Conductive adhesive with spherical graphene and manufacturing method thereof

Patent metadata

Field	Value
Publication number	US-9725625-B2
Application number	US-201414398978-A
Country	US
Kind code	B2
Filing date	Aug 14, 2014
Priority date	Jul 22, 2014
Publication date	Aug 8, 2017
Grant date	Aug 8, 2017

Abstract

The invention provide a manufacturing method for producing conductive adhesive with spherical graphene, and the steps comprise as following: step 1 : preparing monomer, initiator, a dispersing agent and solvent to manufacture a monomer compound, and use the monomer compound to produce polymer micro ball; step 2 : heating pre-treatment or plasma etching pre-treatment to the said polymer micro ball; step 3 : by chemical vapor deposition, the polymer micro ball after pre-treatment from step 2 to grow graphene outside surfaces or inside polymer micro ball, and then obtain the spherical graphene; step 4 : producing epoxy gel system made by epoxy, hardener and accelerant with a certain ratio mixing homogeneously; step 5 : dispersing the spherical graphene from step 3 into the epoxy gel system to produce pre-material of conductive adhesive of spherical graphene; Step 6 : deforming the pre-material of conductive adhesive of spherical graphene, and then obtain conductive adhesive of spherical graphene.

First claim

The invention claimed is:

1. A manufacturing method for producing conductive adhesive with spherical graphene, comprising:
step 1 : preparing a monomer, an initiator, a dispersing agent and a solvent to manufacture a monomer mixture, and using the monomer mixture to produce a polymer microsphere;
step 2 : heating pre-treatment or plasma etching pre-treatment to the polymer microsphere;
step 3 : by chemical vapor deposition, the polymer microsphere after pre-treatment from step 2 to grow graphene on the surface of or inside the polymer microsphere, and then obtain the spherical graphene;
step 4 : producing an epoxy gel system made by epoxy, hardener and accelerant with a certain ratio mixing homogeneously;
step 5 : dispersing the spherical graphene from step 3 into the epoxy gel system to produce a pre-material of conductive adhesive with spherical graphene; and
Step 6 : defoaming the pre-material of conductive adhesive of spherical graphene, and then obtain the conductive adhesive with spherical graphene;
wherein the plasma etching pre-treatment in step 2 is to obtain an active polymer microsphere by etching the polymer microsphere with inductively coupled plasma in sulfur hexafluoride and dioxygen, at 80-150° C. for 2 min˜1 h; and
wherein the chemical vapor deposition in step 3 is dispersing the pretreated polymer microspheres from step 2 into a sealed space of chemical vapor deposition; next, inserting a mixture gas of methane, hydrogen and other auxiliary gas inside the sealed space after vacuuming; and then growing graphene on the surfaces of or inside the polymer microsphere by heating the polymer microsphere pretreated from step 2 with at least one way following:
infrared ray, thermal radiation, laser, micro-wave, plasma, ultraviolet ray or induction heating.

2. A manufacturing method for producing conductive adhesive with spherical graphene according to claim 1 , wherein in step 1 , the monomer is acrylic acid, phenylethene, methyl methacrylate or divinylbenzene; the initiator is comprising at least one selected from azobisisobutyronitrile or benzoyl peroxide; the dispersing agent is polyvinylpyrrolidone, polyethylene glycol, polyglycolic acid or polyacrylic acid; the solvent is comprising water and a composition mixed at least one selected from ethanol, methanol or isopropanol.

3. A manufacturing method for producing conductive adhesive with spherical graphene according to claim 1 , wherein an amount of the monomer to the monomer mixture is 8 wt %˜42 wt %; an amount of the initiator to the monomer mixture is 0.11 wt %˜5.2 wt %; an amount of the dispersing agent to the monomer mixture is 4.9 wt %˜21 wt %; an amount of the solvent to the monomer mixture is 3 wt %˜56 wt %.

4. A manufacturing method for producing conductive adhesive with spherical graphene according to claim 1 , wherein the heating pre-treatment in step 2 is to obtain a porous polymer microsphere by dispersing the polymer microsphere into inert atmosphere at 100-500° C. for 0.5-5 h.

5. A manufacturing method for producing conductive adhesive with spherical graphene according to claim 1 , wherein a volume ratio for the methane to the mixture gas is 1%˜10%; a volume ratio for the hydrogen to the mixture gas is 50%˜99%; and the other auxiliary gas is comprising at least one selected from vapor, nitrogen, or argon.

6. A method for producing conductive adhesive with spherical graphene according to claim 1 , wherein in step 4 , the epoxy is bisphenol A epoxy resins E44, bisphenol A epoxy resins E51, bisphenol A epoxy resins E54, bisphenol A epoxy resins EPON826 or bisphenol A epoxy resins EPON828; the hardener is hexahydrophthalic anhydride, tetrahydrophthalic anhydride, succinic dihydrazide, adipic acid dihydrazide, dicyandiamide or phenylenediamine; the accelerant is 2-ethyl-4-methylimidazole, imidazole, 2-methylimidazole or triethylamine;
an amount of the epoxy to the epoxy gel system is 80 wt %˜95 wt %; an amount of the hardener to the epoxy gel system is 1 wt %˜12 wt %; and an amount of the accelerant to the epoxy gel system is 0.3 wt %˜5 wt %.

7. A manufacturing method for producing graphene sphere conductive adhesive according to claim 1 , wherein in step 5 , a mass ratio for the epoxy gel system to the spherical graphene is 100:2˜30.

8. A manufacturing method for producing conductive adhesive with spherical graphene, comprising:
step 1 : preparing a monomer, an initiator, a dispersing agent and a solvent to manufacture a monomer mixture, and using the monomer mixture to produce a polymer microsphere;
step 2 : heating pre-treatment or plasma etching pre-treatment to the polymer microsphere;
step 3 : by chemical vapor deposition, the polymer micro ball after pre-treatment from step 2 to grow graphene inside or outside the polymer microsphere, and then obtain the spherical graphene;
step 4 : producing an epoxy gel system made by epoxy, hardener and accelerant with a certain ratio mixing homogeneously;
step 5 : dispersing the spherical graphene from step 3 into the epoxy gel system to produce a pre-material of conductive adhesive with spherical graphene; and
Step 6 : defoaming the pre-material of conductive adhesive with spherical graphene, and then obtain the conductive adhesive with spherical graphene;
wherein in step 1 , the monomer is acrylic acid, phenylethene, methyl methacrylate or divinylbenzene; the initiator is comprising at least one from azobisisobutyronitrile or benzoyl peroxide; the dispersing agent is polyvinylpyrrolidone, polyethylene glycol, polyglycolic acid or polyacrylic acid; the solvent is comprising water and a composition mixed at least one selected from ethanol, methanol or isopropanol; wherein an amount of the monomer to the monomer mixture is 8 wt %˜42 wt %; an amount of the initiator to the monomer mixture is 0.11 wt %˜5.2 wt %; an amount of the dispersing agent to the monomer mixture is 4.9 wt %˜21 wt %; an amount of the solvent to the monomer mixture is 3 wt %˜56 wt %;
wherein in step 2 , the pre-treatment is to obtain a porous polymer microsphere by dispersing the polymer microsphere into inert atmosphere at 100-500° C. for 0.5-5 h;
wherein in step 2 , the plasma etching pre-treatment is to obtain an active polymer microsphere by etching the polymer microsphere with inductively coupled plasma in sulfur hexafluoride and dioxygen, at 80-150° C. for 2 min˜1 h;
wherein in step 3 , steps of the chemical vapor deposition are dispersing the pretreated polymer microsphere from step 2 into a sealed space of chemical vapor deposition; next, inserting a mixture gas of methane, hydrogen and other auxiliary gas inside the sealed space after vacuuming; and then growing graphene on the surfaces of or inside the polymer microsphere by heating the polymer microsphere pretreated from step 2 with at least one way listed as following: infrared ray, thermal radiation, laser, micro-wave, plasma, ultraviolet ray or induction heating; wherein a volume ratio for the methane to the mixture gas is 1%˜10%; a volume ratio for the hydrogen to the mixture gas is 50%˜99%; the other auxiliary gas is comprising at least one selected from vapor, nitrogen, or argon;
wherein in step 4 , the epoxy is bisphenol A epoxy resins E44, bisphenol A epoxy resins E51, bisphenol A epoxy resins E54, bisphenol A epoxy resins EPON826 or bisphenol A epoxy resins EPON828; the hardener is hexahydrophthalic anhydride, tetrahydrophthalic anhydride, succinic dihydrazide, adipic acid dihydrazide, dicyandiamide or phenylenediamine; the accelerant is 2-ethyl-4-methylimidazole, imidazole, 2-methylimidazole or triethylamine;
an amount of the epoxy to the epoxy gel system is 80 wt %˜95 wt %; an amount of ratio for the hardener to the epoxy gel system is 1 wt %˜12 wt %;

Assignees

• Shenzhen China Star Optoelect
• Shenzhen China Star Optoelect

Inventors

• Lee Yungjui
• Zhang Xia
• Li Ji
• Chen Yahui

Classifications

• B01J2/003

  followed by coating of the granules (to prevent the granules sticking together B01J2/30) · CPC title

• C08J7/00

  Chemical treatment or coating of shaped articles made of macromolecular substances (coating with metallic material C23C; electrolytic deposition of metals C25) · CPC title

• C09J163/00

  Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins · CPC title

• C08K9/12

  Adsorbed ingredients {, e.g. ingredients on carriers} · CPC title

• B01J2/06

  in a liquid medium · CPC title