CN111118459A - Preparation method of high-performance ferromagnetic target material - Google Patents
Preparation method of high-performance ferromagnetic target material Download PDFInfo
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- CN111118459A CN111118459A CN201911395580.8A CN201911395580A CN111118459A CN 111118459 A CN111118459 A CN 111118459A CN 201911395580 A CN201911395580 A CN 201911395580A CN 111118459 A CN111118459 A CN 111118459A
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
- H01F41/18—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates by cathode sputtering
- H01F41/183—Sputtering targets therefor
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Abstract
The invention discloses a preparation method of a high-performance ferromagnetic target material, which belongs to the technical field of target material preparation, and comprises the steps of firstly preparing a target blank and a back plate, processing the target blank to the thickness size of a finished product, then adopting a temperature difference method for welding, ensuring the flatness of the target material, eliminating the welding internal stress through vibration aging, and finally completing the preparation of the target material finished product through processing the back plate, wherein the method is suitable for preparing a large-area target blank with the diameter of phi 300 and 450 mm. The large-area high-purity ferromagnetic metal target prepared by the method has good thickness uniformity, small welding stress, uniform magnetic permeability distribution and good target sputtering film uniformity.
Description
Technical Field
The invention belongs to the technical field of target preparation, and particularly relates to a preparation method of a high-performance ferromagnetic target. The high-purity ferromagnetic sputtering target material provided by the invention is suitable for the field of semiconductor and integrated circuit manufacturing.
Background
With the continuous progress of semiconductor manufacturing technology, the line width of the front-end logic circuit of the semiconductor integrated circuit has reached 90-28nm, and will be further popularized to the deep nanometer level of 14-10nm in the future. As line widths decrease, metal Co, Ni (Pt) silicides replace Ti silicides for use as electrical contacts (contacts), such as cobalt targets, nickel platinum alloy targets, etc. used in strained silicon technology in CMOS devices and modulated work function technology in novel finfets, with the electrical contacts being formed by PVD. Since these targets have ferromagnetism, the uniformity of the distribution of magnetic energy becomes a key to the uniformity of sputtered thin films.
There are many factors that affect the uniformity of the magnetic performance of the ferromagnetic target material, mainly including microstructure texture, thickness and internal stress distribution uniformity. If the thickness distribution of the target is not uniform, the magnetic field distribution on the surface of the target is not uniform. In addition, the welding stress of the target is large, which causes poor control of the thickness uniformity in the target processing process. Therefore, the processing of ferromagnetic targets has a large impact on the sputtering performance of the targets. For the 8-12 inch ferromagnetic metal target with higher requirement, the target is usually deformed by 1-2mm after welding because the diameter of the target surface is too large (> 300 mm). After the leveling is carried out by adopting a common leveling method, the flatness of the target is still larger (more than 0.2mm), so that a special method is required to ensure that the welding stress of the target is lower, and the target has higher thickness uniformity (less than 0.2 mm).
The temperature difference method can be used for eliminating welding stress and deformation, and comprises a flame water spraying method, an induction heating method, a heat dissipation method and the like. It was reported that the Hervey laboratory in the united states studied the reduction of bowing in aluminum parts in 1968 using a method of controlling the heat distribution profile of the weld. The principle is that a distortion temperature field is formed by cryogenic liquid and an auxiliary heat source, so that metal near a welding seam contracts and expands to counteract expansion and contraction generated by welding. However, the above methods are mainly used in butt welding structures, and cannot solve the deformation generated by the plane welding of large-area thin plates, and the prior art vibration aging is mostly used for small workpieces, so a technical scheme is urgently needed to solve the problems of welding deformation of large-area ferromagnetic targets and internal stress elimination.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of a high-performance ferromagnetic target material, which comprises the following steps:
1) firstly, preparing a target blank and a back plate;
2) processing the target blank to the thickness size of the finished target material;
3) welding the processed target blank and the back plate by adopting a temperature difference method, ensuring the flatness and low stress of the target material and obtaining a welded assembly;
4) eliminating welding residual internal stress of the welding assembly through vibration aging to obtain a blank;
5) and processing the blank into a required specification and size to obtain the finished target.
The target blank in the step 1) is a brazing type ferromagnetic target material.
The diameter of the target blank in the step 1) is phi 300-450 mm.
And 2) the target blank processing mode is high-precision processing.
In the step 3), the target blank is heated by the temperature difference method, so that the deformation between the target blank and the back plate is reduced.
In the step 3), the welding by the temperature difference method is to control the temperature reduction speed of the target blank by a heater so that the temperature reduction speed of the target blank is controlled to be 1-2 ℃/min.
In the step 3), the temperature difference method welding is to control the temperature reduction speed of the target blank 1 through a cooling plate, so that the temperature reduction speed of the back plate is controlled at 3-10 ℃/min.
And the vibration aging time in the step 4) is 10-20 min.
The target in the step 5) is a ferromagnetic target for 8-inch or 12-inch wafers.
According to the high-performance ferromagnetic target prepared by the method, the flatness of the target is less than or equal to 0.2mm, the uniformity of the film is less than or equal to 2.2%, and the magnetic permeability of the sputtering surface of the target is uniformly distributed.
The invention has the beneficial effects that:
1. the ferromagnetic metal ferromagnetic target material prepared by the invention has the advantages of uniform thickness, small welding stress, uniform sputtering film and uniform distribution of the magnetic permeability of the surface of the target material, and can meet the use requirements of advanced semiconductor chips.
2. The invention adopts a temperature difference method to reduce the welding deformation of the large-area ferromagnetic target material. And the internal stress of the large-area target material is eliminated by combining with the vibratory stress relief, so that the flatness is further reduced.
Drawings
FIG. 1 is a process flow diagram of the high performance ferromagnetic target of the present invention;
FIG. 2 is a schematic view of a target blank 1 of the target material of the present invention;
FIG. 3 is a schematic view of a backing plate 2 of the target of the present invention;
FIG. 4 is a schematic diagram of the deformation after welding the target blank 1 and the backing plate 2 according to the comparative example method;
FIG. 5 is a schematic view of the welding of the present invention by temperature differential welding;
fig. 6 is a schematic view of stress relief of the target material of the present invention by vibrational aging.
Wherein:
1-target blank, 2-back plate, 3-heater, 4-cooling plate, 5-objective table, 6-vibration exciter and 7-sensor.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
first, a target blank 1 and a backing plate 2 are prepared. The ferromagnetic metal target blank 1 containing Co, Ni and Fe mainly comprises a high-purity Co target, a NiPt target, a NiFe target and the like. The material of the backplate 2 is usually copper alloy, such as CuCr and CuZn alloy.
The target blank 1 is 8-12 inches in size, typically with a diameter of phi 300 and 450 mm. And (3) processing the target blank 1 to the thickness size of a finished product, and processing by adopting a lathe or a grinding machine to ensure the thickness uniformity of the target blank. The welding surfaces of the target blank 1 and the back plate 2 are coated with solder, and the solder is high-purity indium. The target blank 1 and the backing plate 2 are welded together.
After the target blank 1 and the back plate 2 are welded, internal welding stress is generated due to the difference of the linear expansion coefficients of the target blank 1 and the back plate 2, so that the target blank 1 and the back plate 2 deform and warp after cooling, as shown in fig. 4. Since the backboard 2 is made of Cu alloy, the linear expansion coefficient of the backboard 2 is large. Therefore, the central positions of the target blank 1 and the backing plate 2 are warped after the temperature is reduced, and the warping amount h is usually 1.5-4 mm. Due to the large warp, a pressing block is usually required for flattening. But the flatness control difficulty is higher, and because the magnetic property of the ferromagnetic target material is sensitive to stress, certain residual stress exists after flattening. Resulting in poor uniformity of target thickness and stress distribution.
In order to reduce the warpage, a heater 3 is used on the surface of the target material, and the temperature reduction speed is controlled to be lower than that of the backing plate 2 for the target blank 1. The temperature reduction speed of the target blank 1 is controlled to be 1-2 ℃/min. The cooling speed of the back plate 2 is controlled to be 3-10 ℃/min by using the cooling plate 4 at the position of the back plate 2. The cooling plate can be designed as a water-cooled copper plate and the complete assembly is placed on the object table 5, as shown in fig. 5. In the process of cooling the target blank and the back plate, the cooling plate 4 is rapidly cooled to the solidification temperature point of the solder, so that the target blank and the back plate generate temperature difference and respectively contract. Thereby ensuring that the final cooling has smaller warping degree.
Compared with the conventional welding method, the warping amount of the target is reduced to 0.3-0.5mm after the target is welded by adopting a temperature difference method. And eliminating welding internal stress by adopting vibration aging. As shown in fig. 6, an exciter 6 is used on the surface of the target blank, and a sensor 7 is used on the edge of the backing plate to obtain a vibration signal. After the target material eliminates the welding stress, the flatness is reduced to be below 0.2mm, the flatness of the target material is obviously improved, and the welding stress is basically eliminated.
And processing the back plate 2 into a required specification to finally obtain the finished target material.
The process flow diagram 1 of the present invention is described below with reference to examples to determine the feasibility of the process. In the examples, high purity NiPt15 target blank 1 and Cu alloy backing plate 2 were selected for experiments.
Comparative example 1
Preparing a high-purity NiPt15 target blank and a Cu alloy back plate, wherein the diameter of the target blank is 330mm, and processing the target blank to the thickness of 3.5mm of a finished product and the thickness of the back plate is 15 mm.
The NiPt15 target blank and the Cu alloy back plate 2 complete indium brazing welding at 220 ℃.
And after welding, measuring the warping h of the target material to be 3 mm.
And mechanically flattening the target material by using a pressing block, and measuring the warping amount h of the target material after flattening to be 0.3 mm.
And (3) finishing the machining of a finished product of the target, machining the NiPt15 target blank part to the thickness of the finished product of 3mm, measuring the thickness range of the NiPt15 part of the target, and finishing welding as shown in figure 4.
Comparative example 2
Preparing a high-purity NiPt15 target blank and a Cu alloy back plate, wherein the diameter of the target blank is phi 450mm, and processing the target blank to the thickness of 3mm of a finished product and the thickness of the back plate is 15 mm.
And completing indium brazing welding of the NiPt15 target blank and the Cu alloy back plate at 180 ℃.
After welding, the warping h of the target material is measured to be 2 mm.
And (3) removing stress when the target vibrates, wherein the warping amount h of the target is 0.25 mm.
And (4) finishing the finished product processing of the target, and measuring the thickness range of the NiPt15 part of the target.
Example 1
Preparing a high-purity NiPt15 target blank and a Cu alloy back plate, wherein the diameter of the target blank is 330mm, and processing the target blank to the thickness of 3mm of a finished product and the thickness of the back plate is 15 mm.
The NiPt15 target blank and the Cu alloy back plate are welded by indium brazing at 220 ℃, the back plate is rapidly cooled by a temperature difference method in the cooling process, and the target blank is slowly cooled. The temperature reduction speed of the target blank is controlled at 1 ℃/min, the temperature reduction speed of the back plate is controlled at 5 ℃/min, and the warping amount h of the target material is measured to be 0.9mm after welding.
And (3) removing stress when the target material is vibrated, wherein the vibration time is 6min, and the warping amount h of the target material after the stress is removed is 0.15 mm.
And (4) finishing the finished product processing of the target, and measuring the thickness range of the NiPt15 part of the target.
Example 2
Preparing a high-purity NiPt15 target blank and a Cu alloy back plate, wherein the diameter of the target blank is 330mm, and processing the target blank to the thickness of 3mm of a finished product and the thickness of the back plate is 15 mm.
The NiPt15 target blank and the Cu alloy backboard finish indium brazing welding at 200 ℃, and the temperature difference method is adopted in the temperature reduction process to realize the quick temperature reduction of the backboard and the slow temperature reduction of the target blank. The temperature reduction speed of the target blank is controlled at 1 ℃/min, the temperature reduction speed of the back plate is controlled at 7 ℃/min, and the warping amount h of the target material is measured to be 0.6mm after welding.
And (3) removing stress when the target material is vibrated, wherein the vibration time is 10min, and the warping amount h of the target material after the stress is removed is 0.1 mm.
And (4) finishing the finished product processing of the target, and measuring the thickness range of the NiPt15 part of the target.
Example 3
Preparing a high-purity NiPt15 target blank and a Cu alloy back plate, wherein the diameter of the target blank is phi 450mm, and processing the target blank to the thickness of 3mm of a finished product and the thickness of the back plate is 15 mm.
The NiPt15 target blank and the Cu alloy backboard finish indium soldering welding at 180 ℃, and the temperature difference method is adopted in the temperature reduction process to realize the quick temperature reduction of the backboard and the slow temperature reduction of the target blank. The temperature reduction speed of the target blank is controlled at 2 ℃/min, the temperature reduction speed of the back plate is controlled at 6 ℃/min, and the warping amount h of the target material is measured to be 0.5mm after welding.
And (3) carrying out vibration aging stress removal on the target material, wherein the vibration time is 7min, and the warping amount h of the target material after stress removal is 0.15 mm.
And (4) finishing the finished product processing of the target, and measuring the thickness range of the NiPt15 part of the target.
The high-purity ferromagnetic NiPt15 target material prepared by the method is used for carrying out sputtering experiments, and the uniformity data of the film obtained by sputtering are shown in Table 1. In the embodiment, the film obtained by sputtering the high-purity ferromagnetic target prepared by the invention has good uniformity, the thickness uniformity can be less than or equal to 3 percent, and the film can meet the use requirement of high-end semiconductor integrated circuits. The ferromagnetic target material prepared by the conventional process has the film uniformity of more than or equal to 5 percent and can not meet the use requirements of high-end semiconductor integrated circuits.
Table 1 comparison table of target material preparation results of inventive example and comparative example
| Amount of warping h (mm) | Levelled flatness (mm) | Extremely poor thickness (mm) | Uniformity of film | |
| Comparative example 1 | 3 | 0.3 | 0.35 | ≤6.5％ |
| Comparative example No. two | 2 | 0.25 | 0.23 | ≤5.5％ |
| Example one | 0.9 | 0.15 | 0.15 | ≤2.1％ |
| Example two | 0.6 | 0.1 | 0.13 | ≤2.2％ |
| Practice ofEXAMPLE III | 0.5 | 0.15 | 0.13 | ≤2.0％ |
Claims (10)
1. The preparation method of the high-performance ferromagnetic target material is characterized by comprising the following steps of:
1) firstly, preparing a target blank and a back plate;
2) processing the target blank to the thickness size of the finished target material;
3) welding the processed target blank and the back plate by adopting a temperature difference method, ensuring the flatness and low stress of the target material and obtaining a welded assembly;
4) eliminating welding residual internal stress of the welding assembly through vibration aging to obtain a blank;
5) and processing the blank into a required specification and size to obtain the finished target.
2. The method of claim 1, wherein the target blank in step 1) is a brazed-type ferromagnetic target material.
3. The method as claimed in claim 1, wherein the diameter of the target blank in step 1) is phi 300-450 mm.
4. The method of claim 1, wherein the target blank processing manner of step 2) is high-precision processing.
5. The method of claim 1, wherein the step 3) of said temperature differential welding is performed by heating the target blank to reduce distortion between the target blank and the backing plate.
6. The method as claimed in claim 1, wherein the step 3) of welding by temperature difference method is to control the temperature reduction rate of the target blank by a heater, so that the temperature reduction rate of the target blank is controlled to be 1-2 ℃/min.
7. The method as claimed in claim 1, wherein the step 3) of welding by temperature difference method is to control the temperature reduction rate of the target blank 1 through the cooling plate, so that the temperature reduction rate of the backing plate is controlled to be 3-10 ℃/min.
8. The method according to claim 1, wherein the vibration aging time in step 4) is 10-20 min.
9. The method of claim 1, wherein the target in step 5) is a ferromagnetic target for 8-inch or 12-inch wafers.
10. The high-performance ferromagnetic target material prepared by the method of any one of claims 1 to 8, wherein the flatness of the target material is less than or equal to 0.2mm, the uniformity of the film is less than or equal to 2.2%, and the magnetic permeability of the sputtering surface of the target material is uniformly distributed.
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Cited By (6)
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| CN111375998A (en) * | 2020-04-03 | 2020-07-07 | 宁波江丰电子材料股份有限公司 | Method for controlling thickness uniformity of magnetic target |
| CN111607752A (en) * | 2020-06-03 | 2020-09-01 | 福建阿石创新材料股份有限公司 | Internal stress removing correction method for sputtering target material |
| CN112808833A (en) * | 2020-12-31 | 2021-05-18 | 有研科技集团有限公司 | Method for preparing high-performance ferromagnetic target material |
| CN112894112A (en) * | 2021-01-18 | 2021-06-04 | 有研亿金新材料有限公司 | Method for reducing diffusion welding deformation of large-size target and target welding assembly |
| CN112917100A (en) * | 2021-01-27 | 2021-06-08 | 宁波江丰电子材料股份有限公司 | Processing method of nickel target material assembly |
| CN113752403A (en) * | 2021-09-17 | 2021-12-07 | 宁波江丰电子材料股份有限公司 | Silicon carbide target material assembly and preparation method thereof |
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| CN112894112A (en) * | 2021-01-18 | 2021-06-04 | 有研亿金新材料有限公司 | Method for reducing diffusion welding deformation of large-size target and target welding assembly |
| CN112917100A (en) * | 2021-01-27 | 2021-06-08 | 宁波江丰电子材料股份有限公司 | Processing method of nickel target material assembly |
| CN113752403A (en) * | 2021-09-17 | 2021-12-07 | 宁波江丰电子材料股份有限公司 | Silicon carbide target material assembly and preparation method thereof |
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