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CN105463395B - A kind of high-performance dilval sputtering target material and preparation method thereof - Google Patents

A kind of high-performance dilval sputtering target material and preparation method thereof Download PDF

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Publication number
CN105463395B
CN105463395B CN201510965185.4A CN201510965185A CN105463395B CN 105463395 B CN105463395 B CN 105463395B CN 201510965185 A CN201510965185 A CN 201510965185A CN 105463395 B CN105463395 B CN 105463395B
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dilval
target
blank
rolling
target material
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CN105463395A (en
Inventor
徐国进
罗俊锋
陈明
李勇军
丁照崇
徐学礼
张巧霞
熊晓东
何金江
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GRINM ADVANCED MATERIALS Co Ltd
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GRINM ADVANCED MATERIALS Co Ltd
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
    • B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1216—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the working step(s) being of interest
    • C21D8/1233—Cold rolling
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1266—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest between cold rolling steps
    • 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
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electromagnetism (AREA)
  • Manufacturing & Machinery (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention belongs to target preparing technical field, and in particular to a kind of high-performance dilval sputtering target material and preparation method thereof.The present invention carries out hot forging to dilval ingot casting first, then the microstructure of dilval is controlled using cold rolling and Technology for Heating Processing, and the magnetic conductivity of target is reduced by the way that target blankss are carried out with the rolling deformation that total deformation is 1%~20%, final machining obtains high-performance dilval sputtering target material.Preparation method of the present invention is simple, is adapted to make various sizes target, can reduce the magnetic conductivity of target, and makes even tissue, average grain size between 20 100 μm, and target as sputter face is in random crystalline orientation.

Description

A kind of high-performance dilval sputtering target material and preparation method thereof
Technical field
The invention belongs to target preparing technical field, and in particular to a kind of high-performance dilval sputtering target material and its preparation Method.
Background technology
Ferronickel system permalloy is extensive due to the excellent magnetic property such as high magnetic permeability and high saturated magnetic induction For clock stator, the pole part of electromagnetic lens, high sensitivity transformer, shielding material and magnetic head device etc..With electronic system To high integration, high-performance development, component gradually minimizes, filming, to occupying larger volume and again in the electronic device The magnetic device of amount, such as inductor, transformer, it is proposed that higher requirement.It is soft using dilval as the permalloy formed Magnetic material, the superlattice film of preparation have high saturated magnetic induction (more than 1.5t), high resistance, low-coercivity and excellent Anisotropic magnetoresistive (AMR), it can be used as giant magnetic resistor material and be applied in MEMS of new generation, such as new sensor, magnetic Record magnetic reading head, giant magnetoresistance random access memory and harmonic filter etc., and the various devices prepared have it is low in energy consumption, sensitive Spend the series of advantages such as height, small volume, reliability height.
Dilval electric thin has a variety of preparation methods, such as vapour deposition method, galvanoplastic, magnetron sputtering method etc., wherein, magnetic Film consistency height prepared by sputtering method is controlled, adhesion is strong, and therefore, corresponding magnetic property is more excellent.But because ferronickel closes Magnetic caused by itself has the function that to magnetic field shielding gold in magnetic field, can lead to not normally sputter.Therefore, it is necessary to pass through Rational preparation technology ensures that sputtering target material has stronger permeability to sputtering source magnetic field, and ensures the film tool of magnetron sputtering There is very strong saturation induction density.
In general dilval target, it is to be forged, rolled by the ingot casting for melting to obtain to high vacuum, is heat-treated and machine What the processes such as processing were process.In this manufacturing process, the forging of ingot casting destroys cast sturcture, expands stomata and segregation Dissipate, disappear, then by being rolled and being heat-treated to it, the uniformity of tissue, crystal grain thinning can be improved, but target is present The problem of magnetic conductivity is high.Typically when implementing to sputter, because the magnetic conductivity of magnetic target is high so that the magnetic line of force on target surface is few, leads Cause sputter rate relatively low, or even can not normally sputter.
For US6267827B1 by being machined out to obtain target to high-purity N iFe18wt.% ingot castings, target is organized as cast condition Tissue, this method is only suitable for doing the target of small size, and because target size is small, the magnetic line of force can bypass target, reach target Surface, magnetic conductivity influence smaller on it；US6190516B1 to a certain region deformation of target by reducing the magnetic of the region target Conductance, target magnetic susceptibility is improved, but the difference of structural state can influence the uniformity of target as sputter film between target region； US6988306B2 increases magnetic susceptibility by changing the thickness of target different parts, but so add target and backboard plus Work and the difficulty of welding；WO03/104521A2 has manufactured the NiFe19wt.% targets of high magnetic susceptibility using powder metallurgy process The nonmetallic inclusion constituent contents such as material, the target that this method obtains, oxygen are high, and target internal gas discharges in sputter procedure, shadow Ring sputtered film quality.
The content of the invention
The invention provides a kind of high-performance dilval sputtering target material and preparation method thereof, concrete technical scheme is as follows：
A kind of preparation method of high-performance dilval sputtering target material, comprises the following steps：
(1) hot forging：Hot forging is carried out to dilval ingot casting, as-cast structure is eliminated, soldering casting flaw, obtains required The blank of shape；
(2) roll：Blank after hot forging is subjected to cold rolling, so that blank is thinned, crystal grain thinning, can be entered according to material thickness The one or many rollings of row；
(3) intermediate heat-treatment：If repeatedly rolling blank, need to carry out intermediate heat-treatment, temperature twice between cold rolling For 600~1000 DEG C, processing hardening is eliminated；
(4) dynamic recrystallization treatment：Dynamic recrystallization treatment is carried out to the blank after finish to gauge, temperature is 700~1100 DEG C, makes group Perfect recrystallization is given birth in hair-weaving；Final heat treatment temperature must be maintained at more than 700 DEG C, can so ensure that blank is being heat-treated Uniform recrystallized structure is obtained afterwards；But otherwise heat treatment temperature can make coarse grains not above 1100 DEG C, reduce The quality of sputter coating；
(5) deform：The rolling deformation that total deformation is 1%~20% is carried out to the blank after dynamic recrystallization treatment, preferably Total deformation be 5%~15%；
(6) finished product finishes：Blank is processed into required specification, obtains dilval sputtering target material.
The purity of the dilval ingot casting be 4N and more than.
Described Ni, Fe atom ratio are (99:1)~(1:99), preferably (80:20) (20 are arrived:80).
In step (1), during ingot casting hot forging, heating-up temperature is 900~1300 DEG C；Heating can increase the plasticity of material, reduce Resistance of deformation, flat-die forging can eliminate as-cast structure, soldering casting flaw, reach broken, crystal grain thinning effect.
In step (2), pass deformation during rolling is 5%~30%, and total deformation is 30~99%, and rolling direction can Unidirection rolling or tandem rolling are used according to target shape.
Dynamic recrystallization treatment can be such that the microstructure of blank fully recrystallizes, and even tissue is tiny.
Preferably, in step (6), tabular target can be processed into by machining.It need to such as be combined, can be used with backboard The methods of soldering, gluing, Diffusion Welding, welds, and reprocesses out finished product.
The high-performance dilval sputtering target material that preparation method as described above obtains, target magnetic conductivity is low, even tissue, puts down Equal crystallite dimension is 20~100 μm, and sputter face is in random crystalline orientation.
Beneficial effects of the present invention are：
(1) preparation method of the present invention is simple, is adapted to make various sizes target, suitable for semiconductor and IC manufacturing Deng field.
(2) present invention reduces the magnetic conductivity of target by increasing a certain amount of deformation after recrystallization annealing, with increase Magnetic susceptibility, realize the sputtering of dilval target.
(3) present invention controls the microstructure of target by thermomechanical processing method, makes dilval target tissue equal For even, average grain size between 20-100 μm, target as sputter face is in random crystalline orientation
(4) present invention solves ferromagnetic sputter target material in sputter procedure, and sputter rate is low, or even what can not be sputtered ask Topic；Meanwhile the reduction of magnetic conductivity also helps the dilval target for making bigger thickness, target utilization ratio is improved, is reduced The frequency is changed, reduces production cost.
Brief description of the drawings
Fig. 1 is the preparation flow figure of high-performance dilval sputtering target material in the present invention.
Fig. 2 is the micro-structure diagram of high-performance dilval sputtering target material in embodiment one.
Fig. 3 is the micro-structure diagram of high-performance dilval sputtering target material in embodiment two.
Fig. 4 is the micro-structure diagram of high-performance dilval sputtering target material in embodiment three.
Fig. 5 is the micro-structure diagram of high-performance dilval sputtering target material in example IV.
Fig. 6 is the micro-structure diagram of high-performance dilval sputtering target material in embodiment five.
Fig. 7 is the micro-structure diagram of high-performance dilval sputtering target material in embodiment six.
Fig. 8 is the micro-structure diagram of dilval sputtering target material in comparative example one.
Fig. 9 is the micro-structure diagram of dilval sputtering target material in comparative example two.
Embodiment
Below by the drawings and specific embodiments, the present invention will be further described, but is not meant to protect the present invention Protect the limitation of scope.
(1) hot forging：The purity of dilval ingot casting be 4N and more than, Ni, Fe atom ratio is (99:1)~(1:99). Dilval ingot casting is subjected to hot forging, heating-up temperature is 900~1300 DEG C.
(2) roll：Blank after hot forging is subjected to cold rolling, blank is thinned, crystal grain thinning, can be carried out according to material thickness One or many rollings；Pass deformation during rolling is 5%~30%, and total deformation is 30~99%, and rolling direction can root Unidirection rolling or tandem rolling are used according to target shape.
(3) intermediate heat-treatment：If repeatedly rolling blank, need to carry out intermediate heat-treatment, temperature twice between cold rolling For 600~1000 DEG C, processing hardening is eliminated.
(4) dynamic recrystallization treatment：Dynamic recrystallization treatment is carried out to the blank after finish to gauge, temperature is 700~1100 DEG C, makes group Perfect recrystallization is given birth in hair-weaving.
(5) deform：The rolling deformation that total deformation is 1%~20% is carried out to the blank after dynamic recrystallization treatment.
(6) finished product finishes：Blank is processed into required specification, obtains dilval sputtering target material.
The preparation method of dilval sputtering target material such as step (1)~(6) are described in specific embodiment, ferronickel in comparative example Without step (5) in the preparation method of alloy sputtering target, related parameter values are as shown in table 1.
Related parameter values in the embodiment of table 1 and comparative example
As can be seen that grain structure is uniform from table 1 and Fig. 2~Fig. 9, average grain size is between 20-100 μm； From Table 2, it can be seen that the tissue obtained in each embodiment and comparative example is distributed in disordered orientation.It is real as can be seen from Table 3 Apply the magnetic conductivity in example and obtain obvious reduction.
Dilval target as sputter covering weave is orientated in the embodiment of table 2 and comparative example
Dilval target magnetic conductivity in the embodiment of table 3 and comparative example
Embodiment one Embodiment two Embodiment three Example IV Embodiment five Embodiment six Comparative example one Comparative example two
Magnetic conductivity 1651 1116 1015 1305 1670 1420 1917 2683

Claims (1)

1. a kind of preparation method of high-performance dilval sputtering target material, it is characterised in that comprise the following steps：
(1) hot forging：The purity of dilval ingot casting be 4N and more than, Ni, Fe atom ratio is 45：55；Dilval is cast Ingot carries out hot forging, and heating-up temperature is 1200 DEG C；
(2) roll：Blank after hot forging is subjected to cold rolling, blank is thinned, crystal grain thinning, is rolled twice；During rolling first Deflection is 60%, and it is 80% that second, which rolls total deformation, and rolling direction can use unidirection rolling or friendship according to target shape Fork rolling；
(3) intermediate heat-treatment：Carry out intermediate heat-treatment between cold rolling to blank twice, temperature is 700 DEG C, eliminates processing hardening；
(4) dynamic recrystallization treatment：Dynamic recrystallization treatment is carried out to the blank after finish to gauge, temperature is 850 DEG C, tissue occurs complete Recrystallization；
(5) deform：The rolling deformation that total deformation is 10% is carried out to the blank after dynamic recrystallization treatment；
(6) finished product finishes：Blank is processed into required specification, obtains dilval sputtering target material.
CN201510965185.4A 2015-12-21 2015-12-21 A kind of high-performance dilval sputtering target material and preparation method thereof Active CN105463395B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112808833B (en) * 2020-12-31 2023-01-10 有研科技集团有限公司 Method for preparing high-performance ferromagnetic target material
CN112941473B (en) * 2021-01-28 2022-06-17 宁波江丰电子材料股份有限公司 MoTiNi alloy target material and preparation method thereof
CN114657345B (en) * 2022-03-31 2024-04-09 先导薄膜材料（广东）有限公司 Iron target, iron-nickel alloy target and grain refinement method of target
CN114934261B (en) * 2022-04-27 2023-12-05 先导薄膜材料（广东）有限公司 Iron target, iron-nickel alloy target and manufacturing method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6190516B1 (en) * 1999-10-06 2001-02-20 Praxair S.T. Technology, Inc. High magnetic flux sputter targets with varied magnetic permeability in selected regions
US6988306B2 (en) * 2003-12-01 2006-01-24 Praxair Technology, Inc. High purity ferromagnetic sputter target, assembly and method of manufacturing same
CN101250618A (en) * 2008-04-03 2008-08-27 上海交通大学 Grain ultra-refining method for Fe-32%Ni alloy
CN104726829A (en) * 2013-12-18 2015-06-24 有研亿金新材料股份有限公司 High purity NiPt alloy target material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6190516B1 (en) * 1999-10-06 2001-02-20 Praxair S.T. Technology, Inc. High magnetic flux sputter targets with varied magnetic permeability in selected regions
US6988306B2 (en) * 2003-12-01 2006-01-24 Praxair Technology, Inc. High purity ferromagnetic sputter target, assembly and method of manufacturing same
CN101250618A (en) * 2008-04-03 2008-08-27 上海交通大学 Grain ultra-refining method for Fe-32%Ni alloy
CN104726829A (en) * 2013-12-18 2015-06-24 有研亿金新材料股份有限公司 High purity NiPt alloy target material and preparation method thereof

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