system
During making, the deformation ratio inside tantalum ingot is low, the defect such as the tantalum target interior laminate layer phenomenon of acquisition is serious.
A kind of manufacture method of tantalum target that the present invention is provided, including：
Tantalum ingot is provided；
Hot forging treatment is carried out to the tantalum ingot, an annealing process is carried out to the tantalum ingot afterwards, the first tantalum target is formed
Blank；
Rolling process is carried out to the first tantalum target blank, the second tantalum target blank is formed；
Double annealing technique is carried out to the second tantalum target blank, tantalum target is obtained.
Alternatively, the hot forging treatment includes：
The tantalum ingot is heated to 800~1100 DEG C, afterwards the tantalum ingot is carried out forging treatment；
It is once described to forge treatment and include at least forging the tantalum ingot along both direction, and once described forge place
Tantalum ingot shape variable after reason is more than or equal to 80%.
Alternatively, hot forging treatment at least includes forging treatment described in 3 times.
Alternatively, the once annealing includes：
Regulation vacuum heat furnace temperature heats 2~4h of the tantalum ingot under vacuum to 1000~1300 DEG C.
Alternatively, the hot forging is repeated to process at least 3 times, carried out once after the treatment of hot forging each time it is described once
Annealing process.
Alternatively, the rolling process is cold-rolling treatment, including：
Cool down the first tantalum target blank；
Along the first tantalum target blank described in different directions repeat-rolling to predetermined thickness, the second tantalum target blank, institute are formed
The deformation quantity for stating the first tantalum target blank is more than 90%.
Alternatively, the rolling process includes：
First stage rolling is carried out to the first tantalum target blank, the deformation quantity for making the first tantalum target blank is
40%~60%；
After first stage rolling, second stage rolling is carried out to the first tantalum target blank, to first tantalum target
The deformation quantity of blank is 70%~80%；
After second stage rolling, phase III rolling is carried out to the first tantalum target blank, to first tantalum target
The deformation quantity of blank is more than or equal to 90%；
After phase III rolling, fourth stage rolling is carried out to the first tantalum target blank, to predetermined thickness.
Alternatively, rolled including multistep during rolling, second stage rolling and phase III rolling in the first stage
Step processed；
Wherein, in rolling in the first stage, the deformation quantity of the first tantalum target blank after each step rolling is step rolling
Preceding 10%~25%；
In second stage rolling, the deformation quantity of the first tantalum target blank after each step rolling is before the step is rolled
10%~20%；
In the phase III rolls, the deformation quantity of the first tantalum target blank after each step rolling is before the step is rolled 8%
~13%；
In fourth stage rolling, the deformation quantity of the first tantalum target blank after each step rolling is before the step is rolled 3%
~7%.
Alternatively, after rolling each time, 120 °~140 ° of the first tantalum target blank is rotated, afterwards, to described first
Tantalum target blank is rolled next time.
Alternatively, the double annealing treatment includes：
Regulation vacuum heat furnace temperature heats 1~3h of tantalum ingot under vacuum to 800~1000 DEG C.
Compared with prior art, technical scheme has advantages below：
In hot forging processing procedure is carried out to tantalum ingot, tantalum ingot is carried out forging treatment under the high temperature conditions, can be effectively increased
Deformation ratio inside tantalum ingot, the original crystal phase structure of tantalum crystal grain in destruction tantalum ingot, while realizing tantalum crystal miniaturization；And at hot forging
In an annealing process after reason, realize that tantalum is recrystallized, make that tantalum is intercrystalline to be bonded and reset, so as to realize tantalum ingot internal junction
Structure is homogenized, it is to avoid occur the defects such as structural stratification inside tantalum ingot；Simultaneously in an annealing process, can also fully discharge and be based on
Hot forging processes the stress produced inside tantalum ingot, optimizes tantalum ingot internal structure；
In rolling process after, while realizing the rolling sizing of the first tantalum target blank, the is further refined
Tantalum crystal grain in one tantalum target blank, improves the uniformity inside the first tantalum target blank, and in double annealing technique, release
Put in the operation of rolling, in the stress that the first tantalum target blank is internally formed, optimize the first tantalum target blank internal structure；
Tiny using above-mentioned technical proposal formation tantalum target internal grain, tantalum target consistent internal structure is prevented effectively from tantalum
There are the defects such as layering in target inside, so that during improving follow-up use, the sputter rate of tantalum target, and the tantalum for being formed is thin
Film quality；And above-mentioned technical proposal is easily controllable, the preparation cost of tantalum target can be effectively reduced.
Further, it is cold-rolling treatment by rolling process, realizing that the first tantalum target blank internal grain fully refines, with
While improving the first tantalum target blank internal structure, process costs, and technique controlling difficulty are effectively reduced；Additionally, institute
Stating rolling process technique includes multiple stages, and each stage includes the different milling step of multistep deformation quantity to realize the first tantalum
Target blank is progressively suppressed, deformation, and above-mentioned technical proposal can effectively be alleviated in the operation of rolling, the shape inside the first tantalum target blank
Into stress, with the defect such as avoid the first tantalum target blank cracking.
Brief description of the drawings
Fig. 1 is the flow chart of the manufacture method of tantalum target of the present invention；
Fig. 2 be tantalum target of the present invention manufacture method in hot forging handling process schematic diagram；
Fig. 3 to Fig. 6 be tantalum target of the present invention manufacture method in roll structural representation.
Specific embodiment
As described in background, the metal structure based on tantalum metal in itself, the included a tantalum target that traditional manufacturing process is formed
Obvious lamination occurs inside material, so that target as sputter speed and stability in influenceing magnetron sputtering process, and by
This reduces the quality of forming film of tantalum films.
If being realized under tantalum recrystallization temperature conditions above, tantalum target plastic deformation can alleviate tantalum target interior laminate layer phenomenon,
But above-mentioned technique is high for the requirement of the process equipments such as equipment of hot rolling, and process conditions are harsh, and operation difficulty is big, the finished product of tantalum target
Rate is low, and above-mentioned technique also greatly increases tantalum target production cost.
Therefore, the invention provides a kind of manufacture method of tantalum target, using the present invention during tantalum target is manufactured, can
The primitive unit cell structure of effectively broken tantalum crystal grain, reduces the deformation resistance of tantalum ingot, it is to avoid lamination occurs in the tantalum target of acquisition, makes
Tantalum target internal structure is more uniformly distributed, optimize the internal structure of tantalum target, so as to improve tantalum target in magnetron sputtering process
Sputter rate, and magnetron sputtering formed tantalum films quality.
Below in conjunction with the accompanying drawings, by specific embodiment, clear, complete description is carried out to technical scheme.
With reference to shown in Fig. 1, step S1 is first carried out, there is provided tantalum ingot.
The tantalum ingot can be obtained by high vacuum electron beam smelting furnace, and its purity reaches 4N（99.99%）More than.It is existing
There is technology, will not be repeated here.
Then step S2 is performed, hot forging treatment is carried out to the tantalum ingot, an annealing process is carried out to the tantalum ingot afterwards,
Form the first tantalum target blank.
In the present embodiment, specifically include：The tantalum ingot is first put into Muffle furnace preheating, until the temperature of the tantalum ingot is more than
Tantalum ingot recrystallization temperature, carries out forging treatment to the tantalum ingot afterwards.
In the present embodiment, the tantalum ingot temperature is alternatively heated in 800~1100 degrees Celsius（℃）.By tantalum ingot heating
To after 800~1100 DEG C, the growth of tantalum crystal grain recrystallization, increases crystallite dimension in tantalum ingot, improves the plasticity of tantalum ingot.
With reference to shown in Fig. 2, the step that forges includes：
Tantalum ingot 10 after preheating is placed in forging machine, applying pressure to the tantalum ingot 10 deforms upon tantalum ingot 10.
During described forging, based on above-mentioned pre-heating process, the growth of tantalum crystal grain recrystallization, increases crystal grain chi in tantalum ingot 10
It is very little, improve the plasticity of tantalum ingot 10.After pressure is applied to the tantalum ingot 10, make to be deformed upon inside the tantalum ingot 10, compel
It is destroyed tantalum crystal grain prototype structure；In addition during forging, the inside tantalum crystal grain of tantalum ingot 10 is by tinyization, so as to be beneficial to follow-up tantalum
Ingot internal structure is moulded again.
In the present embodiment, during forging, constantly change the compression direction of tantalum ingot 10, realize it is multi-direction forge, improve
The uniform force of tantalum ingot 10, realizes the homogenization of the internal structure of tantalum ingot 10.Such as, can first along the thickness direction of tantalum ingot 10 forge
Tantalum ingot 10 obtains tantalum ingot 11, overturns tantalum ingot 11 again afterwards, is forged to the other direction pressure of tantalum ingot 11 and obtains tantalum ingot 12.It is so anti-
It is multiple to forge tantalum ingot by multiple directions, the original structure of tantalum crystal grain in tantalum ingot can be effectively destroyed, while improving the equal of tantalum ingot internal structure
Even property.
In the present embodiment, after a pre-heating technique for tantalum ingot, tantalum ingot is at least forged repeatedly 3 times, and tantalum ingot forging each time
Deformation quantity after beating is greater than equal to 80%, so as to preferably change the original structure in tantalum ingot inside, and makes the tantalum ingot internal structure
Evenly, it is to avoid lamination occurs in the tantalum ingot for obtaining afterwards.
After hot forging treatment, an annealing process is carried out to the tantalum ingot 12.Annealing process includes, incites somebody to action
The tantalum ingot 12 is heated on recrystallization temperature so that recrystallization occurs in the inside of tantalum ingot 12, reinvents the internal structure of tantalum ingot 12.
In the present embodiment, an annealing process is chosen as vacuum annealing process, and its detailed process includes：
The tantalum ingot 12 obtained after being processed through hot forging is positioned in vacuum heat treatment furnace, adjusts the vacuum heat treatment furnace
Temperature is to 1000~1300 DEG C, and tantalum ingot 2~4 hours described in Heat preservation at the temperature disclosed above（h）.
In an annealing process procedure, after being processed through hot forging, tantalum intercrystalline occurs being bonded and resets, after crushing
Tantalum crystal grain realizes recrystallization, and original grainiess is disappeared, and the grainiess inside tantalum ingot is reinvented, so that tantalum ingot internal structure
Evenly, it is to avoid occur the defects such as lamination inside tantalum ingot.
In an annealing process, if temperature is too low（Such as）, annealing temperature is higher, and the time is more long, and recrystallization is formed
Tantalum crystal grain it is bigger, the plasticity of tantalum crystal grain is stronger, but the tantalum ingot consistency for obtaining, and hardness is impacted.In the present embodiment,
If the temperature once annealed is too low（Less than 1000 DEG C）, the heat time is too short（Less than 2h）Then tantalum recrystallization is not thorough enough, it is impossible to
Obtain the tantalum ingot of even structure；If temperature is too high（More than 1300 DEG C）, the heat time is long（More than 4h）, then tantalum grain growth
Greatly, the first tantalum target blank hardness and consistency for obtaining are reduced, is unfavorable for follow-up rolling process, and the included a tantalum target for ultimately forming
The mass parameters such as hardness, the consistency of material.
Additionally, in above-mentioned hot forging processing procedure, based on applied external force is forged, internal stress is formed in tantalum ingot,
These stress defect such as tantalum ingot may be caused cracking, in an above-mentioned annealing process, can fully discharge these stress, from
And optimize tantalum ingot internal structure.
And the annealing process of the carrying out under vacuum condition, can be prevented effectively from heating process, based on the oxygen in air
Reacted Deng composition and tantalum, and the defect such as cause tantalum ingot to be oxidized.The tantalum target mass defect for causing to ultimately form is avoided, and it is right
The additional process input in significant loss and subsequent manufacturing processes, to increase preparation cost.
In the manufacture method of the tantalum target that the present embodiment is provided, at least above-mentioned in triplicate hot forging handling process, and
After each hot forging process, an annealing process is carried out once, to form the first tantalum target blank 13, so that it is guaranteed that through institute
After stating hot forging handling process and an annealing process, the quality of the internal structure of the first tantalum target blank 13 of formation.
With continued reference to shown in Fig. 1, after step S2, step S3 is performed, the first tantalum target blank 13 is rolled
Treatment, forms the second tantalum target blank.
The rolling process technique of the present embodiment is cold-rolling treatment, is obtained through above-mentioned hot forging and an annealing process
After the first tantalum target blank 13, cool down the first tantalum target blank, afterwards, roll the first tantalum target blank 13 to
Predetermined thickness, forms the second tantalum target blank.Wherein, the deformation quantity of the first tantalum target blank 13 is more than 90%.
Fig. 3 to Fig. 6 be the present embodiment in, the rolling process process schematic representation of the first tantalum target blank.
With reference to shown in Fig. 3 and Fig. 4, Fig. 3 is the stereogram of rolling mill practice, and Fig. 4 is the plan of rolling mill practice in Fig. 3.
In the present embodiment, the mode of the cold-rolling treatment is double roller cylinder rolling mill practice.Specifically, by the first tantalum target blank
13 in calender（calender）Two rollers 20a and 20b between extruded, to obtain specific plane size and thickness
The second tantalum target blank.
In the present embodiment, the cold-rolling treatment is divided into multiple stages, and progressively rolling is completed, so as to reduce in the operation of rolling
In, stress is formed in the first tantalum target blank 13, it is to avoid the defect such as target blank is cracking.
Specifically, in the present embodiment, the cold-rolling treatment to the first tantalum target blank 13 is divided into four-stage completion.Its
In, in each stage, multistep milling step is divided into again.
First stage rolls：The deformation quantity for making the first tantalum target blank is 40%~60%.Alternatively, described in each step
The deformation quantity of the first tantalum target blank 13 after milling step is 10%~25% before the step is rolled.
With reference to shown in Fig. 5.Before with a certain step milling step, the thickness of the first tantalum target blank 13 is h1, the rolling
The thickness of the first tantalum target blank 13 after step is h2, in the milling step, the deformation of the first tantalum target blank 13
Amount △ H=| h1-h2 |/h1=10%~25%.
Second stage is rolled：After first stage rolling, second stage rolling is carried out to the first tantalum target blank 13, made
The deformation quantity for obtaining the first tantalum target blank is 70%~80%.
Alternatively, the deformation quantity of the first tantalum target blank 13 after each step rolling is 10%~20% before the step is rolled,
That is, △ H=| h1-h2 |/h1=10%~20%.
Phase III rolls：After second stage rolling, phase III rolling is carried out to the first tantalum target blank 13, extremely
The deformation quantity of the first tantalum target blank 13 is more than or equal to 90%.
Alternatively, the deformation quantity of the first tantalum target blank 13 after each step rolling is 8%~13% before the step is rolled,
That is, △ H=| h1-h2 |/h1=8%~13%.
Fourth stage is rolled：After phase III rolling, fourth stage rolling is carried out to the first tantalum target blank 13, extremely
Predetermined thickness.
Alternatively, the deformation quantity of the first tantalum target blank after each step rolling is 3%~7% before the step is rolled, i.e. △
H=| h1-h2 |/h1=3%~7%.
With after the hot forging handling process, the size of the first target blank 130 of acquisition is：Diameter d is 130mm, height
It is 160mm；After rolling process technique, it is contemplated that obtaining size is：Diameter d is 520mm, highly for the tantalum target of 10mm is example.
In the first stage operation of rolling, the amount of rolling of each step milling step is 20~30mm, after multistep rolling, makes institute
The thickness for stating the first tantalum target blank 13 is suppressed to 1/2 or so of original thickness.
In the second stage operation of rolling, for the first tantalum target blank each step milling step of examples detailed above
Amount of rolling is 8~10mm, after multistep rolling, the thickness of the first tantalum target blank 13 is suppressed to the 1/4 of original thickness
Left and right.
In the phase III operation of rolling, for the first tantalum target blank each step milling step of examples detailed above
Amount of rolling is 3~5mm, after multistep rolling, the thickness of the first tantalum target blank 13 is suppressed to the 1/10 of original thickness
Left and right.
In the fourth stage operation of rolling, for the first tantalum target blank each step milling step of examples detailed above
Amount of rolling is 0.5~1mm, and after multistep rolling, the thickness for making the first tantalum target blank 13 is 10mm.
In the present embodiment, each deformation rate of each step cold-rolling treatment technique is all smaller, it is to avoid the first tantalum target base
There are the defects such as crackle during cold rolling this strong plastic deformation in material 13.And in practical operation technique, each
After step pressing step, whether have fold and fracture phenomenon, under deciding whether to enter if checking the edge of the tantalum target blank for being formed
One technique.Such as, if there is fold and slight crack, illustrate that tantalum target consistent internal structure degree is poor, then by tantalum target blank again
Carry out hot forging process.
Table 1 below is for before rolling process, diameter d is 130mm, is highly 160mm, after rolling process technique, it is contemplated that obtain chi
It is very little to be：Diameter d be 520mm, highly for 10mm the first tantalum target blank one group of specific rolling process data：
Table 1
Alternatively, during aforementioned four rolling sequence, the first tantalum target blank 13 is often once rolled
After step, can all specific predetermined angle be rotated to the first tantalum target blank 13, carry out milling step next time again afterwards, from
And cause calendering after the first tantalum target blank 13 various pieces structure than it is more uniform with it is consistent.
In the present embodiment, the predetermined angle is at 120 °~140 °.
Specific steps are referred to shown in Fig. 6, and the direction in Fig. 6 shown in four-headed arrow is directly carried out for the first tantalum target blank 13
The direction of calendering, the direction shown in unidirectional arrow is the direction that the first tantalum target blank 13 is rotated, shown in Fig. 6 1~8
It is the mark for determining to set the angle rotated after the first tantalum target blank 13 calendering for convenience.
Such as, some o'clock on the first tantalum target blank 13 8 position has been rotated counterclockwise to from 3 position, then may be used
To know the first tantalum target blank 13 135 ° of rotate counterclockwise in the hot rolling.In the present embodiment, the first tantalum target
After blank 13 often carries out a milling step, the rotation that equal angular is carried out to it with ensure calendering after the second tantalum target blank
Each several part all receives abundant and close pressure rolling, so as to obtain the second tantalum target blank of even structure.It is specific to use many
The big anglec of rotation, and rolling number of times by actual conditions depending on.
After through the rolling handling process, the tantalum crystallite dimension inside the first tantalum target blank 13 is further refined, and
So that forming the second tantalum target blank internal structure evenly.
Compared to hot rolling technology, must assure that the heat of the first tantalum target blank 13 is more than in the operation of rolling and tie again
Brilliant temperature（More than 800 DEG C）So that in the operation of rolling, realize that tantalum crystal grain is crushed and recrystallization process repeatedly, so as to destroy
Tantalum target inside original structure, it is to avoid lamination occur inside the target after rolling.Hot rolling technology is high for equipment requirement, high
It is harsh to not operation technological requirement during warm-rolling system.
What the present embodiment was provided, the mode that hot forging and cold-rolling process are combined is ensuring to obtain internal structure even tissue
Tantalum target blank simultaneously, greatly reduce process equipment requirement, and operating procedure difficulty.
After rolling process technique, the second tantalum target blank to obtaining carries out double annealing technique, so as to further release
Put after stating rolling process technique, the stress formed in the second tantalum target blank improves the second tantalum target internal structure.
In the present embodiment, the double annealing technique is vacuum annealing handling process.Specific steps include：It is described obtaining
After second tantalum target blank, the second tantalum target blank is positioned in vacuum heat treatment furnace, and adjust vacuum heat furnace temperature
To 800~1000 DEG C, second 1~3h of tantalum target blank is heated under vacuum.
In above-mentioned double annealing handling process, between the tantalum crystal grain in the second tantalum target blank, it is bonded again
And rearrangement, and during the tantalum crystal grain reinvented fully discharges the rolling processing procedure, what is produced inside the second tantalum target blank should
Power, to optimize tantalum ingot internal structure.
It is worth noting that, in the present embodiment, the double annealing technological temperature is less than above-mentioned single treatment annealing temperature,
Its reason is, in thermal anneal process, annealing temperature is higher, and the heat time is more long, and the tantalum grain particles of formation are bigger, if included a tantalum target
Material grain particles are excessive, directly affect the consistency and hardness of tantalum target blank.In the present embodiment, in an annealing treating process
In, the temperature for using is 1000~1300 DEG C so that the tantalum grain particles in the tantalum target blank are suitably grown up, so as to improve
The plasticity of tantalum target blank, in order to the follow-up operation of rolling in, for further grain particles tinyization of tantalum target blank
Technique, and the rolling of tantalum target blank is shaped.And in double annealing handling process, rolled its object is to fully release
Cheng Zhong, the stress formed in the tantalum target blank, to optimize the tantalum target blank internal structure for obtaining, while must ensure to obtain
The tantalum target internal grain size for obtaining can not be excessive.In the present embodiment, if temperature is too high（More than 1100 DEG C）, the heat time is long
（More than 3h）, the tantalum crystal grain being likely to result in tantalum target blank is excessive and influences the consistency and hardness of tantalum target.If temperature
It is too low（Less than 800 DEG C）, the heat time is too short（Less than 1h）, then answering inside the second tantalum target blank cannot fully be discharged
Power.
100 μm or so of tantalum target internal grain can be obtained in the manufacture method of the tantalum target provided using the present embodiment, and
Consistent internal structure, the tantalum target for not having substantially specific crystal phase structure.So that the magnetron sputtering of tantalum target can be effectively improved
The quality of the tantalum films obtained after stability, and tantalum target magnetron sputtering technique.
Although present disclosure is as above, the present invention is not limited to this.Any those skilled in the art, are not departing from this
In the spirit and scope of invention, can make various changes or modifications, therefore protection scope of the present invention should be with claim institute
The scope of restriction is defined.
Claims (6)
1. a kind of manufacture method of tantalum target, it is characterised in that including：
Tantalum ingot is provided；
Hot forging treatment is carried out to the tantalum ingot；
The tantalum ingot is carried out after hot forging treatment, an annealing process is carried out to the tantalum ingot, form the first tantalum target blank；
The hot forging is repeated to process at least 3 times, an annealing process is carried out once after the treatment of hot forging each time；
Rolling process is carried out to the first tantalum target blank, the second tantalum target blank is formed, the rolling process is cold rolling place
Reason；
Double annealing technique is carried out to the second tantalum target blank, tantalum target is formed；
The rolling process includes：
Cool down the first tantalum target blank；
First stage rolling is carried out to the first tantalum target blank, make the deformation quantity of the first tantalum target blank for 40%~
60%；
After first stage rolling, second stage rolling is carried out to the first tantalum target blank, to the first tantalum target blank
Deformation quantity be 70%~80%；
After second stage rolling, phase III rolling is carried out to the first tantalum target blank, to the first tantalum target blank
Deformation quantity be more than or equal to 90%；
After phase III rolling, fourth stage rolling is carried out to the first tantalum target blank, to predetermined thickness；
After each step rolling, 120 °~140 ° of the first tantalum target blank is rotated, afterwards, then to the first tantalum target blank
Carry out next step rolling；Along the first tantalum target blank described in different directions repeat-rolling to predetermined thickness, the second tantalum target is formed
Blank；And after the rolling process, the deformation quantity of the first tantalum target blank is more than 90%.
2. the manufacture method of tantalum target according to claim 1, it is characterised in that the hot forging treatment includes：
The tantalum ingot is heated to 800~1100 DEG C, afterwards the tantalum ingot is carried out forging treatment；
Once it is described forge treatment include the tantalum ingot is forged along multiple directions at least, and once it is described forge treatment after
Tantalum ingot shape variable be more than or equal to 80%.
3. the manufacture method of tantalum target according to claim 2, it is characterised in that hot forging treatment at least includes 3 times
It is described to forge treatment.
4. the manufacture method of tantalum target according to claim 1, it is characterised in that described once to make annealing treatment as vacuum is moved back
Fiery handling process, including：
Regulation vacuum heat furnace temperature heats 2~4h of the tantalum ingot under vacuum to 1000~1300 DEG C.
5. the manufacture method of the tantalum target stated according to claim 1, it is characterised in that roll in the first stage,
During second stage is rolled and the phase III rolls, including multistep milling step；
Wherein, in rolling in the first stage, the deformation quantity of the first tantalum target blank after each step rolling is before the step is rolled
10%~25%；
In second stage rolling, the deformation quantity of the first tantalum target blank after the rolling of each step be before step rolling 10%~
20%；
In the phase III rolls, the deformation quantity of the first tantalum target blank after the rolling of each step be before step rolling 8%~
13%；
In fourth stage rolling, the deformation quantity of the first tantalum target blank after the rolling of each step be before step rolling 3%~
7%.
6. the manufacture method of tantalum target according to claim 1, it is characterised in that the double annealing is processed as vacuum and moves back
Fiery handling process, including：
Regulation vacuum heat furnace temperature to 800~1000 DEG C, heat under vacuum the second tantalum target blank 1~
3h。
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| CN106521434B (en) * | 2016-11-07 | 2019-01-22 | 长沙南方钽铌有限责任公司 | A kind of preparation method of the high-purity tantalum target with preferred orientation |
| CN108611607A (en) * | 2016-12-09 | 2018-10-02 | 宁波江丰电子材料股份有限公司 | The forming method of powder metallurgy process and target |
| CN108687158B (en) * | 2018-05-11 | 2019-12-17 | 成都联虹钼业有限公司 | preparation method of isotropic molybdenum plate |
| CN109338316B (en) * | 2018-09-12 | 2020-04-28 | 中南大学 | Ultra-pure tantalum with controllable structure and texture and preparation method and application thereof |
| CN111088481A (en) * | 2018-10-23 | 2020-05-01 | 宁波江丰电子材料股份有限公司 | Nickel target blank and method for manufacturing target material |
| CN112877629A (en) * | 2021-01-14 | 2021-06-01 | 重庆大学 | Processing method for improving microstructure uniformity of tantalum plate for thick target |
| CN113909414B (en) * | 2021-09-30 | 2023-12-29 | 宁波江丰电子材料股份有限公司 | Preparation method of tantalum target blank |
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| US6331233B1 (en) * | 2000-02-02 | 2001-12-18 | Honeywell International Inc. | Tantalum sputtering target with fine grains and uniform texture and method of manufacture |
| KR100966682B1 (en) * | 2001-02-20 | 2010-06-29 | 에이치. 씨. 스타아크 아이앤씨 | Refractory metal plates with uniform texture and methods of making the same |
| JP2004535933A (en) * | 2001-07-19 | 2004-12-02 | ハネウェル・インターナショナル・インコーポレーテッド | Method of preparing sputtering target, sputter reactor, cast ingot and method of preparing metal article |
| JP4110476B2 (en) * | 2001-11-26 | 2008-07-02 | 日鉱金属株式会社 | Sputtering target and manufacturing method thereof |
| EP1704266A2 (en) * | 2003-12-22 | 2006-09-27 | Cabot Corporation | High integrity sputtering target material and method for producing bulk quantities of same |
| EP2418299A4 (en) * | 2009-05-22 | 2013-05-01 | Jx Nippon Mining & Metals Corp | Tantalum sputtering target |
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