CN113540001A - Kovar/silver alloy composite material for microelectronic packaging and preparation method thereof - Google Patents
Kovar/silver alloy composite material for microelectronic packaging and preparation method thereof Download PDFInfo
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- CN113540001A CN113540001A CN202110707913.7A CN202110707913A CN113540001A CN 113540001 A CN113540001 A CN 113540001A CN 202110707913 A CN202110707913 A CN 202110707913A CN 113540001 A CN113540001 A CN 113540001A
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- 239000002131 composite material Substances 0.000 title claims abstract description 66
- 229910000833 kovar Inorganic materials 0.000 title claims abstract description 52
- 229910001316 Ag alloy Inorganic materials 0.000 title claims abstract description 37
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 14
- 238000004377 microelectronic Methods 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 238000000137 annealing Methods 0.000 claims abstract description 37
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 28
- 239000000956 alloy Substances 0.000 claims abstract description 28
- 238000010273 cold forging Methods 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000005219 brazing Methods 0.000 claims abstract description 27
- 229910052751 metal Inorganic materials 0.000 claims abstract description 26
- 239000002184 metal Substances 0.000 claims abstract description 26
- 238000009792 diffusion process Methods 0.000 claims abstract description 25
- 238000005096 rolling process Methods 0.000 claims abstract description 25
- 239000000945 filler Substances 0.000 claims abstract description 22
- 229910000679 solder Inorganic materials 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 238000007731 hot pressing Methods 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 45
- 238000013329 compounding Methods 0.000 claims description 18
- 238000004381 surface treatment Methods 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 10
- 238000005242 forging Methods 0.000 claims description 7
- 238000010030 laminating Methods 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000919 ceramic Substances 0.000 abstract description 14
- 238000012858 packaging process Methods 0.000 abstract description 4
- 238000005538 encapsulation Methods 0.000 abstract description 3
- 238000005476 soldering Methods 0.000 abstract description 3
- 239000010949 copper Substances 0.000 description 13
- 239000010936 titanium Substances 0.000 description 12
- 239000005022 packaging material Substances 0.000 description 8
- 238000000227 grinding Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000004615 ingredient Substances 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- NEIHULKJZQTQKJ-UHFFFAOYSA-N [Cu].[Ag] Chemical compound [Cu].[Ag] NEIHULKJZQTQKJ-UHFFFAOYSA-N 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000004100 electronic packaging Methods 0.000 description 2
- 238000004573 interface analysis Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
- H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L24/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
- H01L24/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
- C22C5/08—Alloys based on silver with copper as the next major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
- H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L24/27—Manufacturing methods
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L2224/27—Manufacturing methods
- H01L2224/271—Manufacture and pre-treatment of the layer connector preform
- H01L2224/2711—Shaping
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L2224/27—Manufacturing methods
- H01L2224/275—Manufacturing methods by chemical or physical modification of a pre-existing or pre-deposited material
- H01L2224/27505—Sintering
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L2224/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
- H01L2224/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
- H01L2224/29001—Core members of the layer connector
- H01L2224/29075—Plural core members
- H01L2224/2908—Plural core members being stacked
- H01L2224/29082—Two-layer arrangements
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L2224/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
- H01L2224/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
- H01L2224/29001—Core members of the layer connector
- H01L2224/29099—Material
- H01L2224/291—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof
- H01L2224/29138—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof the principal constituent melting at a temperature of greater than or equal to 950°C and less than 1550°C
- H01L2224/29139—Silver [Ag] as principal constituent
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L2224/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
- H01L2224/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
- H01L2224/29001—Core members of the layer connector
- H01L2224/29099—Material
- H01L2224/291—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof
- H01L2224/29138—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof the principal constituent melting at a temperature of greater than or equal to 950°C and less than 1550°C
- H01L2224/29147—Copper [Cu] as principal constituent
Abstract
A kovar/silver alloy composite material for microelectronic packaging and a preparation method thereof are provided, wherein the Cu content in a silver alloy solder layer in the composite material is 30-35 wt%, the Ti content is 0.1-5.0 wt%, the Ni content is 0.1-1.0 wt%, and the balance is Ag; the kovar alloy layer is 4J29 or 4J 34. The preparation method comprises the following steps: preparing a brazing filler metal ingot blank by adopting a vacuum pressure sintering method, obtaining a composite ingot blank in a hot-pressing diffusion mode, and obtaining a layered composite material with the thickness of 0.15-1.5 mm through cold forging forming, intermediate annealing, precision rolling and finished product annealing, wherein the thickness of the kovar alloy layer is 0.1-1 mm, and the thickness of the silver alloy brazing filler metal layer is 0.01-0.5 mm. The kovar/silver alloy composite material has good matching property with the thermal expansion coefficient of ceramics, and can realize good encapsulation with ceramics. The soldering temperature is moderate, the packaging process is simple and efficient, the device is not easy to crack after being sealed, and the yield is high.
Description
Technical Field
The invention relates to the technical field of electronic packaging materials, in particular to a kovar/silver alloy composite material for microelectronic packaging and a preparation method thereof.
Background
In recent years, with rapid development of microelectronic technology, miniaturization, densification, high power and multiple functions of electronic devices, components and the like have required that a packaging process and a packaging material matched with the electronic devices and the components have high stability and high reliability. The packaging material is used for supporting and protecting semiconductor chips and electronic circuits, assisting in dissipating heat of electronic elements, transferring signals and the like, and is of great importance to the service life of microelectronic components. Electronic packaging materials can be divided into plastic packaging materials, ceramic materials for packaging and metal packaging materials according to material components. The metal packaging material has the irreplaceable characteristics of high mechanical strength, good heat dissipation performance and the like. Conventional metal encapsulation materials include Cu, Al, Mo, kovar, and the like. Wherein the kovar alloy has a thermal expansion coefficient similar to oxygen-free copper, ceramic materials and the like, and good vacuum brazing performance, and is widely applied to the electronic industry. It can be used to make high-air-tightness element and device by sealing with hard glass, or used to make high-frequency power tube and rectifier tube by sealing with ceramic, and used as leading-out wire and lead frame in transistor and integrated circuit. However, when pure copper is used as a brazing filler metal to braze kovar, the chip is damaged due to high packaging temperature, and when silver-copper alloy and other brazing filler metals are used, the cracking phenomenon which cannot be repaired is often caused in the sealing process, so that the problems of micro-cracking, air leakage and the like of a tube shell are caused, the reliability of a device is seriously influenced, and even the device is failed. The application party tries to adopt a silver-copper and kovar alloy stacking assembly mode for packaging, but the problems of low yield, poor air tightness and the like exist.
Disclosure of Invention
The invention mainly aims to provide a kovar/silver alloy composite material for microelectronic packaging, wherein brazing filler metal and a packaging material are combined through metallurgy to form a layered composite material, so that the problems of chip fracture, pipe shell microcrack, air leakage and the like caused by high temperature and thermal stress between metal layers in the sealing process of high-power vacuum pipe fittings, semiconductor devices and the like are solved, and the packaging yield and service reliability of microelectronic components are improved.
The invention also aims to provide the preparation method of the composite material, the method is simple and convenient to operate, the Kovar/silver, copper and titanium composite material can be highly reliably compounded, and the prepared composite material is moderate in thickness and beneficial to subsequent preforming of the material.
In order to achieve the above purpose, the invention provides the following technical scheme:
a kovar/silver alloy composite material for microelectronic packaging is a double-layer layered composite material formed by metallurgical bonding of a kovar alloy layer and a silver alloy solder layer; the content of Cu in the silver alloy brazing filler metal layer is 30-35 wt%, the content of Ti is 0.1-5.0 wt%, the content of Ni is 0.1-1.0 wt%, and the balance is Ag; the kovar alloy layer is made of 4J29 or 4J 34; the thickness of the composite material is 0.15-1.5 mm, wherein the thickness of the kovar alloy layer is 0.1-1 mm, and the thickness of the silver alloy brazing filler metal layer is 0.01-0.5 mm.
In the kovar/silver alloy composite material, preferably, the silver alloy solder layer contains 32 to 34 wt% of Cu, 0.5 to 4.5 wt% of Ti, 0.2 to 0.8 wt% of Ni and the balance of Ag.
In the kovar/silver alloy composite material, the thickness of the kovar alloy sheet is preferably 0.2-0.5 mm, and the thickness of the silver alloy solder sheet is preferably 0.02-0.2 mm.
In another aspect, the present invention provides a method for preparing a kovar/silver alloy composite material as described above, which adopts a process flow of "solder powder mixture-solder ingot blank preparation-ingot blank surface treatment-ingot blank compounding-cold forging forming-intermediate annealing-precision rolling-finished product annealing", and comprises the following steps:
(1) solder mixed powder
Weighing several raw material powders according to the mass percentage, wherein the content of Cu is 30-35 wt%, the content of Ti is 0.1-5.0 wt%, the content of Ni is 0.1-1.0 wt%, and the balance is Ag, and mixing the powders in a ball mill;
(2) preparing a brazing filler metal ingot blank: preparing the solder alloy powder subjected to ball milling into an ingot blank by adopting a vacuum pressure sintering method;
(3) and (3) ingot blank surface treatment: performing surface treatment on the brazing filler metal ingot blank and the kovar alloy by using a double-sided grinder;
(4) compounding an ingot blank: laminating the silver alloy ingot blank subjected to surface treatment and a 4J29 or 4J34 kovar alloy matrix by adopting a hot-pressing diffusion method for primary compounding;
(5) cold forging and forming: cold forging the composite ingot blank by using a small hydraulic cold forging machine;
(6) intermediate annealing: placing the cold-forged composite blank into a vacuum furnace for annealing;
(7) precision rolling: performing multi-pass precision rolling on the annealed composite blank until the size of a finished product is reached;
(8) annealing of a finished product: and (4) placing the composite sheet in a vacuum furnace for annealing.
In the method described above, preferably, in the raw materials in step (1), the purities of the Cu powder, the Ni powder and the Ag powder are 99.99%, the purity of the Ti powder is 99.9%, the particle sizes of the powders are 200-400 mesh, the ball milling speed is 100-200 rad/min, and the ball milling time is 2-4 hours.
In the method as described above, preferably, in the step (2), the pressure of the vacuum pressure sintering is 40 to 60MPa, and the degree of vacuum is 1.0 × 10-3Pa～1.0×10-4pa, the sintering temperature is 700-750 ℃.
In the method, preferably, the thickness of the kovar alloy ingot blank in the step (4) is 1-8 mm, and the thickness of the silver alloy solder ingot blank is 0.1-1 mm; the composite pressure is 30 MPa-50 MPa, the diffusion temperature is 700 ℃ to 750 ℃, and the diffusion time is 5 min-15 min.
In the method, the cold forging deformation amount in the step (5) is preferably 20-40%, and the forging rate is preferably 1-2 mm · s-1.
In the method as described above, it is preferable that the degree of vacuum in the step (6) is 1.0X 10-3pa～1.0×10-4Pa, the annealing temperature is 580-600 ℃, and the heat preservation time is 60-120 min;
in the method, preferably, in the step (7), the single-pass rolling deformation rate is 20-35%, and the total deformation rate is less than 90%;
in the method as described above, it is preferable that the degree of vacuum in the step (8) is 1.0X 10-3Pa～1.0×10-4Pa, annealing temperature of 550-580 deg.C, and holding time of 60-90 min.
The beneficial effects of the invention are as follows:
(1) the composite material is suitable for being directly connected with a ceramic part in microelectronic packaging, and effectively solves the problems of complex process, time and cost consumption, poor batch stability and the like of the traditional indirect connection of ceramics and kovar.
(2) The composite material comprises a brazing filler metal layer and a kovar matrix layer, the thickness proportion of the brazing filler metal layer and the kovar matrix layer is moderate, the brazing filler metal layer and the kovar matrix layer can be processed into required shapes and sizes and then quickly assembled with a ceramic device, the problems of low welding rate and the like caused by assembly dislocation and the like in the packaging process at present are effectively solved, and the packaging efficiency is improved.
(3) The brazing material layer of the composite material contains active elements Ti and Ni, the Ti element can react with ceramic to form intermetallic compounds in the brazing process, the wetting of the silver alloy brazing filler metal to the ceramic can be improved, the similar intermiscibility of the brazing material layer and the kovar alloy can be improved by adding the Ni element, the interface diffusion effect of the brazing material layer and the kovar layer is promoted through the reaction of Fe and Ni elements, the silver alloy brazing filler metal and the kovar alloy can form good metallurgical bonding, and the bonding strength of the ceramic/kovar interface is enhanced.
(4) The preparation method of the composite material adopts the cold forging process to improve the forming performance of the composite material, is beneficial to subsequent rolling forming and ensures the dimensional stability of the composite material. The intermediate annealing and finished product annealing processes are carried out twice, so that on one hand, the components of the composite material are fully homogenized, element diffusion is realized by combining an interface, on the other hand, the residual stress generated in the processing process of the material can be eliminated, and the reliable compounding of the composite material and ceramic in the connection process is ensured.
(5) The composite material has good matching property with the thermal expansion coefficient of ceramics, and the device is not easy to crack after being sealed, thereby improving the packaging yield of the device.
Drawings
FIG. 1 is a metallographic microscope photograph of the AgCuTiNi/4J29 layered composite material prepared in example 1.
Detailed Description
Preferred embodiments of the present invention are described in further detail below. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not constitute a limitation on the invention.
Example 1: preparing AgCuTiNi/4J29 layered composite material
Step 1: solder ingredient mixed powder
Respectively weighing 126 g of Ag powder with the powder granularity of 200 meshes to 400 meshes and the purity of 99.99 percent, 64 g of Cu powder, 1.0 g of Ni powder and 9.0 g of Ti powder with the purity of 99.9 percent, mixing the powders in a ball mill at the ball milling speed of 150rad/min for 2 hours.
Step 2: blank making
The ball-milled powder is sintered under vacuum pressure with the vacuum degree of 1.0 multiplied by 10-4Pa, temperature 730 ℃, pressure 40MPa, ingot blank diameter 100 mm.
And step 3: surface treatment of ingot blank
The sintered ingot blank with the thickness of 0.62mm and 4J29 kovar alloy with the diameter of 100mm and the thickness of 4mm are placed in a double-sided grinding machine for surface treatment.
And 4, step 4: ingot blank compounding
And laminating and assembling the AgCuTiNi subjected to surface grinding and a 4J29 blank, and then performing thermal diffusion pressure compounding, wherein the compounding pressure is 40MPa, the diffusion temperature is 720 ℃, and the diffusion time is 10 min.
And 5: cold forging to form
And (3) performing cold forging on the diffusion compounded ingot blank by using a small hydraulic cold forging machine, wherein the cold forging deformation is 20-30%, and the forging speed is 1-2 mm & s < -1 >.
Step 6: intermediate annealing
Putting the cold-forged composite blank into a vacuum furnaceAnnealing is carried out with a degree of vacuum of 1.0X 10-4pa, annealing temperature of 580 ℃ and heat preservation time of 60 min.
And 7: precision rolling
And (3) carrying out multi-pass rolling on the annealed composite blank by using a precision rolling mill, wherein the single-pass rolling deformation rate is 20-25% until the size of a finished product is 0.35 mm.
And 8: annealing the finished product
The rolled laminated composite sheet is placed in a vacuum furnace with the vacuum degree of 1.0 multiplied by 10-3Pa, annealing temperature of 550 ℃ and heat preservation time of 60 min.
The metallographic microscopic photograph of the obtained AgCuTiNi/4J29 layered composite material is shown in figure 1, and the photograph shows that the silver alloy layer and the kovar alloy layer are well combined and have no defects such as holes, gaps and the like.
Example 2: preparing AgCuTiNi/4J29 layered composite material
Step 1: solder ingredient mixed powder
Respectively weighing 124 g of Ag powder with the powder granularity of 200 meshes-400 meshes and the purity of 99.99%, 68 g of Cu powder, 1.0 g of Ni powder and 7.0 g of Ti powder with the purity of 99.9%, and mixing the powders in a ball mill at the ball milling speed of 150rad/min for 2 hours.
Step 2: blank making
The ball-milled powder is sintered under vacuum pressure with the vacuum degree of 1.0 multiplied by 10-4Pa, the temperature is 720 ℃, the pressure is 50MPa, and the diameter of the ingot blank is 100 mm.
And step 3: surface treatment of ingot blank
The sintered ingot blank with the thickness of 0.60mm and 4J29 kovar alloy with the diameter of 100mm and the thickness of 5mm are placed in a double-sided grinding machine for surface treatment.
And 4, step 4: ingot blank compounding
And laminating and assembling the AgCuTiNi subjected to surface grinding and a 4J29 blank, and then performing thermal diffusion pressure compounding, wherein the compounding pressure is 50MPa, the diffusion temperature is 710 ℃, and the diffusion time is 5 min.
And 5: cold forging to form
The diffusion compounded ingot blank is subjected to cold forging by a small hydraulic cold forging machine to obtain the cold forging deformation30 to 40 percent of the forging rate, and the forging rate is 1 to 2 mm.s-1。
Step 6: intermediate annealing
Annealing the cold-forged composite blank in a vacuum furnace with a vacuum degree of 1.0 × 10-4Pa, annealing temperature of 590 ℃, and heat preservation time of 60 min.
And 7: precision rolling
And (3) carrying out multi-pass rolling on the annealed composite blank by using a precision rolling mill, wherein the single-pass rolling deformation rate is 30-35% until the size of a finished product is 0.5 mm.
And 8: annealing the finished product
The rolled laminated composite sheet is placed in a vacuum furnace with the vacuum degree of 1.0 multiplied by 10-3pa, annealing temperature 560 ℃, and heat preservation time 60 min.
Example 3: preparing AgCuTiNi/4J34 layered composite material
Step 1: solder ingredient mixed powder
Respectively weighing 132 g of Ag powder with the powder granularity of 200 meshes-400 meshes and the purity of 99.99%, 66 g of Cu powder, 0.8 g of Ni powder and 1.2 g of Ti powder with the purity of 99.9%, and mixing the powders in a ball mill at the ball milling speed of 150rad/min for 2 hours.
Step 2: blank making
The ball-milled powder is sintered under vacuum pressure with the vacuum degree of 1.0 multiplied by 10-4pa, temperature 740 ℃, pressure 40MPa, ingot blank diameter 100 mm.
And step 3: surface treatment of ingot blank
The sintered ingot with a thickness of 0.64mm and 4J34 kovar alloy with a diameter of 100mm and a thickness of 5.8mm were placed in a double-sided grinder for surface treatment.
And 4, step 4: ingot blank compounding
And laminating and assembling the AgCuTiNi subjected to surface grinding and a 4J34 blank, and then performing thermal diffusion pressure compounding, wherein the compounding pressure is 40MPa, the diffusion temperature is 730 ℃, and the diffusion time is 15 min.
And 5: cold forging to form
The diffusion compounded ingot blank is subjected to cold forging by a small hydraulic cold forging machine, and the cold forging deformation is 30Percent to 40 percent and forging and pressing rate of 1 to 2mm s-1。
Step 6: intermediate annealing
Annealing the cold-forged composite blank in a vacuum furnace with a vacuum degree of 1.0 × 10-4Pa, the annealing temperature is 580 ℃, and the heat preservation time is 90 min.
And 7: precision rolling
And (3) carrying out multi-pass rolling on the annealed composite blank by using a precision rolling mill, wherein the single-pass rolling deformation rate is 30-35% until the size of a finished product is 0.8 mm.
And 8: annealing the finished product
The rolled laminated composite sheet is placed in a vacuum furnace with the vacuum degree of 1.0 multiplied by 10-3Pa, annealing temperature of 550 ℃ and heat preservation time of 90 min.
Example 4: preparing AgCuTiNi/4J34 layered composite material
Step 1: solder ingredient mixed powder
Respectively weighing 129.6 g of Ag powder with the powder granularity of 200 meshes to 400 meshes and the purity of 99.99 percent, 62 g of Cu powder, 0.4 g of Ni powder and 8 g of Ti powder with the purity of 99.9 percent, and mixing the powders in a ball mill at the ball milling speed of 150rad/min for 2 hours.
Step 2: blank making
The ball-milled powder is sintered under vacuum pressure with the vacuum degree of 1.0 multiplied by 10-4Pa, 750 ℃, 60MPa pressure and 100mm diameter of the ingot blank.
And step 3: surface treatment of ingot blank
The sintered ingot blank with the thickness of 0.62mm and 4J34 kovar alloy with the diameter of 100mm and the thickness of 5mm are placed in a double-sided grinding machine for surface treatment.
And 4, step 4: ingot blank compounding
And laminating and assembling the AgCuTiNi subjected to surface grinding and a 4J34 blank, and then performing thermal diffusion pressure compounding, wherein the compounding pressure is 30MPa, the diffusion temperature is 740 ℃, and the diffusion time is 5 min.
And 5: cold forging to form
The ingot blank after diffusion compounding is subjected to cold forging by a small hydraulic cold forging machine, and the cold forging deformation is 20-30 percentPercent, forging rate of 1-2 mm · s-1。
Step 6: intermediate annealing
Annealing the cold-forged composite blank in a vacuum furnace with a vacuum degree of 1.0 × 10-4Pa, annealing temperature of 600 ℃ and heat preservation time of 120 min.
And 7: precision rolling
And (3) carrying out multi-pass rolling on the annealed composite blank by using a precision rolling mill, wherein the single-pass rolling deformation rate is 30-35% until the size of a finished product is 0.6 mm.
And 8: annealing the finished product
The rolled laminated composite sheet is placed in a vacuum furnace with the vacuum degree of 1.0 multiplied by 10-3Pa, the annealing temperature is 580 ℃, and the heat preservation time is 90 min.
Experimental example 1 Performance test
The composite materials prepared in examples 1 to 4 were subjected to mechanical property test and interface analysis, respectively, and subjected to Al-interface analysis2O3The results of the hermetic seal test performed after the ceramic was soldered and sealed are shown in Table 1.
TABLE 1
| Soldering temperature | Peel strength | Silver alloy/kovar layer thickness ratio | Air tightness | |
| Example 1 | 850℃ | 6.5N/m | 1∶6 | ＜1.0×10-13Pa·m3/s |
| Example 2 | 850℃ | 6.0N/m | 1∶8 | ＜1.0×10-13Pa·m3/s |
| Example 3 | 850℃ | 5.9N/m | 1∶9 | ＜1.0×10-13Pa·m3/s |
| Example 4 | 850℃ | 6.1N/m | 1∶8 | ＜1.0×10-13Pa·m3/s |
The experimental results show that the Kovar/silver alloy composite material has good matching property with the thermal expansion coefficient of ceramic, and can realize good encapsulation with ceramic parts. The soldering temperature is moderate, the packaging process is simple and efficient, the device is not easy to crack after being sealed, and the yield is high.
The above examples only show some examples of the kovar/silver alloy composite material and the preparation method thereof, and in the above technical solution of the present invention: the contents of the alloy components Ag, Cu, Ni and Ti can be freely selected within the specified ranges, and are not listed here, so the technical solutions included in the above description should be regarded as illustrative examples, and are not intended to limit the scope of the present invention.
Claims (10)
1. A kovar/silver alloy composite material for microelectronic packaging is characterized in that: the kovar/silver alloy composite solder is a double-layer layered composite material formed by metallurgical bonding of a kovar alloy layer and a silver alloy solder layer; the content of Cu in the silver alloy brazing filler metal layer is 30-35 wt%, the content of Ti is 0.1-5.0 wt%, the content of Ni is 0.1-1.0 wt%, and the balance is Ag; the kovar alloy layer is made of 4J29 or 4J 34; the thickness of the composite material is 0.15-1.5 mm, wherein the thickness of the kovar alloy layer is 0.1-1 mm, and the thickness of the silver alloy brazing filler metal layer is 0.01-0.5 mm.
2. The kovar/silver alloy composite according to claim 1, wherein: the silver alloy brazing filler metal layer contains 32-34 wt% of Cu, 0.5-4.5 wt% of Ti, 0.2-0.8 wt% of Ni and the balance of Ag.
3. The kovar/silver alloy composite according to claim 1, wherein: the thickness of the kovar alloy sheet is 0.2-0.5 mm, and the thickness of the silver alloy brazing filler metal sheet is 0.02-0.2 mm.
4. The method of making a kovar/silver alloy composite according to claim 1, wherein: the technological process of 'brazing filler metal mixed powder-brazing filler metal ingot blank preparation-ingot blank surface treatment-ingot blank compounding-cold forging forming-intermediate annealing-precision rolling 1 finished product annealing' comprises the following steps:
(1) solder mixed powder
Weighing several raw material powders according to the mass percentage, wherein the content of Cu is 30-35 wt%, the content of Ti is 0.1-5.0 wt%, the content of Ni is 0.1-1.0 wt%, and the balance is Ag, and mixing the powders in a ball mill;
(2) preparing a brazing filler metal ingot blank: preparing the solder alloy powder subjected to ball milling into an ingot blank by adopting a vacuum pressure sintering method;
(3) and (3) ingot blank surface treatment: performing surface treatment on the brazing filler metal ingot blank and the kovar alloy by using a double-sided grinder;
(4) compounding an ingot blank: laminating the silver alloy ingot blank subjected to surface treatment and a 4J29 or 4J34 kovar alloy matrix by adopting a hot-pressing diffusion method for primary compounding;
(5) cold forging and forming: cold forging the composite ingot blank by using a small hydraulic cold forging machine;
(6) intermediate annealing: placing the cold-forged composite blank into a vacuum furnace for annealing;
(7) precision rolling: performing multi-pass precision rolling on the annealed composite blank until the size of a finished product is reached;
(8) annealing of a finished product: and (4) placing the composite sheet in a vacuum furnace for annealing.
5. The method as claimed in claim 4, wherein the purity of Cu powder, Ni powder and Ag powder in the raw materials in step (1) is 99.99%, the purity of Ti powder is 99.9%, the particle sizes of the powders are all 200-400 meshes, the ball milling speed is 100-200 rad/min, and the ball milling time is 2-4 hours.
6. The method according to claim 4, wherein in the step (2), the pressure of the vacuum pressure sintering is 40MPa to 60MPa, and the degree of vacuum is 1.0X 10-3Pa～1.0×10-4Pa, and the sintering temperature is 700-750 ℃.
7. The method as claimed in claim 4, wherein in the step (4), the thickness of the kovar alloy ingot is 1-8 mm, and the thickness of the silver alloy solder ingot is 0.1-1 mm; the composite pressure is 30 MPa-50 MPa, the diffusion temperature is 700 ℃ to 750 ℃, and the diffusion time is 5 min-15 min.
8. The method as claimed in claim 4, wherein the cold forging deformation in the step (5) is 20-40%, and the forging rate is 1-2 mm-s-1。
9. The method of claim 4, wherein the vacuum in step (6)Degree of 1.0X 10-3Pa～1.0×10-4pa, the annealing temperature is 580-600 ℃, and the heat preservation time is 60-120 min.
10. The method as claimed in claim 4, wherein the single-pass rolling deformation rate in the step (7) is 20-35%, and the total deformation rate is less than 90%;
the vacuum degree in the step (8) is 1.0 x 10-3pa～1.0×10-4Pa, annealing temperature of 550-580 deg.C, and holding time of 60-90 min.
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| CN117282771A (en) * | 2023-11-21 | 2023-12-26 | 西安稀有金属材料研究院有限公司 | Preparation method of AgCu15/4J29 composite strip for electronic packaging |
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