CN104694904A - Hollow-pipe micro-lattice ceramic material constructed by adopting template method and preparation method thereof - Google Patents
Hollow-pipe micro-lattice ceramic material constructed by adopting template method and preparation method thereof Download PDFInfo
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- CN104694904A CN104694904A CN201510044149.4A CN201510044149A CN104694904A CN 104694904 A CN104694904 A CN 104694904A CN 201510044149 A CN201510044149 A CN 201510044149A CN 104694904 A CN104694904 A CN 104694904A
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Abstract
The invention discloses a hollow-pipe micro-lattice ceramic material constructed by adopting a template method and a preparation method thereof. The method comprises the steps: preparing a three-dimensional micro-lattice polymer template of a designed structure by adopting a rapid forming technology; depositing ceramics on the surface of the micro-lattice polymer template so as to prepare a preformed body; removing a template, thereby obtaining the hollow-pipe micro-lattice ceramic material. According to the hollow-pipe micro-lattice ceramic material constructed by adopting the template method and the preparation method thereof, the template method and a thin-film deposition method are organically combined, and the prepared lightweight and porous hollow-pipe micro-lattice ceramic material has the characteristic of low density and the properties of high strength, high modulus, high hardness, high-temperature resistance, corrosion resistance, radiation resistance, small thermal expansion coefficient and the like and is a multifunctional, lightweight and porous micro-lattice material. The hollow-pipe micro-lattice ceramic material is applied to the fields of aviation, aerospace, electronic information and the like.
Description
Technical field
The present invention relates to the preparation of stupalith, more particularly, refer to that a kind of template that adopts constructs open tube microarray stupalith and preparation method thereof, belong to light porous technical field of function materials.
Background technology
The progress of human society develops into prerequisite with material, and the material of excellent performance facilitates the development of society, and the appearance of novel material is also called in the high development of society simultaneously.Along with the development of science and technology, also more and more higher to the performance requriements of material, low density material is also more and more subject to people and payes attention to, and super light material has excellent specific tenacity, specific rigidity and thermotolerance, also has good structure properties and physics and chemical property.In addition, super light material also demonstrates the functional performance of many uniquenesses such as excellent damping noise reduction performance, good energy-absorbing buffering performance, outstanding sound absorption and shielding properties, desirable filtration and absorption property, is called structure-function integrated material.
3D prints also referred to as the manufacture of increasing material, and it does not need cutter and mould, utilizes three-dimensional CAD model can produce parts with complex structures fast and accurately on an equipment, thus realizes " freely manufacturing ", solves traditional technology difficulty and processes the limitation maybe cannot processed.Current three-dimensional modeling can be realize in the softwares such as Solidworks, UG, Pro/E and CAD.
Why material can have ultralight density, and reason is that solid material is porous.The porosity of different porous material is not identical with pore size, and general porosity is 20% ~ 99%, and pore size is also from nano level to grade.In general, nanometer and micrometer level porous material lay particular emphasis on the functional property of material, and as electrical properties, magnetic, optical property, lightweight is in second.And millimetre-sized porous material, except very light weight, the character such as the thermodynamics of light porous metallic substance excellence also can meet different civil and military demand, and some material can also a large amount of low cost production.Different methods is certain the class material in different range for the preparation of relative density and aperture size.
The periodic structure material that lattice material is made up of connecting rod unit between node and node.Its cell element configuration is similar to the lattice structure of crystalline material, and therefore the periodic structure of this Space Beam body of rod system is referred to as lattice material.
Lattice material is that the class constantly developing and occur along with the preparation of Aeronautics and Astronautics large-scale component structure and material molding technology is in recent years novel, the multifunctional material of lightweight, there are ultralight, some excellent mechanical propertys such as high porosity, high-strong toughness, high specific strength, high specific stiffness, high-energy absorption, and the property such as damping, electromagnetic shielding, sound absorption, lattice material has function and structure dual function concurrently, is a kind of multifunctional engineering material of excellent performance.Development has the three-dimensional lattice structured material of lightweight, efficient, high porosity, is to advance the lightweight of material and equipment, precision, high efficiency, realizes key measure that is energy-conservation, purification.
At present, in laboratory and industry member, the main template used has biomaterial template, organic compound template and mineral compound template etc.Wherein, organic compound, if various plastics, synthon etc. are due to the designability of its pattern and structure and stability, is widely used in the synthesis of inorganic nano material.Template can be prepared material according to the wish of people and can easily obtain good array.
Pottery due to its there is low density, high strength, high-modulus, high rigidity, characteristic and superior optical, electrical, thermal and magnetic, the mechanical property such as high temperature resistant, anticorrosive, radiation hardness, thermal expansivity are little, in high-tech sectors such as Aeronautics and Astronautics, electronic information, national defence, there is extensive and irreplaceable effect, development has the high performance ceramic material of three-dimensional lattice structure of lightweight, efficient, high porosity, be the lightweight of propelling material and equipment, precision, high efficiency, realize key measure that is energy-conservation, purification.
Summary of the invention
An object of the present invention is to provide a kind of preparation method adopting template to construct open tube microarray stupalith.When preparing light porous open tube microarray stupalith by the inventive method, first prepare the three-dimensional microarray polymer template of desired structure by rapid shaping technique; Then at microarray polymer template surface deposition pottery preform processed, object forms uniform ceramic membrane on its surface, controls the thickness of various complex model surface ceramic film by depositing time; Last ablation or chemical etching fall template, the light porous open tube microarray stupalith obtained, and the density of obtained light porous open tube microarray stupalith is decided by the factor such as thickness of the structure of microarray template, size, ceramic membrane.
Another object of the present invention is to provide a kind of stupalith with light porous open tube microarray.Stupalith prepared by the present invention has 3-D ordered multiporous structure, has the feature of low density, high strength.
The object of the invention is to be achieved through the following technical solutions:
Step one: adopt rapid shaping technique to prepare three-dimensional microarray template;
Step 11, select template starting material:
Step 12, select quick shaping process:
Step 13, arranges the lattice structure of template:
Step 14, arranges the lattice parameter of template:
In the present invention, quick shaping process includes stereolithograghy technology (SLA), selective laser sintering (SLS) or fused deposition modeling (FDM);
In the present invention, template starting material are high molecular polymer, it comprises light-sensitive resin EX-200 type, light-sensitive resin DXZ-100 type, light-sensitive resin DSM somos14120 type, acrylic resin, epoxy resin, polystyrene (PS), polyethylene terephthalate (PET), acrylonitrile-butadiene-styrene copolymer (ABS), polycarbonate (PC), polymethylmethacrylate (PMMA), polyoxymethylene (POM), polyvinyl chloride (PVC), polypropylene (PP), or poly(lactic acid) (PLA) etc.
In the present invention, the lattice structure of template includes: simple cubic, body-centered cubic, face-centered cubic, simple six sides, simple tetragonal, body-centered teteragonal, the R heart six side, simple orthorhombic, the C heart are orthogonal, C heart monocline, body-centered orthorhombic, face-centered orthorhombic, simple tiltedly side, simple triclinic or diamond positive tetrahedron structure.
Comprehensive above condition, adopts rapid shaping technique to prepare the template of unlike material, different microarray structure and parameter.
Step 2: at three-dimensional microarray template surface deposition ceramic membrane processed, obtain preform constructions body;
Step 21, cleaning template:
Step 22, deposits ceramic membrane processed:
By through the obtained three-dimensional microarray template ultrasonic cleaning 15 ~ 30min in acetone of step one, then ultrasonicly in deionized water embathe 15 ~ 30min, finally ultrasonic cleaning 10 ~ 20min in ethanol, seasoning, obtains clean template;
Select deposition method, and arrange deposition parameter, in three-dimensional microarray template surface deposit ceramic materials, deposit thickness is designated as h, obtains preform constructions body;
Described deposition method includes: chemical gaseous phase depositing process, physical gas-phase deposite method and sol-gel method; Described chemical gaseous phase depositing process has aumospheric pressure cvd (APCVD), low-pressure chemical vapor deposition (LPCVD), plasma reinforced chemical vapour deposition (PECVD), light to strengthen chemical vapour deposition (PCVD), ald (ALD) etc.; Described physical gas-phase deposite method has vacuum evaporation, radio-frequency sputtering, magnetron sputtering, ion plating etc.
In the present invention, ceramic membrane material includes oxide compound and the mixtures thereof such as titanium oxide, silicon oxide, aluminum oxide, zirconium white, nickel oxide, ferric oxide, stannic oxide, vanadium oxide, barium oxide, Tungsten oxide 99.999, carbide and the mixtures thereof such as norbide, silicon carbide, wolfram varbide, titanium carbide, tantalum carbide, niobium carbide, vanadium carbide, nitride and the mixtures thereof such as silicon nitride, boron nitride, titanium nitride.
The processing parameter that chemical gaseous phase depositing process comprises is: depositing temperature 25 DEG C ~ 1000 DEG C, and chamber pressure 10 ~ 100Pa, radio frequency power is 100 ~ 250W, depositing time 20 ~ 60min.
The processing parameter that physical gas-phase deposite method comprises is: vacuum tightness >=0.1Pa, and base reservoir temperature is 25 DEG C ~ 300 DEG C, and vaporization temperature is 1000 ~ 2000 DEG C, and depositing time is 10 ~ 90min.
The processing parameter that sol-gel method comprises is: first obtain solution, obtains colloidal sol after ageing.
Step 3: adopt the three-dimensional microarray polymer template removed in the obtained preform constructions body of form technology removing step two, obtain light porous open tube microarray stupalith;
Remove form technology and can adopt ablating technics, its condition is: adopt retort furnace, the argon gas being 99.99% in percent by volume is protective atmosphere, is heated to 450 ~ 600 DEG C, roasting 60min ~ 120min with the temperature rise rate of 1 ~ 10 DEG C/min.
Remove form technology and can adopt chemical etching process, its condition is: under etching liquid, process 60min ~ 120min, and described etching liquid can be chloroform, sodium hydroxide, acetone.
Light porous open tube microarray stupalith provided by the invention is a kind of lightweight functional materials of excellent performance, and compared with prior art, the advantage of present invention process and products therefrom is:
1. microarray stay in place form used in the present invention has designability.
2. Introduction To Stereolithography used in the present invention can prepare the microarray structural models of arbitrary structures, and precision is high and preparation cycle is short.
What 3. ceramic membrane deposition method used in the present invention reached is effective, and rete tack is good, and surface compact is even, and thicknesses of layers is controlled.
4. the preparation-obtained light porous open tube microarray stupalith of the present invention has 3-D ordered multiporous structure, has low density, high strength, the feature such as high temperature resistant, corrosion-resistant.
Accompanying drawing explanation
Fig. 1 is the shaping schema of the microarray node configuration of hollow cylinder template-ceramic deposition-removal template.
Fig. 2 is the shaping schema of the microarray node configuration of solid cylindrical template-ceramic deposition-removal template.
Fig. 3 is the shaping schema of the microarray node configuration of solid cubes template-ceramic deposition-removal template.
Fig. 4 is the shaping schema of the microarray node configuration of solid six prism template-ceramic deposition-removal templates.
Fig. 5 A is the photo that embodiment 1 rapid shaping obtains diamond lattice structure template.
Fig. 5 B is that embodiment 1 adopts sol-gel-dip painting technique to obtain the photo of the diamond lattice structure template of film.
Fig. 5 C is the light porous hollow microarray SiO 2-ceramic material photo after embodiment 1 removes diamond lattice structure template.
Fig. 5 D is the electromicroscopic photograph that embodiment 1 obtains light porous open tube microarray SiO 2-ceramic material.
Fig. 5 E is the electromicroscopic photograph that embodiment 1 obtains light porous open tube microarray SiO 2-ceramic layer thickness.
Fig. 5 F is the stress-strain curve that embodiment 1 obtains light porous open tube microarray SiO 2-ceramic material.
Fig. 6 is the structure iron that embodiment 2 rapid shaping obtains arrayed column structure template.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
The present invention proposes a kind of method building the preparation light porous open tube microarray stupalith of template-ceramic deposition-removal template, specifically include three steps:
Step one: adopt rapid shaping technique to prepare three-dimensional microarray template;
Step 11, selects template starting material;
Step 12, selects quick shaping process;
Step 13, arranges the lattice structure of template;
Step 14, arranges the lattice parameter of template;
In the present invention, template starting material are high molecular polymer, it comprises light-sensitive resin EX-200 type, light-sensitive resin DXZ-100 type, light-sensitive resin DSM somos14120 type, acrylic resin, epoxy resin, polystyrene (PS), polyethylene terephthalate (PET), acrylonitrile-butadiene-styrene copolymer (ABS), polycarbonate (PC), polymethylmethacrylate (PMMA), polyoxymethylene (POM), polyvinyl chloride (PVC), polypropylene (PP), or poly(lactic acid) (PLA) etc.
In the present invention, the lattice structure of template includes: simple cubic, body-centered cubic, face-centered cubic, simple six sides, simple tetragonal, body-centered teteragonal, the R heart six side, simple orthorhombic, the C heart are orthogonal, C heart monocline, body-centered orthorhombic, face-centered orthorhombic, simple tiltedly side, simple triclinic or diamond positive tetrahedron structure.Concrete template lattice structure please refer to Zhou Gongdu, " structural chemistry basis (second edition) " that Duan Lianyun writes, September nineteen ninety-five the second edition, the 347th page 14 kinds spatial point formation patterns.Described diamond positive tetrahedron structure please refer to " carbon-base film preparation and the Field Electron Emission " that Zhang Binglin writes, September in 2009 the 1st edition, the 61st page.
Because microarray structure has the cycle characteristics of multiple dot array, in order to describe the configuration characteristic of template in detail, as shown in Figure 1, Figure 2, Figure 3 and Figure 4, Reference numeral number 1,1A, 1B, 1C represent the template under different configuration, and 2 represent stupalith.The dimensional parameters of the present invention to lattice structure is introduced, and be designated as a, the wide b of being designated as long, height is designated as c, diameter is designated as d, central point is designated as r to the distance of the length of side, these lattice dimensions all must not be greater than 1 millimeter.The not all template of lattice structure size is all comprised.By the template that the recirculation of microarray structure obtains, wherein multiple somes array elements will be had.
Comprehensive above condition, adopts rapid shaping technique to prepare the template of unlike material, different dot matrix structure and parameter.
In the present invention, quick shaping process includes stereolithograghy technology (SLA), selective laser sintering (SLS) or fused deposition modeling (FDM).
In the present invention, Stereolithography technique (Stereo Lithography Apparatus, SLA) parameter is: fill sweep velocity 200 ~ 500mm/s, sweep span: 0.1 ~ 0.5mm, light-dark cycle diameter: 0.1 ~ 0.3mm, supports sweep velocity: 80 ~ 120mm/s, jump across speed: 300 ~ 800mm/s, the interlayer waiting time: 1 ~ 5s, table feed speed: 2 ~ 10mm/s, worktable immersion depth: 5 ~ 10mm.
In the present invention, the parameter of selective laser sintering technique (Selective laser Sintering, SLS) is: laser power 10 ~ 50W, preheating temperature 60 ~ 180 DEG C, slice thickness 0.1 ~ 2mm, sweep velocity 1000 ~ 2000mm/s.AFS-320 rapidform machine selected by SLS agglomerating plant, CO
2laser apparatus, wavelength is 10.6 microns, and maximum laser output rating is 50W, and Beijing Longyuan Prototyping System Co., Ltd produces.SLS manufactures thought, with solid powder material straight forming Three-dimensional Entity Components, not by the restriction of part shape complexity, without any need for moulds of industrial equipment, cad model is directly changed into physical prototypes or part, because of but the material forming techniques of a kind of advanced person, can shorten and manufacture and design the cycle.
In the present invention, the parameter of fusion sediment quick shaping process (Fused Deposition Modeling, FDM) is: lift height 0.05 ~ 1.0mm, nozzle temperature 100 ~ 400 DEG C.
Step 2: at three-dimensional microarray template surface deposition ceramic membrane processed, obtain preform constructions body;
Step 21, cleaning template;
Step 22, deposits ceramic membrane processed;
By through the obtained three-dimensional microarray template ultrasonic cleaning 15 ~ 30min in acetone of step one, then ultrasonicly in deionized water embathe 15 ~ 30min, finally ultrasonic cleaning 10 ~ 20min in ethanol, seasoning, obtains clean template;
Select deposition method, and deposition parameter is set, in three-dimensional microarray template surface deposit ceramic materials, obtain preform constructions body;
Described deposition method includes: chemical gaseous phase depositing process, physical gas-phase deposite method and sol-gel method; Described chemical gaseous phase depositing process has aumospheric pressure cvd (APCVD), low-pressure chemical vapor deposition (LPCVD), plasma reinforced chemical vapour deposition (PECVD), light to strengthen chemical vapour deposition (PCVD), ald (ALD) etc.; Described physical gas-phase deposite method has vacuum evaporation, radio-frequency sputtering, magnetron sputtering, ion plating etc.
The processing parameter that chemical gaseous phase depositing process comprises is: depositing temperature 25 DEG C ~ 1000 DEG C, and chamber pressure 10 ~ 100Pa, radio frequency power is 100 ~ 250W, depositing time 20 ~ 60min.
The processing parameter that physical gas-phase deposite method comprises is: vacuum tightness >=0.1Pa, and base reservoir temperature is 25 DEG C ~ 300 DEG C, and vaporization temperature is 1000 ~ 2000 DEG C, and depositing time is 10 ~ 90min.
The processing parameter that sol-gel method comprises is: first obtain solution, obtains colloidal sol after ageing.
Particularly, aumospheric pressure cvd (APCVD) processing parameter can be arranged: depositing temperature >=600 DEG C, chamber pressure 20 ~ 100Pa, and radio frequency power is 100 ~ 250W, depositing time 20 ~ 60min.
Particularly, low-pressure chemical vapor deposition (LPCVD) processing parameter can be arranged: depositing temperature >=450 DEG C, chamber pressure 10 ~ 40Pa, and radio frequency power is 150 ~ 190W, depositing time 20 ~ 120min.
Particularly, plasma reinforced chemical vapour deposition (PECVD) processing parameter can be arranged: depositing temperature 20 ~ 600 DEG C, chamber pressure 20 ~ 60Pa, and radio frequency power is 150 ~ 220W, depositing time 20 ~ 80min.
Particularly, ald (ALD) processing parameter can be arranged: depositing temperature 50 ~ 400 DEG C, reaction chamber operating pressure 200 ~ 800Pa.
Particularly, vacuum evaporation process parameter can be arranged: vacuum tightness >=0.1Pa, and base reservoir temperature is 25 DEG C ~ 300 DEG C, and vaporization temperature is 1000 ~ 2000 DEG C.
Particularly, radio-frequency sputtering processing parameter can be arranged: underlayer temperature >=25 DEG C, substrate and sputtering target distance 0.5 ~ 2mm, ar pressure 0.5 ~ 25Pa, sputtering power 50 ~ 170W, pre-sputtering time 0 ~ 30min, sputtering time 10 ~ 90min;
Particularly, magnetron sputtering technique parameter can be arranged: underlayer temperature >=25 DEG C, substrate and sputtering target distance 0.5 ~ 2mm, ar pressure 0.5 ~ 10Pa, sputtering power 70 ~ 200W, sputtering voltage 180 ~ 220V, sputtering current 0.1 ~ 5mA, pre-sputtering time 0 ~ 30min, sputtering time 10 ~ 200min.
In the present invention, ceramic membrane material includes titanium oxide (TiO
2), silicon oxide (SiO
2), aluminum oxide (Al
2o
3), zirconium white, nickel oxide, ferric oxide, stannic oxide, vanadium oxide, barium oxide, Tungsten oxide 99.999, norbide (B
4c), silicon carbide (SiC), wolfram varbide, titanium carbide, tantalum carbide, niobium carbide, vanadium carbide, silicon nitride (Si
3n
4), boron nitride, titanium nitride etc. and their mixture thereof, as SiO
2/ TiO
2, SiO
2/ Al
2o
3, Si
3n
4/ B
4c etc.
Step 3: adopt the three-dimensional microarray polymer template removed in the obtained preform constructions body of form technology removing step two, obtain open tube microarray stupalith;
Remove form technology and can adopt ablating technics, its condition is: adopt retort furnace, the argon gas being 99.99% in percent by volume is protective atmosphere, is heated to 450 ~ 600 DEG C, roasting 60 ~ 120min with the temperature rise rate of 1 ~ 10 DEG C/min.
Remove form technology and can adopt chemical etching process, its condition is: under etching liquid, process 60 ~ 120min, described etching liquid can be chloroform, sodium hydroxide, acetone.
Further illustrate advantage of the present invention and other details in the examples below, but the concrete materials and structures size quoted in embodiment and other conditions and details should not be regarded as to invention has been inappropriate restriction.
embodiment 1
That embodiment 1 proposes is a kind of preparation light porous open tube microarray silicon-dioxide (SiO adopting SLA to build template-sol-gel deposition pottery-removal template
2) method of stupalith, specifically include three steps:
Step one: adopt rapid shaping technique to prepare three-dimensional microarray template;
Stereolithograghy technology (Stereo Lithography Appearance, SL or SLA) is adopted to prepare the template of diamond microarray structure, shown in Fig. 5 A.
The processing parameter of Stereolithography is: filling sweep velocity is 300mm/s, sweep span is 0.1mm, light-dark cycle diameter is 0.2mm, support sweep velocity is 100mm/s, jumping across speed is 600mm/s, the interlayer waiting time is 5s, and table feed speed is 5mm/s, and worktable immersion depth is 6mm.
The mould material that Stereolithography adopts is: light-sensitive resin EX-200 type, its main component is acrylic resin.The smooth surface of this kind of resin mould, is conducive at its surface deposition ceramic membrane.
In diamond microarray stay in place form, dot matrix is of a size of: the diameter of every root post is 0.6mm, and the spacing between node and node is 2mm.
Shown in Fig. 5 A, adopting the light-sensitive resin EX-200 type diamond microarray stay in place form that SLA technique is obtained, through observing, clearly can see the structure of duct, dot matrix post.This structure that first step through embodiment 1 obtains has very high structural stability, and the physical stability of elasticity and resistance to rupture.
Step 2: at three-dimensional microarray template surface deposition ceramic membrane processed, obtain preform constructions body;
Diamond microarray stay in place form prepared by step one adopts sol-gel-dip be coated with process layer method deposition of silica ceramic membrane, obtain preform constructions body;
Its concrete operation step comprises:
A () template surface cleans: ultrasonic cleaning 30min in acetone, and deionized water for ultrasonic embathes 30min, ultrasonic cleaning 20min in ethanol, seasoning;
(b) template surface deposition of silica ceramic membrane: the superpolymer template of having cleaned Dipping in the silicon dioxide gel of preparation is obtained 20 μm of thick silica membranes, and drying obtains preform constructions body;
Described silicon dioxide gel is formulated by the molar ratio of 1:6.4:3.8:0.085 by tetraethyl silicate, ethanol, nitric acid.
In described Dipping method, dipping, pull rate are 10mm/min, and dipping time is 15min, often lift one deck, put into the dry 30min of thermostatic drying chamber of 60 DEG C immediately, after taking out naturally cooling, repeat above-mentioned steps again, lift number of times reaches desired thickness 5 times.Obtained preform constructions body is see shown in Fig. 5 B.
Step 3: adopt the three-dimensional microarray polymer template removed in the obtained preform constructions body of form technology removing step two, obtain light porous open tube microarray stupalith;
Preform constructions body step 2 obtained puts into retort furnace; the argon gas being 99.99% in percent by volume is protective atmosphere; 500 DEG C are heated to the temperature rise rate of 10 DEG C/min; insulation 120min; after retort furnace Temperature fall; taking-up obtains light porous open tube microarray earth silicon material, shown in Fig. 5 C.
Weighed by light porous open tube microarray earth silicon material obtained for embodiment 1, calculating density is 23mg/cm
3, this light porous open tube microarray earth silicon material belongs to low density material.
By light porous open tube microarray earth silicon material obtained for embodiment 1 through electron-microscope scanning, inflated diameter is 540.7 μm, shown in Fig. 5 D; Obtained silicon dioxide thickness is 60.49 μm, shown in Fig. 5 E.
Light porous open tube microarray earth silicon material obtained for embodiment 1 is carried out compression performance test, INSTRUMENT MODEL INSTRON 5565 mechanics machine, and translational speed is 5mm/min, and obtaining material greatest compressive strength is 1.57MPa, shown in Fig. 5 F.
Light porous open tube microarray earth silicon material obtained for embodiment 1 is carried out adsorption of cupper ions test in solution, diamond lattic structure open tube silicon-dioxide microarray material is put in the copper solutions of the 200mg/L of the 100mL of configuration, samples after shaking 24h under 190 rotating speeds at 25 DEG C with constant temperature oscillator.Calculating silicon-dioxide microarray material to the adsorptive capacity of cupric ion is 22.5mg/g, and visible diamond lattic structure open tube silicon-dioxide microarray material has good adsorption of cupper ions.
embodiment 2
That embodiment 2 proposes is a kind of preparation light porous open tube microarray silicon nitride (Si adopting SLA to build template-PECVD ceramic deposition-removal template
3n
4) method of stupalith, specifically include three steps:
Step one: adopt rapid shaping technique to prepare three-dimensional microarray template;
Stereolithograghy technology (Stereo Lithography Appearance, SL or SLA) is adopted to prepare the template of simple tetragonal microarray structure, shown in Figure 6.
The processing parameter of Stereolithography technology (SLA) is: filling sweep velocity is 300mm/s, sweep span is 0.1mm, light-dark cycle diameter is 0.2mm, support sweep velocity is 100mm/s, jumping across speed is 600mm/s, the interlayer waiting time is 5s, and table feed speed is 5mm/s, and worktable immersion depth is 6mm.
The mould material that Stereolithography technology (SLA) adopts is: light-sensitive resin EX-200 type, and its main component is acrylic resin.The smooth surface of this kind of resin mould, is conducive at its surface deposition ceramic membrane.
In the template of simple tetragonal microarray structure, dot matrix is of a size of: the diameter of every root post is 0.4mm, and the spacing between node and node is 2.4mm.
Step 2: at three-dimensional microarray template surface deposition ceramic membrane processed, obtain preform constructions body;
The template of the simple tetragonal microarray structure prepared by step one adopts plasma reinforced chemical vapour deposition method (PECVD) deposited silicon nitride ceramic membrane, obtain preform constructions body;
Its concrete operation step comprises
A () template surface cleans: ultrasonic cleaning 30min in acetone, and deionized water for ultrasonic embathes 20min, ultrasonic cleaning 20min in ethanol, seasoning;
B () deposited silicon nitride ceramic membrane: the reaction chamber template of having cleaned being put into PECVD device, is heated to the temperature of reaction 80 DEG C of needs and keeps 30min by reaction chamber; Pass into reactant gases NH
3, adjust flux meter is to 60ml/min; Open 800W radio frequency power source, radio frequency power is adjusted to the power 200W that experiment needs; Pass into reactant gases SiH
4, adjust flux meter is to 30ml/min; Depositing time 20min, obtained silicon nitride film thickness is the preform constructions body of 29 microns.
Step 3: adopt the three-dimensional microarray polymer template removed in the obtained preform constructions body of form technology removing step two, obtain open tube microarray stupalith;
Preform constructions body step 2 obtained puts into retort furnace; the argon gas being 99.99% in percent by volume is protective atmosphere, is heated to 600 DEG C with the temperature rise rate of 3 DEG C/min, insulation 90min; after retort furnace Temperature fall, take out and obtain light porous open tube microarray silicon nitride material.
Weighed by light porous open tube microarray silicon nitride material obtained for embodiment 2, calculating density is 13mg/cm
3, this light porous open tube microarray silicon nitride material belongs to low density material.Obtained silicon nitride thickness is 29 microns, and material greatest compressive strength is 5.93MPa.
Light porous open tube microarray silicon nitride material obtained for embodiment 2 is carried out thermal conductivity test, and adopt System of Physical Properties Test PPMS-9T to carry out performance test, the thermal conductivity recording sample under room temperature is 0.17Wm
-1k
-1, this open tube microarray silicon nitride material has good heat-proof quality.
embodiment 3
The present invention proposes a kind of method adopting FDM to build the preparation light porous open tube microarray stupalith of template-PECVD ceramic deposition-removal template, specifically include three steps:
Step one: adopt rapid shaping technique to prepare three-dimensional microarray template;
Fused deposition modeling (Fused Deposition Modeling, FDM) is adopted to prepare the template of diamond microarray structure.
The processing parameter that fused deposition modeling (FDM) adopts is: lift height: 0.1mm, nozzle temperature 230 DEG C.
The mould material of fused deposition modeling (FDM) is: poly(lactic acid) (PLA).
In diamond microarray stay in place form, dot matrix is of a size of: the diameter of every root post is 0.6mm, and the spacing between node and node is 1.2mm.
Step 2: at three-dimensional microarray template surface deposition ceramic membrane processed, obtain preform constructions body;
Diamond microarray stay in place form prepared by step one adopts plasma reinforced chemical vapour deposition method (PECVD) deposited silicon nitride ceramic membrane, obtains preform constructions body:
Its concrete operation step comprises:
A () template surface cleans: ultrasonic cleaning 30min in acetone, and deionized water for ultrasonic embathes 30min, ultrasonic cleaning 15min in ethanol, seasoning;
B () deposited silicon nitride ceramic membrane: the reaction chamber polymer template cleaned being put into PECVD device, is heated to the temperature of reaction 80 degree of needs and keeps 30min by reaction chamber; Pass into reactant gases NH
3, adjust flux meter is to 60ml/min; Open 800W radio frequency power source, radio frequency power is adjusted to the power 200W that experiment needs; Pass into reactant gases SiH
4, adjust flux meter is to 30ml/min; Depositing time 20min; Obtained silicon nitride (Si
3n
4) film thickness is the preform constructions body of 8 microns.
Step 3: adopt the three-dimensional microarray polymer template removed in the obtained preform constructions body of form technology removing step two, obtain light porous open tube microarray stupalith;
Removing template is process 100min under chloroform etching liquid, then obtain light porous open tube microarray Si
3n
4material.
By light porous open tube microarray Si obtained for embodiment 3
3n
4material is weighed, and calculating density is 21mg/cm
3, this light porous open tube microarray Si
3n
4material belongs to low density material.Obtained Si
3n
4thickness is 8 microns, and material greatest compressive strength is 13MPa.
Light porous open tube microarray silicon nitride material obtained for embodiment 3 is carried out thermal conductivity test, and adopt System of Physical Properties Test PPMS-9T to test, the thermal conductivity recording sample under room temperature is 0.14Wm
-1k
-1, this open tube microarray silicon nitride material has good heat-proof quality.
embodiment 4
The present invention proposes a kind of preparation light porous open tube microarray B adopting FDM to build template-PECVD ceramic deposition-removal template
4the method of C stupalith, specifically includes three steps:
Step one: adopt rapid shaping technique to prepare three-dimensional microarray template;
Fused deposition modeling (Fused Deposition Modeling, FDM) is adopted to prepare the template of diamond microarray structure.
The processing parameter that fused deposition modeling (FDM) adopts is: lift height: 0.1mm, nozzle temperature 180 DEG C.
The mould material of fused deposition modeling (FDM) is: light-sensitive resin DXZ-100 type.The smooth surface of this kind of resin mould, is conducive at its surface deposition ceramic membrane.
In diamond microarray stay in place form, dot matrix is of a size of: the diameter of every root post is 0.3mm, and the spacing between node and node is 1mm.
Step 2: at three-dimensional microarray template surface deposition ceramic membrane processed, obtain preform constructions body;
Diamond lattice structure template prepared by step one adopt PECVD deposit B
4c ceramic membrane, obtains preform constructions body;
Its concrete operation step comprises
A () template surface cleans: ultrasonic cleaning 15min in acetone, and deionized water for ultrasonic embathes 20min, ultrasonic cleaning 15min in ethanol, seasoning;
B () cvd nitride boron ceramic membrane: the reaction chamber polymer template cleaned being put into PECVD device, is heated to the temperature of reaction 350 degree of needs and keeps 30min by reaction chamber; Pass into Ar, adjust flux meter, to 19ml/min, passes into reaction gas N2, and adjust flux meter is to 0.7ml/min; Open 800W radio frequency power source, radio frequency power is adjusted to the power 160W that experiment needs; Pass into reactant gases B
2h
6, adjust flux meter is to 0.7ml/min; Depositing time 60min; Obtained boron nitride film thickness is the preform constructions body of 8 microns.
Step 3: adopt the three-dimensional microarray polymer template removed in the obtained preform constructions body of form technology removing step two, obtain light porous open tube microarray stupalith;
Preform constructions body step 2 obtained puts into retort furnace, and the argon gas being 99.99% in percent by volume is protective atmosphere, is heated to 450 DEG C with the temperature rise rate of 7 DEG C/min, insulation 120min, after retort furnace Temperature fall, takes out and obtains open tube microarray B
4c material.
By open tube microarray B obtained for embodiment 4
4c material is weighed, and calculating density is 14mg/cm
3, this open tube microarray B
4c material belongs to low density material.B
4c thickness is 8 μm, and material greatest compressive strength is 5.5MPa.
Light porous open tube microarray boron carbide material obtained for embodiment 4 is carried out resistance to elevated temperatures test, ceramic fiber retort furnace is adopted to calcine at different temperatures, recording the most ablation temperature of open tube microarray boron carbide material is 2100 DEG C, and this boron carbide material has resistance to elevated temperatures as seen.
embodiment 5
The present invention proposes a kind of method preparing open tube microarray stupalith that SLS of employing builds template-sol-gel deposition pottery-removal template, specifically include three steps:
Step one: adopt rapid shaping technique to prepare three-dimensional microarray template;
Selective laser sintering (Selective Laser Sintering, SLS) is adopted to prepare the template of diamond microarray structure.
The processing parameter of selective laser sintering (SLS) is: laser power: 30W, preheating temperature 100 DEG C, slice thickness 0.2mm, sweep velocity 1800mm/s.
The mould material that selective laser sintering (SLS) adopts is: light-sensitive resin DSM somos14120 type, its main component is epoxy acrylic resin.The smooth surface of this kind of resin mould, is conducive at its surface deposition ceramic membrane.
In diamond microarray stay in place form, dot matrix is of a size of: the diameter of every root post is 0.5mm, and the spacing between node and node is 1.5mm.
Step 2: at three-dimensional microarray template surface deposition ceramic membrane processed, obtain preform constructions body;
Diamond lattice structure template prepared by step one adopts sol-gel dip coating deposition of silica ceramic membrane, obtain preform constructions body;
Its concrete operation step comprises
A () template surface cleans: ultrasonic cleaning 30min in acetone, and deionized water for ultrasonic embathes 30min, ultrasonic cleaning 20min in ethanol, seasoning;
(b) deposition of silica ceramic membrane: the superpolymer template of having cleaned Dipping in the silicon dioxide gel of preparation is obtained the silica membrane of 29 micron thickness, and drying obtains preform constructions body;
Described silicon dioxide gel is formulated by the molar ratio of 1:6.4:3.8:0.085 by tetraethyl silicate, ethanol, nitric acid.
In described Dipping method, dipping, pull rate are 10mm/min, and dipping time is 10min, lift number of times 5 times.
Step 3: adopt the three-dimensional microarray polymer template removed in the obtained preform constructions body of form technology removing step two, obtain light porous open tube microarray stupalith;
Preform constructions body step 2 obtained puts into retort furnace; the argon gas being 99.99% in percent by volume is protective atmosphere, is heated to 600 DEG C with the temperature rise rate of 5 DEG C/min, insulation 60min; after retort furnace Temperature fall, take out and obtain light porous open tube microarray earth silicon material.
By light porous open tube microarray SiO obtained for embodiment 5
2material is weighed, and calculating density is 27mg/cm
3, this light porous open tube microarray SiO
2material belongs to low density material.Obtained silicon dioxide thickness is 29 μm, and material greatest compressive strength is 1.9MPa.
Light porous open tube microarray earth silicon material obtained for embodiment 5 is carried out adsorption of cupper ions test in solution, diamond lattic structure open tube silicon-dioxide microarray material is put in the copper solutions of the 200mg/L of the 100mL of configuration, samples after shaking 24h under 190 rotating speeds at 25 DEG C with constant temperature oscillator.Calculating silicon-dioxide microarray material to the adsorptive capacity of cupric ion is 25mg/g, and visible diamond lattic structure open tube silicon-dioxide microarray material has good adsorption of cupper ions.
embodiment 6
The present invention proposes a kind of preparation light porous open tube microarray SiO adopting FDM to build template-sol-gel deposition pottery-removal template
2/ TiO
2the method of composite ceramic material, specifically includes three steps:
Step one: adopt rapid shaping technique to prepare three-dimensional microarray template;
Fused deposition modeling (Fused Deposition Modeling, FDM) is adopted to prepare the template of diamond microarray structure.
The processing parameter that fused deposition modeling (FDM) adopts is: lift height: 0.1mm, nozzle temperature 180 DEG C.
The mould material of fused deposition modeling (FDM) is: ABS resin.The smooth surface of this kind of resin mould, is conducive at its surface deposition ceramic membrane.
In diamond microarray stay in place form, dot matrix is of a size of: the diameter of every root post is 0.3mm, and the spacing between node and node is 2mm.
Step 2: at three-dimensional microarray template surface deposition ceramic membrane processed, obtain preform constructions body;
Diamond lattice structure template prepared by step one adopt sol-gel dip coating deposit SiO
2/ TiO
2ceramic thin sheet, obtains preform constructions body;
Its concrete operation step comprises
A () template surface cleans: ultrasonic cleaning 30min in acetone, and deionized water for ultrasonic embathes 30min, ultrasonic cleaning 20min in ethanol, seasoning;
(b) deposition SiO
2/ TiO
2composite ceramic film: the superpolymer template of having cleaned Dipping in the silicon-dioxide and titanium oxide complex sol of preparation is obtained the SiO of 34 micron thickness
2/ TiO
2laminated film, drying obtains preform constructions body;
Described SiO
2/ TiO
2complex sol is that the silicon dioxide gel of ageing 24h and titanium oxide sol are made its Homogeneous phase mixing by the ratio being 1:1 according to silicon-dioxide and titanium oxide mol ratio under room temperature and violent stirring state, add the HCl adjust ph of 1mol/L therebetween between 2.0 ~ 3.0, after stirring 3h, add a certain amount of film coalescence aid N, dinethylformamide (DMF), continue to stir 1h, obtain complex sol.
Described silicon dioxide gel is formulated by the molar ratio of 1:6.4:3.8:0.085 by tetraethyl silicate, ethanol, nitric acid.
Described titanium oxide sol is formulated by the molar ratio of 1:24:0.4:1,2:2 by tetrabutyl titanate, dehydrated alcohol, nitric acid, Glacial acetic acid, deionized water.
In described Dipping method, dipping, pull rate are 10mm/min, and dipping time is 10min, lift number of times 5 times.
Step 3: adopt the three-dimensional microarray polymer template removed in the obtained preform constructions body of form technology removing step two, obtain open tube microarray stupalith;
Preform constructions body step 2 obtained puts into retort furnace; the argon gas being 99.99% in percent by volume is protective atmosphere; 450 DEG C are heated to the temperature rise rate of 10 DEG C/min; insulation 100min; after retort furnace Temperature fall, take out and obtain light porous open tube microarray earth silicon/titanic oxide material.
By light porous open tube microarray SiO obtained for embodiment 6
2/ TiO
2matrix material is weighed, and calculating density is 23mg/cm
3, this light porous open tube microarray SiO
2/ TiO
2matrix material belongs to low density material.Obtained SiO
2/ TiO
2composite thickness is 34 μm, and material greatest compressive strength is 3.7MPa.
Light porous open tube microarray earth silicon/titanic oxide matrix material obtained for embodiment 6 is carried out adsorption of cupper ions test in solution, diamond lattic structure open tube earth silicon/titanic oxide matrix material is put in the copper solutions of the 200mg/L of the 100mL of configuration, samples after shaking 24h under 200 rotating speeds at 25 DEG C with constant temperature oscillator.Calculating earth silicon/titanic oxide matrix material to the adsorptive capacity of cupric ion is 26.5mg/g, and visible diamond lattic structure open tube earth silicon/titanic oxide matrix material also has good adsorption of cupper ions.
embodiment 7
The present invention proposes a kind of method adopting SLS to build the preparation light porous open tube microarray stupalith of template-magnetron sputtering deposition pottery-removal template, specifically include three steps:
Step one: adopt rapid shaping technique to prepare three-dimensional microarray template;
Selective laser sintering (Selective Laser Sintering, SLS) is adopted to prepare the template of diamond microarray structure.
The processing parameter of selective laser sintering (SLS) is: laser power: 30W, preheating temperature 100 DEG C, slice thickness 0.2mm, sweep velocity 1800mm/s.
The mould material that selective laser sintering (SLS) adopts is: light-sensitive resin DSM somos14120 type, its main component is epoxy acrylic resin.The smooth surface of this kind of resin mould, is conducive at its surface deposition ceramic membrane.
In diamond microarray structure, dot matrix is of a size of: the diameter of every root post is 0.4mm, and the spacing between node and node is 0.8mm.
Step 2: at three-dimensional microarray template surface deposition ceramic membrane processed, obtain preform constructions body;
Magnetron sputtering TiO in diamond lattice structure template prepared by step one
2film, obtains preform constructions body.
Its concrete operation step comprises
A () template surface cleans: ultrasonic cleaning 30min in acetone, and deionized water for ultrasonic embathes 30min, ultrasonic cleaning 20min in ethanol, seasoning;
(b) depositing Ti O
2film: by purity be 99.99% titanium target and cleaned model put into sputtering chamber, oxygen makes reactant gases, sputtering obtain TiO
2film;
Splash-proofing sputtering process parameter is: background vacuum 3 × 10
-3pa, be filled with argon gas and the oxygen of purity 99.999%, ratio is 3:2, and vacuum tightness reaches 8 × 10
-1pa, sputtering current is 0.3A, and voltage is 200V, sputtering power 140W, and sputtering time is 1h.
Step 3: adopt the three-dimensional microarray polymer template removed in the obtained preform constructions body of form technology removing step two, obtain light porous open tube microarray stupalith;
Preform constructions body step 2 obtained puts into retort furnace; the argon gas being 99.99% in percent by volume is protective atmosphere, is heated to 500 DEG C with the temperature rise rate of 10 DEG C/min, insulation 60min; after retort furnace Temperature fall, take out and obtain light porous open tube microarray TiO
2material.
By light porous open tube microarray titanium dioxide (TiO obtained for embodiment 8
2) material weighs, calculating density is 15mg/cm
3, this light porous open tube microarray TiO
2material belongs to low density material.Obtained TiO
2thickness is 4 μm, and material greatest compressive strength is 1.2MPa.
Light porous open tube microarray titanic oxide material obtained for embodiment 7 is carried out photocatalysis performance test, diamond lattic structure open tube titanium dioxide microarray material is put in the 40mg/L rhodamine B solution of the 100mL of configuration, under ultraviolet lamp, 90min is irradiated after mixing, reference solution is done at 550nm wavelength with distilled water with spectrophotometry, measure the absorbancy of rhodamine B, the degradation rate calculating rhodamine B reaches 87%, and visible diamond lattic structure open tube titanium dioxide microarray material has good photocatalysis performance.
Claims (10)
1. adopt template to construct a method for open tube microarray stupalith, it is characterized in that specifically including three steps:
Step one: adopt rapid shaping technique to prepare three-dimensional microarray template;
Step 11, selects template starting material;
Step 12, selects quick shaping process;
Quick shaping process includes stereolithograghy technology (SLA), selective laser sintering (SLS) or fused deposition modeling (FDM);
Step 13, arranges the lattice structure of template;
Step 14, arranges the lattice parameter of template;
Step 2: at three-dimensional microarray template surface deposition ceramic membrane processed, obtain preform constructions body;
Step 21, cleaning template;
By template ultrasonic cleaning 15 ~ 30min in acetone, then ultrasonicly in deionized water embathe 15 ~ 30min, finally ultrasonic cleaning 10 ~ 20min in ethanol, seasoning, obtains clean template;
Step 22, deposits ceramic membrane processed; By selecting deposition method, and deposition parameter being set, in three-dimensional microarray template surface deposit ceramic materials, obtaining preform constructions body;
Step 3: adopt the three-dimensional microarray polymer template removed in the obtained preform constructions body of form technology removing step two, obtain open tube microarray stupalith;
Remove form technology and can adopt ablating technics, its condition is: adopt retort furnace, the argon gas being 99.99% in percent by volume is protective atmosphere, is heated to 450 ~ 600 DEG C, roasting 60 ~ 120min with the temperature rise rate of 1 ~ 10 DEG C/min.
Remove form technology and can adopt chemical etching process, its condition is: under etching liquid, process 60 ~ 120min, described etching liquid can be chloroform, sodium hydroxide, acetone.
2. employing template according to claim 1 constructs open tube microarray stupalith and preparation method thereof, it is characterized in that: the parameter of Stereolithography technique (SLA) is: fill sweep velocity 200 ~ 500mm/s, sweep span: 0.1 ~ 0.5mm, light-dark cycle diameter: 0.1 ~ 0.3mm, support sweep velocity: 80 ~ 120mm/s, jump across speed: 300 ~ 800mm/s, the interlayer waiting time: 1 ~ 5s, table feed speed: 2 ~ 10mm/s, worktable immersion depth: 5 ~ 10mm.
3. employing template according to claim 1 constructs open tube microarray stupalith and preparation method thereof, it is characterized in that: the parameter of selective laser sintering technique (SLS) is: laser power 10 ~ 50W, preheating temperature 60 ~ 180 DEG C, slice thickness 0.1 ~ 2mm, sweep velocity 1000 ~ 2000mm/s.
4. employing template according to claim 1 constructs open tube microarray stupalith and preparation method thereof, it is characterized in that: the parameter of fusion sediment quick shaping process (FDM) is: lift height 0.05 ~ 1.0mm, nozzle temperature 100 ~ 400 DEG C.
5. employing template according to claim 1 constructs open tube microarray stupalith and preparation method thereof, it is characterized in that: template starting material are high molecular polymer, it comprises light-sensitive resin EX-200 type, light-sensitive resin DXZ-100 type, light-sensitive resin DSM somos14120 type, acrylic resin, epoxy resin, polystyrene, polyethylene terephthalate, acrylonitrile-butadiene-styrene copolymer, polycarbonate, polymethylmethacrylate, polyoxymethylene, polyvinyl chloride, polypropylene or poly(lactic acid); Ceramic membrane material includes titanium oxide, silicon oxide, aluminum oxide, zirconium white, nickel oxide, ferric oxide, stannic oxide, vanadium oxide, barium oxide, Tungsten oxide 99.999, norbide, silicon carbide, wolfram varbide, titanium carbide, tantalum carbide, niobium carbide, vanadium carbide, silicon nitride, boron nitride, titanium nitride etc. and their mixture thereof, as SiO
2/ TiO
2, SiO
2/ Al
2o
3, Si
3n
4/ B
4c.
6. employing template according to claim 1 constructs open tube microarray stupalith and preparation method thereof, it is characterized in that: aumospheric pressure cvd (APCVD) processing parameter can be arranged: depositing temperature >=600 DEG C, chamber pressure 20 ~ 100Pa, radio frequency power is 100 ~ 250W, depositing time 20 ~ 60min.Low-pressure chemical vapor deposition (LPCVD) processing parameter can be arranged: depositing temperature >=450 DEG C, chamber pressure 10 ~ 40Pa, and radio frequency power is 150 ~ 190W, depositing time 20 ~ 120min.
7. employing template according to claim 1 constructs open tube microarray stupalith and preparation method thereof, it is characterized in that: magnetron sputtering technique parameter can be arranged: underlayer temperature >=25 DEG C, substrate and sputtering target distance 0.5 ~ 2mm, ar pressure 0.5 ~ 10Pa, sputtering power 70 ~ 200W, sputtering voltage 180 ~ 220V, sputtering current 0.1 ~ 5mA, pre-sputtering time 0 ~ 30min, sputtering time 10 ~ 200min.
8. employing template according to claim 1 constructs open tube microarray stupalith and preparation method thereof, it is characterized in that: plasma reinforced chemical vapour deposition (PECVD) processing parameter can be arranged: depositing temperature 20 ~ 600 DEG C, chamber pressure 20 ~ 60Pa, radio frequency power is 150 ~ 220W, depositing time 20 ~ 80min.
9. employing template according to claim 1 constructs open tube microarray stupalith and preparation method thereof, it is characterized in that: ald (ALD) processing parameter can be arranged: depositing temperature 50 ~ 400 DEG C, reaction chamber operating pressure 200 ~ 800Pa.
10. employing template according to claim 1 constructs open tube microarray stupalith and preparation method thereof, it is characterized in that: obtained open tube microarray stupalith has resistance to elevated temperatures, heat-proof quality, photocatalysis performance or heavy metal ion attraction performance.
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| CN114540782A (en) * | 2022-02-26 | 2022-05-27 | 西安交通大学 | Preparation method of metal-ceramic multilayer film hollow micro-lattice material |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105599299A (en) * | 2016-01-07 | 2016-05-25 | 北京无线电测量研究所 | 3D printing processing technology of LTCC substrate cavity filling mold |
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| CN109722654A (en) * | 2017-10-31 | 2019-05-07 | 北京航空航天大学 | The method that ultralight metal hollow pipe lattice material is constructed using high-molecular lattice template |
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| CN114525487A (en) * | 2022-02-26 | 2022-05-24 | 西安交通大学 | Preparation method of metal-high-entropy alloy multilayer film hollow micro-lattice material |
| CN114540782A (en) * | 2022-02-26 | 2022-05-27 | 西安交通大学 | Preparation method of metal-ceramic multilayer film hollow micro-lattice material |
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