CN111354514A - Packaging paste based on multi-dimensional nano material and preparation method thereof - Google Patents
Packaging paste based on multi-dimensional nano material and preparation method thereof Download PDFInfo
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- CN111354514A CN111354514A CN202010153063.6A CN202010153063A CN111354514A CN 111354514 A CN111354514 A CN 111354514A CN 202010153063 A CN202010153063 A CN 202010153063A CN 111354514 A CN111354514 A CN 111354514A
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000004806 packaging method and process Methods 0.000 title abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 88
- 239000002184 metal Substances 0.000 claims abstract description 88
- 238000002156 mixing Methods 0.000 claims abstract description 26
- 239000002923 metal particle Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 238000005530 etching Methods 0.000 claims abstract description 16
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 55
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 30
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 26
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 20
- 229910052802 copper Inorganic materials 0.000 claims description 20
- 239000010949 copper Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 14
- 239000011668 ascorbic acid Substances 0.000 claims description 13
- 229960005070 ascorbic acid Drugs 0.000 claims description 13
- 235000010323 ascorbic acid Nutrition 0.000 claims description 13
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 229910052709 silver Inorganic materials 0.000 claims description 11
- 239000004332 silver Substances 0.000 claims description 11
- 235000015165 citric acid Nutrition 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 9
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 9
- 229940116411 terpineol Drugs 0.000 claims description 9
- 239000012459 cleaning agent Substances 0.000 claims description 7
- 238000001312 dry etching Methods 0.000 claims description 7
- 150000002739 metals Chemical class 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 7
- 229920005989 resin Polymers 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052737 gold Inorganic materials 0.000 claims description 5
- 239000010931 gold Substances 0.000 claims description 5
- 150000007524 organic acids Chemical class 0.000 claims description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 3
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 3
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 2
- 239000011258 core-shell material Substances 0.000 claims description 2
- 229910052741 iridium Inorganic materials 0.000 claims description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 239000008393 encapsulating agent Substances 0.000 claims 8
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 26
- 239000002245 particle Substances 0.000 description 15
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 14
- 238000005245 sintering Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 11
- 230000010355 oscillation Effects 0.000 description 9
- 238000009210 therapy by ultrasound Methods 0.000 description 9
- 239000007769 metal material Substances 0.000 description 8
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 7
- 239000001361 adipic acid Substances 0.000 description 7
- 235000011037 adipic acid Nutrition 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 239000002135 nanosheet Substances 0.000 description 7
- 239000002070 nanowire Substances 0.000 description 7
- 229920001568 phenolic resin Polymers 0.000 description 7
- 239000005011 phenolic resin Substances 0.000 description 7
- 238000002791 soaking Methods 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 6
- 238000002390 rotary evaporation Methods 0.000 description 6
- 238000009792 diffusion process Methods 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 5
- 239000002042 Silver nanowire Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000002082 metal nanoparticle Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 239000002055 nanoplate Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004100 electronic packaging Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000001052 transient effect Effects 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009459 flexible packaging Methods 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- 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
- B23K37/00—Auxiliary devices or processes, not specially adapted to a procedure covered by only one of the preceding main groups
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Optics & Photonics (AREA)
- Conductive Materials (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention provides a nano-material-based packaging paste and a preparation method thereof, wherein the nano-material comprises at least two nano-metals with different dimensions, and the preparation method comprises the following preparation steps: the first step is as follows: etching holes on the surfaces of the first nano metal wires and/or the first nano metal sheets to form second nano metal wires and/or second nano metal sheets, wherein the diameters of the holes are 10-40 nm; secondly, cleaning the first nano metal particles, the second nano metal wires and/or the second nano metal sheets by using a first solvent to obtain second nano metal particles, third nano metal wires and/or third nano metal sheets; the third step: mixing second nano metal particles, third nano metal wires and/or third nano metal sheets to obtain a first mixture, and mixing the first mixture and a second solvent to obtain a second mixture; the fourth step: concentrating the second mixture to obtain an encapsulated paste. The method has simple process and mild execution conditions, and is suitable for mass production with low cost.
Description
Technical Field
The invention relates to the technical field of semiconductor interconnection materials, in particular to a packaging paste based on a multi-dimensional nano material and a preparation method thereof.
Background
In the emerging field of flexible electronic packaging and the like, the demand of lead-free solders is increasing, the welding temperature of the traditional Sn-based lead-free solders is usually over 200 ℃, and sintering interconnection on a heat-sensitive organic substrate (such as polymer and paper) is not facilitated in flexible packaging.
The low-temperature packaging interconnection process can effectively solve the technical problems, and certain solutions can be realized by the advantages of nano metal materials on nano sintering. In the nano-sintering process, the nano-materials are sintered together by diffusion, relying on the driving force from high surface energy, to form the encapsulating paste.
In the research and development process, no matter which kind of metal material is used to prepare the packaging paste, the adhesive strength and the fracture resistance strength of the packaging paste in the related art can not meet the use requirement, and the technical personnel in the field can not find an effective solution.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a preparation method of an encapsulating paste based on a multi-dimensional nano material, which is characterized by comprising the following steps: the nanometer material comprises nanometer metals with at least two different dimensions, and specifically comprises the following steps:
the first step is as follows: etching holes on the surface of the first nano metal wire and/or the first nano metal sheet to form a second nano metal wire and/or a second nano metal sheet, wherein the diameter of each hole is 10-40 nm;
the specific surface area and the roughness of the metal nano-sheets are increased due to the existence of the holes, and the existence of the holes of 10-40 nm is beneficial to improving the mutual binding force and the friction force among the nano-metal particles, the metal nano-wires and the metal nano-sheets during blending, so that the compactness of the paste is improved, and the subsequent sintering interconnection and the bonding strength are improved.
Secondly, cleaning the first nano metal particles, the second nano metal wires and/or the second nano metal sheets by using a first solvent to obtain second nano metal particles, third nano metal wires and/or third nano metal sheets;
the cleaning process is that the first solvent soaks the first nano metal particles, the second nano metal wires and/or the second nano metal sheets; then centrifuging, separating, washing and drying the soaked nano material to obtain second nano metal particles, third nano metal wires and/or third nano metal sheets;
the third step: mixing second nano metal particles, third nano metal wires and/or third nano metal sheets to obtain a first mixture, and mixing the first mixture and a second solvent to obtain a second mixture;
the fourth step: concentrating the second mixture to obtain an encapsulated paste.
Specifically, the second mixture is subjected to ultrasonic treatment, oscillation, dispersion and low-pressure rotary evaporation and concentration in sequence to obtain a packaged paste body, and the ultrasonic treatment is carried out for 20min to 50min and the oscillation treatment is carried out for 1h to 2 h.
Preferably, the mass ratio of the first nano metal particles to the second nano metal wires to the second nano metal sheets is 8-10: 3-5: 4.
the nano metal particle component can be a particle of a single metal or a particle of a core-shell structure consisting of two or more metals, wherein the core part of the metal constitutes one of gold, silver and copper, and the shell part of the metal constitutes one or more of tin, bismuth, iridium and titanium.
Preferably, the packaging paste of the multi-dimensional nano material is welded by adopting a transient liquid phase diffusion method.
Preferably, the length of the second nano metal wire is 30-50 μm, the diameter is 40nm, the length of the second nano metal sheet is 50-250 μm, the thickness is 10-20 nm, and the size of the first nano metal particle is 10-500 μm.
Preferably, the nano metal is one or more of gold, silver and copper.
Preferably, the etching is dry etching.
Preferably, the first solvent comprises an organic solvent and a cleaning agent, and the organic solvent is selected from ethanol, isopropanol, acetone, ethyl acetate and glycol; the cleaning agent is selected from ascorbic acid, citric acid and sodium dihydrogen phosphate; the mass ratio of the organic solvent to the cleaning agent is 15-25: 1.
Preferably, the mass ratio of the first mixture to the second solvent is 0.5-1: 0.2-0.4; the second solvent comprises organic acid, resin and a third solvent, wherein the third solvent is selected from ethanol, isopropanol, terpineol, glycol, glycerol and diglycol.
Preferably, the mass ratio of the organic acid to the resin to the third solvent is 0.05-0.1:0.01-0.03: 0.2-0.5.
The packaging paste prepared by the preparation method of the packaging paste based on the multi-dimensional nano material has the nano metal accounting for 75-85% of the weight of the material.
Compared with the paste of the simple metal particles, the paste of the metal nano-sheets and the metal nanowires with the holes is mixed with the metal particles, the interconnection temperature is lower, the time is shorter, and the shearing strength of the interconnection device is higher.
The beneficial effects of the invention at least comprise:
(1) the preparation method of the packaging paste provided by the invention has the advantages of simple process and mild execution conditions, and is suitable for mass low-cost production.
(2) The combination of a plurality of different dimensions of etched hole nano metals is beneficial to atomic diffusion and compact interconnection among particles during sintering, the shear strength, the bonding strength and the fracture resistance of the sintered paste are improved, and pressureless sintering can be better realized at a lower sintering temperature.
(3) The sintered paste manufactured based on the invention can be widely applied to a plurality of emerging microelectronic interconnection fields such as flexible electronic packaging, thermosensitive organic substrates, sensing lead-free microcircuits and the like.
Drawings
FIG. 1 is a microstructure diagram of an encapsulating paste prepared based on the method provided by the present invention；
FIG. 1a is a transmission electron microscope image of a mixed paste of metal nanowires and metal nanoparticles；
FIG. 1b is a transmission electron microscope image of the mixed paste of metal nanoparticles and metal nanosheets；
FIG. 1c is a transmission electron microscope image of the mixed paste of metal nanoparticles, metal nanowires and metal nanosheets；
FIG. 2 is a transmission electron microscope image and a scanning electron microscope image of the metal nano-sheet etched with holes under different magnifications.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the scope of the present invention.
During research and practical application, the applicant finds that different sintering effects can be achieved for different forms of nano-metals, for example, when one-dimensional nanowires and nanotube materials are used for interconnection, the maximum bonding strength of pure silver nanowire sintering is about 9MPa, and the maximum bonding strength is lower than that of zero-dimensional nanoparticle paste, because the capability of the nanowires to diffuse to form interconnection network is weaker than that of nanoparticles during sintering. A large number of experiments repeatedly verify that the low activation energy and the high surface energy are enhanced in nano-scale diffusion based on the size effect and the shape effect, the sintering temperature is obviously reduced, and the sintering rate is greatly improved. In order to combine nano metals with different morphologies, such as zero-dimensional nano particles, one-dimensional nano wires or nano tubes, two-dimensional nano sheets and other multi-dimensional nano metals, so as to provide an encapsulating paste material with better sintering performance. Meanwhile, in order to further improve the sintering interconnection capacity, a transient liquid phase diffusion method is introduced. The invention provides a preparation method of a multi-dimensional nanomaterial-doped packaging paste, wherein the nanomaterial comprises at least two different dimensions of nano metals, and the preparation method specifically comprises the following steps:
the first step is as follows: etching holes on the surface of the first nano metal wire and/or the first nano metal sheet to form a second nano metal wire and/or a second nano metal sheet, wherein the diameter of each hole is 10-40 nm;
secondly, cleaning the first nano metal particles, the second nano metal wires and/or the second nano metal sheets by using a first solvent to obtain second nano metal particles, third nano metal wires and/or third nano metal sheets;
the third step: mixing second nano metal particles, third nano metal wires and/or third nano metal sheets to obtain a first mixture, and mixing the first mixture and a second solvent to obtain a second mixture;
the fourth step: concentrating the second mixture to obtain an encapsulated paste.
Shear force test method:
the model is as follows: MCR high-grade rheometer
1. A circular flat head indenter with a diameter of 20mm was used to apply a pressure of 30N on the data line 4mm from the edge of the I/O port.
2. And inserting the plug into the female testing seat in the plane direction.
3. Applying 30N pressure to the front and back planes of the plug in the horizontal direction for 5min, and repeating the steps for 5 times.
4. And fixing the test female seat in the test fixture in the horizontal direction.
In some alternative embodiments, the nanomaterial may include, but is not limited to, two or more of a metal particle, a nano-metal wire, and a nano-metal sheet.
In some alternative embodiments, the metal is one or more of gold, silver and copper.
In some alternative embodiments, the organic solvent is ethanol, isopropanol, acetone, ethyl acetate, or ethylene glycol, and the cleaning agent is ascorbic acid, citric acid, or sodium dihydrogen phosphate.
In some optional embodiments, the length of the nano metal wire is 30-50 μm, the diameter is 40nm, and/or the length of the nano metal sheet is 50-250 μm, the thickness is 10-20 nm, and the size of the nano metal particle is 10-500 μm.
In some alternative embodiments, the organic acid is succinic acid, phthalic acid, adipic acid, malonic acid, pimelic acid, malic acid, salicylic acid, or glutaric acid, and/or the resin is a phenolic resin, an epoxy resin, or a polyvinyl butyral resin, and/or the third solvent is ethanol, isopropanol, terpineol, ethylene glycol, glycerol, or diethylene glycol.
In some alternative embodiments, ultrasonic treatment is performed for 20min, oscillation treatment is performed for 1h, and the nano metal accounts for 80% of the weight of the material after concentration.
Based on the method, the embodiment of the invention provides the encapsulating paste based on the nano material, and the encapsulating paste is manufactured based on the method.
Example 1
In a preferred embodiment 1 of the present invention, the following procedure is used to prepare the encapsulating paste:
forming a plurality of holes with the diameter of 10nm on the surfaces of the nano silver wires and the nano silver sheets by using dry etching, configuring an ascorbic acid solution with the mass concentration of 0.5 wt%, and respectively soaking the nano silver particles, the nano silver wires after etching and the nano silver sheets after etching for 24 hours by using the ascorbic acid solution, wherein the mass ratio of the ascorbic acid solution to each nano silver material is 5: 2; and then centrifuging, separating, washing and drying the soak solution, and mixing the washed nano silver particles, nano silver wires and nano silver sheets according to a mass ratio of 8: 3: and 4, mixing, namely mixing the mixed nano-silver material with adipic acid, phenolic resin and terpineol respectively according to the mass ratio of 0.8:0.05:0.01:0.2, and performing ultrasonic treatment for 20min and oscillation for 1h to perform reduced pressure rotary evaporation on the mixed solution to obtain a uniformly dispersed paste, wherein the nano-silver material accounts for 80% of the mass of the paste.
Example 2
In a preferred embodiment 2 of the present invention, the following procedure was used to prepare the encapsulating paste:
forming a plurality of holes with the diameter of 40nm on the surfaces of the nano silver wires and the nano silver sheets by using dry etching, configuring an ascorbic acid solution with the mass concentration of 0.5 wt%, and respectively soaking the nano silver particles, the nano silver wires after etching and the nano silver sheets after etching for 24 hours by using the ascorbic acid solution, wherein the mass ratio of the ascorbic acid solution to each nano silver material is 5: 2; and then centrifuging, separating, washing and drying the soak solution, and mixing the washed nano silver particles, nano silver wires and nano silver sheets according to a mass ratio of 8: 3: and 4, mixing, namely mixing the mixed nano-silver material with adipic acid, phenolic resin and terpineol respectively according to the mass ratio of 0.8:0.05:0.01:0.2, and performing ultrasonic treatment for 20min and oscillation for 1h to perform reduced pressure rotary evaporation on the mixed solution to obtain a uniformly dispersed paste, wherein the nano-silver material accounts for 80% of the mass of the paste.
Example 3
In a preferred embodiment 3 of the present invention, the following procedure is used to prepare the encapsulating paste:
forming a plurality of holes with the diameter of 10nm on the surfaces of the nano copper wires and the nano copper sheets by using dry etching, configuring a citric acid solution with the mass concentration of 0.5 wt%, and respectively soaking the nano copper particles, the nano copper wires after etching and the nano copper sheets after etching for 24 hours by using the citric acid solution, wherein the mass ratio of the citric acid solution to each nano copper material is 3: 1; and then centrifuging, separating, washing and drying the soak solution, and mixing the washed nano copper particles, nano copper wires and nano copper sheets according to a mass ratio of 8: 3: and 4, mixing, namely mixing the mixed nano copper material with adipic acid, phenolic resin and terpineol respectively according to the mass ratio of 0.8:0.05:0.01:0.2, and performing ultrasonic treatment for 20min and oscillation for 1h to reduce pressure and perform rotary evaporation on the mixed solution to obtain a uniformly dispersed paste, wherein the nano copper material accounts for 80% of the mass of the paste.
Example 4
In a preferred embodiment 4 of the present invention, the following procedure is used to prepare the encapsulating paste:
forming a plurality of holes with the diameter of 10nm on the surfaces of the nano silver wires and the nano silver sheets by using dry etching, configuring a citric acid solution with the mass concentration of 0.5 wt%, and respectively soaking the nano copper particles, the nano silver wires after etching and the nano silver sheets after etching for 24 hours by using the citric acid solution, wherein the mass ratio of the ascorbic acid solution to each nano metal material is 5: 2; and then centrifuging, separating, washing and drying the soak solution, and mixing the washed nano copper particles, nano silver wires and nano silver sheets according to a mass ratio of 8: 3: 4, mixing, namely mixing the mixed nano metal material with adipic acid, phenolic resin and terpineol respectively according to the mass ratio of 0.8:0.05:0.01:0.2, and performing ultrasonic treatment for 20min and oscillation for 1h to perform reduced pressure rotary evaporation on the mixed solution to obtain a uniformly dispersed paste, wherein the nano metal material accounts for 80% of the mass of the paste.
Example 5
In a preferred embodiment of the invention 5, the following procedure is used to prepare the encapsulating paste:
forming a plurality of holes with the diameter of 10nm on the surfaces of the nano silver wires and the nano silver sheets by using dry etching, configuring a citric acid solution with the mass concentration of 0.5 wt%, and respectively soaking the nano copper particles, the nano silver wires after etching and the nano silver sheets after etching for 24 hours by using the citric acid solution, wherein the mass ratio of the ascorbic acid solution to each nano metal material is 5: 2; and then centrifuging, separating, washing and drying the soak solution, and mixing the washed nano tin-coated copper particles, nano silver wires and nano silver sheets according to a mass ratio of 8: 3: 4, mixing, namely mixing the mixed nano metal material with adipic acid, phenolic resin and terpineol respectively according to the mass ratio of 0.8:0.05:0.01:0.2, and performing ultrasonic treatment for 20min and oscillation for 1h to perform reduced pressure rotary evaporation on the mixed solution to obtain a uniformly dispersed paste, wherein the nano metal material accounts for 80% of the mass of the paste.
Comparative example 1
The diameter of the surface hole of the silver nanowire and the silver nanoplate in the comparative example is 5nm, and other experimental conditions are the same as those in example 1.
Comparative example 2
The diameter of the surface hole of the silver nanowire and the silver nanoplate in the comparative example is 50nm, and other experimental conditions are the same as those in example 1.
Comparative example 3
The diameter of the surface hole of the silver nanowire and the silver nanoplate in the comparative example is 100nm, and other experimental conditions are the same as those in example 1.
Comparative example 4
Preparing an ascorbic acid solution with the mass concentration of 0.5 wt%, wherein the ascorbic acid solution comprises the following components in a mass ratio of 5: 2, respectively soaking the nano silver particles, the nano silver wires and the nano silver sheets for 24 hours, then centrifuging, separating, washing and drying the soaking solution, and mixing the washed silver nano materials according to the mass ratio of the nano silver particles: nano silver wire: and (3) nano silver sheets 8: 3: and 4, mixing the mixed silver nano material with adipic acid, phenolic resin and terpineol respectively according to the mass ratio of 0.8:0.05:0.01:0.2, and carrying out ultrasonic treatment on the mixed solution for 20min and oscillation for 1h to obtain a uniformly dispersed paste, wherein the silver nano material accounts for about 80% of the interconnected material.
Table 1 table comparing the properties of each group
| Sample(s) | Shear strength (Mpa) |
| Example 1 | 30 |
| Example 2 | 32 |
| Example 3 | 33 |
| Example 4 | 31 |
| Example 5 | 32 |
| Comparative example 1 | 15 |
| Comparative example 2 | 19 |
| Comparative example 3 | 16 |
| Comparative example 4 | 17 |
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of an encapsulating paste based on a multi-dimensional nano material is characterized by comprising the following steps: the nano material comprises nano metals with at least two different dimensions, and comprises the following preparation steps:
the first step is as follows: etching holes on the surfaces of the first nano metal wires and/or the first nano metal sheets to form second nano metal wires and/or second nano metal sheets, wherein the diameters of the holes are 10-40 nm;
secondly, cleaning the first nano metal particles, the second nano metal wires and/or the second nano metal sheets by using a first solvent to obtain second nano metal particles, third nano metal wires and/or third nano metal sheets;
the third step: mixing second nano metal particles, third nano metal wires and/or third nano metal sheets to obtain a first mixture, and mixing the first mixture and a second solvent to obtain a second mixture;
the fourth step: concentrating the second mixture to obtain an encapsulated paste.
2. The method for preparing the multi-dimensional nanomaterial-based encapsulant paste as claimed in claim 1, wherein: the mass ratio of the first nano metal particles to the second nano metal wires to the second nano metal sheets is 8-10: 3-5: 4.
3. the method for preparing the multi-dimensional nanomaterial-based encapsulant paste as claimed in claim 1, wherein: the length of the second nano metal wire is 30-50 mu m, the diameter of the second nano metal wire is 40nm, the length of the second nano metal sheet is 50-250 mu m, the thickness of the second nano metal sheet is 10-20 nm, and the size of the first nano metal particle is 10-500 mu m.
4. The method for preparing the multi-dimensional nanomaterial-based encapsulant paste as claimed in claim 1, wherein: the nano metal is one or more of gold, silver and copper.
5. The method for preparing the multi-dimensional nanomaterial-based encapsulant paste as claimed in claim 1, wherein: the nano metal particles are of a core-shell structure, the metal of the core part is selected from gold, silver and copper, and the metal of the shell part is selected from one or more of tin, bismuth, iridium and titanium.
6. The method for preparing the multi-dimensional nanomaterial-based encapsulant paste as claimed in claim 1, wherein: the etching is dry etching.
7. The method for preparing the multi-dimensional nanomaterial-based encapsulant paste as claimed in claim 1, wherein: the first solvent comprises an organic solvent and a cleaning agent, wherein the organic solvent is selected from ethanol, isopropanol, acetone, ethyl acetate and glycol; the cleaning agent is selected from ascorbic acid, citric acid and sodium dihydrogen phosphate; the mass ratio of the organic solvent to the cleaning agent is 15-25: 1.
8. The method for preparing the multi-dimensional nanomaterial-based encapsulant paste as claimed in claim 1, wherein: the mass ratio of the first mixture to the second solvent is 0.5-1: 0.2-0.4; the second solvent comprises organic acid, resin and a third solvent, wherein the third solvent is selected from ethanol, isopropanol, terpineol, glycol, glycerol and diglycol.
9. The method for preparing the multi-dimensional nanomaterial-based encapsulant paste as claimed in claim 8, wherein: the mass ratio of the organic acid to the resin to the third solvent is 0.05-0.1:0.01-0.03: 0.2-0.5.
10. An encapsulating paste prepared by the method for preparing an encapsulating paste based on multi-dimensional nanomaterials as claimed in claims 1-9, wherein: the nano metal accounts for 75-85% of the weight of the material.
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