CN115896722B - Method for improving wear resistance and conductivity of Cu-Ni-Sn alloy - Google Patents
Method for improving wear resistance and conductivity of Cu-Ni-Sn alloy Download PDFInfo
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- CN115896722B CN115896722B CN202211470804.9A CN202211470804A CN115896722B CN 115896722 B CN115896722 B CN 115896722B CN 202211470804 A CN202211470804 A CN 202211470804A CN 115896722 B CN115896722 B CN 115896722B
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 57
- 239000000956 alloy Substances 0.000 title claims abstract description 57
- 229910018100 Ni-Sn Inorganic materials 0.000 title claims abstract description 39
- 229910018532 Ni—Sn Inorganic materials 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 27
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 16
- 229910052786 argon Inorganic materials 0.000 claims abstract description 11
- 230000004907 flux Effects 0.000 claims abstract description 8
- 238000004544 sputter deposition Methods 0.000 claims description 35
- 239000000758 substrate Substances 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 10
- 239000011521 glass Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000002474 experimental method Methods 0.000 claims description 3
- 238000000151 deposition Methods 0.000 abstract description 10
- 238000002360 preparation method Methods 0.000 abstract description 10
- 230000008021 deposition Effects 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 4
- 229910000881 Cu alloy Inorganic materials 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000004377 microelectronic Methods 0.000 abstract description 2
- 238000002161 passivation Methods 0.000 abstract 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract 1
- 229910052782 aluminium Inorganic materials 0.000 abstract 1
- 230000001276 controlling effect Effects 0.000 abstract 1
- 238000005457 optimization Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 58
- 239000010409 thin film Substances 0.000 description 13
- 239000010949 copper Substances 0.000 description 12
- 239000000203 mixture Substances 0.000 description 9
- 230000032683 aging Effects 0.000 description 4
- 229910001128 Sn alloy Inorganic materials 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- VRUVRQYVUDCDMT-UHFFFAOYSA-N [Sn].[Ni].[Cu] Chemical compound [Sn].[Ni].[Cu] VRUVRQYVUDCDMT-UHFFFAOYSA-N 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 229910002058 ternary alloy Inorganic materials 0.000 description 1
Abstract
The invention discloses a method for improving wear resistance and conductivity of Cu-Ni-Sn alloy, and relates to the technical field of microelectronic integrated circuit interconnection; the Cu-Ni-Sn alloy is prepared into a film through magnetron sputtering, and the Cu-Ni-Sn uniform combined film with different application requirements and various components can be prepared through regulating and controlling parameters such as magnetron sputtering power, deposition time, argon flow and the like. The invention adopts the high flux 6 target magnetron sputtering film codeposition preparation technology, so that the alloy film has low resistivity and higher electromigration resistance, and compared with an aluminum-based alloy film which is used as an interconnection wire material, the alloy film has a wide passivation interval and low passivation current density, thereby further realizing the great optimization of the comprehensive performance of the combined film; the Cu-Ni-Sn alloy film completely meets the use requirement of the copper alloy film in the field of interconnection of very large scale integrated circuits.
Description
Technical Field
The invention relates to the technical field of microelectronic integrated circuit interconnection, in particular to a method for improving the wear resistance and conductivity of Cu-Ni-Sn alloy.
Background
The Cu-Ni-Sn alloy is widely applied to the fields of aerospace parts, automatic lead frames, electronic elastic components, electronic packaging and the like as a conductive elastic copper alloy has good conductivity, creep resistance and other comprehensive properties. However, as integrated circuits move to large/very large scale integration, lead frames have more, finer pins and pitches, thereby placing higher demands on the performance of Cu-Ni-Sn alloys.
At present, the main technical route for preparing the copper-nickel-tin alloy is as follows: casting, homogenizing treatment, solution treatment, cold deformation and aging. The performance of the alloy is controlled mainly by controlling the aging temperature and the aging time, but in the aging process, the precipitation amount of nano-scale precipitated phases is small, and the strength, the plasticity and the conductivity of the alloy cannot be greatly improved, so that the hardness is reduced. The strength of the alloy block body in the casting process is only 0.5GPa, the hardness is only 1.18GPa, and the conductivity is less than 10% IACS due to the segregation of Sn element in the casting process; for modern high-performance compound interconnection (Multilevel Interconnections) circuits, the alloy often cannot meet the use requirements in precision electronic elastic components, micro-interconnection and heat-load environments.
Disclosure of Invention
The invention aims to provide a method for improving the wear resistance and conductivity of a Cu-Ni-Sn alloy, which is characterized in that the Cu-Ni-Sn alloy is prepared into a film with uniform components by controlling sputtering according to the following weight percentages of 75-80% of Cu, 10-20% of Ni and 0.9-10% of Sn.
Preferably, the preparation method of the Cu-Ni-Sn alloy film comprises the following steps of:
(1) Cleaning the vacuum cavity: before experiments are carried out, the vacuum cavity and the sample table of the high-flux 6-target magnetron sputtering equipment are required to be polished and wiped by ethanol.
(2) And (3) installing a target: in the high flux 6-target magnetron sputtering system, a No. 1 target, a No. 3 target and a No. 5 target are strong magnetic targets; the target No. 2, the target No. 4 and the target No. 6 are weak magnetic targets; and mounting a inlaid high-purity Ni target, a high-purity Sn target and a high-purity Cu target on the target No. 1, the target No. 2 and the target No. 4 respectively.
(3) Cleaning the glass sheet: 1 or more glass sheets are selected as the substrates, which are arranged in a row along the diameter direction and fixed on a sample stage, and the substrates are sent to a main chamber by feeding the sheets.
(4) The process is operated: the system starts film pre-sputtering firstly, and after the pre-sputtering is correct, the equipment automatically opens the target cover to formally start sputtering.
Preferably, the purity of the high-purity Ni target is more than 99.99 percent; the purity of the high-purity Sn target is more than 99.99 percent; the purity of the high-purity Cu target is more than 99.99 percent.
Preferably, the pre-sputtering time in the step (4) is 30-60 s.
Preferably, the sputtering time is 30-60 min, the argon flow is 200-230 SCCM, the sputtering power of the No. 1 target is 50-60W, the sputtering power of the No. 2 target is 30-40W, and the sputtering power of the No. 4 target is 80-90W.
The Cu-Ni-Sn alloy is prepared into the film, so that the application field of a copper-nickel-tin alloy system is further expanded; the film prepared by the method has small size, uniform components, hardness of more than 3GPa and conductivity of up to 30% IACS; this results in unprecedented improvement in the reliability of the film for use in precision electronic elastic components and high performance micro interconnect circuits, which is not achievable with alloy blocks.
The invention adopts the high flux 6 target magnetron sputtering film codeposition preparation technology, the purity of the prepared alloy film is high, the components are controllable, the material gene high flux concept is integrated, the alloy film can be prepared in large batch, and the large-scale application is satisfied.
The invention has the beneficial effects that:
(1) The Cu-Ni-Sn alloy film prepared by the reasonable sputtering process parameters selected by the high flux 6 target magnetron sputtering film codeposition preparation method has uniform structure, high film density and flatness, greatly reduces stress concentration, and improves the thermal stability and comprehensive performance of the substrate Cu film; from fig. 2, it can be observed that the contrast of the SEM morphology of the Cu-Ni-Sn alloy film is remarkable, which indicates that the film has surface relief, and Cu, ni and Sn components are uniformly distributed in the observation range, so as to form a good solid solution.
(2) The invention adopts a high flux 6 target magnetron sputtering film codeposition technology; the distance and angle between the target and the Si wafer substrate are consistent, the film deposition is more accurate than the sputtering systems of the traditional process 2 targets, the traditional process 4 targets and the like, the sputtering efficiency is high, the structure of the film is uniform, and the high-performance alloy film can be prepared.
(3) It can be observed from fig. 2 that the bonding performance of the glass substrate and the film interface is better; in the nanoindentation test system, the Cu-Ni-Sn alloy thin film data presented in tables 1 to 4 show significant changes in conductivity and hardness. This also verifies that the hardness of the film is significantly improved at different sputter powers, different sputter times and different argon flows; meanwhile, the Cu-Ni-Sn alloy film has fewer defects, and the increase of Ni content and the generation of new solid solution phase lead to the increase of the conductivity of the film.
(4) In example 1, a component of a film prepared by magnetron sputtering was selected, and a Cu-Ni-Sn alloy block of a corresponding component was prepared by a conventional vacuum induction melting method, and performance comparison was made, as shown in Table 1. By comparing the properties, we clearly see that the hardness and conductivity of the Cu-Ni-Sn alloy film are greatly increased compared to bulk alloys. This also shows that it is very feasible to improve the wear resistance and conductivity of the Cu-Ni-Sn alloy by the preparation of the thin film.
Drawings
FIG. 1 is a schematic diagram of a Cu-Ni-Sn alloy film prepared by codeposition of a multi-target magnetron sputtering film;
FIG. 2 Cu-Ni-Sn ternary alloy film surface morphology diagram.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the scope of the present invention is not limited to the above.
Example 1
Film deposition raw materials: self-made inlaid high-purity Cu target (> 99.99%), self-made inlaid high-purity Ni target (> 99.99%), self-made inlaid high-purity Sn target (> 99.99%).
The preparation method of the Cu-Ni-Sn alloy film in the embodiment 1 adopts a high flux 6 target magnetron sputtering film codeposition preparation technology and mainly comprises a vacuum control system, a turntable controller, a heating system, a radio frequency sputtering power supply, a direct current sputtering power supply and the like.
The method described in this example 1 includes the steps of:
(1) Cleaning the vacuum cavity: before experiments are carried out, the vacuum cavity and the sample table of the high-flux 6-target magnetron sputtering equipment are required to be polished and wiped by ethanol.
(2) And (3) installing a target: as shown in FIG. 1, a high purity Ni target (> 99.99%), a high purity Sn target (> 99.99%) and a high purity Cu target (> 99.99%) were mounted on the target No.1, the target No.2 and the target No. 4, respectively.
(3) Cleaning the glass sheet: 15 glass sheets with the dimensions of 10mm multiplied by 3mm multiplied by 1mm are selected as substrates, which are arranged in a row along the diameter direction as shown in fig. 1, A-B, and fixed on a sample stage by using a high-temperature adhesive tape, and the substrates are sent to a main chamber to wait for process editing and pre-sputtering.
(4) And (3) process editing: the pre-sputter time was 30s (to remove target surface oxides and contaminants), the sputter time was 30min, the argon flow was 200SCCM, and different sputter powers were used in this example, with specific parameters as shown in table 1.
(5) The process is operated: and (3) starting the operation of the process parameters set in the step (4), performing film sputtering, starting film pre-sputtering by the system, and automatically opening a target cover to formally start sputtering after the pre-sputtering is correct.
(6) Taking a piece: and (3) after the sputtering of the film in the step (5) is finished, taking out the sample by the main piece, and placing the sample in a self-adsorption box for vacuum preservation.
The composition and properties of the resulting films at different sputter powers were investigated in this example and are shown in Table 1.
TABLE 1 preparation of high Performance Cu-Ni-Sn alloy thin film Co-deposition sputter Power parameters in this example
TABLE 2 high performance Cu-Ni-Sn alloy film composition and Performance Table prepared in this example
It can be seen from tables 1 and 2 that the alloy thin films prepared by different sputtering powers have different compositions, and the hardness and the conductivity of the thin films show different changes, when the content of Cu is 75.93%, the content of Ni is 15.78%, and the content of Sn is 8.29%, the hardness of the alloy thin films can reach 2.87GPa, and the conductivity can reach 20.80% IACS. This is because the hardness and thermoelectric properties can be remarkably improved and the temperature coefficient of resistivity can be reduced when the Ni content is relatively high. And Sn in the film is dissolved into Cu and Ni in a solid manner, so that the conductivity and the wear resistance of the film are further improved.
For comparison, the Cu-15Ni-8Sn alloy is prepared by a vacuum induction melting method, and the corresponding performances are as follows: the average hardness of the as-cast alloy is only 1.13GPa, and the average conductivity of the as-cast alloy is 7.78 percent IACS; the composition was similar to that of sample 2, and it can be seen that the as-cast Cu-15Ni-8Sn alloy was far less excellent than the Cu-15.02Ni-8.05Sn alloy film prepared by magnetron sputtering. When the Cu content is 76.93%, the Ni content is 15.02%, and the Sn content is 8.05%, the hardness of the alloy film can reach 3.12GPa, and the conductivity can reach 30.98% IACS. Thus, films of different compositions exhibit different hardness and conductivity.
As shown in fig. 2, which shows the microscopic surface morphology of sample 2, it can be seen that the film prepared by the high-flux sputtering process has better surface flatness, and the addition of Ni and Sn elements significantly improves the hardness and conductivity of the film compared to the pure copper film;
Example 2
The preparation method of the Cu-Ni-Sn alloy film in this embodiment is the same as that of the Cu-Ni-Sn alloy film in embodiment 1, and is different in that: the sputtering times were varied and specific parameters are shown in table 3.
TABLE 3 Cu-Ni-Sn alloy film composition and Performance Table at different sputtering times of this example
It can be seen from table 3 that the alloy thin film composition after deposition by different sputtering times is different, and a significant improvement in hardness and electrical conductivity is obtained. Particularly, when the Cu content is 76.62%, the Ni content is 19.25% and the Sn content is 4.13%, the hardness of the alloy film can reach 3.54GPa, and the conductivity can reach 30.52% IACS. Compared with the change of sputtering power, the different deposition time has larger influence on the performance of the film; this is mainly reflected in that when the sputtering time of the thin film is long, the thickness of the thin film is increased, and the degree of uniformity of the thin film is greatly improved with the extension of the deposition time, thus enabling the hardness and conductivity of the thin film to be significantly increased.
Example 3
The preparation method of the Cu-Ni-Sn alloy film in this embodiment is the same as that of the Cu-Ni-Sn alloy film in embodiment 1, and is different in that: the argon flows were varied and specific parameters are shown in table 4.
TABLE 4 Cu-Ni-Sn alloy film composition and Performance Table for different argon flows of this example
It can be seen from table 4 that the composition is different in the different argon flow atmospheres and the vapor pressure of the deposition main chamber is different, thereby affecting the overall performance of the film. When the air pressure is too high, ions cannot be well deposited on the wafer substrate due to the fact that the pressure of the deposition chamber is too high, so that the film is not uniform, the surface of the film is rough, and performance is deteriorated; when the air pressure is too low, the argon content of the deposition chamber is insufficient, the vacuum degree is insufficient, and the obtained film has uneven structure and low density. Therefore, in the film deposition process, a proper argon flow is required to be ensured, and when the argon flow is 220SCCM as in example 3, the hardness of the film can reach 3.12GPa, and the conductivity can reach 22.58% iacs. Therefore, when the vapor pressure is too high or too low, the influence on the hardness and conductivity of the cu—ni—sn alloy thin film is remarkable.
The above examples are only illustrative to help understand a method of improving wear resistance and electrical conductivity of Cu-Ni-Sn alloy and a novel thin film fabrication method and core ideas thereof according to the present invention. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
Claims (5)
1. A method for improving the wear resistance and the conductivity of a Cu-Ni-Sn alloy, which is characterized by comprising the following steps: the Cu-Ni-Sn alloy is prepared into a film by magnetron sputtering, and the method specifically comprises the following steps:
(1) Cleaning the vacuum cavity: before the experiment is carried out, the vacuum cavity and the sample table of the high-flux 6-target magnetron sputtering equipment are required to be polished and wiped by ethanol;
(2) And (3) installing a target: in the high flux 6-target magnetron sputtering system, a No. 1 target, a No. 3 target and a No. 5 target are strong magnetic targets; the target No. 2, the target No. 4 and the target No. 6 are weak magnetic targets; the embedded high-purity Ni target, the high-purity Sn target and the high-purity Cu target are respectively arranged on the target No. 1, the target No. 2 and the target No. 4; the sputtering power of the No. 1 target is 50-60W, the sputtering power of the No. 2 target is 30-40W, and the sputtering power of the No. 4 target is 80-90W;
(3) Cleaning the glass sheet: selecting 1 or more glass sheets as a substrate, arranging the substrates into a row along the diameter direction, fixing the substrates on a sample table, and feeding the substrates to a main chamber;
(4) The process is operated: the system starts film pre-sputtering firstly, and after the pre-sputtering is correct, the equipment automatically opens the target cover to formally start sputtering.
2. The method for improving the wear resistance and the electrical conductivity of a Cu-Ni-Sn alloy of claim 1, wherein: the Cu-Ni-Sn film comprises 75-80% of Cu, 10-20% of Ni and 0.9-10% of Sn by weight percent of each element.
3. The method for improving the wear resistance and the electrical conductivity of a Cu-Ni-Sn alloy of claim 1, wherein: the purity of the high-purity Ni target is more than 99.99 percent; the purity of the high-purity Sn target is more than 99.99 percent; the purity of the high-purity Cu target is more than 99.99 percent.
4. The method for improving the wear resistance and the electrical conductivity of a Cu-Ni-Sn alloy of claim 1, wherein: and (3) the pre-sputtering time in the step (4) is 30-60 s.
5. The method for improving the wear resistance and the electrical conductivity of a Cu-Ni-Sn alloy of claim 1, wherein: the sputtering time is 30-60 min, and the argon flow is 200-230 SCCM.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211470804.9A CN115896722B (en) | 2022-11-23 | Method for improving wear resistance and conductivity of Cu-Ni-Sn alloy |
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| CN202211470804.9A CN115896722B (en) | 2022-11-23 | Method for improving wear resistance and conductivity of Cu-Ni-Sn alloy |
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| Publication Number | Publication Date |
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| CN115896722A CN115896722A (en) | 2023-04-04 |
| CN115896722B true CN115896722B (en) | 2024-07-16 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014218706A (en) * | 2013-05-09 | 2014-11-20 | 出光興産株式会社 | Sputtering target, oxide semiconductor thin film, and manufacturing method of them |
| JP2016156087A (en) * | 2015-02-19 | 2016-09-01 | 株式会社神戸製鋼所 | Cu LAMINATED FILM AND Cu ALLOY SPUTTERING TARGET |
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014218706A (en) * | 2013-05-09 | 2014-11-20 | 出光興産株式会社 | Sputtering target, oxide semiconductor thin film, and manufacturing method of them |
| JP2016156087A (en) * | 2015-02-19 | 2016-09-01 | 株式会社神戸製鋼所 | Cu LAMINATED FILM AND Cu ALLOY SPUTTERING TARGET |
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