CN103834924A - Method for preparing ultra-high purity aluminium and ultra-high purity aluminium alloy sputtering target material - Google Patents
Method for preparing ultra-high purity aluminium and ultra-high purity aluminium alloy sputtering target material Download PDFInfo
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- CN103834924A CN103834924A CN201310721649.8A CN201310721649A CN103834924A CN 103834924 A CN103834924 A CN 103834924A CN 201310721649 A CN201310721649 A CN 201310721649A CN 103834924 A CN103834924 A CN 103834924A
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Abstract
The invention discloses a method for preparing ultra-high purity aluminium and an ultra-high purity aluminium alloy sputtering target material. The method comprises the following steps of keeping the material for 24-48 hours at a temperature of 200 DEG C-500 DEG C; air cooling the material to a room temperature; putting a cast ingot into an elliptical mold; forging along an X direction until a deformation amount reaches 20%-40%; putting the cast ingot into a circular mold; forging along an Y direction until the deformation amount reaches 20%-40%; taking the cast ingot out from the mold; forging along a Z direction until the deformation amount reaches 70%; annealing the forged cast ingot at a temperature of 200-400 DEG C; rolling a forged sheet material for 8-20 times at a room temperature with the rolling amount of each time not less than 25%; rolling alternatively along the X direction and the Y direction; and annealing at the temperature of 200-400 DEG C to eliminate internal stress and refine grains of the material below 200 [mu]m. The ultra-high purity aluminium target material prepared by the method is fine and uniform in grains, stable in texture and high in material yield. The method is easy to operate and is convenient for large-scale production.
Description
Technical field
The invention belongs to metal, alloy material processing technology, be specifically related to a kind of ultra-pure aluminum and ultra-pure aluminum alloy sputtering targets material preparation method.
Technical background
Magnetron sputtering plating is a kind of novel physical vapor plated film mode, the evaporation coating mode of comparing, and its very many-sided advantage is quite obvious, as larger in the bonding force of rete and workpiece surface, the hardness of rete is higher, and wear resistance and erosion resistance are better, and the performance of rete is also more stable.As a comparatively proven technique having developed, magnetron sputtering has been applied to many fields.All be widely used at aspects such as semiconductor integrated circuit, recording medium, plane demonstration and surface coatings.
In the situation that sputtering technology is identical, the microstructure of sputtering target material directly affects the performance of sputtered film and the work-ing life of target, and target crystalline grains is more tiny, even, and sputter rate is faster, and the thickness evenness of sputtering deposit film is better.
Purity is up to the ultra-pure aluminum ingot casting of 5N-6N, and foreign matter content is very low, and the mechanism that hinders grain growth is little, larger to the control difficulty of its grain fineness number.Wherein viscous deformation is the comparatively common of ultra-pure aluminum grain refining, is also effective means comparatively.In order to obtain the tiny uniform rafifinal target of crystal grain, do a lot of research both at home and abroad.As waited corner extrusion method, multiway forging, hubbing etc.But for the large-sized ultra-pure aluminum target of preparation, and energy large-scale production, certain deficiency had.Chinese patent application, the patent No.: CN 1928129A, denomination of invention: a kind of method of preparing sputter target material, propose to adopt air hammer to carry out plastic working to aluminium ingot, by the method for plastic working and combined with heat treatment, reach the object of crystal grain thinning.Patent application, the patent No.: CN 102002653A, denomination of invention: the preparation method of a kind of superhigh-purity aluminum fine grain, high orientation target, this invention feature is to adopt the cold rolling working method of multidirectional flat-die forging and 0 ℃～5 ℃ to carry out crystal grain thinning.These method lumber recoverys are lower above, Working environment required also harsh.
Summary of the invention
The deficiency that object of the present invention exists for prior art, the present invention adopts die forging to be combined with free forging process, and the method for cold rolling and combined with heat treatment under room temperature is prepared the method for ultra-pure aluminum and ultra-pure aluminum alloy sputtering target.The present invention has overcome flat-die forging and the low problem of corner extrusion lumber recovery, greatly improves lumber recovery, because adopt the technique of rational rolling and heat treatment phase combination, can prepare the tiny even target of crystal grain simultaneously, meets the service requirements of PVD filming equipment.Lumber recovery is high, easy handling, be applicable to large-scale industrialization produce.
For achieving the above object, the present invention adopts technical scheme: the method that this prepares ultra-pure aluminum and ultra-pure aluminum alloy sputtering target, is characterized in that comprising the following steps:
(1) homogenizing: ultra-pure aluminum ingot casting or ultra-pure aluminum alloy cast ingot, at 200 ℃～500 ℃, are incubated after 24～48 hours, and air cooling is to room temperature;
(2) oval mould put into by ingot casting after treatment homogenizing by die forging: a., forges and presses along directions X, and deflection reaches 20%～40%; B. ingot casting is put into circular die, forge and press along Y-direction, deflection reaches 20%～40%;
(3) flat-die forging: ingot casting is taken out from mould, forge and press along Z direction, deflection reaches 70%;
(4) thermal treatment: the ingot casting after forging and stamping is carried out to anneal under 200～400 ℃ of conditions;
(5) rolling: by forging into aluminium sheet or the pure aluminum alloy plate of sheet material, at room temperature carry out 8～20 passage rollings, every time is pricked lower amount and is not less than 25%, and directions X and Y-direction replace rolling, and directions X is vertical with Y-direction;
(6) thermal treatment: the aluminium sheet after rolling or pure aluminum alloy plate are carried out to anneal under 200～400 ℃ of conditions, both eliminated internal stress, material grains is refined to below 200 μ m again, texture is take (200) as main.
Anneal in described step (4) is: take X → Y → Z+ thermal treatment as a circulation, and 8～10 circulations so repeatedly.
Adopt the beneficial effect of technique scheme: a kind of method of preparing ultra-pure aluminum and ultra-pure aluminum alloy sputtering target of the present invention, to adopt die forging to be combined with free forging process, the method of cold rolling and combined with heat treatment under room temperature, prepare the tiny uniform ultra-pure aluminum target of crystal grain, meet the service requirements of PVD filming equipment.Overcome flat-die forging and the low problem of corner extrusion lumber recovery, greatly improved lumber recovery, the ultra-pure aluminum target that uses present method to make, crystal grain is tiny evenly, and texture is stable, and lumber recovery is high, and easy handling, is convenient to large-scale industrial production.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, specific examples of the present invention is described in further detail.
Fig. 1 is ultra-pure aluminum forging and stamping schematic diagram, and the ingot casting that indicates X, Y-direction is put into oval mould, depresses along directions X, and circular ingot casting is pressed into oval ingot casting.
Fig. 2 is that oval ingot casting is pressed into circular ingot casting process schematic diagram.
Fig. 3 is the schematic diagram to the forging and stamping of ultra-pure aluminum ingot casting along Z direction.
Fig. 4 is in embodiment 1, the polarisation tissue of the large size ultra-pure aluminum sheet material being prepared into through forging and stamping mill-annealed.
Fig. 5 is in embodiment 1, the crystal grain texture structure of the large size ultra-pure aluminum sheet material being prepared into through forging and stamping mill-annealed.
Fig. 6 is in embodiment 2, the polarisation tissue of the large size ultra-pure aluminum sheet material being prepared into through forging and stamping mill-annealed.
Fig. 7 is in embodiment 2, the crystal grain texture structure of the large size ultra-pure aluminum sheet material being prepared into through forging and stamping mill-annealed.
Embodiment
Adopt die forging and cold-rolling process to prepare a method for ultra-pure aluminum target, adopt die forging to be combined with free forging process, under room temperature, the method for cold rolling and combined with heat treatment, prepares the tiny uniform ultra-pure aluminum target of crystal grain.
embodiment 1
A method of preparing ultra-pure aluminum and ultra-pure aluminum alloy sputtering target, specifically comprises the steps:
(1) homogenizing: the 5N ultra-pure aluminum ingot casting of Ф 400mm × 396mm, at 380 ℃, is incubated after 45 hours, and air cooling is to room temperature, and demarcates X, Y-direction on aluminium ingot cross section, and X, Y-direction are mutually vertical, demarcate Z direction in short transverse;
(2) oval mould put into by ingot casting after treatment homogenizing by die forging: a., forges and presses along directions X, and deflection reaches 25%, sees Fig. 1; B. ingot casting is put into circular die, forge and press along Y-direction, deflection reaches 25%, sees Fig. 2;
(3) flat-die forging: ingot casting is taken out from mould, forge and press with air hammer along Z direction, deflection reaches 70%, sees Fig. 3;
(4) anneal: the ingot casting after forging and stamping is carried out to anneal under 320 ℃ of conditions.Take X → Y → Z+ thermal treatment as a circulation, 8～10 circulations so repeatedly;
(5) rolling: will forge into the aluminium sheet of sheet material, at room temperature replace rolling 8～10 passages along directions X and Y-direction, every time rolls lower amount and is not less than 25%, and the final size after rolling is 1700 × 1500 × 19mm;
(6) thermal treatment: the ingot casting after forging and stamping is carried out to anneal according to certain program under 280 ℃ of conditions, eliminate internal stress, the grain-size of the ultra-pure aluminum target finally obtaining can reach below 200 μ m, and texture, take (200) as main, is shown in shown in Fig. 4,5.
embodiment 2
This prepares the method for ultra-pure aluminum and ultra-pure aluminum alloy sputtering target, and with embodiment 1 same steps, described ultra-pure aluminum ingot casting is that purity is 6N, is of a size of Ф 380mm × 420mm, and homogenizing treatment temp is 430 ℃, is incubated 35 hours, and air cooling is to room temperature.Die forging is totally 3 circulations, and rolling pass deflection is controlled at 35% left and right, finally must be of a size of 2100
×1400
×the aluminium sheet of 16mm.Aluminium sheet is carried out to 300 ℃ of insulations thermal treatment of 5 hours, obtain average grain size and be about 168 μ m, texture take (200) as main heterogeneous microstructure.As shown in Fig. 6 six, 7.
Claims (2)
1. a method of preparing ultra-pure aluminum and ultra-pure aluminum alloy sputtering target, is characterized in that comprising the following steps:
(1) homogenizing: ultra-pure aluminum ingot casting or ultra-pure aluminum alloy cast ingot, at 200 ℃～500 ℃, are incubated after 24～48 hours, and air cooling is to room temperature;
(2) oval mould put into by ingot casting after treatment homogenizing by die forging: a., forges and presses along directions X, and deflection reaches 20%～40%; B. ingot casting is put into circular die, forge and press along Y-direction, deflection reaches 20%～40%;
(3) flat-die forging: ingot casting is taken out from mould, forge and press along Z direction, deflection reaches 70%;
(4) thermal treatment: the ingot casting after forging and stamping is carried out to anneal under 200～400 ℃ of conditions;
(5) rolling: by forging into aluminium sheet or the pure aluminum alloy plate of sheet material, at room temperature carry out 8～20 passage rollings, every time is pricked lower amount and is not less than 25%, and directions X and Y-direction replace rolling, and directions X is vertical with Y-direction;
(6) thermal treatment: the aluminium sheet after rolling is carried out to anneal under 200～400 ℃ of conditions, both eliminated internal stress, and material grains is refined to below 200 μ m.
2. the method for preparing ultra-pure aluminum and ultra-pure aluminum alloy sputtering target as claimed in claim 1, is characterized in that the anneal in described step (4) is: take the thermal treatment of directions X → Y-direction → Z+ direction as a circulation, and 8～10 circulations so repeatedly.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104928625A (en) * | 2015-05-22 | 2015-09-23 | 沈阳富创精密设备有限公司 | Method for preparing high temperature creep resistant grounded substrate for semiconductor equipment through physical vapor deposition (PVD) |
| CN105525149A (en) * | 2014-09-29 | 2016-04-27 | 有研亿金新材料有限公司 | Method for preparing aluminum alloy sputtering target material |
| CN106282945A (en) * | 2016-09-26 | 2017-01-04 | 中铝瑞闽股份有限公司 | A kind of preparation method of ultra-pure aluminum target |
| CN106947926A (en) * | 2017-04-21 | 2017-07-14 | 中铝瑞闽股份有限公司 | A kind of preparation method of large scale rafifinal target |
| CN107119244A (en) * | 2017-06-06 | 2017-09-01 | 东南大学 | A kind of preparation method of high preferred orientation fine grain ultra-pure aluminum target |
| CN109518140A (en) * | 2018-11-28 | 2019-03-26 | 河北冠靶科技有限公司 | A kind of preparation method of ultra-pure, isometric fine grain aluminium target |
| CN110000211A (en) * | 2018-01-05 | 2019-07-12 | 宁波江丰电子材料股份有限公司 | Target milling method |
| CN110709532A (en) * | 2017-06-22 | 2020-01-17 | 株式会社Uacj | Sputtering target material, sputtering target, aluminum plate for sputtering target, and method for producing same |
| CN112538598A (en) * | 2020-12-02 | 2021-03-23 | 爱发科电子材料（苏州）有限公司 | Manufacturing method of aluminum-silicon target material |
| CN113025972A (en) * | 2021-03-01 | 2021-06-25 | 宁波江丰电子材料股份有限公司 | Manufacturing method of aluminum target material |
| CN113755801A (en) * | 2021-09-17 | 2021-12-07 | 福州大学 | Preparation method of high-purity aluminum target material with uniform orientation |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105525149A (en) * | 2014-09-29 | 2016-04-27 | 有研亿金新材料有限公司 | Method for preparing aluminum alloy sputtering target material |
| CN104928625A (en) * | 2015-05-22 | 2015-09-23 | 沈阳富创精密设备有限公司 | Method for preparing high temperature creep resistant grounded substrate for semiconductor equipment through physical vapor deposition (PVD) |
| CN104928625B (en) * | 2015-05-22 | 2017-06-16 | 沈阳富创精密设备有限公司 | A kind of PVD prepares the method that semiconductor equipment high temperature creep-resisting is grounded substrate |
| CN106282945A (en) * | 2016-09-26 | 2017-01-04 | 中铝瑞闽股份有限公司 | A kind of preparation method of ultra-pure aluminum target |
| CN106947926B (en) * | 2017-04-21 | 2018-04-03 | 中铝瑞闽股份有限公司 | A kind of preparation method of large scale rafifinal target |
| CN106947926A (en) * | 2017-04-21 | 2017-07-14 | 中铝瑞闽股份有限公司 | A kind of preparation method of large scale rafifinal target |
| CN107119244A (en) * | 2017-06-06 | 2017-09-01 | 东南大学 | A kind of preparation method of high preferred orientation fine grain ultra-pure aluminum target |
| CN110709532A (en) * | 2017-06-22 | 2020-01-17 | 株式会社Uacj | Sputtering target material, sputtering target, aluminum plate for sputtering target, and method for producing same |
| US11618942B2 (en) | 2017-06-22 | 2023-04-04 | Uacj Corporation | Sputtering-target material, sputtering target, sputtering-target aluminum plate, and method of manufacturing the same |
| CN110000211A (en) * | 2018-01-05 | 2019-07-12 | 宁波江丰电子材料股份有限公司 | Target milling method |
| CN109518140A (en) * | 2018-11-28 | 2019-03-26 | 河北冠靶科技有限公司 | A kind of preparation method of ultra-pure, isometric fine grain aluminium target |
| CN112538598A (en) * | 2020-12-02 | 2021-03-23 | 爱发科电子材料（苏州）有限公司 | Manufacturing method of aluminum-silicon target material |
| CN113025972A (en) * | 2021-03-01 | 2021-06-25 | 宁波江丰电子材料股份有限公司 | Manufacturing method of aluminum target material |
| CN113755801A (en) * | 2021-09-17 | 2021-12-07 | 福州大学 | Preparation method of high-purity aluminum target material with uniform orientation |
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