CN102000702A - Processing technology of high-purity tantalum sputtering target material - Google Patents
Processing technology of high-purity tantalum sputtering target material Download PDFInfo
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Abstract
The invention discloses a processing technology of a high-purity tantalum sputtering target material. By the processing technology, a round billet of the hammer cogged tantalum sputtering target material is subjected to the rolling treatment. The processing technology is characterized in that the rolling can be carried out after the rolling direction is rotated by 135 degrees when a pass is rolled in the rolling process and the arc-thickness ratio of reduction in pass is controlled to be 2-3. The total rolling passes are required to be matched with the arc-thickness ratio and the total deformation quantity which is 90 percent. According to the processing technology provided by the invention, by adjusting process parameters, the crystallite dimension on the sputtering surface can be controlled to be 100+/-20mu m, the content of a gamma structure can be controlled to be 30-60 percent and the content of a random texture can be controlled to be 30-60 percent. The center and middle of the sputtering surface, the crystallite dimension and the texture distribution can reach the standards and the crystallite dimension can be controlled to be 100+/-15mu m along the thickness direction. The crystallite dimension and the texture distribution can completely meet the industrial production requirement. The processing technology is simple and the control means is reliable and effective.
Description
Technical field
The present invention relates to the sputtering target material technical field, particularly a kind of processing technology of High-purity Tantalum sputtering target material.
Background technology
Sputter is the main mode of preparation thin-film material, the ion that it utilizes ion gun to produce, assemble through quickening in a vacuum, and formation has the ion beam current of high energy, bombard the surface of solids, ion and surface of solids atom generation exchange of kinetic energy are bombarded the atom of the surface of solids, thereby are left solid and be deposited on substrate surface.The solid that is bombarded is with the raw material of sputtering method deposit film, is called sputtering target material, and sputtering target material is the crucial consumptive material that is used for this technology.
The grain size of sputtering target material and grain orientation directly influence the quality of its sputtering performance and sputtered film, and main performance has: along with the increase of crystallite dimension, film deposition rate is and reduces trend gradually.The target crystallite dimension is in OK range, and then film deposition rate height and film gauge uniformity are good during sputter.Therefore, the uniformity of the average grain size of target size and crystallite dimension is one of key element that influences the target as sputter performance.Great scale integrated circuit should have suitable crystallite dimension with the semiconductor sputtering target material, and guarantees its uniformity, and in certain grain size range, the grain orientation uniformity of target is strong more good more.
High-purity Ta (tantalum) sputtering target material is widely used in the electronics and information products manufacturing, as the sputter barrier layer, will progressively replace aluminium to become the material of metallization wiring on the silicon chip with high purity copper, is used widely.The crystallite dimension size of high-purity Ta sputtering target material, structural homogenity and grain orientation distribute has fundamental influence to sputtering performance.Along with the increase of semiconductor silicon chip size, the size of sputtering target material is also to large scale development, for guaranteeing the uniformity of quality between same target and the different batches large scale semiconductor sputtering target material, thereby guarantees the quality and the yield rate of different batches sputtered film.To target thickness direction, sputter face direction Microstructure Uniformity, distribution of orientations control has proposed strict more requirement.
Plastic deformation and heat treatment process are the microstructure of control sputtering target material and the key production technology thereof of orientation control, comprise the homogenising heat treatment of ingot casting, circumferential/axially operations such as hammer cogging, annealing in process, cold rolling, recrystallization annealing.Usually can pass through annealing in process for the former billet behind circumferential/axially hammer cogging, the cold rolling pass deformation quantity, crystallization heat processing etc. cooperatively interacts to adjust and controls the target quality again.
At present and since to microstructure in plastic processing and the heat treatment process develop and and processing technology between relation understanding not enough, the microstructure of high-purity Ta sputtering target material and orientation control are the key problem in technology points of high-purity Ta sputtering target material processing.Therefore, the structural homogenity how to control as far as possible on the thickness direction under microstructure on the assurance sputter face and the inhomogeneity prerequisite of orientation control is the problem that semiconductor sputtering target material manufacture field is needed solution badly.
Summary of the invention
In view of this, the invention provides a kind of processing technology of High-purity Tantalum sputtering target material, with the purpose of microstructure and orientation stability on the sputter face that realizes sputtering target material and the thickness direction.
For achieving the above object, the invention provides following technical scheme:
A kind of processing technology of High-purity Tantalum sputtering target material, tantalum spattering target material behind hammer cogging circle base is rolled processing, every rolling a time is rolled behind 5 ° of the rolling direction ROT13s in the operation of rolling, and until a rolling week, and the arc thickness rate of reduction in pass is controlled at 2～3.
Preferably, in the processing technology of above-mentioned High-purity Tantalum sputtering target material, the arc thickness rate of reduction in pass is controlled at 2.5.
Preferably, in the processing technology of above-mentioned High-purity Tantalum sputtering target material, described arc thickness rate L/d=R * arccos (1-Δ h/2R)/(H-Δ h/2), wherein R is the milling train radius, and Δ h is a reduction in pass, and H is the original depth of each passage.
Preferably, in the processing technology of above-mentioned High-purity Tantalum sputtering target material, be tantalum spattering target material circle base more than 90% for deformation quantity, deformation quantity is distributed in 16 passages.
Preferably, in the processing technology of above-mentioned High-purity Tantalum sputtering target material, be 90% tantalum spattering target material circle base for deformation quantity, after rolling, carry out vacuum annealing, annealing temperature is controlled at 1050 ± 10 ℃, and vacuum values sets 0.8 * 10
-2Pa～1 * 10
-2Pa, annealing time were controlled at 35～55 minutes, and cool off with stove the annealing back.
Preferably, in the processing technology of above-mentioned High-purity Tantalum sputtering target material, described vacuum values is 10
-2Pa, annealing time were controlled at 45 minutes.
From above-mentioned technical scheme as can be seen, by adopting processing technology provided by the invention, empirical tests as can be known, the crystallite dimension of sputter face can be controlled at 150 ± 15 μ m, grain orientation can be realized 80% γ texture and 20% texture at random, sputter face distributes along radial direction heart portion, middle part, limit portion crystallite dimension and texture all can reach above standard, can be controlled at 100 ± 10 μ m along the thickness direction crystallite dimension.Above crystallite dimension and texture distribute can satisfy the industrial production demand fully, and processing technology is simple, and control device is reliably effective.
The specific embodiment
The invention discloses a kind of processing technology of High-purity Tantalum sputtering target material, with the purpose of microstructure and orientation stability on the sputter face that realizes sputtering target material and the thickness direction.
Below in conjunction with the accompanying drawing in the embodiment of the invention, the technical scheme in the embodiment of the invention is clearly and completely described, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills belong to the scope of protection of the invention not making the every other embodiment that is obtained under the creative work prerequisite.
The processing technology of High-purity Tantalum sputtering target material provided by the invention, need the circle of the tantalum spattering target material behind hammer cogging base is rolled processing, of the present invention focusing on, every rolling a time is rolled behind 0～140 ° of the rolling direction ROT13 in the operation of rolling, until a rolling week.Be that each passage rolling direction and last a time rolling direction angle are controlled in 130～140 ° of scopes.For the circle base, about 8 passages of every process can be finished the rolling of whole disc direction.The arc thickness rate of every time drafts is controlled in 2～3 scopes.
By adopting processing technology provided by the invention, empirical tests as can be known, the crystallite dimension of sputter face can be controlled at 150 ± 15 μ m, grain orientation can be realized 80% γ texture and 20% texture at random, sputter face distributes along radial direction heart portion, middle part, limit portion crystallite dimension and texture all can reach above standard, can be controlled at 100 ± 10 μ m along the thickness direction crystallite dimension.Above crystallite dimension and texture distribute can satisfy the industrial production demand fully, and processing technology is simple, and control device is reliably effective.
Every rolling a time can be preferential in the operation of rolling with 5 ° of rolling direction ROT13s, promptly for the circle base, whenever can finish the rolling of whole disc direction through 8 passages.For deformation quantity is tantalum spattering target material circle base more than 90%, and deformation quantity is matched with the arc thickness rate is distributed in 16 passages,
The arc thickness rate of reduction in pass preferentially is controlled at 2.5.Wherein, arc thickness rate L/d=R * arccos (1-Δ h/2R)/(H-Δ h/2), wherein R is the milling train radius, and Δ h is a reduction in pass, and H is the original depth of each passage, and L is the arc length of reduction in pass, d is the thickness of reduction in pass.
For deformation quantity is 90% tantalum spattering target material circle base, also can carry out vacuum annealing after rolling, and annealing temperature is controlled at 1050 ± 10 ℃, and vacuum values sets 0.8 * 10
-2Pa～1 * 10
-2Pa, annealing time were controlled at 35～55 minutes, and cool off with stove the annealing back.Preferred vacuum values is 10-2Pa, and annealing time was controlled at 45 minutes.
Each embodiment adopts the mode of going forward one by one to describe in this specification, and what each embodiment stressed all is and the difference of other embodiment that identical similar part is mutually referring to getting final product between each embodiment.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be conspicuous concerning those skilled in the art, and defined herein General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet and principle disclosed herein and features of novelty the wideest corresponding to scope.
Claims (6)
1. the processing technology of a High-purity Tantalum sputtering target material, tantalum spattering target material behind hammer cogging circle base is rolled processing, it is characterized in that, be rolled behind 5 ° of the rolling direction ROT13s in the every rolling a time of the operation of rolling, until a rolling week, and the arc thickness rate of reduction in pass is controlled at 2～3.
2. the processing technology of High-purity Tantalum sputtering target material as claimed in claim 1 is characterized in that, the arc thickness rate of reduction in pass is controlled at 2.5.
3. the processing technology of High-purity Tantalum sputtering target material as claimed in claim 1 is characterized in that, described arc thickness rate L/d=R * arccos (1-Δ h/2R)/(H-Δ h/2), and wherein R is the milling train radius, and Δ h is a reduction in pass, and H is the original depth of each passage.
4. the processing technology of High-purity Tantalum sputtering target material as claimed in claim 1 is characterized in that, is tantalum spattering target material circle base more than 90% for deformation quantity, and deformation quantity is distributed in 16 passages.
5. as the processing technology of each described High-purity Tantalum sputtering target material of claim 1-4, it is characterized in that, is 90% tantalum spattering target material circle base for deformation quantity, carries out vacuum annealing after rolling, and annealing temperature is controlled at 1050 ± 10 ℃, and vacuum values sets 0.8 * 10
-2Pa～1 * 10
-2Pa, annealing time were controlled at 35～55 minutes, and cool off with stove the annealing back.
6. the processing technology of High-purity Tantalum sputtering target material as claimed in claim 5 is characterized in that, described vacuum values is 10
-2Pa, annealing time were controlled at 45 minutes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010599296A CN102000702B (en) | 2010-12-21 | 2010-12-21 | Processing technology of high-purity tantalum sputtering target material |
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| CN201010599296A CN102000702B (en) | 2010-12-21 | 2010-12-21 | Processing technology of high-purity tantalum sputtering target material |
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| CN102000702A true CN102000702A (en) | 2011-04-06 |
| CN102000702B CN102000702B (en) | 2012-09-26 |
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| CN201010599296A Expired - Fee Related CN102000702B (en) | 2010-12-21 | 2010-12-21 | Processing technology of high-purity tantalum sputtering target material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102296272A (en) * | 2011-08-17 | 2011-12-28 | 宁波江丰电子材料有限公司 | Manufacturing method of tantalum target material |
| CN102350439A (en) * | 2011-09-23 | 2012-02-15 | 宁波江丰电子材料有限公司 | Hot rolling method for nickel target billet used for semiconductor |
| CN112410699A (en) * | 2020-11-11 | 2021-02-26 | 西安诺博尔稀贵金属材料股份有限公司 | Method for optimizing grain size and uniformity of tantalum plate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002014576A1 (en) * | 2000-08-15 | 2002-02-21 | Honeywell International Inc. | Sputtering target |
| CN1370853A (en) * | 2001-02-23 | 2002-09-25 | 光洋应用材料科技股份有限公司 | Production process of metal sputtering target |
| CN1524977A (en) * | 1999-12-23 | 2004-09-01 | 西南交通大学 | Artificial organs surface treatment method using sputtering technology |
-
2010
- 2010-12-21 CN CN201010599296A patent/CN102000702B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1524977A (en) * | 1999-12-23 | 2004-09-01 | 西南交通大学 | Artificial organs surface treatment method using sputtering technology |
| WO2002014576A1 (en) * | 2000-08-15 | 2002-02-21 | Honeywell International Inc. | Sputtering target |
| CN1370853A (en) * | 2001-02-23 | 2002-09-25 | 光洋应用材料科技股份有限公司 | Production process of metal sputtering target |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102296272A (en) * | 2011-08-17 | 2011-12-28 | 宁波江丰电子材料有限公司 | Manufacturing method of tantalum target material |
| CN102296272B (en) * | 2011-08-17 | 2013-09-04 | 宁波江丰电子材料有限公司 | Manufacturing method of tantalum target material |
| CN102350439A (en) * | 2011-09-23 | 2012-02-15 | 宁波江丰电子材料有限公司 | Hot rolling method for nickel target billet used for semiconductor |
| CN102350439B (en) * | 2011-09-23 | 2014-04-23 | 宁波江丰电子材料有限公司 | Hot rolling method for nickel target billet used for semiconductor |
| CN112410699A (en) * | 2020-11-11 | 2021-02-26 | 西安诺博尔稀贵金属材料股份有限公司 | Method for optimizing grain size and uniformity of tantalum plate |
| CN112410699B (en) * | 2020-11-11 | 2022-05-27 | 西安诺博尔稀贵金属材料股份有限公司 | Method for optimizing grain size and uniformity of tantalum plate |
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| CN102000702B (en) | 2012-09-26 |
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