CN116770247A - Nanometer twin crystal silver material and preparation method thereof - Google Patents
Nanometer twin crystal silver material and preparation method thereof Download PDFInfo
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- CN116770247A CN116770247A CN202310758841.8A CN202310758841A CN116770247A CN 116770247 A CN116770247 A CN 116770247A CN 202310758841 A CN202310758841 A CN 202310758841A CN 116770247 A CN116770247 A CN 116770247A
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- 239000000463 material Substances 0.000 title claims abstract description 79
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 69
- 239000004332 silver Substances 0.000 title claims abstract description 69
- 239000013078 crystal Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000758 substrate Substances 0.000 claims abstract description 72
- 238000000151 deposition Methods 0.000 claims abstract description 22
- 230000008021 deposition Effects 0.000 claims abstract description 22
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 19
- 238000004544 sputter deposition Methods 0.000 claims abstract description 18
- 239000013077 target material Substances 0.000 claims abstract description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000004140 cleaning Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 16
- 229910052710 silicon Inorganic materials 0.000 claims description 16
- 239000010703 silicon Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 13
- 238000005516 engineering process Methods 0.000 description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 8
- 238000003384 imaging method Methods 0.000 description 7
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000010884 ion-beam technique Methods 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- -1 and power: 250W Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 230000001687 destabilization Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012536 packaging technology Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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Abstract
The invention provides a nano twin crystal silver material and a preparation method thereof, wherein the preparation method comprises the following steps: step S1, cleaning and drying a substrate; s2, selecting a silver target as the target material, placing the substrate and the target material into a magnetron sputtering device, vacuumizing, applying negative bias to the substrate for direct-current magnetron sputtering deposition, wherein the bias of the substrate is-50 to-200V, the temperature of the substrate is 25-50 ℃, the flow rate of argon is 30-50 sccm, the vacuum degree of a sputtering chamber is 0.3-1.0 Pa, and the deposition time is 15-90min. By adopting the technical scheme, the nano twin crystal silver material prepared by the method has high-density nano twin crystals, the twin crystal boundary accounts for more than 90 percent, and the hardness, electromigration resistance and thermal stability of the material are improved under the conditions of high electric conductivity and high heat conductivity; the obtained nano twin crystal silver material has excellent comprehensive performance.
Description
Technical Field
The invention belongs to the technical field of advanced preparation of metal materials, and particularly relates to a nano twin crystal silver material and a preparation method thereof.
Background
With the gradual development of packaging technology to high density and high reliability, the packaging technology requires that the interconnection material have a series of excellent characteristics of high strength, good heat and electrical conductivity, thermal stability, electromigration resistance, wen Fuyi energy and the like. Silver is one of the key materials for realizing electrical interconnection in electronic circuit fabrication as a metal having excellent electrical and thermal conductivity and oxidation resistance. However, the problems of low strength of metallic silver and easy electromigration failure in service as an interconnection material severely limit the application of the metallic silver in the field of electronic package interconnection.
Disclosure of Invention
Aiming at the technical problems, the invention discloses a nano twin crystal silver material and a preparation method thereof, and the obtained silver material has excellent characteristics of high strength, electromigration resistance, high thermal stability, high heat conduction and electric conduction and the like.
In this regard, the invention adopts the following technical scheme:
a preparation method of a nano twin crystal silver material comprises the following steps:
step S1, cleaning and drying a substrate;
s2, selecting a silver target as the target material, placing the substrate and the target material into a magnetron sputtering device, vacuumizing, applying negative bias to the substrate for direct-current magnetron sputtering deposition, wherein the bias of the substrate is-50 to-200V, the temperature of the substrate is 25-50 ℃, the flow rate of argon is 30-50 sccm, the vacuum degree of a sputtering chamber is 0.3-1.0 Pa, and the deposition time is 15-90min.
The nano twin crystal silver material obtained by adopting the technical scheme has high density, and has higher strength and good electromigration resistance under the condition of keeping the electric conduction and heat conduction properties of the silver material. Because the grain boundary energy of the coherent nanometer twin grain boundary is lower and is only about 10 percent of that of the large-angle grain boundary, the nanometer twin crystal in the material can also effectively improve the thermal stability of the material at high temperature. The high-density nano twin crystal silver is used as an interconnection material, is expected to solve the problems of low shearing strength and poor electromigration resistance of a silver interconnection layer, and improves service temperature and reliability of interconnection welding spots.
As a further improvement of the invention, in the step S2, the power is 100-300W.
As a further improvement of the invention, the target is a 99.999% silver target.
As a further improvement of the present invention, in step S2, the distance between the substrate and the target is 10-20cm.
As a further improvement of the present invention, the substrate is a silicon substrate or a copper substrate.
As a further improvement of the invention, the thickness of the substrate is 200-500 μm.
As a further improvement of the present invention, step S1 includes cleaning the polished substrate with an acid solution, then cleaning with deionized water, spin-drying the surface moisture, and then drying.
The invention also discloses a nano twin crystal silver material which is prepared by adopting the preparation method of the nano twin crystal silver material.
As a further improvement of the invention, the internal microstructure of the nano twin crystal silver material consists of columnar crystals which grow along the deposition direction and have the width of 200-1000 nm, the nano twin crystal layers perpendicular to the deposition direction are positioned in the columnar crystals, and the average thickness of the nano twin crystal layers is 10-100nm.
As a further improvement of the invention, the columnar crystal surface has a preferred orientation of (111).
As a further improvement of the invention, the thickness of the nano twin crystal silver material is 2-50 μm.
Compared with the prior art, the invention has the beneficial effects that:
firstly, by adopting the technical scheme of the invention, the prepared nano twin crystal silver material has high-density nano twin crystals, the twin crystal boundary accounts for more than 90 percent, and the hardness, electromigration resistance and thermal stability of the material are greatly improved under the condition of high electric conductivity and high heat conductivity; the obtained nano twin crystal silver material has excellent comprehensive performance, can solve the problems of low strength, poor electromigration resistance and the like of the silver material at present, and can be used as an interconnection layer to be applied to the fields of power device packaging, advanced packaging, electromechanical system (MEMS) packaging and the like.
Secondly, the technical scheme of the invention adopts the magnetron sputtering technology to prepare the nano twin crystal silver material, and has the advantages of uniform thickness, uniform and easily controlled structure, strong adhesive force and the like; meanwhile, the physical vapor deposition technology is compatible with microelectronic fabrication processes.
Drawings
Fig. 1 is a Focused Ion Beam (FIB) imaging picture of a cross section of a nano-twin silver material deposited on a silicon substrate according to example 1 of the present invention.
Fig. 2 is a transmission electron microscope picture of a nano-twin silver material deposited on a silicon substrate according to example 1 of the present invention, showing a high density nano-twin layer perpendicular to the deposition direction, with arrows indicating the deposition direction of the material.
Fig. 3 is a Focused Ion Beam (FIB) imaging picture of a cross section of silver material deposited on a silicon substrate according to comparative example 1 of the present invention.
Fig. 4 is a FIB imaging photograph of nano-twin silver material deposited on a silicon substrate according to example 3 of the present invention.
Fig. 5 is a FIB imaging photograph of nano-twin silver material deposited on a silicon substrate according to example 4 of the present invention.
Detailed Description
Preferred embodiments of the present invention are described in further detail below.
Example 1
And preparing the high-density nanocrystalline silver material on the <111> monocrystalline silicon substrate by using a bias DC magnetron sputtering technology. The method for preparing the nano twin crystal silver material by the magnetron sputtering technology comprises the following steps:
s1, cleaning a 2 inch <100> single crystal silicon substrate subjected to chemical mechanical polishing by adopting a solution of hydrofluoric acid and water in a mass ratio of 1:50, and removing a natural oxidation layer; then, adopting deionized water for cleaning; and spin-drying the surface moisture by a spin dryer and then drying for later use;
s2, putting the silicon substrate with the surface oxide film removed and a 99.999% silver target material into a magnetron sputtering workbench, and adjusting the distance between the substrate and the target material to be 15cm;
s3, setting the following technological parameters of sputtering deposition after vacuumizing: applying-100V bias voltage to the deposition substrate, and power: 250W, substrate temperature: 25 ℃, argon flow: 40sccm, sputtering chamber vacuum: 0.5Pa, followed by sputter deposition on the substrate;
and S4, maintaining the step S3 for 20min to obtain the high-density nano twin crystal silver material with the thickness of about 3 mu m.
Fig. 1 is a Focused Ion Beam (FIB) imaging image of a cross section of a nano twin silver material deposited on a silicon substrate according to example 1 of the present invention, and it can be seen from the figure that almost all grains in the columnar crystal of the material contain nano twin crystals with high density, and the grains with high density of nano twin crystals account for about 100%. Fig. 2 is a Transmission Electron Microscope (TEM) image of a nano-twin silver material deposited on a silicon substrate, wherein the nano-twin can be clearly seen.
Example 2
The method for preparing the nano twin crystal silver material by utilizing the bias DC magnetron sputtering technology comprises the following steps of:
s1, cleaning a mechanically polished polycrystalline copper substrate by using 5% (mass percent) citric acid aqueous solution, and cleaning by using deionized water; and spin-drying the surface moisture by a spin dryer and then drying for later use;
s2, putting the polycrystalline copper substrate with the surface oxide film removed and 99.999% of silver target material into a magnetron sputtering workbench, and adjusting the distance between the substrate and the target material to be 20cm;
s3, setting the following technological parameters of sputtering deposition after vacuumizing: applying-100V bias voltage to the deposition substrate, and power: 300W, substrate temperature: 25 ℃, argon flow: 50sccm, sputtering chamber vacuum: 0.5Pa, followed by sputter deposition on the substrate;
and S4, maintaining the step S3 for 30min to obtain the high-density nano twin crystal silver material with the thickness of about 10 mu m.
Comparative example 1
The comparative example comprises the following steps:
s1, cleaning a 2 inch <100> monocrystalline silicon substrate subjected to chemical mechanical polishing by adopting a solution of hydrofluoric acid and water (1:50), and removing a natural oxidation layer; then, adopting deionized water for cleaning; and spin-drying the surface moisture by a spin dryer and then drying for later use;
s2, putting the silicon substrate with the surface oxide film removed and a 99.999% silver target material into a magnetron sputtering workbench, and adjusting the distance between the substrate and the target material to be 15cm;
s3, setting the following technological parameters of sputtering deposition after vacuumizing: no bias voltage is applied to the deposition substrate, power: 250W, substrate temperature: 25 ℃, argon flow: 40sccm, sputtering chamber vacuum: 0.5Pa, followed by sputter deposition on the substrate;
and S4, maintaining the step S3 for 20min to obtain the nano silver material with the thickness of about 3 mu m.
Fig. 3 is a Focused Ion Beam (FIB) imaging picture of a cross section of a nano-twin silver material deposited on a silicon substrate according to comparative example 3, and it can be found from the microstructure that the bottom of the deposited material is an equiaxed crystal transition layer without applying a negative bias, and only few grains have nano-twin crystals, and a high-density nano-twin material is not obtained.
Example 3
And preparing the high-density nanocrystalline silver material on the <111> monocrystalline silicon substrate by using a bias DC magnetron sputtering technology. The method for preparing the nano twin crystal silver material by the magnetron sputtering technology comprises the following steps:
s1, cleaning a 2 inch <100> single crystal silicon substrate subjected to chemical mechanical polishing by adopting a solution of hydrofluoric acid and water in a mass ratio of 1:50, and removing a natural oxidation layer; then, adopting deionized water for cleaning; and spin-drying the surface moisture by a spin dryer and then drying for later use;
s2, putting the silicon substrate with the surface oxide film removed and a 99.999% silver target material into a magnetron sputtering workbench, and adjusting the distance between the substrate and the target material to be 15cm;
s3, setting the following technological parameters of sputtering deposition after vacuumizing: applying a bias voltage of-50V to the deposition substrate, and applying power: 250W, substrate temperature: 25 ℃, argon flow: 40sccm, sputtering chamber vacuum: 0.5Pa, followed by sputter deposition on the substrate;
and S4, maintaining the step S3 for 20min to obtain the high-density nano twin crystal silver material with the thickness of about 3 mu m.
Fig. 4 is a FIB image of a nano-twin silver material deposited on a silicon substrate under a substrate bias of-50V in this example 4, and it can be seen from the figure that there is an equiaxed transition layer at the bottom of the material obtained under this condition, and the volume fraction of grains of the high-density nano-twin is about 50%.
Example 4
And preparing the high-density nanocrystalline silver material on the <111> monocrystalline silicon substrate by using a bias DC magnetron sputtering technology. The method for preparing the nano twin crystal silver material by the magnetron sputtering technology comprises the following steps:
s1, cleaning a 2 inch <100> single crystal silicon substrate subjected to chemical mechanical polishing by adopting a solution of hydrofluoric acid and water in a mass ratio of 1:50, and removing a natural oxidation layer; then, adopting deionized water for cleaning; and spin-drying the surface moisture by a spin dryer and then drying for later use;
s2, putting the silicon substrate with the surface oxide film removed and a 99.999% silver target material into a magnetron sputtering workbench, and adjusting the distance between the substrate and the target material to be 15cm;
s3, setting the following technological parameters of sputtering deposition after vacuumizing: -200V bias voltage, power, applied to the deposition substrate: 250W, substrate temperature: 25 ℃, argon flow: 40sccm, sputtering chamber vacuum: 0.5Pa, followed by sputter deposition on the substrate;
and S4, maintaining the step S3 for 20min to obtain the high-density nano twin crystal silver material with the thickness of about 3 mu m.
Fig. 5 is a FIB imaging picture of the nano-twin silver material deposited on a silicon substrate under a substrate bias of-200V in this example 5, under which it can be seen that a high density nano-twin silver material can be obtained.
The magnetron sputtered Ag materials of examples 1 to 4 and comparative example 1 were subjected to hardness test using a nano hardness tester, and the results are shown in table 1 below. It can be seen that the hardness of the Ag material of comparative example 1, which has a low twin density, was 0.88GPa, and the hardness of example 1, which has high-density twin (90% -Nt), was 1.95GPa, which is 2.21 times that of comparative example 1.
TABLE 1 nanometer hardness test results for examples and comparative examples
| Material | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 |
| hardness/GPa | 1.95 | 1.86 | 1.43 | 1.69 | 0.88 |
The magnetron sputtered Ag materials of examples 1 to 4 and comparative example 1 were incubated at different temperatures for 1 hour to test the thermal stability of the materials, and the critical temperature at which the materials began to de-twine and grain growth occurred was determined to evaluate the thermal stability of the materials. The critical temperature of the material for de-twinning is shown in table 2, and compared with the material of comparative example 1, the destabilization temperature of the high-density twin Ag material of the example is increased to 350 ℃.
Table 2 results of thermal stability test of examples and comparative examples
| Material | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 |
| Destabilization temperature/. Degree.C | 350 | 350 | 300 | 300 | 200 |
The foregoing is a further detailed description of the invention in connection with the preferred embodiments, and it is not intended that the invention be limited to the specific embodiments described. It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.
Claims (10)
1. The preparation method of the nano twin crystal silver material is characterized by comprising the following steps:
step S1, cleaning and drying a substrate;
s2, selecting a silver target as the target material, placing the substrate and the target material into a magnetron sputtering device, vacuumizing, applying negative bias to the substrate for direct-current magnetron sputtering deposition, wherein the bias of the substrate is-50 to-200V, the temperature of the substrate is 25-50 ℃, the flow rate of argon is 30-50 sccm, the vacuum degree of a sputtering chamber is 0.3-1.0 Pa, and the deposition time is 15-90min.
2. The method for preparing nano twin crystal silver material according to claim 1, wherein: in step S2, the power is 100-300W.
3. The method for preparing nano twin crystal silver material according to claim 2, wherein: the target material is a 99.999% silver target.
4. The method for preparing nano twin crystal silver material according to claim 3, wherein: in the step S2, the distance between the substrate and the target is 10-20cm.
5. The method for preparing nano twin crystal silver material according to claim 1, wherein: the substrate is a silicon substrate or a copper substrate.
6. The method for preparing nano twin crystal silver material according to claim 5, wherein: the thickness of the substrate is 200-500 mu m.
7. The method for preparing nano twin crystal silver material according to claim 1, wherein: in step S1, the polished substrate is cleaned with an acid solution, then cleaned with deionized water, and dried after the surface moisture is spin-dried.
8. A nanometer twin crystal silver material is characterized in that: which is prepared by the preparation method of the nano twin crystal silver material as claimed in any one of claims 1 to 7.
9. The nano-twin silver material according to claim 8, wherein: the internal microstructure of the nano twin crystal silver material consists of columnar crystals which grow along the deposition direction and have the width of 200-1000 nm, the nano twin crystal layer vertical to the deposition direction is positioned in the columnar crystals, and the average thickness of the nano twin crystal layer is 10-100nm.
10. The nano-twin silver material according to claim 8, wherein: the columnar crystal surface has (111) optimal orientation, and the thickness of the nano twin crystal silver material is 2-50 mu m.
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| TWI762342B (en) * | 2021-06-03 | 2022-04-21 | 國立臺灣大學 | Methods for forming bonding structures |
| CN115642140A (en) * | 2021-07-20 | 2023-01-24 | 乐鑫材料科技股份有限公司 | Bonding structure and method for forming the same |
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| TWI762342B (en) * | 2021-06-03 | 2022-04-21 | 國立臺灣大學 | Methods for forming bonding structures |
| CN115642140A (en) * | 2021-07-20 | 2023-01-24 | 乐鑫材料科技股份有限公司 | Bonding structure and method for forming the same |
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