Low thermal conductivity and low-k dielectric aerogel material and preparation method therefor
View Patent ↗The present invention discloses the an aerogel material featuring of low thermal conductivity, low dielectric constant (low-D K ) and low dielectric-loss (low-D F ) and a preparation method therefor. The method comprises steps of: (1) mix and hydrolysis, (2) dispersion and condensation, (3) molding, and (4) drying. The prepared pure aerogel or fiber/aerogel composite is further processed by steps of: (5) polymer solution impregnating, (6) solvent drying and (7) crosslinking-solidifying to obtain a polymer/aerogel composite or a polymer/fiber/aerogel composite featuring of high strength, low thermal conductivity, low-D K and low-D F . The method provided by the present invention does not involve highly conductive solvents or additives, and a highly porous structure is formed so that the dielectric constant and dielectric loss of the aerogel material are significantly reduced, suitable for 5G communications, microwave circuits, protection and insulation for electric vehicle lithium battery modules.
1. A method for making a low thermal conductivity and low-k dielectric aerogel material, wherein the aerogel material comprises a pure aerogel, a fiber/aerogel composite, a polymer/aerogel composite, or a polymer/fiber/aerogel composite and the method comprising steps of:
mixing and hydrolysis step: adding a siloxane precursor to an ethanol water solution to form a mixed solution and then adding an acid catalyst to the mixed solution to perform a hydrolysis reaction, wherein the siloxane precursor comprises a hydrophobic siloxane compound, a siloxane compound or a combination thereof;
dispersion and condensation step: adding a dispersing solution to the mixed solution and then using an emulsifier or a stirring equipment to disperse the siloxane precursor to form a homogeneous sol, wherein the dispersing solution comprises a base catalyst;
molding step: injecting the sol to a mold so as to promote the sol to further condense into a solid-like aerogel wet-gel structure, wherein the mold comprises a molding mold or a molding mold comprising a fiber;
drying step: at atmospheric pressure, drying the solid-like aerogel wet-gel structure at a drying temperature so as to obtain the low thermal conductivity and low-k dielectric aerogel material with a homogeneous structure, wherein the drying temperature ranges from 60 to 150° C., the pure aerogel with thermal conductivity k ranging from 0.0113 to 0.018 W/(m·K), and the fiber/aerogel composite with thermal conductivity k ranging from 0.022 W/(m·K) to 0.032 W/(m·K); and
polymer solution impregnating step: preparing a polymer solution and injecting the polymer solution into the low thermal conductivity and low-k dielectric aerogel material so that a polymeric chain penetrates homogeneously into interior of the low thermal conductivity and low-k dielectric aerogel material to form a polymer solution-containing pure aerogel composite or a polymer solution-containing fiber/aerogel composite, wherein the polymer solution comprises a polymer and a mixing solvent, and the polymer comprises a thermosetting polymer, a thermoplastic polymer, a liquid crystalline polymer or a combination thereof; and
solvent drying step: placing the polymer solution-containing pure aerogel composite or the polymer solution-containing fiber/aerogel composite at a solvent drying temperature so as to vaporize the mixing solvent of the polymer solution, so that the polymer coats a network structure surface inside the pure aerogel or the fiber/aerogel composite or a fiber surface inside the fiber/aerogel composite to form the polymer/aerogel composite or the polymer/fiber/aerogel composite, wherein the solvent drying temperature ranges from 60 to 115° C.; wherein the polymer concentration in the polymer solution ranges from 0.01 wt % to 80.0 wt %.
2. The method as claimed in claim 1 , wherein the drying step comprises steps of:
solvent vaporizing step: placing the solid-like aerogel structure at an azeotropic vaporizing temperature so that the ethanol water solution in the solid-like aerogel wet-gel structure accomplishes azeotropic vaporization, and then distilling and drying the ethanol water solution to obtain a half-dried aerogel structure, wherein the azeotropic vaporizing temperature ranges from 60 to 110° C.; and
solvent bumping step: adjusting the azeotropic vaporizing temperature of the half-dried aerogel structure to a bumping temperature so that trace amount of a water of the ethanol water solution in the half-dried aerogel structure bumps with water molecules of the water of the ethanol water solution to produce a positive vapor pressure, and the positive vapor pressure produces micropores in the half-dried aerogel structure, wherein the bumping temperature ranges from 110 to 150° C.
3. The method as claimed in claim 1 , wherein the siloxane compound comprises tetramethoxysilane (TMOS), tetraethoxysilane (TEOS) or the combination thereof; the hydrophobic siloxane compound comprises methyltrimethoxysilane (MTMS), methyltriethoxysilane (MTES) or the combination thereof, wherein in the siloxane precursor, a molar ratio of the siloxane compound to the hydrophobic siloxane compound ranges from 0:100 to 40:60.
4. The method as claimed in claim 1 , wherein the ethanol water solution comprises (1) ethanol, and (2) deionized water, distilled water or secondary distilled water.
5. The method as claimed in claim 1 , wherein the fiber comprises glass fiber, ceramic fiber, rock wool fiber, polypropylene fiber, nylon fiber or polyester fiber; wherein the fiber comprises multi-porous glyph, multi-porous paper, multi-porous blanket, multi-porous rope, multi-porous plate or a combination thereof.
6. The method as claimed in claim 1 , wherein the low thermal conductivity and low-k dielectric aerogel material is a multi-porous structure with porosity ranging from 40.0 to 95%, density ranging from 0.180 to 0.600 g/cm 3 , dielectric constant ranging from 1.20 to 1.87 and dielectric loss ranging from 0.0026 to 0.0078.
7. The method as claimed in claim 1 , wherein the thermoplastic polymer comprises polyethylene, polypropylene, PTFE, polycarbonate, polyamide, polyamide, polyester, polyetherimide, polyphenylene ether, polyphenylene sulfide, polyether ketone or a combination thereof.
8. The method as claimed in claim 7 , wherein the polymer concentration in the polymer solution ranges from 5.0 wt % to 30.0 wt %.
9. The method as claimed in claim 1 , wherein the polymer is the thermosetting polymer, and the method further comprising a step of:
crosslinking-solidifying step: placing the polymer/aerogel composite or the polymer/fiber/aerogel composite at a specific crosslinking-solidifying temperature, and crosslinking the polymeric chain of the polymer coating the network structure surface and silica-based aerogel molecule to obtain a thermosetting polymer/aerogel composite or a thermosetting polymer/fiber/aerogel composite, wherein the thermosetting polymer/aerogel composite or the thermosetting polymer/fiber/aerogel composite features density ranging from 0.180 g/cm 3 to 0.600 g/cm 3 .
10. The method as claimed in claim 9 , wherein the polymer concentration in the polymer solution ranges from 5.0 wt % to 30.0 wt %.
11. The method as claimed in claim 10 , wherein when the thermosetting polymer is epoxy, the crosslinking-solidifying temperature ranges from 150 to 180° C.
12. The method as claimed in claim 10 , wherein when the thermosetting polymer is polyimide, the crosslinking-solidifying temperature ranges from 120 to 325° C.
13. The method as claimed in claim 9 , wherein the thermosetting polymer comprises epoxy, polyimide, phenolic plastic ester, polymelamine-formaldehyde plastic ester or a combination thereof.