CN106399954A - Processing method of long-service-life copper manganese alloy target material - Google Patents
Processing method of long-service-life copper manganese alloy target material Download PDFInfo
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- CN106399954A CN106399954A CN201610786648.5A CN201610786648A CN106399954A CN 106399954 A CN106399954 A CN 106399954A CN 201610786648 A CN201610786648 A CN 201610786648A CN 106399954 A CN106399954 A CN 106399954A
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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
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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- Mechanical Engineering (AREA)
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- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a processing method of a long-service-life copper manganese alloy target material, and belongs to the technical field of sputtering target material manufacturing. The method mainly comprises the steps that a copper manganese alloy cast ingot is processed by a conventional heat mechanical treatment method to obtain an original blank; the original blank is subjected to grain refinement through stirring and friction processing; the preparation of the long-service-life copper manganese alloy target material is realized; the service life of the target material can be effectively prolonged; and the utilization rate of the target material is improved. The obtained long-service-life copper manganese alloy target material has the advantages that the average grain size is less than 5 [mu]m; the service life can reach 3000kwh; and the texture orientation is in random distribution, so that the requirement of the technical process of 45nm or lower of an integrated circuit can be met.
Description
Technical field
The invention belongs to target manufacturing technology field, particularly to a kind of processing method of long-life cupromanganese target.
Background technology
Sputtering target material is one of important raw material in semiconductor integrated circuit preparation process, and the material of target mainly includes
Al, Cu, Ti, WTi, NiV, NiPt etc., are mainly used in the physics such as contact, through hole, interconnection line, barrier layer, encapsulation in integrated circuit
The preparation of vapor deposition film.In sputter procedure, with the Ions Bombardment target material surface accelerating, the atomic deposition making surface is in substrate
Surface.In order to reduce IC manufacturing cost, simple effective method is to improve target life, conventional raising target life
Method be increase sputter area thickness.
Patent CN 204097558 U, CN 201793723 U, CN 201793726 the patent such as U pass through to increase sputtering zone
Domain thickness improves target service life, and the edge having neither part nor lot in sputtering keeps life size, so can avoid affecting target install and
Overall sputtering performance.It is ledge structure or ramp structure in target rim, its effect is to prevent from producing in target as sputter process
Backwash material contact with board cathodic protection frame and lead to short circuit.
And the patent such as patent CN 201962347 U, US2009/0045051 A1 then to be improved using reducing back plate thickness
The thickness of sputtering part target, thus reach the purpose improving target life.
But the limitation of above method is, target life, life-span are improved by the method increasing sputter area thickness
Lifting typically within 30%, for example traditional copper alloy target life-span is 1800kwh；Designed by the rational long-life,
The life-span that target can be made brings up to 2200kwh, but this life-span has reached the limit of traditional target processing method.
Super fine crystal material refers to crystallite dimension in 0-10 μm of nanocrystalline material or sub-micron crystal material, due to its have bright
Performance and the superior mechanical properties such as the aobvious optics being different from traditional material, electricity, magnetics, so always investigation of materials scholar
Primary study direction.
Ultra-fine Grained CuMn target has the performance of brilliance.Because Ultra-fine Grained can be greatly improved target intensity, hardness, make target
Integrated design can be carried out using one block of metal, this had both extended the service life of target, eliminate again loaded down with trivial details target with
Backboard connects operation.The service life of conventional 1800kwh can be significantly promoted to 3000kwh, pole by Ultra-fine Grained CuMn target
The big utilization rate that improve target, saves the time and efforts that target is changed and board maintenance is required, drops to greatest extent
The low production cost of semiconductor producer, has broad application prospects.
The method of the processing Ultra-fine Grained target being current international mainstream Deng groove angle extruding (ECAE).The method is passed through repeatedly many
Inferior groove angle extruding makes the strain of target be up to 6-8, thus obtaining ultrafine-grained (UFG) microstructure.But due to equipment limit, the whole world at present
Only Honeywell have large-scale wait groove angle extrusion equipment can using the method processing large scale Ultra-fine Grained target it is therefore desirable to
Develop other Novel super-thin crystalline substance target processing methods.
Patent CN1484711A discloses physical vapor deposition target and the method manufacturing metal material, and the method is with predetermined
Path and number of times such as carry out at the groove angle extruding, and carry out tandem rolling or forging after waiting groove angle to extrude, and eventually pass recrystallization
Annealing, obtains average grain size and is 1-30 μm, (220) are orientated percentage>90% target blankss.
Patent CN1592797A discloses a kind of high-strength sputtering target and its manufacture method, and the groove angle extruding such as the method employing is thin
Change crystal grain, the final target crystalline grains size obtaining<1 μm, be orientated random sputtering target material, sputtering target material material mainly comprise Al,
Ti、Cu、Ta、Ni、Mo、Au、Ag、Pt.
Patent CN1681960 discloses a kind of copper sputtering target material and the method forming copper sputtering target material, and the method adopts 300
DEG C hot forging, makes height drop to and is at least about 40%, only carry out extrusion process, makes forge hot blank pass through equal channel angular
Extruding at least 4 times, period is heat-treated, and is finally cold-rolled to drafts and is less than 90%, thus forming semi-finished product, the target of acquisition
Average grain diameter is less than 1 μm, and in whole target, grain size uniformity standard deviation is less than or equal to 15%.
Patent CN102925832A discloses a kind of large plastometric set method preparing ultra-fine contraction crystalline substance copper, and the method is using many
Shear stress during the asynchronous ply rolling of passage and accumulation strain effect promote the wrong row of the stacking of material internal, the refinement of crystal grain and
Being combined of interface, passes through the sliding of annealing process Dislocations afterwards and climbs, and so that local dot matrix and crystal boundary planar orientation is changed, promotes
The brilliant formation of contraction in annealing process, then cools to room temperature with the furnace and removes, that is, obtain ultra-fine contraction crystalline substance copper material.But the method is only suitable
Process it is impossible to be applied to sputtering target material manufacture field for thin strip.
Based on the principle of agitating friction welding, Mishra etc. has developed mixing yoghurt technology, for the local of material
Modified.The principle very simple of mixing yoghurt, the stirring-head high-speed rotation being made up of the shaft shoulder and mixing needle, so that mixing needle is squeezed
Enter workpiece to be processed until the shaft shoulder is contacted with surface of the work, the shaft shoulder and surface of the work friction make material softening, mixing needle drives and adds
Work area material produces violent plastic flow, so that processing district structure refinement, densified and homogenization.In recent years, agitating friction
Process technology also becomes a kind of effective means preparing bulk ultrafine-grained materials.But on the one hand due to mixing yoghurt process
Middle can produce severe plastic deformation it is therefore desirable to control stirring-head rotating speed, it is to avoid lead to feeding occurs not because rotating speed is too fast
Good situation；On the other hand because the temperature rise that the severe plastic deformation of mixing yoghurt process in which materials produces can make recrystallization
Crystal grain is grown up it is therefore desirable to make the material after processing still maintain Ultra-fine Grained yardstick using forcing to cool down.
Patent CN105039670A discloses a kind of two-sided mixing yoghurt Ultra-fine Grained sheet material Apparatus and method for, the method
Design two-sided mixing yoghurt Apparatus and method for by rational, can effectively eliminate the heat engine impact between adjacent stirring area
Area and heat affected area, effectively improve the mechanical property of Ultra-fine Grained sheet material.Refer to agitating friction weldering in document and prepare Ultra-fine Grained aluminium
And aluminum alloy plate materials, but it is not directed to the processing of copper system strake material, and the purpose of this patent is not configured to improve target
Life-span.
Article " microstructure of agitating friction weldering processing Ultra-fine Grained and nanostructured Cu-Al alloy and mechanical property research "
In refer to obtain Ultra-fine Grained and nano junction in Cu-Al alloy by forcing mixing yoghurt (FSP) technology that cools down
The microstructure of structure, Al content is respectively 10at% and 15at%.The Cu-Al alloy being obtained is uniform, equiaxial recrystallization
Tissue, with the reduction of stacking fault energy, crystallite dimension constantly reduces, and in the FSP Cu-Al alloy of low stacking fault energy, Ultra-fine Grained
Intragranular portion generates abundant nano twin crystal lamellar structure, has refined microstructure further.Cu-Al alloy is proposed in article
Ultra-fine Grained processing method, but be not related to Cu-Mn alloy target material.
Content of the invention
It is an object of the invention to provide a kind of processing method of long-life cupromanganese target is it is characterised in that comprise to walk
Suddenly as follows：
1) using conventional thermal mechanical processing method, cupromanganese ingot casting is processed, obtains original blank；
2) using mixing yoghurt, crystal grain refinement is carried out to original blank, obtain the length of below 5 μm of average grain size
Life-span cupromanganese sputtering target material；Its life-span reaches 3000kwh.
In described cupromanganese, Mn content is 0.5at%-2at%.
Described traditional thermo-mechanical processi method is：Hot forging, it is cold roller and deformed to carry out 60%-90% afterwards, then warp
Cross 400-600 DEG C of dynamic recrystallization treatment, temperature retention time is 2-3h, is processed under air or vacuum condition；
Described mixing yoghurt, stirring-head rotating speed is 400-600r/min.
Described mixing yoghurt, carries out water-cooled to blank in process.
Described mixing yoghurt, carries out Low-temperature stress-relief annealing to blank after processing, and annealing temperature is 250-350
℃.
Beneficial effects of the present invention：The processing method of the present invention can realize the preparation of long-life cupromanganese target, can
To effectively improve target life, promoting utilization rate of target.The long-life cupromanganese target average grain size that the present invention obtains
Below 5 μm, texture is orientated random distribution, disclosure satisfy that integrated circuit 45nm and the requirement of following manufacturing process.
Brief description
Fig. 1 is long-life cupromanganese target SEM photograph (rotating speed 500r/min).
Fig. 2 is long-life cupromanganese target metallograph (rotating speed 350r/min).
Fig. 3 is stirring-head feeding material object photo (top view) (rotating speed 650r/min).
Specific embodiment
The present invention provides a kind of processing method of long-life cupromanganese target, comprises step as follows：
1) using conventional thermal mechanical processing method, cupromanganese ingot casting is processed, obtains original blank；
2) using mixing yoghurt, crystal grain refinement is carried out to original blank, obtain the length of below 5 μm of average grain size
Life-span cupromanganese sputtering target material；Its life-span reaches 3000kwh.It is explained with reference to the accompanying drawings and examples.
Embodiment 1-5：The results are shown in Table shown in 1 and Fig. 1-Fig. 3；
Cupromanganese ingot casting specification is φ 200 × 260t, carries out forge hot under the conditions of 500-800 DEG C, and forging mode is X/
Y/Z tri- direction jumping-up pulling, upsetting pull ratio is for 2:1, through cold rolling and roll φ 580 × 30t；Then carry out dynamic recrystallization treatment,
Obtain original blank.
Carry out crystal grain refinement using mixing yoghurt under conditions of rotating speed is for 400-600r/min, obtain long-life copper
Manganese alloy sputtering target material, carries out water-cooled in grain refinement process, and afterwards blank is carried out with 300 DEG C of stress relief annealings.
Obtain the results are shown in Table 1 it can be seen that using mixing yoghurt under conditions of rotating speed is for 400-600r/min
Carry out crystal grain refinement, the long-life cupromanganese sputtering target material average grain size obtaining below 5 μm, with the fall of rotating speed
Low, average grain size is gradually increased.
Comparative example 1-2：
In order to obtain the range of speeds of long-life cupromanganese target mixing yoghurt, carry out the slow-speed of revolution and high turn respectively
Speed test, is contrasted with embodiment.
Cupromanganese ingot casting specification is φ 200 × 260t, carries out forge hot under the conditions of 500-800 DEG C, and forging mode is X/
Y/Z tri- direction jumping-up pulling, upsetting pull ratio is for 2:1, through cold rolling and roll φ 580 × 30t；Then carry out dynamic recrystallization treatment,
Obtain original blank.
Carry out crystal grain refinement using mixing yoghurt under conditions of rotating speed is 350,650r/min, obtain cupromanganese
Sputtering target material.Obtain the results are shown in Table 1 it can be seen that when rotating speed is relatively low, plastic deformation is not violent, and average grain size is relatively
Greatly, more than 5 μm；When rotating speed is higher, stirring-head feeding situation is poor, and stirring-head feeding hole is deeper, causes target to lose efficacy (see figure
3).
The embodiment result of table 1 cupromanganese sputtering target material
Claims (6)
1. a kind of processing method of long-life cupromanganese target it is characterised in that：Comprise step as follows：
1) using conventional heat engine tool processing method, cupromanganese ingot casting is processed, obtains original blank；
2) using mixing yoghurt, crystal grain refinement is carried out to original blank, obtain the long-life of below 5 μm of average grain size
Cupromanganese sputtering target material, its life-span is up to 3000kwh.
2. a kind of processing method of the long-life cupromanganese target according to claims 1 is it is characterised in that described
In cupromanganese, Mn content is 0.5at%-2at%.
3. a kind of processing method of the long-life cupromanganese target according to claims 1 is it is characterised in that described
Conventional thermo-mechanical processi method is：Hot forging, it is cold roller and deformed to carry out 60%-90% afterwards, then ties through 400-600 DEG C again
Brilliant heat treatment；Temperature retention time is 2-3h, is processed under air or vacuum condition.
4. a kind of processing method of the long-life cupromanganese target according to claims 1 is it is characterised in that described
Mixing yoghurt, stirring-head rotating speed is 400-600r/min.
5. a kind of processing method of the long-life cupromanganese target according to claims 1 is it is characterised in that described
Mixing yoghurt, carries out water-cooled to blank in process.
6. a kind of processing method of long-life cupromanganese target according to claim 1 is it is characterised in that described stirs
Mix friction processing, after processing Low-temperature stress-relief annealing is carried out to blank, annealing temperature is 200-350 DEG C.
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Cited By (8)
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|---|---|---|---|---|
| CN109338314A (en) * | 2018-12-04 | 2019-02-15 | 有研亿金新材料有限公司 | A kind of processing method of Ultra-fine grain copper manganese alloy target |
| TWI684652B (en) * | 2017-10-13 | 2020-02-11 | 美商哈尼威爾國際公司 | Copper manganese sputtering target |
| US11035036B2 (en) | 2018-02-01 | 2021-06-15 | Honeywell International Inc. | Method of forming copper alloy sputtering targets with refined shape and microstructure |
| CN114310159A (en) * | 2021-12-02 | 2022-04-12 | 上海交通大学 | Method for regulating and controlling rolling texture of in-situ synthesized particle reinforced aluminum-based composite material |
| CN114574822A (en) * | 2022-03-02 | 2022-06-03 | 基迈克材料科技（苏州）有限公司 | Preparation process and application of silver alloy target |
| CN115029668A (en) * | 2022-06-02 | 2022-09-09 | 有研亿金新材料有限公司 | Method for preparing high-performance tantalum sputtering target material through pack rolling |
| CN115161603A (en) * | 2022-05-17 | 2022-10-11 | 广东欧莱高新材料股份有限公司 | Production process of high-purity multi-element alloy rotary sputtering target for high-generation high-definition liquid crystal display |
| CN115369365A (en) * | 2022-10-24 | 2022-11-22 | 有研亿金新材料有限公司 | Long-life sputtering target material and preparation method thereof |
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|---|---|---|---|---|
| JP7297741B2 (en) | 2017-10-13 | 2023-06-26 | ハネウェル・インターナショナル・インコーポレーテッド | copper manganese sputtering target |
| TWI684652B (en) * | 2017-10-13 | 2020-02-11 | 美商哈尼威爾國際公司 | Copper manganese sputtering target |
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| JP2020537046A (en) * | 2017-10-13 | 2020-12-17 | ハネウェル・インターナショナル・インコーポレーテッドＨｏｎｅｙｗｅｌｌ Ｉｎｔｅｒｎａｔｉｏｎａｌ Ｉｎｃ． | Copper manganese sputtering target |
| US11035036B2 (en) | 2018-02-01 | 2021-06-15 | Honeywell International Inc. | Method of forming copper alloy sputtering targets with refined shape and microstructure |
| CN109338314A (en) * | 2018-12-04 | 2019-02-15 | 有研亿金新材料有限公司 | A kind of processing method of Ultra-fine grain copper manganese alloy target |
| CN114310159A (en) * | 2021-12-02 | 2022-04-12 | 上海交通大学 | Method for regulating and controlling rolling texture of in-situ synthesized particle reinforced aluminum-based composite material |
| CN114574822A (en) * | 2022-03-02 | 2022-06-03 | 基迈克材料科技（苏州）有限公司 | Preparation process and application of silver alloy target |
| CN114574822B (en) * | 2022-03-02 | 2024-01-30 | 基迈克材料科技（苏州）有限公司 | Silver alloy target preparation process and application |
| CN115161603A (en) * | 2022-05-17 | 2022-10-11 | 广东欧莱高新材料股份有限公司 | Production process of high-purity multi-element alloy rotary sputtering target for high-generation high-definition liquid crystal display |
| CN115161603B (en) * | 2022-05-17 | 2023-02-21 | 广东欧莱高新材料股份有限公司 | Production process of high-purity multi-element alloy rotary sputtering target for high-definition liquid crystal display of high generation |
| CN115029668A (en) * | 2022-06-02 | 2022-09-09 | 有研亿金新材料有限公司 | Method for preparing high-performance tantalum sputtering target material through pack rolling |
| CN115369365A (en) * | 2022-10-24 | 2022-11-22 | 有研亿金新材料有限公司 | Long-life sputtering target material and preparation method thereof |
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Application publication date: 20170215 |