CN100420757C - Method for preparing sputtering target material - Google Patents
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- CN100420757C CN100420757C CNB2006100537163A CN200610053716A CN100420757C CN 100420757 C CN100420757 C CN 100420757C CN B2006100537163 A CNB2006100537163 A CN B2006100537163A CN 200610053716 A CN200610053716 A CN 200610053716A CN 100420757 C CN100420757 C CN 100420757C
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Abstract
The sputtering target material preparing process includes mutually combined plastic working and heat treatment. During the preparing process, are used a pneumatic hammer as plastic working unit, a range limiting standard block for the control of material deformation, a unit to change the stress surface and thus the material deformation direction and a surface temperature detector to monitor the temperature. Compared with available technology, the present invention has the advantages of ensured working repeatability and controllability, simple working process, low cost, high efficiency, etc.
Description
Technical field
The present invention relates to a kind of method of material preparation, particularly a kind of method for preparing sputter target material.
Background technology
The quality of the film that forms on silicon chip by the physical vapor deposition sputtering method can be subjected to being used for the influence of the target material surface roughness of sputter.The surfaceness of target is relevant with the grain size of target.Generally speaking, crystal grain is thin more, and the surfaceness of target is more little.Therefore, can be by reducing target grain-size size, crystal grain thinning correspondingly reduces the target surfaces roughness, and sputtering sedimentation goes out than the better film of the film quality that is formed by the target with greater particle size crystal grain thus.The factor that influences the target performance is except that grain size, and also having an important factor is target tissue, it is generally acknowledged＜220〉orientation account for leading crystal structure in the target performance that has the best aspect deposition and the film equality.
Many materials can be used for making target, more representational aluminium and aluminium alloy, refractory metal base alloy (W, Mo, Ti, Ta, Zr, Nb), metal silicide (MoSix, WSix, NiSix etc.), platinum metals etc. of being to use.In the target that these materials are made important a kind of be aluminium and the aluminium alloy target that forms aluminium wiring usefulness.Target also can comprise the high-purity forms of concrete metallic substance, exemplary target is made up of (or basically by) rafifinal and aluminium alloy, wherein rafifinal is the aluminium of at least 99.99% (4N) purity, and preferred at least 99.9999% (5N) purity, and percentage ratio is atomic percent.Except that aluminium, described alumina-bearing material also comprises elements Si, Cu, Ti, Cr, Mn, Zr, Hf and rare earth element etc.Other element total amounts that join in the target material aluminium are generally 0.01-10% weight.
Had multiple about forming the method for improved target structure before.For example: Chinese patent CN1409773A " method for preparing sputtering target material ", this patent has been introduced a kind of method for preparing sputtering target material.This method is that the processing speed of processing per-cent and at least 100%/second with at least 5% is carried out plastic working to metallic substance.And the temperature variation in the control material course of processing.Grain fineness number size that like this can the good control material.Be mainly used in the making of targets such as fine aluminium, pure titanium, fine copper.But greater than 100%/second the plastic working of two-forty in actually operating, be very difficult to control, the speed of each plastic working and distortion of materials amount also are difficult to calculate and determine.Aspect commercial scale production, be difficult to very high repeatability that requires processing units and production technique and controllability.Therefore demand developing the alternative method of new preparation sputtering target material urgently.
Summary of the invention
Technical problem to be solved by this invention provides the method for preparing sputter target material that a kind of controllability and good reproducibility and suitable large-scale industrialization are produced.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: this prepares the method for sputter target material, and it comprises: utilize the effect of mutually combining of plastic working and thermal treatment process, aluminum or aluminum alloy is prepared into sputter target material, concrete steps are as follows:
(1) utilize process furnace that material evenly is preheated to 130-170 ℃;
(2) utilize plastic working equipment that material is carried out plastic working perpendicular to axial direction, process temperature is controlled at below 250 ℃;
(3) use heat treatment furnace that material is carried out temperature 250-500 ℃ heat treatment process, carry out water-cooled behind the insulation certain hour;
(4) this material evenly is preheated to 130-170 ℃ once more;
(5) utilize plastic working equipment that material is parallel to axial plastic working, process temperature is controlled at below 250 ℃.
In order to obtain the material grains of desired different size, can make described step (1)-(5) repeated interaction effect three to five times, the material deformation amount is controlled at 70-80%.
Plastic working equipment can be chosen general forging equipment etc., but preferably air hammer is a plastic working equipment, and mode is simple, and equipment drops into little, and the working (machining) efficiency height, process repeatability, and controllability is good.
Utilize air hammer as controllability plastic working equipment, accurate control plastic history that can be more convenient is by limit journey spare part calibrated bolck control material deflection, by the variation control material deformation direction of thrust surface.
For the temperature of strictness control plastic history, can pass through surface temperature detector observation process temperature.
Materials such as aluminium, titanium, copper can be used as through the material of suitable processing with crystal grain thinning, are preferably aluminium or aluminium alloy.
Described material has aluminium grain after processing, the average crystal grain size is lower than 100 μ m.
Described material has certain microstructure texture orientation after processing.
During plastic working, can be sputtering target with material forming.
Compared with prior art, the invention has the advantages that utilization by this controllability plastic working of air hammer equipment, make that not only repeatability, the controllability of processing units and complete processing are guaranteed, and processing mode is simple, equipment drops into little, efficient is also higher, and is also more simple to operator's requirement; By controlling, can realize control simultaneously, obtain desired grain size of people and microstructure texture orientation the material grains size with the various combination of thermal treatment process.
Description of drawings
Fig. 1 is embodiment of the invention plastic working facilities air hammer action principle figure;
Fig. 2 is an embodiment of the invention plastic processing synoptic diagram.
Embodiment
As shown in Figure 1, use air hammer to be plastic working equipment, the specification of air hammer is that to fall nominal weight be 750 kilograms to tup 1, hammer stem helical pitch bottom surface to the distance of air hammering platform 3 is 670mm, it is 105 times/minute that tup 1 impacts number of times, by using the limit journey spare part calibrated bolck 2 control material deflections of 0-670mm, by cylindrical aluminium ingot being processed into tetrahedron, hexahedron controlled deformation direction; Aluminum ingot temperature is controlled at below 250 ℃ in the process, monitors by surface temperature detector, and heat treatment process is carried out in box heat treatment furnace, and temperature is controlled at 250-500 ℃.
Embodiment one
Prepare φ 180X60L, purity is that the thermoplasticity procedure of processing (a) that the cylindrical aluminium ingot of 99.99% weight carries out as shown in Figure 2 arrives (e).At first, use preheating oven to material preheater to 130 ℃, utilize air hammer to obtain workpiece (a) φ 110X160L by the cylindrical aluminium ingot of starting material through processing perpendicular to axial direction, need in the process to expend the long time, about 20 minutes, materials processing finishes the back temperature test and reaches about 240 ℃, and temperature test finishes the back material and carries out water-cooled to room temperature at once; Reuse preheating oven to material preheater to 130 ℃, obtain workpiece (b) φ 87.5X237L through axial plastic working, in the process about 20 minutes consuming time, materials processing finished the back temperature test and reaches about 240 ℃, and temperature test finishes the back material and carries out water-cooled to room temperature at once; Obtain workpiece (c) φ 87.5X237L by heat treatment process then, again through using preheating oven to material preheater to 130 ℃, processing perpendicular to axial direction obtains workpiece (d) φ 162X68L workpiece, in the process 20 minutes consuming time approximately, the materials processing end is after temperature test reaches about 240 ℃, and temperature test finishes back material horse back water-cooled to room temperature; Use rolling press to carry out processing perpendicular to axial direction at last and obtain (e) φ 210X40L target.Concrete parameter is shown in Table 1; Described thermoplasticity procedure of processing (a) to (d) is carried out three times continuously.
Table 1 thermoplasticity machined parameters
| Processing mode | Processing per-cent (%) | Condition | Final size (diameter mm * length) | |
| (a) | Axially plastic working | 38.9％ | The calibrated bolck of H=110mm | 110X160 |
| (b) | Axially plastic working | 20.5％ | The calibrated bolck of H=87.5mm | 87.5X237 |
| (c) | Thermal treatment | 490℃X15min | 87.5X237 | |
| (d) | The vertical axial plastic working | 71.3％ | The calibrated bolck of H=68mm | 162X68 |
| (e) | The vertical axial plastic working | 41.2％ | Use rolling press | 210X40 |
With the target material surface that sand paper polishes or machined into obtained, the necessary turning in surface is greater than 1mm, carry out electropolishing and corrosion then and demonstrate its crystal boundary, observe down and take a picture at 100 times by opticmicroscope, it is 100 μ m that the photo that obtains is measured the average crystal grain size by the straight line resection, homogeneous grain size on the whole observation surface;
With the surface of sand paper polishing or target that machined into obtains, the necessary turning in surface uses the XRD-X x ray diffractometer x to detect greater than 1mm then, analyzes as can be known by the data that draw, and workpiece survey face (220) texture orientation accounts for leading.
Each viscous deformation first being processed uses process furnace that material is carried out preheating in the above operation, mainly is in order to improve the flowability of material in the viscous deformation course of processing, to prevent the material cracking.If but preheating temperature is lower than 130 ℃, because itself having heat, the viscous deformation course of processing produces, the materials processing temperature is raise, through long viscous deformation, after viscous deformation finished, what material temperature raise probably surpassed 250 ℃, caused the internal performance of target to change.
Embodiment two
Prepare φ 180X60L, purity is that the thermoplasticity procedure of processing (a) that the cylindrical aluminium ingot of 99.99% weight carries out as shown in Figure 2 arrives (e).At first, use preheating oven to material preheater to 150 ℃, utilize air hammer to obtain workpiece (a) φ 110X160L by the cylindrical aluminium ingot of starting material through processing perpendicular to axial direction, in the process about 15 minutes consuming time, materials processing finishes the back temperature test and reaches about 220 ℃, and temperature test finishes the back material and carries out water-cooled to room temperature at once; Reuse preheating oven to material preheater to 150 ℃, obtain workpiece (b) φ 87.5X237L through axial plastic working, in the process about 10 minutes consuming time, materials processing finished the back temperature test and reaches about 220 ℃, and temperature test finishes the back material and carries out water-cooled to room temperature at once; Obtain workpiece (c) φ 87.5X237L by heat treatment process then, again through using preheating oven to material preheater to 150 ℃, processing perpendicular to axial direction obtains workpiece (d) φ 162X68L workpiece, in the process about 10 minutes consuming time, materials processing finishes the back temperature test and reaches about 220 ℃, and temperature test finishes the back material and carries out water-cooled to room temperature at once; Use rolling press to carry out processing perpendicular to axial direction at last and obtain (e) φ 210X40L target.Concrete parameter is shown in Table 1; Described thermoplasticity procedure of processing (a) to (d) is carried out three times continuously,
With the target material surface that sand paper polishes or machined into obtained, the necessary turning in surface is greater than 1mm, carry out electropolishing and corrosion then and demonstrate its crystal boundary, observe down and take a picture at 100 times by opticmicroscope, it is 100 μ m that the photo that obtains is measured the average crystal grain size by the straight line resection, homogeneous grain size on the whole observation surface;
With the surface of sand paper polishing or target that machined into obtains, the necessary turning in surface uses the XRD-X x ray diffractometer x to detect greater than 1mm then, analyzes as can be known by the data that draw, and workpiece survey face (220) texture orientation accounts for leading.
Each viscous deformation first being processed uses process furnace that material is carried out preheating in the above operation, mainly is in order to improve the flowability of material in the viscous deformation course of processing, to prevent the material cracking.With material preheater to 150 ℃, the flowability of material has improved, and has prevented the cracking of material in plastic history among the above embodiment.And after viscous deformation finished, material temperature raise and is no more than 250 ℃, and the internal performance of material does not change, and satisfies the target performance requriements.
Embodiment three
Prepare φ 180X60L, purity is that the thermoplasticity procedure of processing (a) that the cylindrical aluminium ingot of 99.99% weight carries out as shown in Figure 2 arrives (e).At first, use preheating oven to material preheater to 170 ℃, utilize air hammer to obtain workpiece (a) φ 110X160L by the cylindrical aluminium ingot of starting material through processing perpendicular to axial direction, in the process about 10 minutes consuming time, materials processing finishes the back temperature test and reaches about 240 ℃, and temperature test finishes the back and material water is chilled to room temperature at once; Reuse preheating oven to material preheater to 170 ℃, obtain workpiece (b) φ 87.5X237L through axial plastic working, in the process about 10 minutes consuming time, materials processing finished the back temperature test and reaches about 240 ℃, and temperature test finishes the back material and carries out water-cooled to room temperature at once; Obtain workpiece (c) φ 87.5X237L by heat treatment process then, again through using preheating oven to material preheater to 170 ℃, processing perpendicular to axial direction obtains workpiece (d) φ 162X68L workpiece, in the process about 10 minutes consuming time, materials processing finishes the back temperature test and reaches about 240 ℃, and temperature test finishes the back material and carries out water-cooled to room temperature at once; Use rolling press to carry out processing perpendicular to axial direction at last and obtain (e) φ 210X40L target.Concrete parameter is shown in Table 1; Described thermoplasticity procedure of processing (a) to (d) is carried out three times continuously,
With the target material surface that sand paper polishes or machined into obtained, the necessary turning in surface is greater than 1mm, carry out electropolishing and corrosion then and demonstrate its crystal boundary, observe down and take a picture at 100 times by opticmicroscope, it is 100 μ m that the photo that obtains is measured the average crystal grain size by the straight line resection, homogeneous grain size on the whole observation surface;
With the surface of sand paper polishing or target that machined into obtains, the necessary turning in surface uses the XRD-X x ray diffractometer x to detect greater than 1mm then, analyzes as can be known by the data that draw, and workpiece survey face (220) texture orientation accounts for leading.
The viscous deformation first being processed uses process furnace that material is carried out preheating in the above operation, mainly is in order to improve the flowability of material in the viscous deformation course of processing, to prevent the material cracking.If but preheating temperature is higher than 170 ℃, because the viscous deformation course of processing itself has heat and produces, the materials processing temperature is raise, viscous deformation always needs certain hour, because preheating temperature height, after viscous deformation finished, what material temperature raise probably surpassed 250 ℃, caused the internal performance of target to change.
More than among three embodiment, one of mode of the grain-size of control machined material is to utilize plastic working.Term " plastic working " is the processing of instigating the starting material distortion.Exemplary plastic processing method is stretched for forging, jumping-up.
This original distortion per-cent in back (per-cent that diameter reduces be satin stretch the per-cent that per-cent, thickness reduces be the per-cent of jumping-up) of handling is called as " processing per-cent ".
For the present invention, heat treatment process all is to need to carry out water-cooled behind the insulation certain hour, this soaking time is relevant with thermal treatment temp and the required grain-size that obtains, published in 1996 in press of Harbin Institute of Technology, provide related description in the 308th to 309 page of Li Chao chief editor's " Principles of Metallography ", supposed D
0Be the mean diameter of initial crystal grain, through the average grain diameter D behind the soaking time t
tFor:
D
t＝k
1e
-Qm/RTt
n
Wherein T is a thermal treatment temp, k
1Be constant, relevant with the metalline of material, Qm is the intensity of activation of crystal boundary migration or the atomic diffusion intensity of activation by crystal boundary, R, e is constant, n be one less than 1/2 empirical constant, can infer according to actual tests.
Can go out needed thermal treatment soaking time according to the above-mentioned derivation of equation.
As in embodiments of the present invention, to wish to obtain the average crystal grain size about 100 μ m, and selected 490 ℃ thermal treatment temp, the thermal treatment soaking time that can calculate needs according to this formula is 15min, and is as shown in table 1.
Claims (8)
1. method for preparing sputter target material, it comprises: utilize the effect of mutually combining of plastic working and thermal treatment process, aluminum or aluminum alloy is prepared into sputter target material, concrete steps are as follows:
(1) utilize process furnace that material evenly is preheated to 130-170 ℃;
(2) utilize plastic working equipment that material is carried out plastic working perpendicular to axial direction, process temperature is controlled at below 250 ℃;
(3) use heat treatment furnace that material is carried out temperature 250-500 ℃ heat treatment process, carry out water-cooled behind the insulation certain hour;
(4) this material evenly is preheated to 130-170 ℃ once more;
(5) utilize plastic working equipment that material is parallel to axial plastic working, process temperature is controlled at below 250 ℃.
2. the method for preparing sputter target material according to claim 1 is characterized in that: described step (1)-(5) repeated interaction effect three to five times, the material deformation amount is controlled at 70-80%.
3. the method for preparing sputter target material according to claim 1 is characterized in that: described plastic working equipment is air hammer.
4. the method for preparing sputter target material according to claim 3 is characterized in that: described air hammer is a controllability plastic working equipment, by limit journey spare part calibrated bolck control material deflection, by the variation control material deformation direction of thrust surface.
5. the method for preparing sputter target material according to claim 1 is characterized in that: described process temperature is monitored by surface temperature detector.
6. the method for preparing sputter target material according to claim 1 is characterized in that: described material has aluminium grain after processing, and the average crystal grain size is lower than 100 μ m.
7. the method for preparing sputter target material according to claim 1 is characterized in that: described material has certain microstructure texture orientation after processing.
8. the method for preparing sputter target material according to claim 1 is characterized in that: also comprise material is configured as sputtering target during plastic working.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624695B (en) * | 2009-08-11 | 2011-02-09 | 宁波江丰电子材料有限公司 | Heat treatment method of target blank |
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| CN101624694B (en) * | 2009-08-11 | 2011-01-26 | 宁波江丰电子材料有限公司 | Target heat treatment method |
| CN104694888B (en) * | 2013-12-09 | 2017-05-10 | 有研亿金新材料股份有限公司 | Preparation method of high-purity copper target |
| CN104746020B (en) * | 2013-12-27 | 2017-07-04 | 有研亿金新材料股份有限公司 | A kind of processing method of copper alloy target |
| CN111001662B (en) * | 2018-10-08 | 2021-05-11 | 合肥江丰电子材料有限公司 | Monitoring method and monitoring system for rolling deformation of test target |
| CN110484874A (en) * | 2019-08-16 | 2019-11-22 | 韶关市欧莱高新材料有限公司 | A kind of preparation method of high-purity aluminum pipe sputtering target material |
| CN112063976B (en) * | 2020-09-11 | 2022-08-30 | 宁波江丰电子材料股份有限公司 | Ultrahigh-purity copper target material and grain control method thereof |
| CN112921287B (en) * | 2021-01-22 | 2022-10-28 | 宁波江丰电子材料股份有限公司 | Ultrahigh-purity copper target material and grain orientation control method thereof |
| CN113046705B (en) * | 2021-03-16 | 2022-08-16 | 宁波江丰电子材料股份有限公司 | Copper target material and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5282946A (en) * | 1991-08-30 | 1994-02-01 | Mitsubishi Materials Corporation | Platinum-cobalt alloy sputtering target and method for manufacturing same |
| US5993575A (en) * | 1996-11-05 | 1999-11-30 | Sony Corporation | Method for fabricating randomly oriented aluminum alloy sputting targets with fine grains and fine precipitates |
| JPH11335826A (en) * | 1998-05-27 | 1999-12-07 | Ryoka Matthey Kk | Production of sputtering target material made of al alloy |
| CN1409773A (en) * | 1999-10-15 | 2003-04-09 | 霍尼韦尔国际公司 | process for producing sputtering target materials |
-
2006
- 2006-09-29 CN CNB2006100537163A patent/CN100420757C/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5282946A (en) * | 1991-08-30 | 1994-02-01 | Mitsubishi Materials Corporation | Platinum-cobalt alloy sputtering target and method for manufacturing same |
| US5993575A (en) * | 1996-11-05 | 1999-11-30 | Sony Corporation | Method for fabricating randomly oriented aluminum alloy sputting targets with fine grains and fine precipitates |
| JPH11335826A (en) * | 1998-05-27 | 1999-12-07 | Ryoka Matthey Kk | Production of sputtering target material made of al alloy |
| CN1409773A (en) * | 1999-10-15 | 2003-04-09 | 霍尼韦尔国际公司 | process for producing sputtering target materials |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624695B (en) * | 2009-08-11 | 2011-02-09 | 宁波江丰电子材料有限公司 | Heat treatment method of target blank |
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Address after: 315400, Zhejiang Yuyao Economic Development Zone, state science and Technology Industrial Park, Ann Road Patentee after: NINGBO JIANGFENG ELECTRONIC MATERIAL CO., LTD. Address before: 315400 Zhejiang Province, Yuyao City Yangming science and Technology Industrial Park No. 1 Jiang Feng Lu Patentee before: Ningbo Jiangfeng Electronic Materials Co., Ltd. |