WO2014005514A1 - 超材料及其制备方法 - Google Patents
超材料及其制备方法 Download PDFInfo
- Publication number
- WO2014005514A1 WO2014005514A1 PCT/CN2013/078714 CN2013078714W WO2014005514A1 WO 2014005514 A1 WO2014005514 A1 WO 2014005514A1 CN 2013078714 W CN2013078714 W CN 2013078714W WO 2014005514 A1 WO2014005514 A1 WO 2014005514A1
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- Prior art keywords
- ceramic
- housing
- dielectric
- layer
- conductive
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 78
- 239000000919 ceramic Substances 0.000 claims description 221
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 59
- 239000000835 fiber Substances 0.000 claims description 59
- 238000005266 casting Methods 0.000 claims description 45
- 239000002002 slurry Substances 0.000 claims description 44
- 239000002131 composite material Substances 0.000 claims description 31
- 239000000758 substrate Substances 0.000 claims description 25
- 239000011230 binding agent Substances 0.000 claims description 23
- 238000007650 screen-printing Methods 0.000 claims description 22
- 238000002360 preparation method Methods 0.000 claims description 21
- 239000012779 reinforcing material Substances 0.000 claims description 21
- 239000004744 fabric Substances 0.000 claims description 19
- 239000005350 fused silica glass Substances 0.000 claims description 17
- 238000009694 cold isostatic pressing Methods 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 14
- 239000012815 thermoplastic material Substances 0.000 claims description 7
- 229920001187 thermosetting polymer Polymers 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- 238000007582 slurry-cast process Methods 0.000 claims description 6
- 239000000853 adhesive Substances 0.000 claims description 5
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- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 241000264877 Hippospongia communis Species 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 claims 1
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- -1 polyethylene Polymers 0.000 description 14
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 11
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- 239000004917 carbon fiber Substances 0.000 description 9
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- 238000005245 sintering Methods 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 6
- 239000002270 dispersing agent Substances 0.000 description 6
- 230000004044 response Effects 0.000 description 6
- 230000035699 permeability Effects 0.000 description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical group [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 229920002125 Sokalan® Polymers 0.000 description 4
- BAECOWNUKCLBPZ-HIUWNOOHSA-N Triolein Natural products O([C@H](OCC(=O)CCCCCCC/C=C\CCCCCCCC)COC(=O)CCCCCCC/C=C\CCCCCCCC)C(=O)CCCCCCC/C=C\CCCCCCCC BAECOWNUKCLBPZ-HIUWNOOHSA-N 0.000 description 4
- PHYFQTYBJUILEZ-UHFFFAOYSA-N Trioleoylglycerol Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC(OC(=O)CCCCCCCC=CCCCCCCCC)COC(=O)CCCCCCCC=CCCCCCCCC PHYFQTYBJUILEZ-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000002708 enhancing effect Effects 0.000 description 4
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- 238000002844 melting Methods 0.000 description 4
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- 239000000203 mixture Substances 0.000 description 4
- 229910052750 molybdenum Inorganic materials 0.000 description 4
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- 239000000377 silicon dioxide Substances 0.000 description 4
- 229920002545 silicone oil Polymers 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- PHYFQTYBJUILEZ-IUPFWZBJSA-N triolein Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CCCCCCCC)COC(=O)CCCCCCC\C=C/CCCCCCCC PHYFQTYBJUILEZ-IUPFWZBJSA-N 0.000 description 4
- 229940117972 triolein Drugs 0.000 description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 239000010937 tungsten Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 241000533950 Leucojum Species 0.000 description 3
- 229910001252 Pd alloy Inorganic materials 0.000 description 3
- 238000005553 drilling Methods 0.000 description 3
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- 239000006260 foam Substances 0.000 description 3
- 238000009766 low-temperature sintering Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229910000431 copper oxide Inorganic materials 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 150000002466 imines Chemical class 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 239000002694 phosphate binding agent Substances 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 230000000379 polymerizing effect Effects 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 2
- SWPMTVXRLXPNDP-UHFFFAOYSA-N 4-hydroxy-2,6,6-trimethylcyclohexene-1-carbaldehyde Chemical compound CC1=C(C=O)C(C)(C)CC(O)C1 SWPMTVXRLXPNDP-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000000992 sputter etching Methods 0.000 description 1
- 238000009849 vacuum degassing Methods 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
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- C04B2237/368—Silicon nitride
Definitions
- the invention relates to the field of metamaterials, in particular to a metamaterial and a preparation method thereof. Background technique
- the dielectric constant and magnetic permeability of each point of the material are the same or different, so that the dielectric constant and magnetic permeability of the material are arranged regularly, and the magnetic permeability and the regular arrangement are regularly arranged.
- the electrical constant allows the material to have a macroscopic response to electromagnetic waves, such as converging electromagnetic waves, diverging electromagnetic waves, and the like. This type of material with regularly arranged magnetic permeability and dielectric constant is called a metamaterial.
- the basic unit of metamaterial includes a conductive geometry and a substrate to which the conductive geometry is attached.
- the conductive geometry is preferably a metal microstructure having a planar or stereo topology capable of responding to an incident electromagnetic wave electric field and/or a magnetic field, changing the pattern and/or size of the metal microstructure on each metamaterial base unit.
- the response of each metamaterial base unit to incident electromagnetic waves can be varied.
- the arrangement of a plurality of metamaterial basic units in a regular pattern allows the metamaterial to have a macroscopic response to electromagnetic waves.
- the material of the dielectric substrate can be a composite material and a ceramic. Most composite substrates have a certain degree of brittleness. When supermaterials are widely used in outdoor environments, the room environment is very different from the ideal environment of the laboratory. Substance which affects properties such as external water vapor easily enters the interior of the metamaterial through the gaps in the substrate, causing oxidation of the conductive geometry and/or aging of the substrate, which affects the properties of the metamaterial. Although the ceramic substrate has good wave transmission performance and high temperature resistance, it cannot satisfy high strength performance. Summary of the invention
- a method for preparing a metamaterial of the present invention which comprises
- Step 1 making a first dielectric housing having a spatial geometry
- Step 2 fabricating a dielectric patch having at least one conductive geometry
- Step 3 attaching the at least one dielectric patch to a part or all of the surface of the first dielectric housing to form at least one dielectric patch layer;
- Step 4 The first medium casing and the dielectric patch layer are integrated into one body.
- the preparation method wherein the first medium casing is a first ceramic casing.
- step 1 a second ceramic housing having a spatial geometry is further fabricated, and in step 3, the second ceramic housing is mated with the first ceramic housing to The dielectric chip layer is encapsulated between the first ceramic housing and the second ceramic housing.
- step 4 the first ceramic housing, the dielectric patch layer, and the second The ceramic shell is integrally sintered.
- step 1 a second ceramic housing having a spatial geometry is further formed, and the first dielectric housing and the second ceramic housing are respectively formed; in step 3, at least one The dielectric patch is bonded to the first dielectric housing; in step 4, the first dielectric housing to which the dielectric patch is bonded is integrated with the second ceramic housing.
- the invention also provides a preparation method of a conformal ceramic metamaterial, the preparation method comprising the following steps Step:
- preparing a green body degassing and pre-polymerizing a suspension containing a ceramic powder and an organic system to obtain a slurry, pouring the slurry into the first mold, inserting the mold core, and solidifying to obtain a gel injection molding Green body
- the ceramic powder is made into a ceramic slurry and cast into a green ceramic sheet, and a conductive geometric structure is prepared on the green ceramic sheet by a screen printing technique;
- step d casting the same slurry as in step a into the second mold, inserting the green body with the conductive geometry in step c, and solidifying to obtain a gel-molded conformal structure blank containing the conductive geometry;
- the conformal structure blank containing the conductive geometry is degreased and sintered to obtain a conformal ceramic metamaterial.
- the first mold and the second mold are both double open molds, and the second mold has a larger diameter than the first mold.
- a surface of the conductive geometric structure is coated with a green sheet of the same composition as in the step b.
- the conformal structure blank containing the conductive geometry is shaped by a cold isostatic pressing technique at a pressure of 100 to 150 MPa before being discharged.
- the inner and outer surfaces of the green body are curved surfaces.
- the organic system includes a dispersant, an organic monomer, and a crosslinking agent.
- the metal used to prepare the conductive geometry is silver, platinum, molybdenum or tungsten.
- a conformal ceramic metamaterial comprising a conformal ceramic metamaterial prepared by the above method.
- the curved conformal ceramic metamaterial prepared by the method for preparing a metamaterial of the present invention not only has good wave transmission performance and high temperature resistance, but also enhances the strength of the metamaterial due to the conformal combination of the ceramic shell and the dielectric patch.
- Fig. 1 is a schematic view of a green ceramic sheet containing a conductive geometry prepared in the step b of an embodiment of the present invention.
- FIG. 2 is a schematic view of a conformal ceramic metamaterial prepared in an embodiment of the present invention.
- Figure 3 is a block diagram showing a method of preparing a metamaterial in another embodiment of the present invention.
- FIG. 4 is a block diagram of a method of fabricating a dielectric patch having a conductive geometry in accordance with another embodiment of the present invention.
- Figure 5 is a longitudinal cross-sectional view of a metamaterial in another embodiment of the present invention.
- Figure 6 is a transverse cross-sectional view of a metamaterial in another embodiment of the present invention.
- Figure 7 is a schematic illustration of a conductive geometry in another embodiment of the invention.
- Figure 8 is a schematic illustration of a conductive geometry in yet another embodiment of the present invention.
- Figure 9 is a block diagram showing a method of preparing a metamaterial in still another embodiment of the present invention.
- Figure 10 is a block diagram showing a method of fabricating a dielectric patch having a conductive geometry in accordance with still another embodiment of the present invention.
- the conductive geometry is generally a microstructure having a specific pattern and material in the field of metamaterials, which modulates electromagnetic waves passing through a specific frequency band of the body, and has substantially the same meaning as the microstructure.
- Embodiment 1 can be understood with reference to Figs. 1 and 2.
- a method for preparing a conformal ceramic metamaterial comprising the steps of:
- preparing a green body degassing and pre-polymerizing a suspension containing a ceramic powder (such as cordierite, alumina or non-oxide Si3N4) and an organic system to obtain a slurry, and pouring the slurry into the first mold, And inserting a mold core, and curing to obtain a gel injection molded green body;
- a ceramic powder such as cordierite, alumina or non-oxide Si3N4
- the specific process is as follows: the organic monomer and the cross-linking agent are dissolved in water, and the water-soluble polymer is added as a dispersing agent to prepare a monomer solution; then the ceramic powder is added to the monomer solution and thoroughly mixed, and after vacuum degassing The initiator and the catalyst are further stirred and pre-polymerized to obtain a desired slurry; the obtained slurry is poured into the first mold, and inserted into the mold core, and cured at room temperature to obtain a gel-molded green body, and The inner and outer surfaces of the finished green body are curved surfaces.
- step b preparing a green ceramic sheet containing a conductive geometry: the same ceramic powder as in step a is made into a ceramic slurry and cast into a green ceramic sheet, and a conductive geometric structure is prepared on the green ceramic sheet by screen printing technology;
- the conductive geometric structure is a plane or a three-dimensional structure composed of a metal wire having a certain geometric shape, such as an I-shaped type, a snowflake type, etc., and the conductive geometric structure can be prepared by using a screen printing technique, and other etching, drilling, and the like can also be adopted.
- the metal used in the processing of conductive geometries is silver, platinum, molybdenum, tungsten, or silver-palladium alloys, such as engraving, electron engraving or ion etching.
- step c affixing the green sheet containing the conductive geometry prepared in step b to the outer surface of the green body in step a to obtain a green body with a conductive geometry
- step d the same slurry as in step a is poured into the second mold, inserted into the green body with conductive geometry in step c, and cured at room temperature to obtain a gel-molded conformal structure blank containing conductive geometry;
- the first mold and the second mold are both double-opening molds, and the diameter of the second mold is larger than the diameter of the first mold.
- the conformal structure blank containing the conductive geometry is shaped by a cold isostatic pressing technique (cold isostatic pressing technique or warm isostatic pressing technique) under a pressure of 100 to 150 MPa;
- the gel-shaped injection molding method is organically combined with LTCC or HTCC technology to prepare a curved conformal ceramic metamaterial, which not only has good wave-transmission performance and high temperature resistance, but also has a conformal combination of internal and external two-layer ceramic sheets and a conductive geometric structure.
- the strength of the conformal ceramic metamaterial is increased between the two ceramic sheets.
- Embodiment 2 can be understood with reference to FIGS. 3 to 7.
- the method for preparing a metamaterial includes the first step of providing a ceramic shell.
- the ceramic housing may be a conventional ceramic housing, and the ceramic housing has a spatial geometry.
- the ceramic housing is divided into a first ceramic housing (outer housing) 1 1 and a second ceramic.
- the casing (inner casing) 12, the ceramic casings 1 1 and 12 are in the shape of a space curved surface.
- first ceramic housing 11 and/or the second ceramic housing 12 are formed by slurry casting, gel casting or cold isostatic pressing.
- the first ceramic housing 11 and/or the second ceramic housing 12 may also be made of fused silica ceramic.
- a ceramic housing is retained, and the second ceramic housing 12 can be omitted.
- the metamaterial preparation method further includes the second step of providing a dielectric patch comprising a conductive geometry.
- the dielectric patch 132 is shown in FIG. 7.
- the horizontal thick line 1323 and the vertical thick line 1321 are electrically conductive structures
- the block portion 1322 is a dielectric substrate, which may be a ceramic substrate or other A substrate prepared from a high temperature resistant material.
- the conductive geometry shown in Figure 5 is suitable for enhancing the wave transmission properties of supermaterials.
- the conductive geometry of this embodiment is not limited thereto, and other corresponding conductive geometries may be made for electromagnetic waves, such as enhanced absorbing properties.
- the method for preparing the dielectric patch can be referred to FIG. 4.
- it may include the steps of fabricating a reinforcing material, such as a step of fabricating a quartz fiber cloth, in which, according to a preferred embodiment, fused silica is first selected.
- the fiber cloth has a plain or twill surface and is impregnated with silicone oil.
- the silica content is 99.95 %
- the temperature is 1200 ° C
- the thickness is between 0.12 mm and 0.70 mm.
- the slurry is mixed with ethanol and methyl ethyl ketone as a mixed solvent, the ball-milled fused silica powder is mixed, the mixed dispersant polyacrylic acid and triolein are added, and then a binder such as prB and plasticizer C is added.
- the alcohol is stirred to form a concentrated slurry having good fluidity.
- the aforementioned quartz fiber can be replaced with other reinforcing materials, such as glass fiber, fang Polyester, polyethylene, carbon or polyester.
- the method for preparing a dielectric patch further includes forming a casting sheet.
- casting is performed on the casting machine, and in a specific implementation process, Casting on a quartz fiber cloth to form a quartz fiber reinforced quartz powder casting tape (ceramic layer) having high strength and high softness, that is, a ceramic substrate or ceramic layer 133 as shown in Fig. 7 can be formed.
- a quartz fiber reinforced quartz powder casting tape ceramic layer having high strength and high softness
- the method for preparing a dielectric patch further includes forming a conductive geometric structure, in which a conductive paste is first prepared, and then a screen printing plate is overlaid on the casting tape to form a plurality of screen plates. a pattern similar to the conductive geometry, followed by coating the conductive paste on a screen printing plate, the conductive paste being attached to the casting tape via a mesh in a plurality of patterns of the screen printing plate, after curing That is, a conductive structure layer is formed, and the conductive structure layer may be a conductive structure composed of a lateral thick line 1323 and a vertical thick line 1321 as shown in FIG.
- a plurality of dielectric patches 13 are disposed partially or entirely on the surface of the housing of the ceramic housing 11 or 12.
- the surface of the casing may be one surface or two surfaces.
- step three in conjunction with FIG. 3 and FIG. 4, the aforementioned casting strip containing the conductive geometry is combined with the ceramic shell, and then sintered to form a metamaterial by sintering.
- an adhesive is applied to the surface of the casing of the ceramic casing (substrate/base) 1 1 , 12 prior to lamination or / And the corresponding media patch on the surface.
- the adhesive layer 14 is in the form of a liquid or a slurry at the time of sticking.
- the binder is a fiber reinforced tie layer and the fibers may be glass fibers, quartz fibers, aramid fibers, polyethylene fibers, carbon fibers or polyester fibers.
- the binder comprises a molten metal and/or a non-metal oxide such as quartz powder, zirconium oxide, copper oxide, silica sol, and the weight percentage thereof is: l ⁇ 20 wt%, l ⁇ 10wt%, l ⁇ 10wt%, l ⁇ 5wt%, and the rest is Al(HPO 4 ) 2 .
- the binder comprises fused silica powder, water glass, zirconium silicate, and alumina, and the weight percentages thereof are: 5 to 35 wt%, 1 to 5 wt%, 5 to 10 wt%, 30 to 40 wt%, respectively. %, the rest is water.
- a flexible casting sheet having a conductive geometric structure is attached to one surface of the ceramic casings 1 1 and 12, and the casting sheet is in a blank state. Before sintering, cold isostatic pressing is preferably performed to shape the ceramic casing.
- a high-temperature binder slurry mixed with a quartz powder filler is applied to coat the desired surface, when coated Before the slurry has not been hardened, another ceramic casing or dielectric patch with or without conductive geometry is closed, and pressure is applied to fill the bonding slurry.
- the low temperature baking causes the binder to undergo a curing reaction.
- the curing reaction chemical formula is:
- the low temperature sintering process temperature is less than the melting point of the conductive geometry, for example 961 °C.
- the phosphate binder may be mixed with fused silica powder, quartz short fibers, or a perforated (punched) quartz fiber cloth having a bonding layer thickness of between 1 mm and 2 mm.
- the dielectric patch layers of the respective sides of the first ceramic housing and/or the second ceramic housing are spliced by a plurality of casting sheets 13 and have a similar composition.
- Embodiment 3 can be understood with reference to FIGS. 3 to 6 and 8.
- the same reference numerals are used to denote the same or similar elements, and the description of the same technical content is omitted, and the same reference numerals are used to denote the same or similar elements.
- Parts similar to those of Embodiment 2 can be referred to FIG. 3, FIG. 4, FIG. 5, and FIG.
- the metamaterial preparation method includes the first step of providing a ceramic shell.
- the ceramic housing may be a conventional housing made of various ceramics having a spatial geometry. As shown in Fig. 5, the ceramic housing 11 has a space curved shape. In a preferred embodiment, the ceramic housing 11 is formed by slurry casting, gel casting or cold isostatic pressing. In a preferred embodiment, the ceramic housing 11 is made of fused quartz ceramic. In other embodiments of the present invention, on the basis of this embodiment, similar to the structure shown in Fig. 3, the second ceramic housing 12 may be added.
- the metamaterial preparation method further includes the second step of providing a dielectric patch comprising a conductive geometry.
- the dielectric patch 132 is shown in Fig. 8.
- the horizontal thick line and the vertical thick line of the conductive geometric layer 132 are electrically conductive structures, and the square portion is a ceramic substrate.
- the conductive geometry shown in Figure 8 is suitable for enhancing the wave transmission properties of metamaterials.
- the conductive geometry of this embodiment is not limited thereto, and other corresponding conductive geometries for electromagnetic waves may be made, such as enhanced absorbing properties.
- the method for preparing the dielectric patch can be referred to FIG. 4.
- it may include the steps of fabricating a reinforcing material, such as a step of fabricating a quartz fiber cloth, in which, according to a preferred embodiment, fused silica is first selected.
- the fiber cloth has a plain or twill surface and is impregnated with silicone oil.
- the silica content is 99.9 %
- the temperature is 1300 ° C
- the thickness is between 0.15 mm and 0.80 mm.
- the method for preparing a dielectric patch without a conductive geometry further includes forming a cast sheet.
- a quartz fiber reinforced quartz powder casting tape (ceramic layer) having high strength and high flexibility, that is, a ceramic substrate or ceramic layer 133 as shown in Fig. 6 can be formed.
- a method of fabricating a dielectric patch containing a conductive geometry further includes forming a conductive geometry, in which a conductive paste is first prepared, and then a screen printing plate is overlaid on the casting tape, using a screen printing Forming a plurality of patterns identical to the conductive geometry, and then coating the conductive paste on a screen printing plate, the conductive paste being attached to the casting by a mesh in a plurality of patterns of the screen printing plate.
- the conductive layer is formed after curing, and the conductive structure layer may be the conductive structure layer 132 as shown in FIG.
- the dielectric patch 13 includes two ceramic layers 133, 131 forming a conductive geometric layer 132 between the two ceramic layers 133, 131.
- a plurality of dielectric patches 13 are disposed partially or entirely on the surface of the housing of the ceramic housing 1 1 or 12.
- the surface of the casing may be one surface or two surfaces.
- the casting tape (ceramic layer) containing the conductive geometry and the casting tape (ceramic layer) not containing the conductive geometry are combined with the ceramic shell. Sintering is then carried out to form a metamaterial by sintering.
- an adhesive is applied to the ceramic casing (substrate/substrate) 1 1 before lamination. Or / and the corresponding media patch on the surface.
- the adhesive layer 14 is in the form of a liquid or a slurry at the time of sticking.
- the binder is a fiber reinforced bonding layer.
- the binder comprises molten metal and/or non-metal oxides such as quartz powder, zirconia, copper oxide, silica sol, and the weight percentages thereof are: 1 ⁇ 20 wt%, 1 to 10 wt%, 1 to 10 wt%, 1 to 5 wt%, and the balance is Al(HPO 4 ) 2 .
- the binder comprises fused silica powder, water glass, zirconium silicate, and aluminum oxide, and the weight percentage thereof is 5 to 35 wt %, 1 to 5 wt %, 5 to 10 wt %, respectively. 30 ⁇ 40wt%, the rest is water.
- a flexible casting sheet (ceramic layer) having a conductive geometric structure and a casting sheet (ceramic layer) are pasted on one surface of the ceramic shell 11 to form a blank state, and before sintering, cold isostatic pressing is preferably performed to make the ceramic
- the housing is shaped. As shown in FIGS. 5 and 6, the entire metamaterial includes 12 layers of dielectric material. In FIG. 6, from top to bottom, the ceramic casing 11 is in turn, the binder layer 14, and the ceramic layer 133 not containing the conductive geometry.
- conductive geometric layer 132 ceramic layer 131 without conductive geometry
- adhesive layer 14 ceramic layer 133 without conductive geometry, conductive geometric layer 132, ceramic layer 131 without conductive geometry, sticky
- the coupon layer 14 a ceramic layer 133 that does not include a conductive geometry, a conductive geometry layer 132, a ceramic layer 131 that does not include a conductive geometry, an adhesive layer 14, and a ceramic housing 12.
- a high-temperature binder slurry mixed with a quartz powder filler is applied to coat the desired surface, when coated Before the slurry has not been hardened, another ceramic casing or dielectric patch with or without conductive geometry is closed, and pressure is applied to fill the bonding slurry.
- the low temperature baking causes the binder to undergo a curing reaction.
- the curing reaction chemical formula is:
- the low temperature sintering process temperature is less than the melting point of the conductive geometry, for example 961 °C.
- the phosphate binder may be mixed with fused silica powder, quartz short fibers, or a perforated (punched) quartz fiber cloth having a bonding layer thickness of between 1 mm and 2 mm.
- the dielectric patch layer on the corresponding side of the ceramic housing 11 is spliced by a plurality of casting sheets 13, which are similarly formed or corresponding to the first ceramic housing.
- a spatial geometry of the shape of the ceramic housing such as a spatial curved surface, ie the shape of the dielectric patch is adapted to the shape of the corresponding side surface of the first or second ceramic housing to allow the dielectric to be attached
- the sheet layer as a whole has no clearance fit with the one side surface of the first or second ceramic housing.
- Embodiment 4 can be understood with reference to Figs. 5 to 7, Fig. 9, and Fig. 10.
- the metamaterial preparation method comprises the first step of providing a first dielectric housing 1 1 and a second ceramic housing 12.
- the first medium casing (outer casing) 1 1 and the second ceramic casing (inner casing) 12 have a space curved shape.
- the first dielectric housing 1 1 may be a ceramic housing, which may be formed by sintering.
- the first dielectric housing 11 is a composite material, and the molding of the first dielectric housing 11 specifically includes curing the first dielectric housing, and the composite material is a thermosetting or thermoplastic material such as a polyacyl group.
- these composite materials may further comprise a reinforcing material, which is at least one of fibers, fabrics, or particles, for example
- the reinforcing material is fiber, such as glass fiber, quartz fiber, aramid fiber, polyethylene fiber, carbon fiber or polyester fiber.
- these composite materials can also be multilayer structures.
- the second ceramic housing 12 is formed by slurry casting, gel casting or cold isostatic pressing.
- the second ceramic housing 12 may also be cast and sintered from a fused silica ceramic slurry.
- the method for preparing a metamaterial further includes the second step of providing a dielectric patch comprising a conductive geometric structure, wherein the conductive geometric structure is a planar or three-dimensional structure having a certain geometric shape, such as an I-shape, a snowflake. Type and so on.
- the dielectric patch 132 is in the embodiment shown in FIG.
- the thick line 1323 and the longitudinal thick line 1321 are metal structures, and the block portion 1322 is a dielectric substrate.
- the conductive geometry shown in Figure 7 is suitable for enhancing the wave transmission properties of metamaterials.
- the conductive geometry of this embodiment is not limited thereto, and other corresponding conductive geometries may be made for electromagnetic waves, such as enhanced absorbing properties.
- the method for preparing the dielectric patch can be referred to FIG. 10.
- it may include the steps of fabricating a reinforcing material, such as a step of fabricating a quartz fiber cloth, in which, according to a preferred embodiment, fused silica is first selected.
- the fiber cloth has a plain or twill surface and is impregnated with silicone oil.
- the silica content is 99.95 %
- the temperature is 1200 ° C
- the thickness is between 0.12 mm and 0.70 mm.
- the slurry is mixed with ethanol and methyl ethyl ketone as a mixed solvent, the ball-milled fused silica powder is mixed, the mixed dispersant polyacrylic acid and triolein are added, and then a binder such as prB and plasticizer C is added.
- the alcohol is stirred to form a concentrated slurry having good fluidity.
- the aforementioned quartz fiber may be replaced with other reinforcing materials such as glass fiber, aramid fiber, polyethylene fiber, carbon fiber or polyester fiber.
- the method for preparing a dielectric patch further includes forming a casting sheet.
- a casting sheet On the basis of the foregoing steps, after the slurry is vacuum defoamed, casting on a quartz fiber cloth on a casting machine to form a high strength.
- the method for preparing a dielectric patch further includes forming a conductive geometric structure, in which a conductive paste is first prepared, and then a screen printing plate is overlaid on the casting tape to form a plurality of screen plates. a pattern similar to the conductive geometry, followed by coating the conductive paste on a screen printing plate, the conductive paste being attached to the casting tape via a mesh in a plurality of patterns of the screen printing plate, after curing That is, a conductive geometric layer is formed, and the conductive geometric layer may be a conductive geometric structure composed of a horizontal thick line 1323 and a vertical thick line 1321 as shown in FIG.
- the substrate of the dielectric patch may also be a composite material, a composite material.
- a composite material such as polyimide, polyester, polytetrafluoroethylene, polyurethane, polyarylate, PET, PE or PVC
- the composite may be one or more layers containing foam and/or honeycomb Layer structure.
- the composite material may contain a reinforcing material, which is at least one of fibers, fabrics, or particles, for example, the reinforcing material is a fiber such as glass fiber, quartz fiber, aramid fiber, polyethylene fiber, carbon fiber or Polyester.
- the conductive geometry can also be formed on the composite by etching, drilling, engraving, electro-engraving or ion engraving.
- the metal used to process the conductive geometry is silver, platinum, molybdenum, tungsten, or silver-palladium alloy.
- a plurality of dielectric patches 13 are disposed on one side of the first dielectric housing 11.
- the dielectric patch 13 is affixed to a portion or all of the surface of the first dielectric housing 1 1 to form at least one first dielectric housing 1 1 having a dielectric patch 13 .
- the dielectric patch containing the conductive geometry is combined with the first dielectric housing 1 1 and then integrated with the second ceramic housing.
- the integrated method includes, but is not limited to:
- the first dielectric housing 1 1 to which the dielectric patch 13 is bonded is engaged with the second ceramic housing 12.
- the low temperature sintering process temperature is lower than the melting point of the conductive geometry, such as 961 °C.
- the dielectric patch layers of the respective sides of the first dielectric housing 1 1 and the second ceramic housing 12 are spliced by a plurality of casting sheets 13 to form a common Similar to or corresponding to a spatial geometry of the shape of the first dielectric housing and the second ceramic housing, such as a spatial curved surface, ie the shape of the dielectric patch and the shape of the corresponding side surface of the first or second ceramic housing Adapting so that the dielectric patch layer as a whole has no gap fit with the one side surface of the first or second ceramic housing.
- Embodiment 4 can be understood with reference to Figs. 5 to 6 and Figs. 8 to 10.
- the metamaterial preparation method includes the first step of providing a first dielectric housing 1 1 and a second ceramic housing 12.
- the first medium casing 1 has a space curved shape.
- the first dielectric housing 1 1 may be a ceramic housing, which may be formed by sintering.
- the first dielectric housing 11 is a composite material, and the molding of the first dielectric housing 11 specifically includes curing the first dielectric housing, and the composite material is a thermosetting or thermoplastic material such as a polyacyl group.
- these composite materials may further comprise a reinforcing material, which is at least one of fibers, fabrics, or particles, for example
- the reinforcing material is fiber, such as glass fiber, quartz fiber, aramid fiber, polyethylene fiber, carbon fiber or polyester fiber.
- these composite materials may also be one or more layers comprising foam and/or honeycomb.
- the second ceramic housing 12 is formed by slurry casting, gel casting or cold isostatic pressing. In a preferred embodiment, the second ceramic housing 12 is cast and sintered from a fused silica ceramic slurry.
- the metamaterial preparation method further includes the second step of providing a dielectric patch comprising a guide Electrical geometry
- conductive geometry is a plane or three-dimensional structure composed of wire with a certain geometric shape, such as I-shaped, snowflake and so on.
- the dielectric patch 132 is in the embodiment shown in FIG. 8, in which the lateral thick lines and the longitudinal thick lines of the conductive geometric layer 132 are metal structures, and the block portions are dielectric substrates.
- the conductive geometry shown in Figure 8 is suitable for enhancing the wave transmission properties of metamaterials.
- the conductive geometry of this embodiment is not limited thereto, and other corresponding conductive geometries may be made for electromagnetic waves, such as enhanced absorbing properties.
- the method for preparing the dielectric patch can be referred to FIG. 10.
- it may include the steps of fabricating a reinforcing material, such as a step of fabricating a quartz fiber cloth, in which, according to a preferred embodiment, fused silica is first selected.
- the fiber cloth has a plain or twill surface and is impregnated with silicone oil.
- the silica content is 99.9 %
- the temperature is 1300 ° C
- the thickness is between 0.15 mm and 0.80 mm.
- the slurry is mixed with ethanol and methyl ethyl ketone as a mixed solvent, the ball-milled fused silica powder is mixed, the mixed dispersant polyacrylic acid and triolein are added, and then a binder such as prB and plasticizer C is added.
- the alcohol is stirred to form a concentrated slurry having good fluidity.
- quartz fiber can be replaced with other reinforcing materials such as glass fiber, aramid fiber, polyethylene fiber, carbon fiber or polyester fiber.
- a method for preparing a dielectric patch without a conductive geometry further includes forming a cast sheet.
- a quartz fiber cloth On the basis of the foregoing steps, after vacuum defoaming the slurry, on a casting machine, on a quartz fiber cloth. Casting, forming a quartz fiber reinforced quartz powder casting tape (ceramic layer) having high strength and high softness, that is, a dielectric substrate or ceramic layer 133 as shown in Fig. 8 can be formed.
- the aforementioned quartz fiber may be replaced by glass fiber, aramid fiber, polyethylene fiber, carbon fiber or polyester fiber.
- a method of fabricating a dielectric patch containing a conductive geometry further includes forming a conductive geometry, in which a conductive paste is first prepared, and then a screen printing plate is overlaid on the casting tape, using a screen printing The plate forms a plurality of patterns identical to the conductive geometry, and then the conductive paste is coated on a screen plate, the conductive paste being attached via a mesh in a plurality of patterns of the screen printing plate.
- a conductive geometric layer is formed, and the conductive geometric layer may be a conductive geometric layer 132 as shown in FIG.
- the substrate of the dielectric patch may also be a composite material
- the composite material is a thermosetting or thermoplastic material such as polyimide, polyester, polytetrafluoroethylene, polyurethane, polyarylate, PET. , PE or PVC
- the composite material may be one or more layers comprising foam and/or honeycomb.
- the composite material may contain a reinforcing material, which is at least one of fibers, fabrics, or particles, for example, the reinforcing material is a fiber such as glass fiber, quartz fiber, aramid fiber, polyethylene fiber, carbon fiber or Polyester.
- the conductive geometry can also be formed on the composite by etching, drilling, engraving, electro-engraving or ion engraving.
- the metal used to process the conductive geometry is silver, platinum, molybdenum, tungsten, or silver-palladium alloy.
- the dielectric patch 13 includes two ceramic layers 133, 131 forming a conductive geometric layer 132 between the two ceramic layers 133, 131.
- the outer dimension W1 of the two ceramic layers 133, 131 may be 2.5 mm * 2.5 mm
- the outer dimension W2 of the conductive geometric layer 132 may be 2.7 mm * 2.7 mm
- the width HI of the conductive geometric structure may be 0.2 mm.
- the dimensions may vary depending on the design of the different purposes, and the implementation of the invention is not limited to the specific dimensions described above.
- a plurality of dielectric patches 13 are disposed on one side of the first dielectric housing 11.
- the dielectric patch 13 is affixed to a portion or all of the surface of the first dielectric housing 1 1 to form at least one first dielectric housing 1 1 having a dielectric patch 13 .
- the foregoing conductive ribbon-containing casting tape (ceramic layer), the first dielectric shell 1 1 and the second ceramic shell not including the conductive geometric layer
- the body is combined and then integrated with the second ceramic housing, and the integrated method includes but is not limited to: Bonding the first dielectric housing 11 and the second ceramic housing 12 to which the dielectric patch 13 is bonded by the molten slurry;
- the first dielectric housing 1 1 to which the dielectric patch 13 is bonded is engaged with the second ceramic housing 12.
- the entire metamaterial includes 12 layers of dielectric material.
- the first dielectric case 1 1 and the adhesive layer 14 are sequentially arranged from top to bottom, and the conductive structure is not included.
- the aforementioned high temperature pressure bonding temperature is less than the melting point of the conductive geometry, for example, 961 °C.
- the dielectric patch layer on the corresponding side of the ceramic housing 11 is spliced by a plurality of dielectric patches 13, which together have a composition similar to or corresponding to the first dielectric shell.
- a spatial geometry of the shape of the body and/or the second ceramic housing, such as a spatial curved surface, ie the shape of the dielectric patch is adapted to the shape of the respective side surface of the first or second ceramic housing, So that the dielectric patch layer as a whole has no gap fit with the one side surface of the first or second ceramic housing.
- the manufacturing medium case and the ceramic case are subjected to a molding step such that when the medium case to which the dielectric patch is bonded is integrated with the ceramic case , to avoid gasification of the conductive geometry.
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Abstract
一种具有空间几何机构的超材料的制备方法,包括步骤1,制作具有空间几何形状的第一介质壳体;步骤2,制作具有至少一个导电几何结构的介质贴片;步骤3,将所述至少一个介质贴片贴附于所述第一介质壳体表面的局部或者全部,以使所述介质贴片拼接在一起而形成至少一层具有空间几何形状的介质贴片层;以及步骤4,将所述第一介质壳体与所述介质贴片层结合成一体。
Description
超材料及其制备方法 技术领域
本发明涉及超材料领域, 尤其涉及一种超材料及其制备方法。 背景技术
光, 作为电磁波的一种, 其在穿过玻璃的时候, 因为光线的波长远大于 原子的尺寸, 因此我们可以用玻璃的整体参数, 例如折射率, 而不是组成玻 璃的原子的细节参数来描述玻璃对光线的响应。 相应的, 在研究材料对其他 电磁波响应的时候, 材料中任何尺度远小于电磁波波长的结构对电磁波的响 应也可以用材料的整体参数, 例如介电常数 ε和磁导率 μ来描述。 通过设计材料 每点的结构使得材料各点的介电常数和磁导率都相同或者不同从而使得材料 整体的介电常数和磁导率呈一定规律排布, 规律排布的磁导率和介电常数即 可使得材料对电磁波具有宏观上的响应, 例如汇聚电磁波、 发散电磁波等。 该类具有规律排布的磁导率和介电常数的材料我们称之为超材料。
超材料的基本单元包括导电几何结构以及该导电几何结构附着的基材。 导电几何结构优选为金属微结构, 金属微结构具有能对入射电磁波电场和 /或 磁场产生响应的平面或立体拓扑结构, 改变每个超材料基本单元上的金属微 结构的图案和 /或尺寸即可改变每个超材料基本单元对入射电磁波的响应。 多 个超材料基本单元按一定规律排列即可使得超材料对电磁波具有宏观的响 应。
目前的超材料都是在平面介质基板上覆上导电几何结构。 介质基板的材 料可为复合材料和陶瓷。 复合材料基板大多数具有一定的脆性, 当超材料广 泛应用于室外环境时, 则由于室外环境与实验室的理想环境的很大不同, 室
外水汽等影响性能的物质很容易通过基材上的缝隙进入超材料内部导致导电 几何结构出现氧化和 /或基材发生老化导致超材料性能受到影响。 陶瓷基板虽 然透波性能好且耐高温, 但满足不了高强度性能。 发明内容
本发明的目的在于提供一种新的超材料及其制备方法, 该超材料为陶瓷 材料。
本发明的超材料的制备方法, 其包括
步骤 1, 制作具有空间几何形状的第一介质壳体;
步骤 2, 制作具有至少一个导电几何结构的介质贴片;
步骤 3, 将所述至少一个介质贴片贴附于所述第一介质壳体表面的局部或 者全部, 形成至少一层介质贴片层; 以及
步骤 4, 将所述第一介质壳体与所述介质贴片层结合成一体。
所述的制备方法, 其中所述第一介质壳体为第一陶瓷壳体。
所述的制备方法, 其中在步骤 1中, 还制作具有空间几何形状的第二陶瓷 壳体, 在步骤 3中将所述第二陶瓷壳体与所述第一陶瓷壳体配合, 以使所述介 质贴片层封装于所述第一陶瓷壳体和所述第二陶瓷壳体之间, 在步骤 4中, 将 所述第一陶瓷壳体、 所述介质贴片层、 所述第二陶瓷壳体一体烧结成型。
所述的制备方法, 其中 在步骤 1中, 还制作具有空间几何形状第二陶瓷 壳体, 分别将所述第一介质壳体和第二陶瓷壳体成型; 在步骤 3中, 将至少一 个所述介质贴片与所述第一介质壳体粘结; 在步骤 4中, 将粘结有介质贴片的 第一介质壳体与所述第二陶瓷壳体结合成一体。
本发明还提供共形陶瓷超材料的制备方法, 所述制备方法包括以下步
骤:
a、 制备生坯: 将含有陶瓷粉料和有机体系的悬浮体脱气、 预聚得到浆 料, 将浆料浇注到第一模具中, 并插入模具芯子, 固化后得到凝胶注模成型 的生坯;
b、 制备含导电几何结构的生瓷片: 将陶瓷粉料制成陶瓷浆料并流延制成 生瓷片, 通过丝网印刷技术在生瓷片上制备导电几何结构;
c、 将制备好的含导电几何结构的生瓷片贴覆于所述生坯外表面, 得到带 导电几何结构的生坯;
d、 将与步骤 a中相同的浆料浇注到第二模具中, 插入步骤 c中带导电几何 结构的生坯, 固化后得到凝胶注模成型的含导电几何结构的共形结构坯料; e、 将含导电几何结构的共形结构坯料排胶、 烧结, 获得共形陶瓷超材 料。
所述第一模具和所述第二模具都为双开模具, 并且所述第二模具的口径 大于所述第一模具的口径。
所述步骤 b中在所述生瓷片上丝网印刷导电几何结构后, 在所述导电几何 结构的表面覆一层与步骤 b中相同成分的生瓷片。
所述含导电几何结构的共形结构坯料在排胶之前通过冷等静压技术在 100〜150MPa的压力下定型。
所述生坯的内外表面为曲面。
所述有机体系包括分散剂、 有机单体和交联剂。
向所述已脱气的浆料中加入引发剂和催化剂并搅拌均匀。
制备所述导电几何结构所用的金属为银、 铂、 钼或钨。
一种共形陶瓷超材料, 包括上述方法制备的共形陶瓷超材料。
本发明的超材料制备方法所制备的曲面共形陶瓷超材料, 不仅透波性能 好、 耐高温, 由于陶瓷壳体和介质贴片共形结合, 提高了这种超材料的强 度。 附图概述
本发明的具体特征、 性能由以下的实施例及其附图进一步给出。
图 1是本发明一实施例的步骤 b中制备的含导电几何结构的生瓷片示意 图。
图 2是本发明一实施例中制备的共形陶瓷超材料示意图。
图 3是本发明另一实施例中超材料制备方法的方框图。
图 4是本发明另一实施例中具有导电几何结构的介质贴片的制备方法的方 框图。
图 5是本发明另一实施例中超材料的纵向剖面图。
图 6是本发明另一实施例中超材料的横向剖面图。
图 7是本发明另一实施例中导电几何结构的示意图。
图 8是本发明再一实施例中导电几何结构的示意图。
图 9是本发明又一实施例中超材料制备方法的方框图。
图 10是本发明又一实施例中具有导电几何结构的介质贴片的制备方法的 方框图。 本发明的最佳实施方式
为了使本发明的目的、 技术方案及优点更加清楚明白, 以下结合附图及 实施例, 对本发明进行进一步详细说明。 应当理解, 此处所描述的具体实施
例仅仅用以解释本发明, 并不用于限定本发明。
在后述各实施例中, 导电几何结构在超材料领域一般是具有特定图案和 材质的微结构, 会对经过其身的特定频段的电磁波产生调制作用, 与微结构 具有实质上相同的含义。
实施例 1
实施例 1可以参照图 1和图 2来进行理解。
一种共形陶瓷超材料的制备方法, 所述制备方法包括以下步骤:
a、 制备生坯: 将含有陶瓷粉料 (如堇青石、 氧化铝或非氧化物 Si3N4 等) 和有机体系的悬浮体脱气、 预聚得到浆料, 将浆料浇注到第一模具中, 并插入模具芯子, 固化后得到凝胶注模成型的生坯;
其中具体过程为: 将有机单体和交联剂溶解于水中, 并加入水溶性高分 子作为分散剂, 制成单体溶液; 再向单体溶液中加入陶瓷粉料充分混合, 真 空脱气后再加入引发剂和催化剂搅拌均匀、 预聚得到所需浆料; 将得到的浆 料浇注到第一模具中, 并插入模具芯子, 室温固化后得到凝胶注模成型的生 坯, 并且所制成的生坯的内外表面为曲面。
b、 制备含导电几何结构的生瓷片: 将与步骤 a中相同的陶瓷粉料制成陶 瓷浆料并流延制成生瓷片, 通过丝网印刷技术在生瓷片上制备导电几何结 构;
其中导电几何结构是由金属丝构成的具有一定几何形状的平面或者立体 结构, 如工字型、 雪花型等, 可以采用丝网印刷技术制备出导电几何结构, 也可以采用其他蚀刻、 钻刻、 雕刻、 电子刻或离子刻等技术, 加工导电几何 结构所采用的金属为银、 铂、 钼、 钨、 或银钯合金等。
当然也可以在导电几何结构的表面再覆上一层相同成分的生瓷片, 使导
电几何结构夹在两层流延而成的生瓷片之间, 如图 1所示, 增强它们的机械强 度。
c、 将步骤 b中制备的含导电几何结构的生瓷片贴覆于步骤 a中的生坯外表 面, 得到带导电几何结构的生坯;
d、 将与步骤 a中相同的浆料浇注到第二模具中, 插入步骤 c中带导电几何 结构的生坯, 室温固化后得到凝胶注模成型的含导电几何结构的共形结构坯 料;
其中第一模具和第二模具都为双开模具, 并且第二模具的口径大于第一 模具的口径。
e、 含导电几何结构的共形结构坯料通过冷等静压技术 (冷等静压技术或 温冷等静压技术) 在 100〜150MPa的压力下定型;
f、 将定型后的含导电几何结构的共形结构坯料排胶、 烧结, 获得共形陶 瓷超材料, 如图 2所示;
g、 对已制成的共形陶瓷超材料进行切割、 打磨等加工, 获得所需形状、 大小的产品; 当然切割、 打磨等加工步骤也可以在冷等静压之后进行, 因为 陶瓷坯料比烧结后的陶瓷更易加工。
采用凝胶注模成型法与 LTCC或 HTCC技术有机地结合起来, 制备的曲面 共形陶瓷超材料, 不仅透波性能好、 耐高温, 由于内外两层陶瓷片共形结合 及导电几何结构也夹在两片陶瓷片之间, 提高了这种共形陶瓷超材料的强 度。 实施例 2
实施例 2可以参照图 3至图 7来理解。
如图 3所示, 超材料制备方法包括步骤一, 提供陶瓷壳体。 陶瓷壳体可以 是常规的各种陶瓷制成的壳体, 陶瓷壳体为空间几何结构, 如图 5所示, 陶瓷 壳体分为第一陶瓷壳体 (外壳体) 1 1和第二陶瓷壳体 (内壳体) 12, 陶瓷壳 体 1 1、 12成空间曲面形状。 需要注意的是, 在图 5至图 8所示的结构中, 这些 以及后续其他的附图均仅作为示例, 其并非是按照等比例的条件绘制的, 并 且不应该以此作为对本发明实际要求的保护范围构成限制。 优选的实施例 中, 第一陶瓷壳体 1 1和 /或第二陶瓷壳体 12利用浆料浇注成型、 凝胶浇注成型 或冷等静压成型制得。 优选的实施例中, 第一陶瓷壳体 1 1和 /或第二陶瓷壳体 12也可以是由熔融石英陶瓷制成。 在本发明的其他实施例中, 保留一层陶瓷 壳体就可以了, 第二陶瓷壳体 12可以省略。
继续参照图 3, 超材料制备方法还包括步骤二, 提供介质贴片, 其包含导 电几何结构。 介质贴片 132如图 7所示, 图中, 横向粗线 1323和纵向粗线 1321 为导电结构, 而方框部分 1322为介质基片, 该介质基片可以是陶瓷基片, 也 可以是其他耐高温材料制备的基片。 图 5所示的导电几何结构适合于增强超材 料的透波性能。 本实施例的导电几何结构不限于此, 还可以是对电磁波作出 其他相应的导电几何结构, 例如是增强吸波性能。
介质贴片的制备方法可以参照图 4, 在具体的实施过程中, 其可以包括制 作增强材料的步骤, 如制作石英纤维布的步骤, 在该步骤中, 根据优选的实 施例, 首先选用熔融石英纤维布, 其表面为平纹或斜纹, 浸润硅油, 二氧化 硅含量 99.95 %, 耐温 1200°C, 厚度 0.12mm至 0.70mm之间。 然后, 配浆料, 以 乙醇和丁酮作为混合溶剂, 混入球磨过的熔融石英粉, 添加混合分散剂聚丙 烯酸和三油酸甘油酯, 再加入粘结剂, 如 prB和增塑剂丙三醇, 经搅拌制成流 动性好的浓浆料。 前述石英纤维可以替换为其他增强材料, 如玻璃纤维、 芳
纶纤维、 聚乙烯纤维、 碳纤维或聚酯纤维。
继续参照图 4, 介质贴片的制备方法还包括形成流延片, 在前述步骤的基 础上, 对浆料真空除泡后, 在流延机上进行流延, 在具体的实施过程中, 可 以在石英纤维布上做流延, 形成强度高, 柔软度高的石英纤维增强石英粉流 延带 (陶瓷层) , 即可以形成如图 7所示的陶瓷基片或陶瓷层 133。
继续参照图 4, 介质贴片的制备方法还包括形成导电几何结构, 在该步骤 中, 首先制备导电浆料, 然后在前述流延带上覆盖丝网印版, 利用丝网印版 形成多个与导电几何结构相同的图案, 接着在丝网印版上涂覆所述导电浆 料, 所述导电浆料经由丝网印版的多个图案内的网眼而附着于前述流延带, 固化后即形成导电结构层, 导电结构层可以是如图 7所示的横向粗线 1323和纵 向粗线 1321组成的导电结构。
继续参照图 5和图 6, 在本发明的一实施例中, 在陶瓷壳体 11或 12的壳体 表面的局部或全部布置有多层介质贴片 13。 在此, 壳体表面可以是一个表 面, 也可以是两个表面。
在步骤三, 结合图 3和图 4, 将前述含导电几何结构的流延带与陶瓷壳体 结合, 然后再进行烧结, 通过烧结形成超材料。 在优选的实施例中, 是通过 将流延带与陶瓷壳体迭合, 在迭合前, 将粘结剂涂敷在陶瓷壳体 (基板 /基 体) 1 1、 12的壳体表面或 /和相应的介质贴片的表面上。 如图 4所示, 所述粘结 剂层 14在粘贴时呈液状或浆料状。 在优选的实施例中, 所述粘结剂是纤维增 强的粘结层, 纤维可以是玻璃纤维、 石英纤维、 芳纶纤维、 聚乙烯纤维、 碳 纤维或聚酯纤维。 在更为优选的实施例中, 所述粘结剂包括熔融金属和 /或非 金属氧化物, 如石英粉、 氧化锆、 氧化铜、 硅溶胶, 其重量百分比分别为: l〜20wt%、 l〜10wt%、 l〜10wt%、 l〜5wt%, 其余为 Al(HPO4)2。在另一优
选的实施例中, 所述粘结剂包括熔融石英粉、 水玻璃、 硅溶锆、 氧化铝, 其 重量百分比分别为: 5〜35wt %、 l〜5wt %、 5〜10wt%、 30〜40wt %, 其余 为水。 在陶瓷壳体 1 1、 12的一表面粘贴丝印有导电几何结构的柔性流延片, 流延片成坯料状态, 在烧结前, 最好进行冷等静压处理, 使陶瓷壳体定型。 在前述步骤中, 待前述粘结剂低温干燥后 (80°C到 120°C之间) , 再用混 有石英粉填料的高温粘结剂浆料, 涂敷要求的表面, 当涂上的浆料尚未硬化 之前, 合上另一含或未含导电几何结构的陶瓷壳体或介质贴片, 拼接时要施 加压力使粘接浆料填实。 低温烘烤, 使粘结剂发生固化反应, 在本发明的一 实施例中, 在小于 250°C时, 固化反应化学式为:
Zr(OH)4+4H3PO4→Zr(H2PO4)4+4H2O
为了烧结流延片坯体 (含导电几何结构) , 和提高粘结剂的结合强度, 低温烧结工艺温度小于导电几何结构的熔点, 例如 961 °C。 在前述实施例中, 磷酸盐粘结剂可混入熔融石英粉, 石英短纤维, 或者 是被穿孔 (打孔) 的石英纤维布, 粘接层厚可达 lmm到 2mm之间。 在前述实施例中, 如图 5和图 6所示, 第一陶瓷壳体和 /或第二陶瓷壳体的 相应侧的介质贴片层由多个流延片 13拼接成的, 共同组成相似于或相应于第 一陶瓷壳体和 /或第二陶瓷壳体的形状的空间几何结构, 该空间几何结构例如 为空间曲面, 即介质贴片的形状与第一或第二陶瓷壳体的相应一侧表面的形 状相适应, 以使所述介质贴片层整体与第一或第二陶瓷壳体的所述一侧表面 无间隙配合。 实施例 3 实施例 3可以参照图 3至图 6、 图 8来理解。
本实施例沿用前述实施例的元件标号与部分内容, 其中采用相同的标号 来表示相同或近似的元件, 并且选择性地省略了相同技术内容的说明。 关于 省略部分的说明可参照前述实施例, 本实施例不再重复赘述。 与实施例 2相似 的部分可以参照图 3、 图 4、 图 5、 图 6。
参照图 3, 超材料制备方法包括步骤一, 提供陶瓷壳体。 陶瓷壳体可以是 常规的各种陶瓷制成的壳体, 陶瓷壳体为空间几何结构, 如图 5所示, 陶瓷壳 体 1 1成空间曲面形状。 优选的实施例中, 陶瓷壳体 1 1利用浆料浇注成型、 凝 胶浇注成型或冷等静压成型制得。 优选的实施例中, 陶瓷壳体 1 1是由熔融石 英陶瓷制成。 在本发明的其他实施例中, 在本实施例的基础上, 类似于图 3所 示的结构, 可以增加第二陶瓷壳体 12。
继续参照图 3, 超材料制备方法还包括步骤二, 提供介质贴片, 其包含导 电几何结构。 介质贴片 132如图 8所示, 图中, 导电几何结构层 132的横向粗线 和纵向粗线为导电结构, 而方框部分为陶瓷基片。 图 8所示的导电几何结构适 合于增强超材料的透波性能。 本实施例的导电几何结构不限于此, 还可以是 对电磁波作出其他相应的导电几何结构, 例如是增强吸波性能。
介质贴片的制备方法可以参照图 4, 在具体的实施过程中, 其可以包括制 作增强材料的步骤, 如制作石英纤维布的步骤, 在该步骤中, 根据优选的实 施例, 首先选用熔融石英纤维布, 其表面为平纹或斜纹, 浸润硅油, 二氧化 硅含量 99.9 %, 耐温 1300°C, 厚度 0.15mm至 0.80mm之间。 然后, 配浆料, 以 乙醇和丁酮作为混合溶剂, 混入球磨过的熔融石英粉, 添加混合分散剂聚丙 烯酸和三油酸甘油酯, 再加入粘结剂, 如 prB和增塑剂丙三醇, 经搅拌制成流 动性好的浓浆料。 前述石英纤维可以替换为其他增强材料, 如玻璃纤维、 芳 纶纤维、 聚乙烯纤维、 碳纤维或聚酯纤维。
继续参照图 4, 未含导电几何结构的介质贴片的制备方法还包括形成流延 片, 在前述步骤的基础上, 对浆料真空除泡后, 在流延机上, 在石英纤维布 上做流延, 形成强度高、 柔软度高的石英纤维增强石英粉流延带 (陶瓷 层) , 即可以形成如图 6所示的陶瓷基片或陶瓷层 133。
继续参照图 4, 含导电几何结构的介质贴片的制备方法还包括形成导电几 何结构, 在该步骤中, 首先制备导电浆料, 然后在流延带上覆盖丝网印版, 利用丝网印版形成多个与导电几何结构相同的图案, 接着在丝网印版上涂覆 所述导电浆料, 所述导电浆料经由丝网印版的多个图案内的网眼而附着于前 述流延带, 固化后即形成导电结构层, 导电结构层可以是如图 8所示的导电结 构层 132。
如图 5和图 6所示, 在本发明的一实施例中介质贴片 13包括两陶瓷层 133、 131, 在两陶瓷层 133、 131之间形成导电几何结构层 132。
继续参照图 5和图 6, 在本发明的一实施例中, 在陶瓷壳体 1 1或 12的壳体 表面的局部或全部布置有多层介质贴片 13。 在此, 壳体表面可以是一个表 面, 也可以是两个表面。
结合图 3、 图 4、 图 5、 图 6和图 8, 将前述含导电几何结构的流延带 (陶瓷 层) 、 未含导电几何结构的流延带 (陶瓷层) 与陶瓷壳体结合, 然后再进行 烧结, 通过烧结形成超材料。 在优选的实施例中, 是通过将呈坯料状态的流 延带 (陶瓷层) 与陶瓷壳体迭合, 在迭合前, 将粘结剂涂敷在陶瓷壳体 (基 板 /基体) 1 1或 /和相应的介质贴片的表面上。 如图 4所示, 所述粘结剂层 14在 粘贴时呈液状或浆料状。 在优选的实施例中, 所述粘结剂是纤维增强的粘结 层。 在更为优选的实施例中, 所述粘结剂包括熔融的金属和 /或非金属氧化 物, 如石英粉、 氧化锆、 氧化铜、 硅溶胶, 其重量百分比分别为: 1〜
20wt%、 l〜10wt%、 l〜10wt%、 l〜5wt%, 其余为 Al(HPO4)2。在另一优选的 实施例中, 所述粘结剂包括熔融石英粉、 水玻璃、 硅溶锆、 氧化铝, 其重量 百分比分别为: 5〜35wt %、 l〜5wt %、 5〜10wt %、 30〜40wt %, 其余为 水。 在陶瓷壳体 11的一表面粘贴丝印有导电几何结构的柔性流延片 (陶瓷 层) , 流延片 (陶瓷层) 成坯料状态, 在烧结前, 最好进行冷等静压处理, 使陶瓷壳体定型。 如图 5和图 6所示, 整个超材料包括 12层介电材料, 在图 6 中, 由上到下依次为陶瓷壳体 11, 粘结剂层 14, 未含导电几何结构的陶瓷层 133 , 导电几何结构层 132, 未含导电几何结构的陶瓷层 131, 粘结剂层 14, 未 含导电几何结构的陶瓷层 133, 导电几何结构层 132, 未含导电几何结构的陶 瓷层 131, 粘结剂层 14, 未含导电几何结构的陶瓷层 133, 导电几何结构层 132, 未含导电几何结构的陶瓷层 131, 粘结剂层 14, 以及陶瓷壳体 12。 在前述步骤中, 待前述粘结剂低温干燥后 (80°C到 120°C之间) , 再用混 有石英粉填料的高温粘结剂浆料, 涂敷要求的表面, 当涂上的浆料尚未硬化 之前, 合上另一含或未含导电几何结构的陶瓷壳体或介质贴片 , 拼接时要施 加压力使粘接浆料填实。 低温烘烤, 使粘结剂发生固化反应, 在本发明的一 实施例中, 在小于 250°C时, 固化反应化学式为:
Zr(OH)4+4H3PO4→Zr(H2PO4)4+4H2O
为了烧结流延片坯体 (含导电几何结构) , 和提高粘结剂的结合强度, 低温烧结工艺温度小于导电几何结构的熔点, 例如 961 °C。 在前述实施例中, 磷酸盐粘结剂可混入熔融石英粉, 石英短纤维, 或者 是被穿孔 (打孔) 的石英纤维布, 粘接层厚可达 lmm到 2mm之间。 在前述实施例中, 如图 5和图 6所示, 陶瓷壳体 11的相应侧的介质贴片层 由多个流延片 13拼接成的, 共同组成相似于或相应于第一陶瓷壳体和 /或第二
陶瓷壳体的形状的空间几何结构, 该空间几何结构例如为空间曲面, 即介质 贴片的形状与第一或第二陶瓷壳体的相应一侧表面的形状相适应, 以使所述 介质贴片层整体与第一或第二陶瓷壳体的所述一侧表面无间隙配合。 实施例 4
实施例 4可以参照图 5至图 7、 图 9和图 10来理解。
如图 9所示, 超材料制备方法包括步骤一, 提供第一介质壳体 1 1和第二陶 瓷壳体 12。 如图 5所示, 第一介质壳体 (外壳体) 1 1和第二陶瓷壳体 (内壳 体) 12成空间曲面形状。 需要注意的是, 在图 5至图 8所示的结构中, 这些以 及后续其他的附图均仅作为示例, 其并非是按照等比例的条件绘制的, 并且 不应该以此作为对本发明实际要求的保护范围构成限制。 第一介质壳体 1 1可 以是陶瓷壳体, 其成形方法可以是烧结成型。 在本发明的其他实施例中第一 介质壳体 1 1为复合材料, 第一介质壳体 1 1成型具体包括将第一介质壳体固化 成型, 复合材料为热固或者热塑性材料, 如聚酰亚胺、 聚酯、 聚四氟乙烯、 聚氨酯、 聚芳酯、 PET、 PE、 或者 PVC, 这些复合材料还可以包含增强材料, 该增强材料为纤维、 织物、 或者粒子中的至少一种, 例如, 增强材料为纤 维, 如玻璃纤维、 石英纤维、 芳纶纤维、 聚乙烯纤维、 碳纤维或聚酯纤维。 此外, 这些复合材料还可以为多层结构。 优选的实施例中, 第二陶瓷壳体 12 利用浆料浇注成型、 凝胶浇注成型或冷等静压成型制得。 优选的实施例中, 第二陶瓷壳体 12也可以是由熔融石英陶瓷浆料浇注、 烧结成型。
继续参照图 9, 超材料制备方法还包括步骤二, 提供介质贴片, 其包含导 电几何结构, 导电几何结构是由金属丝构成的具有一定几何形状的平面或者 立体结构, 如工字型、 雪花型等。 介质贴片 132在如图 7所示的实施例中, 横
向粗线 1323和纵向粗线 1321为金属结构, 而方框部分 1322为介质基片。 图 7所 示的导电几何结构适合于增强超材料的透波性能。 本实施例的导电几何结构 不限于此, 还可以是对电磁波作出其他相应的导电几何结构, 例如是增强吸 波性能。
介质贴片的制备方法可以参照图 10, 在具体的实施过程中, 其可以包括 制作增强材料的步骤, 如制作石英纤维布的步骤, 在该步骤中, 根据优选的 实施例, 首先选用熔融石英纤维布, 其表面为平纹或斜纹, 浸润硅油, 二氧 化硅含量 99.95 %, 耐温 1200°C, 厚度 0.12mm至 0.70mm之间。 然后, 配浆料, 以乙醇和丁酮作为混合溶剂, 混入球磨过的熔融石英粉, 添加混合分散剂聚 丙烯酸和三油酸甘油酯, 再加入粘结剂, 如 prB和增塑剂丙三醇, 经搅拌制成 流动性好的浓浆料。 前述石英纤维可以替换为其他增强材料, 如玻璃纤维、 芳纶纤维、 聚乙烯纤维、 碳纤维或聚酯纤维。
继续参照图 10, 介质贴片的制备方法还包括形成流延片, 在前述步骤的 基础上, 对浆料真空除泡后, 在流延机上, 在石英纤维布上做流延, 形成强 度高, 柔软度高的石英纤维增强石英粉流延带 (陶瓷层) , 即可以形成如图 5 所示的介质基片或陶瓷层 133。
继续参照图 10, 介质贴片的制备方法还包括形成导电几何结构, 在该步 骤中, 首先制备导电浆料, 然后在前述流延带上覆盖丝网印版, 利用丝网印 版形成多个与导电几何结构相同的图案, 接着在丝网印版上涂覆所述导电浆 料, 所述导电浆料经由丝网印版的多个图案内的网眼而附着于前述流延带, 固化后即形成导电几何结构层, 导电几何结构层可以是如图 10所示的横向粗 线 1323和纵向粗线 1321组成的导电几何结构。
在本发明的其他实施例中介质贴片的基材也可以为复合材料, 复合材料
为热固或者热塑性材料, 如聚酰亚胺、 聚酯、 聚四氟乙烯、 聚氨酯、 聚芳 酯、 PET、 PE或 PVC, 该复合材料可以是包含泡沬和 /或蜂窝的一层或者多层 结构。 另外, 复合材料可以含有增强材料, 所述增强材料为纤维、 织物、 或 者粒子中的至少一种, 例如, 增强材料为纤维, 如玻璃纤维、 石英纤维、 芳 纶纤维、 聚乙烯纤维、 碳纤维或聚酯纤维。
除了前述丝印方法外, 导电几何结构还可以通过蚀刻、 钻刻、 雕刻、 电 子刻或离子刻成型在所述复合材料上。 加工导电几何机构所采用的金属为 银、 铂、 钼、 钨、 或银钯合金等。
继续参照图 9和图 10, 在本发明的一实施例中, 在第一介质壳体 1 1的一侧 面布置有多层介质贴片 13。 介质贴片 13粘贴在第一介质壳体 1 1表面的局部或 者全部, 形成至少一层具有介质贴片 13的第一介质壳体 1 1。
结合图 9和图 10, 将前述含导电几何结构的介质贴片与第一介质壳体 1 1结 合, 然后再与第二陶瓷壳体结成一体, 结合成一体的方法包括但不限于:
通过熔融的浆料将粘结有介质贴片 13的第一介质壳体 1 1与第二陶瓷壳体 12粘接;
或者通过紧固件将粘结有介质贴片 13的第一介质壳体 1 1与第二陶瓷壳体 12连接;
或者将粘结有介质贴片 13的第一介质壳体 1 1与第二陶瓷壳体 12卡接。
在高温压力粘接步骤中, 为了固化介质贴片坯体 (含导电几何结构) , 和提高粘结剂的结合强度, 低温烧结工艺温度小于导电几何结构的熔点, 例 如 961 °C。
在前述实施例中, 如图 9和图 10所示, 第一介质壳体 1 1和第二陶瓷壳体 12 的相应侧的介质贴片层由多个流延片 13拼接成的, 共同组成相似于或相应于
第一介质壳体和第二陶瓷壳体的形状的空间几何结构, 该空间几何结构例如 为空间曲面, 即介质贴片的形状与第一或第二陶瓷壳体的相应一侧表面的形 状相适应, 以使所述介质贴片层整体与第一或第二陶瓷壳体的所述一侧表面 无间隙配合。 实施例 5
实施例 4可以参照图 5至图 6、 图 8至图 10来理解。
本实施例沿用前述实施例的元件标号与部分内容, 其中采用相同的标号 来表示相同或近似的元件, 并且选择性地省略了相同技术内容的说明。 关于 省略部分的说明可参照前述实施例, 本实施例不再重复赘述。 与实施例 4相似 的部分可以参照图 9、 图 10、 图 5、 图 6。
参照图 9, 超材料制备方法包括步骤一, 提供第一介质壳体 1 1和第二陶瓷 壳体 12。 如图 5所示, 第一介质壳体 1 1成空间曲面形状。 第一介质壳体 1 1可以 是陶瓷壳体, 其成形方法可以是烧结成型。 在本发明的其他实施例中第一介 质壳体 1 1为复合材料, 第一介质壳体 1 1成型具体包括将第一介质壳体固化成 型, 复合材料为热固或者热塑性材料, 如聚酰亚胺、 聚酯、 聚四氟乙烯、 聚 氨酯、 聚芳酯、 PET、 PE、 或者 PVC, 这些复合材料还可以包含增强材料, 该 增强材料为纤维、 织物、 或者粒子中的至少一种, 例如, 增强材料为纤维, 如玻璃纤维、 石英纤维、 芳纶纤维、 聚乙烯纤维、 碳纤维或聚酯纤维。 此 外, 这些复合材料还可以为包含泡沬和 /或蜂窝的一层或者多层结构。 第二陶 瓷壳体 12利用浆料浇注成型、 凝胶浇注成型或冷等静压成型制得。 优选的实 施例中, 第二陶瓷壳体 12是由熔融石英陶瓷浆料浇注、 烧结成型。
继续参照图 9, 超材料制备方法还包括步骤二, 提供介质贴片, 其包含导
电几何结构, 导电几何结构是由金属丝构成的具有一定几何形状的平面或者 立体结构, 如工字型、 雪花型等。 介质贴片 132在如图 8所示的实施例中, 图 中, 导电几何结构层 132的横向粗线和纵向粗线为金属结构, 而方框部分为介 质基片。 图 8所示的导电几何结构适合于增强超材料的透波性能。 本实施例的 导电几何结构不限于此, 还可以是对电磁波作出其他相应的导电几何结构, 例如是增强吸波性能。
介质贴片的制备方法可以参照图 10, 在具体的实施过程中, 其可以包括 制作增强材料的步骤, 如制作石英纤维布的步骤, 在该步骤中, 根据优选的 实施例, 首先选用熔融石英纤维布, 其表面为平纹或斜纹, 浸润硅油, 二氧 化硅含量 99.9 %, 耐温 1300°C, 厚度 0.15mm至 0.80mm之间。 然后, 配浆料, 以乙醇和丁酮作为混合溶剂, 混入球磨过的熔融石英粉, 添加混合分散剂聚 丙烯酸和三油酸甘油酯, 再加入粘结剂, 如 prB和增塑剂丙三醇, 经搅拌制成 流动性好的浓浆料。 其中, 石英纤维可以替换为其他增强材料, 如玻璃纤 维、 芳纶纤维、 聚乙烯纤维、 碳纤维或聚酯纤维。
继续参照图 10, 未含导电几何结构的介质贴片的制备方法还包括形成流 延片, 在前述步骤的基础上, 对浆料真空除泡后, 在流延机上, 在石英纤维 布上做流延, 形成强度高, 柔软度高的石英纤维增强石英粉流延带 (陶瓷 层) , 即可以形成如图 8所示的介质基片或陶瓷层 133。 前述石英纤维可以替 换为玻璃纤维、 芳纶纤维、 聚乙烯纤维、 碳纤维或聚酯纤维。
继续参照图 10, 含导电几何结构的介质贴片的制备方法还包括形成导电 几何结构, 在该步骤中, 首先制备导电浆料, 然后在流延带上覆盖丝网印 版, 利用丝网印版形成多个与导电几何结构相同的图案, 接着在丝网印版上 涂覆所述导电浆料, 所述导电浆料经由丝网印版的多个图案内的网眼而附着
于前述流延带, 固化后即形成导电几何结构层, 导电几何结构层可以是如图 8 所示的导电几何结构层 132。
在本发明的其他实施例中介质贴片的基材也可以为复合材料, 复合材料 为热固或者热塑性材料, 如聚酰亚胺、 聚酯、 聚四氟乙烯、 聚氨酯、 聚芳 酯、 PET、 PE或 PVC, 该复合材料可以是包含泡沬和 /或蜂窝的一层或者多层 结构。 另外, 复合材料可以含有增强材料, 所述增强材料为纤维、 织物、 或 者粒子中的至少一种, 例如, 增强材料为纤维, 如玻璃纤维、 石英纤维、 芳 纶纤维、 聚乙烯纤维、 碳纤维或聚酯纤维。
除了前述丝印方法外, 导电几何结构还可以通过蚀刻、 钻刻、 雕刻、 电 子刻或离子刻成型在所述复合材料上。 加工导电几何机构所采用的金属为 银、 铂、 钼、 钨、 或银钯合金等。
如图 5和图 6所示, 在本发明的一实施例中介质贴片 13包括两陶瓷层 133、 131, 在两陶瓷层 133、 131之间形成导电几何结构层 132。 两陶瓷层 133、 131 的外形尺寸 W1可以为 2.5mm*2.5mm, 导电几何结构层 132的外形尺寸 W2可以 为 2.7mm*2.7mm, 而其中导电几何结构的宽度 HI可以为 0.2mm, 这些具体的 尺寸可以根据不同目的的设计进行改变, 本发明的实施不限于前述具体的尺 寸。
继续参照图 5和图 6, 在本发明的一实施例中, 在第一介质壳体 1 1的一侧 面布置有多层介质贴片 13。 介质贴片 13粘贴在第一介质壳体 1 1表面的局部或 者全部, 形成至少一层具有介质贴片 13的第一介质壳体 1 1。
结合图 9、 图 10、 图 5、 图 6和图 7, 将前述含导电几何结构的流延带 (陶 瓷层) 、 未含导电几何结构层的第一介质壳体 1 1与第二陶瓷壳体结合, 然后 与第二陶瓷壳体结成一体, 结合成一体的方法包括但不限于:
通过熔融的浆料将粘结有介质贴片 13的第一介质壳体 1 1与第二陶瓷壳体 12粘接;
或者通过紧固件将粘结有介质贴片 13的第一介质壳体 1 1与第二陶瓷壳体 12连接;
或者将粘结有介质贴片 13的第一介质壳体 1 1与第二陶瓷壳体 12卡接。 如图 5和图 6所示, 整个超材料包括 12层介电材料, 在图 6中, 由上到下依 次为第一介质壳体 1 1, 粘结剂层 14, 未含导电几何结构的介质贴片层 133, 导 电几何结构层 132, 未含介质贴片层的陶瓷层 131, 粘结剂层 14, 未含导电几 何结构的介质贴片层 133, 导电几何结构层 132, 未含导电几何结构的介质贴 片层 131, 粘结剂层 14, 未含导电几何结构的介质贴片层 133, 导电几何结构 层 132, 未含导电几何结构的介质贴片层, 粘结剂层 14, 以及陶瓷壳体 12。
为了固化介质贴片坯体 (含导电几何结构) , 和提高粘结剂的结合强 度, 前述高温压力粘结的温度小于导电几何结构的熔点, 例如 961 °C。
在前述实施例中, 如图 5和图 6所示, 陶瓷壳体 1 1的相应侧的介质贴片层 由多个介质贴片 13拼接成的, 共同组成相似于或相应于第一介质壳体和 /或第 二陶瓷壳体的形状的空间几何结构, 该空间几何结构例如为空间曲面, 即介 质贴片的形状与第一或第二陶瓷壳体的相应一侧表面的形状相适应, 以使所 述介质贴片层整体与第一或第二陶瓷壳体的所述一侧表面无间隙配合。
前述实施例 4、 5在制备的过程中, 对于制作的介质壳体和陶瓷壳体进行 了成型步骤, 使得在将粘结有介质贴片的介质壳体与所述陶瓷壳体结合成一 体时, 避免导电几何结构的气化。
本发明虽然以较佳实施例公开如上, 但其并不是用来限定本发明, 任何 本领域技术人员在不脱离本发明的精神和范围内, 都可以做出可能的变动和
修改。 因此, 凡是未脱离本发明技术方案的内容, 依据本发明的技术实质对 以上实施例所作的任何修改、 等同变化及修饰, 均落入本发明权利要求所界 定的保护范围之内。
Claims
1 . 一种超材料的制备方法, 其特征在于, 包括:
步骤 1, 制作具有空间几何形状的第一介质壳体;
步骤 2, 制作具有至少一个导电几何结构的介质贴片;
步骤 3, 将所述至少一个介质贴片贴附于所述第一介质壳体表面的局部或 者全部, 形成至少一层介质贴片层; 以及
步骤 4, 将所述第一介质壳体与所述介质贴片层结合成一体。
2. 如权利要求 1所述的制备方法, 其特征在于, 所述第一介质壳体为第 一陶瓷壳体。
3. 如权利要求 2所述的制备方法, 其特征在于, 在步骤 1中, 还制作具有 空间几何形状的第二陶瓷壳体, 在步骤 3中将所述第二陶瓷壳体与所述第一陶 瓷壳体配合, 以使所述介质贴片层封装于所述第一陶瓷壳体和所述第二陶瓷 壳体之间, 在步骤 4中, 将所述第一陶瓷壳体、 所述介质贴片层、 所述第二陶 瓷壳体一体烧结成型。
4. 如权利要求 2或者 3所述的制备方法, 其特征在于, 在步骤 1中, 所述 第一陶瓷壳体和 /或所述第二陶瓷壳体利用浆料浇注成型、 凝胶浇注成型或冷 等静压成型制得。
5 . 如权利要求 4所述的制备方法, 其特征在于, 所述步骤 3之前, 还包 括:
在所述第一陶瓷壳体表面和所述第二陶瓷壳体的相应表面、 和 /或所述介
质贴片相应的表面上涂覆粘结剂;
相应的, 在所述冷等静压处理之后, 还包括:
对所述第一陶瓷壳体和 /或所述第二陶瓷壳体加热, 使所述粘结剂发生反 应而固化。
6. 如权利要求 2或者 3所述的制备方法, 其特征在于, 在步骤 1中, 所述 第一陶瓷壳体和 /或所述第二陶瓷壳体由熔融石英陶瓷制成。
7. 如权利要求 3所述的制备方法, 其特征在于, 所述介质贴片的基片是 陶瓷。
8. 如权利要求 7所述的制备方法, 其特征在于, 一个所述介质贴片的制 备方法包括:
配制陶瓷浆料;
用陶瓷浆料形成一陶瓷层;
在所述陶瓷层上形成具有所述导电几何结构的导电结构层;
在所述导电结构层上形成另一陶瓷层。
9. 如权利要求 8所述的制备方法, 其特征在于, 所述用陶瓷浆料形成陶 瓷层之前, 还包括:
在所述陶瓷浆料中加入增强材料。
10. 如权利要求 8或 9所述的制备方法, 其特征在于, 所述陶瓷层是用流 延法形成的陶瓷坯料层。
1 1 . 如权利要求 8所述的制备方法, 其特征在于, 在所述陶瓷层上形成具 有所述导电几何结构的导电结构层, 具体包括:
制备导电浆料;
在所述陶瓷层上覆盖丝网印版, 所述丝网印版形成多个与所述导电几何 结构相同的图案;
在所述丝网印版上涂覆所述导电浆料, 所述导电浆料经由所述丝网印版 的多个图案内的网眼而附着于所述陶瓷层, 固化后即形成所述导电结构层。
12. 如权利要求 2所述的制备方法, 其特征在于, 将所述至少一个介质贴 片贴附于所述第一陶瓷壳体表面的局部或全部之前, 将所述至少一个介质贴 片贴覆于所述第一陶瓷壳体表面时预先在所述第一陶瓷壳体表面和 /或相应的 所述介质贴片的表面上涂覆粘结剂。
13 . 如权利要求 5所述的制备方法, 其特征在于, 所述步骤 3之前, 还包 括:
在所述第一陶瓷壳体的一侧表面和所述第二陶瓷壳体的相应表面、 和 /或 所述介质贴片相应的表面上涂覆粘结剂;
相应的, 在所述冷等静压处理之后, 还包括:
对所述第一陶瓷壳体和 /或所述第二陶瓷壳体烘烤, 使所述粘结剂发生反 应而固化。
14. 如权利要求 2所述的制备方法, 其特征在于, 所述空间几何形状为空 间曲面。
15、 如权利要求 1所述的制备方法, 其特征在于, 在步骤 1中, 还制作具 有空间几何形状第二陶瓷壳体, 分别将所述第一介质壳体和第二陶瓷壳体成 型;
在步骤 3中, 将至少一个所述介质贴片与所述第一介质壳体粘结; 在步骤 4中, 将粘结有介质贴片的第一介质壳体与所述第二陶瓷壳体结合 成一体。
16、 如权利要求 15所述的制备方法, 其特征在于, 所述第一介质壳体为 陶瓷壳体;
所述第一介质壳体成型具体包括: 通过浆料浇注成型、 凝胶浇注成型或 冷等静压成型。
17、 如权利要求 15或者 16所述的制备方法, 其特征在于, 所述介质贴片 的基底是陶瓷, 所述介质贴片的制备方法包括:
配制陶瓷浆料;
用陶瓷浆料形成第一陶瓷层;
在所述第一陶瓷层上形成包含至少一个导电几何结构的导电结构层; 在所述导电结构层上形成第二陶瓷层。
18、 如权利要求 17所述的制备方法, 其特征在于, 所述用陶瓷浆料形成 第一陶瓷层之前, 还包括:
在所述陶瓷浆料中加入增强材料, 所述增强材料为纤维、 织物、 或者粒 子中的至少一种。
19、 如权利要求 17所述的制备方法, 其特征在于, 所述第一陶瓷层与第 二陶瓷层为采用流延法形成的陶瓷坯料层。
20、 如权利要求 17所述的制备方法, 其特征在于, 在所述第一陶瓷层上 形成导电结构层包括:
制备导电浆料;
在所述第一陶瓷层上覆盖丝网印版, 所述丝网印版形成与所述导电几何 结构相同的图案;
在所述丝网印版上涂覆导电浆料, 所述导电浆料经由所述丝网印版的图 案内的网眼而附着于所述第一陶瓷层, 形成所述导电几何结构层。
21、 如权利要求 17所述的制备方法, 其特征在于, 将粘结有介质贴片的 第一介质壳体与所述第二陶瓷壳体结合成一体, 具体包括:
通过浆料将粘结有介质贴片的第一介质壳体与所述第二陶瓷壳体粘接; 或者通过紧固件将粘结有介质贴片的第一介质壳体与所述第二陶瓷壳体 连接;
或者将粘结有介质贴片的第一介质壳体与所述第二陶瓷壳体卡接。
22、 如权利要求 15所述的制备方法, 其特征在于, 所述第一介质壳体为 复合材料, 所述第一介质壳体成型具体包括:
将所述第一介质壳体固化成型。
23、 如权利要求 22所述的制备方法, 其特征在于, 所述复合材料为热固
或者热塑性材料。
24、 如权利要求 22所述的制备方法, 其特征在于, 所述复合材料为包含 泡沬和 /或蜂窝的一层或者多层结构。
25、 如权利要求 15所述的制备方法, 其特征在于, 所述介质贴片的基材 为复合材料, 该复合材料为热固或者热塑性材料。
26、 如权利要求 25所述的制备方法, 其特征在于, 所述复合材料含有增 强材料, 所述增强材料为纤维、 织物、 或者粒子中的至少一种。
27、 如权利要求 25所述的制备方法, 其特征在于, 所述介质贴片上的导 电几何结构通过蚀刻、 钻刻、 雕刻、 电子刻或离子刻成型在所述复合材料 上。
28、 如权利要求 25所述的制备方法, 其特征在于, 所述将至少一个所述 介质贴片与所述第一介质壳体粘结, 具体包括:
将所述介质贴片粘贴在所述第一介质壳体表面的局部或者全部, 形成至 少一层具有介质贴片的第一介质壳体。
29、 如权利要求 28所述的制备方法, 其特征在于, 所述将至少一个所述 介质贴片与所述第一介质壳体粘结之后, 进一步包括:
在具有介质贴片的第一介质壳体表面形成复合材料层; 其中, 所述复合 材料层具有导电几何结构。
30、 如权利要求 25所述的制备方法, 其特征在于,
将粘结有介质贴片的第一介质壳体与所述第二陶瓷壳体结合成一体, 具 体包括:
通过复合材料将粘结有介质贴片的第一介质壳体与所述第二陶瓷壳体粘 接, 该复合材料为热固或者热塑性材料;
或者通过紧固件将粘结有介质贴片的第一介质壳体与所述第二陶瓷壳体 连接;
或者将粘结有介质贴片的第一介质壳体与所述第二陶瓷壳体卡接。
31、 如权利要求 15所述的制备方法, 其特征在于, 所述空间几何形状为 空间曲面。
32、 一种超材料, 其特征在于, 采用权利要求 1至 31中任一项所述的制备 方法制备。
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CN102757229A (zh) * | 2012-07-03 | 2012-10-31 | 深圳光启创新技术有限公司 | 一种共形陶瓷超材料及其制备方法 |
CN104282998B (zh) * | 2013-07-03 | 2020-11-06 | 深圳光启高等理工研究院 | 超材料及其制备方法 |
CN104557099B (zh) * | 2013-10-25 | 2017-03-01 | 深圳光启创新技术有限公司 | 用于将导电几何结构贴压到陶瓷基板上的方法及制得组件和超材料 |
CN104649678B (zh) * | 2013-11-21 | 2017-01-04 | 深圳光启创新技术有限公司 | 在陶瓷材料表面形成导电几何结构的方法以及陶瓷基超材料 |
CN104934717A (zh) * | 2014-03-18 | 2015-09-23 | 深圳光启创新技术有限公司 | 频选蒙皮、天线罩及天线系统 |
US9896954B2 (en) * | 2014-10-14 | 2018-02-20 | Rolls-Royce Corporation | Dual-walled ceramic matrix composite (CMC) component with integral cooling and method of making a CMC component with integral cooling |
CN106032326B (zh) * | 2015-03-20 | 2020-12-01 | 深圳光启高等理工研究院 | 多层复合陶瓷板及其制备方法 |
CN106147703A (zh) * | 2015-04-03 | 2016-11-23 | 深圳光启尖端技术有限责任公司 | 一种吸波复合材料及其制备方法 |
CN106299715B (zh) * | 2015-05-18 | 2020-09-22 | 深圳光启高等理工研究院 | 超材料及其制备方法 |
DE102015220395A1 (de) | 2015-10-20 | 2017-04-20 | Bayerische Motoren Werke Aktiengesellschaft | Rußpartikelsensor |
CN107173849B (zh) * | 2016-03-11 | 2019-11-22 | 周宏明 | 一种导电陶瓷膜多孔陶瓷发热体及其应用 |
CN105702589B (zh) * | 2016-03-31 | 2018-06-29 | 中国电子科技集团公司第五十四研究所 | 一种用于ltcc多层布线曲面基板的制造方法 |
US11011834B2 (en) * | 2017-06-27 | 2021-05-18 | Florida State University Research Foundation, Inc. | Metamaterials, radomes including metamaterials, and methods |
CN108724434B (zh) * | 2018-05-30 | 2023-09-08 | 安徽中科新研陶瓷科技有限公司 | 一种相转化流延机及以其制备陶瓷平板生坯的方法 |
CN111646805B (zh) * | 2019-03-04 | 2022-05-13 | Oppo广东移动通信有限公司 | 陶瓷结构件的制作方法和移动终端 |
CN114851654B (zh) * | 2022-04-21 | 2023-06-30 | 中北大学 | 一种基于短切纤维混杂毡的集成抗高速冲击和吸波功能的纤维树脂超材料及其制备 |
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US20150152013A1 (en) | 2015-06-04 |
EP2871172A4 (en) | 2016-07-13 |
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