CN116140866A - Novel copper-based solder paste for low-melting-point VC soaking plate - Google Patents
Novel copper-based solder paste for low-melting-point VC soaking plate Download PDFInfo
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- CN116140866A CN116140866A CN202310227613.8A CN202310227613A CN116140866A CN 116140866 A CN116140866 A CN 116140866A CN 202310227613 A CN202310227613 A CN 202310227613A CN 116140866 A CN116140866 A CN 116140866A
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- 239000010949 copper Substances 0.000 title claims abstract description 137
- 229910000679 solder Inorganic materials 0.000 title claims abstract description 102
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 91
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 238000002791 soaking Methods 0.000 title abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 238000005219 brazing Methods 0.000 claims description 33
- 229910052751 metal Inorganic materials 0.000 claims description 22
- 239000002184 metal Substances 0.000 claims description 22
- 238000005476 soldering Methods 0.000 claims description 20
- 239000000945 filler Substances 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 15
- 230000004907 flux Effects 0.000 claims description 12
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 16
- 238000002844 melting Methods 0.000 description 13
- 230000008018 melting Effects 0.000 description 13
- 238000003466 welding Methods 0.000 description 13
- 230000008569 process Effects 0.000 description 5
- 238000010008 shearing Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/302—Cu as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Electric Connection Of Electric Components To Printed Circuits (AREA)
Abstract
The invention discloses a novel copper-based solder paste for a low-melting-point VC soaking plate, which relates to the field of material preparation and connection, wherein the mass ratio of copper-based solder components in the solder paste is Cu 67.5-67.9%, sn 22.6-23.0%, ni 3.7-3.9% and P5.6-5.8%.
Description
Technical Field
The invention relates to the field of material preparation and connection, in particular to a novel copper-based solder paste for a low-melting-point VC soaking plate.
Background
A Vacuum Chamber (VC) soaking plate is a plate-shaped heat transfer device capable of performing phase change heat transfer, which is formed by injecting a working liquid into a near vacuum Chamber having a capillary structure inside. It is mainly composed of shell, capillary liquid absorbing core, working liquid and supporting column. The VC vapor chamber is a planar heat pipe, and can radiate heat in two directions. The upper and lower shells of the vapor chamber are made of oxygen-free copper, and the welding process directly restricts the production yield of the vapor chamber and influences the service performance of the vapor chamber. While the brazing filler metal is an important influencing factor of the welding process of the upper and lower shells of the vapor chamber, in the industry of producing the VC vapor chamber, copper-based brazing filler metal is generally adopted to weld the upper and lower shells of the vapor chamber in consideration of the quality of vapor chamber materials. Brazing can be classified into soldering and brazing by taking temperature as a distinguishing standard. The brazing performed at a liquidus temperature of the brazing filler metal lower than 450 ℃ is defined as soldering, and the brazing performed at a temperature higher than 450 ℃ is defined as brazing. The brazing material has high strength, can be used for brazing stressed members and has wide application, and comprises aluminum-based brazing material, silver-based brazing material, copper-based brazing material, manganese-based brazing material, nickel-based brazing material, gold-based brazing material and palladium-based brazing material. The copper-based brazing filler metal is used as hard brazing filler metal, has the characteristic of high melting point, but the copper material is easy to oxidize at high temperature, so that the production cost can be effectively reduced by reducing the welding temperature on the premise of ensuring the use performance.
Disclosure of Invention
The invention aims to provide a novel copper-based solder paste for a low-melting-point VC soaking plate, which solves the problems of high melting point and easy oxidization of copper-based materials in the prior art.
In order to achieve the above object, the present invention provides the following solutions:
one of the technical schemes of the invention is as follows: the copper-based brazing filler metal comprises the following components in percentage by mass: 67.5 to 67.9 percent of Cu, 22.6 to 23.0 percent of Sn, 3.7 to 3.9 percent of Ni and 5.6 to 5.8 percent of P.
The second technical scheme of the invention is as follows: the preparation method of the copper-based brazing filler metal comprises the following steps: and (3) carrying out component adjustment on the PH600 copper-based solder by utilizing metallic tin to obtain the copper-based solder.
Further, the copper-based brazing filler metal can be directly prepared according to the mass percentages of the components.
The third technical scheme of the invention: provided is a copper-based solder paste containing the copper-based solder and a flux.
The technical scheme of the invention is as follows: the preparation method of the copper-based solder paste comprises the following steps: and (3) performing component adjustment on the PH600 copper-based solder by utilizing metallic tin to obtain copper-based solder powder, and adding soldering flux to obtain the copper-based solder paste.
Further, the specific preparation steps of the copper-based solder paste comprise:
s1, preparing copper-based solder powder: ultrasonically cleaning and drying PH600 copper-based brazing filler metal with the components of Cu75.0%, P5.2%, sn15.6% and Ni4.2% to obtain copper-based brazing filler metal powder;
s2, preparing the copper-based solder paste: and uniformly mixing the copper-based solder powder and the metal tin powder, and adding the soldering flux to uniformly mix to obtain the copper-based solder paste.
Further, the addition amount of the metal tin powder is 10.0% by weight of the copper-based solder powder.
Further, the metallic tin powder has a purity of greater than 99.99wt.%.
Further, the flux is ALPHA POP707, and the addition amount of the flux is 12+ -0.5% of the solder powder mass by weight.
The fifth technical scheme of the invention is as follows: the copper-based solder or the copper-based solder paste is applied to the preparation of copper-based soldered joints.
Further, the copper-based soldered joint is a Cu/copper-based solder/Cu sandwich soldered joint.
Further, the preparation step of the Cu/Cu-based solder/Cu sandwich solder joint comprises the following steps:
s1, placing an anaerobic Cu sheet into 30% HNO 3 Soaking in aqueous solution, and then carrying out ultrasonic cleaning and drying;
s2, smearing the copper-based solder paste on a Cu sheet to form a solder paste with a certain thickness on the Cu sheet, and horizontally covering the other Cu sheet above the solder paste to form a Cu/copper-based solder/Cu sandwich structure;
s3, welding the sandwich structure in the S2 under the nitrogen atmosphere, wherein the welding temperature is about +40 ℃ of the melting point of the brazing filler metal, and cooling along with a furnace after welding for 10min to obtain the Cu/copper-based brazing filler metal/Cu sandwich brazing joint.
Further, the purity of the oxygen-free Cu sheet is greater than 99.99wt.%.
Further, when preparing the Cu/copper-based solder/Cu sandwich solder joint, the solder paste thickness in step S2 is 200 μm.
The sixth technical scheme of the invention: the copper-based solder or the copper-based solder paste is applied to the preparation of the copper-based VC vapor chamber.
The invention discloses the following technical effects:
(1) The invention overcomes the defects of high melting point and easy oxidation of the copper-based solder as hard solder, realizes that the melting point of the prepared solder is 505-510 ℃ and is reduced by about 90 ℃ relative to the PH600 solder paste on the premise of ensuring good service performance by adjusting components, has the advantages of saving energy and reducing cost, and can reduce the oxidation degree of Cu at lower heating temperature and ensure excellent service performance.
(2) The invention provides a low-melting-point copper-based solder paste, which reduces the soldering temperature and energy loss in the soldering process, further reduces the heating cost, is suitable for preparing soldering butt joints of copper and copper alloy in a furnace for soldering, flame soldering, high-frequency soldering, resistance welding and other processes, and meanwhile, the soldering joint prepared by adopting the technical scheme of the invention can meet various requirements of tensile and shearing tests, and further can obtain accurate joint use performance data and joint reliability evaluation.
(3) The technical scheme of the invention can reduce the melting point of the copper-based brazing filler metal in the prior art, and reduce the welding cost, i.e. the process is simple and the cost is low; meanwhile, the method can be applied to the preparation of VC vapor chamber and welding joints, and can be applied to the research on the reliability of mechanics and heat of microelectronic connection.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a DSC of a solder before component adjustment in example 1;
FIG. 2 is a DSC of the solder after component adjustment in example 1;
FIG. 3 is an SEM image and an EDS image of the joint after component adjustment in example 2; wherein FIG. a is an SEM image of the component-adjusted joint of example 2 and FIG. b is an EDS image of the component-adjusted joint of example 2;
fig. 4 is a schematic diagram of an application example of preparing solder paste in example 1;
FIG. 5 is a graph showing the strength comparison of Cu/Cu-based solder/Cu sandwich braze joints before and after composition adjustment in example 2.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
The solder paste according to this embodiment is generally stored in a refrigerator, and needs to be taken out of the refrigerator 4-8 hours in advance and placed in a room temperature environment to restore the viscosity of the solder paste, and needs to be sufficiently stirred before use.
Example 1
The method for preparing the copper-based solder paste containing Cu67.7%, sn22.8%, ni3.8% and P5.7% in the embodiment comprises the following steps:
s1, preparing solder powder
30g of PH600 copper-based brazing filler metal with the melting point temperature of 596-608 ℃ and the components of Cu75.0%, P5.2%, sn15.6% and Ni4.2% are weighed and placed in a beaker, acetone is added into the beaker for ultrasonic cleaning for 15 minutes, then liquid in the cup is poured out to leave sediment, the steps are repeated for 4 times, organic solvents such as soldering flux and the like in the soldering paste are fully removed, finally alcohol is added into the sediment, and the sediment is placed in a drying box for drying at 60 ℃ to obtain brazing filler metal powder.
S2, preparing copper-based solder paste
30g of the solder powder in the step S1 is weighed and put into a test tube, 10% Sn metal powder (with purity more than 99.99 wt%) is weighed and mixed fully, and then 12.0% soldering flux ALPHA POP707 is added into the mixture and stirred again to prepare the copper-based solder paste.
The performance test of the copper-based solder paste prepared in example 1 was performed in the present invention:
melting point test: the copper-based solder paste prepared in this example was sampled with the original PH600 copper-based solder paste according to DSC equipment requirements, and DSC curves of the two pastes were measured to measure melting point temperatures.
FIG. 1 is a DSC of a solder before component adjustment in example 1; fig. 2 is a DSC diagram of the solder after component adjustment in example 1, and it can be seen that the technical solution of the present invention reduces the melting point of the PH600 copper-based solder paste by about 80 ℃, so as to achieve the effect of significantly reducing the melting point of the original copper-based solder, and further reducing the soldering cost.
Fig. 4 is a schematic diagram of an application example of the solder paste preparation in example 1.
Example 2
The preparation steps of the Cu/Cu-based solder/Cu sandwich braze joint with the cross section dimension of 5mm multiplied by 5mm and the weld width of 200 mu m are as follows:
s1, putting anaerobic Cu sheets (purity is more than 99.99 wt%) with the size of 3mm multiplied by 5mm into prepared 30% HNO 3 Soaking in aqueous solution to remove oxide and pollutants on the surface of a Cu sheet, then placing the Cu sheet into acetone for ultrasonic cleaning, and drying;
s2, horizontally placing the anaerobic Cu sheet cleaned in the step S1, placing a mask plate with the thickness of 200 mu m above the anaerobic Cu sheet, smearing the copper-based solder paste on the mask plate by using a fine paper cotton swab to form solder paste with the thickness of 200 mu m on the Cu sheet, removing the mask plate, placing another Cu sheet on the smeared copper-based solder paste and ensuring the horizontal placement to form a Cu/copper-based solder/Cu sandwich structure;
s3, welding the sandwich structure by adopting a tube furnace under the nitrogen atmosphere, wherein the welding temperature of the PH600 soldering paste is 630 ℃, the welding temperature of the soldering paste after component adjustment is 540 ℃, and cooling along with the furnace after welding for 10min, so that the Cu/copper-based solder/Cu sandwich soldered joint is obtained.
The performance test of the Cu/Cu-based solder/Cu sandwich braze joint prepared in example 2 is carried out by the invention:
mechanical property test: the mechanical properties (tensile strength and shearing strength) of the Cu/copper-based solder/Cu sandwich braze joint prepared in the example 2 are tested by using a WDW-1 universal tester and a TEST4500 shearing tester, the tensile strength of the original PH600 solder alloy is 396+/-5 MPa, the tensile strength of the solder alloy after component adjustment is 389+/-8 MPa, the shearing strength of the solder joint of the original PH600 solder sandwich structure is 356+/-7 MPa, and the shearing strength of the solder joint of the solder sandwich structure after component adjustment is 352+/-4 MPa without obvious strength reduction phenomenon.
Fig. 3 is an SEM image of the post-component adjustment joint of example 2 and an EDS image, wherein fig. a is an SEM image of the post-component adjustment joint of example 2 and fig. b is an EDS image of the post-component adjustment joint of example 2: the Cu/copper-based solder/Cu sandwich soldered joint is subjected to wire cutting and grinding to remove redundant solder, and then a designated section of the solder is subjected to fine polishing to obtain a metallographic structure of the section of the soldered joint, and the morphology of the metallographic structure is observed by a Scanning Electron Microscope (SEM).
FIG. 5 is a graph showing the comparison of the strength of Cu/Cu-based solder/Cu sandwich braze joints, specifically tensile and shear strength, before and after composition adjustment in example 2.
According to the invention, the component adjustment is carried out on the PH600 copper-based solder or soldering paste by utilizing the metallic tin, so that the solder or soldering paste with a relatively low melting point is manufactured on the premise of ensuring good use performance, the defect that the copper-based solder is high in melting point and easy to oxidize when being used as hard solder is overcome, the method has the advantages of saving energy and reducing cost, and meanwhile, the oxidation degree of Cu can be reduced by the lower heating temperature, so that the use performance is good.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (9)
1. The copper-based brazing filler metal is characterized by comprising the following components in percentage by mass: 67.5 to 67.9 percent of Cu, 22.6 to 23.0 percent of Sn, 3.7 to 3.9 percent of Ni and 5.6 to 5.8 percent of P.
2. The method for producing a copper-based solder according to claim 1, wherein the copper-based solder is obtained by adjusting the composition of a PH600 copper-based solder with metallic tin.
3. A copper-based solder paste comprising the copper-based solder of claim 1 and a flux.
4. A method of preparing a copper-based solder paste according to claim 3, wherein the copper-based solder paste is prepared by adding a flux after the composition of the copper-based solder powder of PH600 is adjusted by means of metallic tin.
5. The method of preparing a copper-based solder paste according to claim 4, comprising the steps of:
s1, preparing copper-based solder powder: ultrasonically cleaning and drying the PH600 copper-based brazing filler metal to obtain copper-based brazing filler metal powder;
s2, preparing the copper-based solder paste: and uniformly mixing the copper-based solder powder and the metal tin powder, and adding the soldering flux to uniformly mix to obtain the copper-based solder paste.
6. The method of preparing a copper-based solder paste according to claim 5, wherein the purity of the metallic tin powder is greater than 99.99wt.%.
7. The method of producing a copper-based solder paste according to claim 5, wherein the flux is ALPHA POP707, and the amount of the flux added is 12.+ -. 0.5% by weight of the copper-based solder powder.
8. Use of a copper-based solder according to claim 1 or a copper-based solder paste according to claim 3 for the preparation of copper-based soldered joints.
9. Use of the copper-based solder according to claim 1 or the copper-based solder paste according to claim 3 for the preparation of a copper-based VC vapor chamber.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310227613.8A CN116140866A (en) | 2023-03-10 | 2023-03-10 | Novel copper-based solder paste for low-melting-point VC soaking plate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310227613.8A CN116140866A (en) | 2023-03-10 | 2023-03-10 | Novel copper-based solder paste for low-melting-point VC soaking plate |
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-
2023
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