WO2017028771A1 - 一种多孔材料 - Google Patents

一种多孔材料 Download PDF

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Publication number
WO2017028771A1
WO2017028771A1 PCT/CN2016/095328 CN2016095328W WO2017028771A1 WO 2017028771 A1 WO2017028771 A1 WO 2017028771A1 CN 2016095328 W CN2016095328 W CN 2016095328W WO 2017028771 A1 WO2017028771 A1 WO 2017028771A1
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Prior art keywords
porous material
mass
average
porous
volume
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English (en)
French (fr)
Inventor
叶雷
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Chongqing Runze Pharmaceutical Co Ltd
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Chongqing Runze Pharmaceutical Co Ltd
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Priority to US15/752,584 priority Critical patent/US10597755B2/en
Priority to EP16836635.9A priority patent/EP3323436A4/en
Publication of WO2017028771A1 publication Critical patent/WO2017028771A1/zh
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/24—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies
    • B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
    • B01D46/2418—Honeycomb filters
    • B01D46/2425—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material
    • B01D46/24492—Pore diameter
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/08—Alloys with open or closed pores
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02—Inorganic materials
    • A61L27/10—Ceramics or glasses
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/14—Macromolecular materials
    • A61L27/18—Macromolecular materials obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2027—Metallic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y80/00—Products made by additive manufacturing
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/661—Metal or alloys, e.g. alloy coatings
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/64—Carriers or collectors
    • H01M4/70—Carriers or collectors characterised by shape or form
    • H01M4/80—Porous plates, e.g. sintered carriers
    • H01M4/808—Foamed, spongy materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/8605—Porous electrodes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/10—Filtering material manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/12—Special parameters characterising the filtering material
    • B01D2239/1208—Porosity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/12—Special parameters characterising the filtering material
    • B01D2239/1291—Other parameters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/10—Copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/20—Refractory metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/11—Making porous workpieces or articles
    • B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
    • B22F3/1137—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers by coating porous removable preforms
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K2103/00—Materials to be soldered, welded or cut
    • B23K2103/02—Iron or ferrous alloys
    • B23K2103/04—Steel or steel alloys
    • B23K2103/05—Stainless steel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/34—Laser welding for purposes other than joining
    • B23K26/342—Build-up welding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C67/00—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00
    • B29C67/20—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00 for porous or cellular articles, e.g. of foam plastics, coarse-pored
    • B29C67/202—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00 for porous or cellular articles, e.g. of foam plastics, coarse-pored comprising elimination of a solid or a liquid ingredient
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2067/00—Use of polyesters or derivatives thereof, as moulding material
    • B29K2067/04—Polyesters derived from hydroxycarboxylic acids
    • B29K2067/046—PLA, i.e. polylactic acid or polylactide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/04—Condition, form or state of moulded material or of the material to be shaped cellular or porous
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00—Electroforming
    • C25D1/08—Perforated or foraminous objects, e.g. sieves
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

Definitions

  • the present invention relates to a porous material.
  • porous materials As a new type of engineering material with excellent performance and structural dual properties, porous materials have been widely used in metallurgical machinery, petrochemical, energy and environmental protection, national defense industry, nuclear technology and bio-pharmaceutical, medical equipment and other industries.
  • porous materials can be used for energy absorption, noise reduction, noise reduction, such as anti-shock for automobiles, as a filter; porous materials can be used to filter and separate gases or liquids to achieve purification and separation of media.
  • porous material can be used in heat exchangers, high efficiency; porous materials such as nickel foam, copper foam can be used as excellent electrode materials, suitable for various batteries, fuel cells and solar cells; porous materials such as porous titanium, porous tantalum, Porous hydroxyapatite or the like can be used as a biological material, such as artificial bone, teeth, etc.; porous ceramic can be used as a catalyst carrier to promote the reaction; rigid polyurethane foam can be used as a thermal insulation material, and is widely used for building energy saving; The polymer foam is used as a housing for the radome and radio emissions.
  • the application requirements of many porous materials require that the material itself is uniform, that is, the pore size and the distribution of the pores are uniform, so that the performance is uniform, but in fact, many porous materials fail to meet the requirements, which is because the uniformity is insufficient. Although some materials have been improved to claim higher homogeneity, their uniformity is still uniform over a large volume scale. If the volume is measured by a small volume scale, for example, the volume of the material is not more than 1 cm.
  • 3 is a three-dimensional body, respectively, measured for mass, which is still very large difference in the degree of non-uniformity, i.e., the current call porous material of uniform scale only in large volume homogeneous, rather than being evenly under small scale, it can be said porous
  • the unevenness of the small volume scale of the material causes various properties of the porous material such as strength, elastic modulus, etc., and thus the true elastic modulus of the porous material cannot be effectively reduced, thereby seriously affecting its function.
  • a porous material having a uniform distribution of pores characterized in that the uniformity distribution of the pores means that each pore has a uniform distribution under arbitrary unit volume on the porous material; and the elastic modulus value of the porous material The modulus of elasticity of the raw material itself used to produce the porous material is reduced by 10-99%.
  • the unit volume described above refers to a cubic centimeter scale or a cubic millimeter scale or smaller unit volume.
  • the uniformity distribution of the above-mentioned pores means that each of the three-dimensional bodies having a volume of not more than 1 cm 3 and the same size on the porous material is substantially equivalent in mass.
  • the mass is substantially equivalent to a plurality of three-dimensional bodies having a volume of not more than 1 cm 3 and the same size, which are respectively referred to as a mass, and the masses thereof are respectively obtained, and the average value of the masses thereof is obtained, and the mass of any three-dimensional body is relative to the mass average value.
  • the absolute value of the deviation is not more than 4% of the average of the three-dimensional body mass.
  • a plurality of three-dimensional bodies of the same size having a volume of not more than 1 cm 3 on the porous material are respectively referred to as masses, and an average value of the masses thereof is obtained, and the absolute value of the deviation of any three-dimensional body mass from the mass average value is not More than 2% of the average value of the three-dimensional body mass, the uniformity is higher, and the performance of the porous material is more stable.
  • the three-dimensional bodies of the same size having a volume of not more than 1 mm 3 on the porous material are substantially equivalent in mass.
  • the mass here basically corresponds to a plurality of three-dimensional bodies of the same size having a volume of not more than 1 mm 3 , which are respectively referred to as porous materials, respectively referred to as masses, and average values of their masses are obtained, and any three-dimensional body mass is compared with mass.
  • the absolute value of the deviation of the average value is not more than 4% of the average value of the three-dimensional body mass.
  • a more uniform case refers to a plurality of three-dimensional bodies of the same size having a volume of not more than 1 mm 3 taken on the porous material, respectively referred to as masses, and an average value of their masses, and the mass of any three-dimensional body relative to the mass average value
  • the absolute value of the deviation is not more than 2% of the average of the three-dimensional body mass.
  • the present invention further provides a porous material which is a hole which is classified by a material pore size and which is formed around a cavity wall which forms a hole, and a lower-order small hole is arranged in a three-dimensional space around a cavity wall constituting the upper-level large hole, and the height is uniform.
  • the porous material has more functions than the porous material of a single pore, and the elastic modulus value of the porous material can be controlled at different scales.
  • the elastic modulus of the porous material decreases by 50-99%.
  • the elastic modulus of the porous material is reduced by 70-99%.
  • the present invention is more specific and specific than the pore distribution of the porous material mentioned in the prior art, and the pore distribution uniformity of the porous material is required at a smaller unit-scale volume, and the pores of such a porous material are highly uniform. Therefore, the uniformity of various properties of the porous material is ensured.
  • the porous material of the present invention has a uniform pore distribution at a unit volume of cubic centimeters or cubic millimeters or less, and its mass is substantially equivalent, thereby truly reducing the overall elastic modulus of the porous material.
  • 1 is a schematic structural view of a porous material according to the present invention, 1-1 is a main view, 1-2 is a left view, and 1-3 is a top view;
  • Embodiment 4 of the porous material of the present invention 2-1 is a main view, 2-2 is a left view, and 2-3 is a top view;
  • Figure 3 is an enlarged view of a portion A of Figure 2;
  • Figure 4 is a cross-sectional view of Figure 3B-B.
  • 1 is a hole
  • 2 is a cavity wall of the hole, and the holes are evenly distributed.
  • the cavity wall 4 of the hole 3 is composed of a smaller hole 5 (lower stage hole) and a cavity wall 6 surrounding the hole 5, and an enlarged view of the cavity wall 4 in conjunction with FIG. 3, and a cross-sectional view of FIG. 4B-B It can be seen that the holes 5 are three-dimensionally penetrated, and the two-stage holes are also three-dimensionally connected to each other.
  • the porous material of the present embodiment is a porous stainless steel 316 having a porosity of 75.5%, and is composed of a square-shaped frame having an edge of 100 ⁇ m and a rib diameter of 30 ⁇ m, and the unit is a 12-edge, and is mechanically processed on the porous material.
  • 10 pieces of 10 mm ⁇ 10 mm ⁇ 10 mm three-dimensional bodies of the same size were tested with a METTLER TOLEDO XP26 Microbalance balance at room temperature 20 ° C. The measurement steps were:
  • Preheat Turn on the power and warm up to the specified time.
  • Calibration is performed by TAR key clearing and CAL subtraction and calibration weight.
  • the compressive stress-strain curve of the above porous stainless steel 316 was tested by a compression test at room temperature 25 °C using an Instron mechanical testing machine.
  • the stress-strain curve showed an initial deformation of elastic deformation.
  • the ratio of the stress value of the elastic deformation portion to the corresponding strain value is the elastic modulus, and the measured elastic modulus value is 35.1 GPa, which is 82% lower than the elastic modulus value of the raw material itself used for the porous material.
  • the preparation method of the porous stainless steel 316 is as follows:
  • This material is used to make the filter element.
  • the porous material of the present embodiment is porous nickel, the porosity is 83%, the average pore diameter is 113 ⁇ m, and 10 pieces of the same size three-dimensional body of 10 mm ⁇ 10 mm ⁇ 8 mm are obtained by mechanical processing on the porous material, using METTLER.
  • METTLER METTLER- Toledo XP26 Microbalance balance test its mass, measuring temperature and steps are the same as in Example 1, the results are shown in Table 2, wherein the absolute value of the deviation from the average value is expressed as a percentage, and the value is absolute with respect to the average value. The value is divided by the mass average value. As can be seen from Table 2, the mass deviation is less than 2%.
  • the elastic modulus of this material was measured by the method of Example 1 to be 15.6 GPa, which was 91% lower than the elastic modulus of the raw material itself used for the porous material.
  • the preparation method of the porous nickel is as follows:
  • Substrate pretreatment a polyurethane sponge having a pore diameter of 152 ⁇ 3 ⁇ m was selected and pretreated with hydrochloric acid;
  • electroplating electroplating the above-mentioned conductive treated polyurethane sponge by pulse current method, and then plating a layer of nickel plating on the sponge edge;
  • Reduction sintering reduction treatment was carried out in a protective atmosphere containing 70% of hydrogen and 30% of nitrogen to obtain a porous nickel material.
  • This material is used to make electrodes.
  • the porous material of the present embodiment is porous polylactic acid, the porosity is 66%, the average pore diameter is 20 ⁇ m, and 10 pieces of the same size of 1 mm ⁇ 1 mm ⁇ 1 mm are taken on the porous material by mechanical processing.
  • the body was tested with a METTLER TOLEDO XP26 Microbalance balance, and the temperature and procedure were the same as in Example 1.
  • the results are shown in Table 3, wherein the absolute value of the deviation from the average value is expressed as a percentage, and the value is expressed as a percentage.
  • the absolute value of the deviation from the average value is divided by the mass average value. As can be seen from Table 3, the mass deviation is less than 4%.
  • the elastic modulus of this material was measured by the method of Example 1 to be 0.96 GPa, which was 68% lower than the elastic modulus of the raw material itself used for the porous material.
  • the preparation method of the porous polylactic acid is as follows:
  • the polylactic acid is frozen in liquid nitrogen, pulverized by a high-speed pulverizer, and sieved particles having a particle size of 20 ⁇ m;
  • This material is used to make medical implants.
  • the porous material of the present embodiment is porous tantalum, has a secondary pore structure, is classified by the pore size of the material, and has three-dimensional penetration between the pores of each level and the pores of each level, and the total effective porosity is 94%, and the average pore diameter of the macropores. At 122 ⁇ m, there were through-holes having an average pore diameter of 10 ⁇ m on the wall of the large pore.
  • Example 1 9 pieces of 10 mm ⁇ 10 mm ⁇ 10 mm three-dimensional bodies of the same size were placed on the porous material by mechanical processing, and the mass was tested with a METTLER TOLEDO XP26 Microbalance balance, and the temperature and procedure were the same as in Example 1. The results are shown in the table. 4, wherein the absolute value of the deviation from the average value is expressed as a percentage, and the value is the absolute value of the deviation from the average value divided by the mass average value. As can be seen from Table 4, the mass deviation is not more than 4%.
  • the elastic modulus of this material was measured by the method of Example 1 to be 1.05 GPa, which was 99% lower than the elastic modulus value of the raw material itself used for the porous material.
  • the preparation method of the porous ruthenium is:
  • the slurry was uniformly filled into a polyester foam having a rib diameter of 160 ⁇ 3 ⁇ m by a foam impregnation method to form a green body and dried, and then crushed to obtain a pulverized powder, a pore former and a polyester foam having a particle diameter of 160 ⁇ 3 ⁇ m. Mixed particles.
  • the dense body is vacuum sintered, and the sintered body is subjected to subsequent treatment according to a conventional process of hydrazine to obtain a porous ruthenium according to this embodiment having a second order of pore size.
  • This material is used to make medical implants.
  • the porous material of the present embodiment is porous copper, the porosity is 45.2%, the average pore diameter is 180 nm, and 10 pieces of three-dimensional bodies of the same size of 1 mm ⁇ 1 mm ⁇ 1 mm are obtained by mechanical processing on the porous material, using METTLER.
  • METTLER METTLER- Toledo XP26 Microbalance balance test its mass, measuring temperature and steps are the same as in Example 1, the results are shown in Table 5, wherein the absolute value of the deviation from the average value is expressed as a percentage, and the value is absolute with respect to the average value. The value is divided by the mass average, as can be seen from Table 5, the mass deviation is less than 2%.
  • the elastic modulus of this material was measured by the method of Example 1 to be 99 GPa, which was 10% lower than the elastic modulus value of the raw material itself used for the porous material.
  • the preparation method of the porous copper is as follows:
  • the nano copper crystal solution is prepared by using a nanocrystalline copper powder having a particle diameter of 30 to 50 nm and deionized water at a concentration of 0.08 g/ml, and the mixture drying temperature is 80 °C.
  • This material is used to make targets.

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Abstract

一种多孔材料，该多孔材料的孔是均匀分布的，该孔的均匀性分布是指各孔在多孔材料上任意单位级体积下均呈均匀性分布；且该多孔材料的弹性模量值比制得该多孔材料所采用的原材料本身的弹性模量值下降10-99％；该种多孔材料保证了其各种性能的均匀一致性，是性能、质量优良的多孔材料，其均匀性还保证了其弹性模量能有效降低。

Description

一种多孔材料 技术领域
本发明涉及一种多孔材料。
背景技术
多孔材料作为一种兼具功能和结构双重属性的性能优异的新型工程材料，在冶金机械、石油化工、能源环保、国防军工、核技术和生物制药、医疗器械等行业得到了广泛应用。例如，多孔材料可用于吸能减震、消音降噪，如用于汽车的防冲档，用作滤音器；多孔材料可用于将气体或液体进行过滤与分离，从而达到介质的净化与分离作用；多孔材料可用于热交换器，效率很高；多孔材料如泡沫镍、泡沫铜可作为优秀的电极材料，适用于各种蓄电池、燃料电池和太阳能电池；多孔材料如多孔钛、多孔钽、多孔羟基磷灰石等可用作生物材料，如人工骨、牙齿等；多孔陶瓷可用作催化剂载体，以促进反应；硬质聚氨酯泡沫塑料可用作隔热保温材料，广泛用于建筑节能；聚合物泡沫材料用作天线罩和无线电发射的外壳。
目前，很多多孔材料的应用要求都需要其材料本身均匀，即孔径大小、孔的分布均匀，使得性能均匀一致，但实际上，有很多多孔材料达不到要求，究其原因是其均匀性不足；尽管有的材料经过改进自称达到了较高的均匀性，但是其均匀性仍是大体积尺度下的均匀性，若用小体积尺度进行衡量比较，比如在材料上任取多块体积不大于1cm3的三维体，分别测其质量，其不均匀程度差异仍然非常大，即目前的多孔材料所称的均匀性只是大体积尺度下的均匀，而不是小体积尺度下的均匀，也可以说多孔材料的小体积尺度的不均匀造成多 孔材料的各种性能如强度、弹性模量等的不均匀，也因此使得多孔材料真正的弹性模量不能有效降低，从而严重影响其功能。
发明内容
本发明的目的在于给出高度均匀的多孔材料，该种多孔材料的弹性模量能有效降低。
本发明目的通过如下技术方案实现：
一种多孔材料，其孔呈均匀性分布，其特征在于：该孔的均匀性分布是指各孔在多孔材料上任意单位级体积下均呈均匀性分布；且该多孔材料的弹性模量值比制得该多孔材料所采用的原材料本身的弹性模量值下降10-99％。
上述单位级体积是指立方厘米级或立方毫米级或更小单位级体积。
上述孔的均匀性分布是指在该多孔材料上任取的体积不大于1cm3且相同大小的各三维体，它们的质量基本相当。
所述质量基本相当是指在多孔材料上任取的多个体积不大于1cm3且相同大小的三维体，分别称其质量，得到它们质量的平均值，任一三维体质量相对于质量平均值的偏差绝对值不大于三维体质量平均值的4％。
进一步说，在多孔材料上任取的多个体积不大于1cm3的相同大小的三维体，分别称其质量，得到它们质量的平均值，任一三维体质量相对于质量平均值的偏差绝对值不大于三维体质量平均值的2％，其均匀性更高，多孔材料的性能更加稳定。
进一步，在该多孔材料上任取的体积不大于1mm3的相同大小的三维体，它们质量基本相当。同样地，这里的质量基本相当是指在多孔材料上任取的多个体积不大于1mm3的相同大小的三维体，分别称其质量，得到它们质量的平均值，任一三维体质量相对于质量平均值的偏差绝对值不大于三维体质量平均值的4％。或者更均匀的情形是指在多孔材料上任取的多个体积不大于1mm3的相同大小的三维体，分别称其质量，得到它们质量的平均值，任一三维体质量相对于质量平均值的偏差绝对值不大于三维体质量平均值的2％。
本发明更进一步提供的多孔材料，它是以材料孔径大小进行分级的孔，及围绕形成孔的腔壁构成，呈三维空间围绕构成上级大孔的腔壁上设置下级小孔，该种高度均匀的多孔材料相对于单一孔隙的多孔材料有更多的功能，该多孔材料的弹性模量值可以在不同的尺度下予以控制。
更进一步说，该多孔材料的弹性模量值下降50-99％。
更进一步说，该多孔材料的弹性模量值下降70-99％。
本发明的有益效果：
1、本发明较现有技术提及的多孔材料的孔分布均匀更为具体明确，是在更小单位级体积的尺度下来要求多孔材料的孔分布均匀性，这样的多孔材料的孔是高度均匀的，从而保证了多孔材料的各种性能的均匀一致性。
2、本发明所述的多孔材料是在立方厘米级或立方毫米级或更小的单位级体积下孔分布均匀，其质量基本相当，从而真正降低多孔材料的整体弹性模量。
附图说明
下面结合附图和实施例，对本发明作进一步说明。
图1为本发明所述多孔材料的结构示意图，1-1为主视图，1-2为左视图，1-3为俯视图；
图2为本发明所述多孔材料实施例4的结构示意图，2-1为主视图，2-2为左视图，2-3为俯视图；
图3为图2局部A放大图；
图4为图3B-B截面图。
具体实施方式
具体实施方式以本发明技术方案为前提，给出了详细的实施方式，但本发明的保护范围不仅限于下述的实施方式。在不脱离和改变本发明上述技术思想情况下，根据本领域的普通技术知识和/或惯用手段，显然还可以做出多种形式的替换或变更，并均应包括在本发明的范围之内。
如图1所示，1为孔，2为孔的腔壁，孔是均匀分布的。
从图2可知，孔3的腔壁4由更小的孔5(下一级孔)及围绕孔5的腔壁6构成，结合图3对腔壁4的放大图、图4B-B截面图可知，孔5是三维贯通的，且两级孔彼此也三维贯通。
以下详细给出本发明的实施例：
实施例1：
本实施例的多孔材料为多孔不锈钢316，孔隙率为75.5％，由棱边为100μm，棱直径为30μm，单元为12棱边的正方体形的框架构成，用机械加工方法在该多孔材料上任取10件10mm×10mm×10mm的相同尺寸的三维体，用梅特勒-托利多XP26Microbalance天平在室温20℃测试其质量，测量步骤为：
1)预热：接通电源，预热至规定时间。
2)天平基本模式的选定：轻按ON键，开启显示器，用“通常情况”模式。
3)校准：用TAR键清零及CAL减、校准砝码进行校准。
4)称量：按TAR键，显示为零后，依次将三维体置于称盘上，待数字稳定即显示器左下角的“0”标志消失后，读出三维体的质量值。
测量结果如表1所示，其中，相对于平均值的偏差绝对值用百分比表示，其值为相对于平均值的偏差绝对值除以质量平均值，由表1可知，其质量偏差小于4％。
表1
件号 质量(mg) 相对于平均值的偏差绝对值(％)
1 1864.521 3.3％
2 1912.954 1.7％
3 1895.510 2.2％
4 1909.078 1.5％
5 1880.005 3％
6 2013.737 3.9％
7 1990.480 2.7％
8 1973.037 1.8％
9 1976.913 2％
10 1963.346 1.3％
质量平均值 1938.150  
按照GBT/7314-2005《金属材料室温压缩试验方法》，采用Instron力学试验机在室温25℃用压缩试验测试上述多孔不锈钢316压缩应力-应变曲线，其应力-应变曲线显示的初始变形为弹性变形，取弹性变形部分应力值与相应应变值之比即为弹性模量，测得弹性模量数值为35.1GPa，比多孔材料采用的原材料本身的弹性模量值下降82％。
该种多孔不锈钢316的制备方法如下：
(1)采用颗粒形状基本为球形的316不锈钢粉末，平均粒度为10±2μm；
(2)用CAD软件造型，作出棱边为102μm，棱直径为30μm，单元为12棱边的正方体形的框架形多孔材料模型；
(3)将多孔材料模型导入HRPM-IIB型选择性激光熔化快速成形系统，按照CAD软件造型扫描，扫描速度为200mm/min，激光束每完成一层切片面积的扫描，工作缸相对于激光束焦平面(成形平面)相应地下降一个切片层厚的高度，切片层厚为30μm；
(4)进行去应力退火处理；
(5)喷砂处理。
该种材料用于制作滤芯。
实施例2：
本实施例的多孔材料为多孔镍，孔隙率为83％，孔径平均值为113μm，用机械加工方法在该多孔材料上任取10件10mm×10mm×8mm的相同尺寸的三维体，用梅特勒-托利多XP26Microbalance天平测试其质量，测量温度及步骤与实施例1相同，结果如表2所示，其中，相对于平均值的偏差绝对值用百分比表示，其值为相对于平均值的偏差绝对值除以质量平均值，由表2可知，其质量偏差小于2％。
表2
件号 质量(mg) 相对于平均值的偏差绝对值(％)
1 1225.532 0.39％
2 1229.165 0.69％
3 1200.100 1.69％
4 1240.796 1.64％
5 1224.320 0.29％
6 1197.412 1.91％
7 1219.475 0.1％
8 1235.220 1.19％
9 1226.740 0.49％
10 1208.562 1％
质量平均值 1220.632  
用实施例1方法测得该种材料的弹性模量为15.6GPa，比多孔材料所采用的原材料本身的弹性模量值下降91％。
该种多孔镍的制备方法如下：
(1)基材预处理：选择孔径为152±3μm的聚氨酯海绵，用盐酸进行预处理；
(2)导电化处理：采用物理气相沉积方式，在聚氨酯海绵上沉积一层镍层；
(3)电镀：用脉冲电流法对上述导电化处理的聚氨酯海绵进行电镀，在海绵棱上再电镀一层镍镀层；
(4)还原烧结：在含70％氢气和30％氮气的保护气氛中进行还原处理，制得多孔镍材料。
该种材料用于制作电极。
实施例3：
本实施例的多孔材料为多孔聚乳酸，孔隙率为66％，孔径平均值为20μm，用机械加工方法在该多孔材料上任取10件1mm×1mm×1mm的相同尺寸的三 维体，用梅特勒-托利多XP26Microbalance天平测试其质量，测量温度及步骤与实施例1相同，结果如表3所示，其中，相对于平均值的偏差绝对值用百分比表示，其值为相对于平均值的偏差绝对值除以质量平均值，由表3可知，其质量偏差小于4％。
表3
件号 质量(mg) 相对于平均值的偏差绝对值(％)
1 0.440 0.5％
2 0.437 1％
3 0.425 3.8％
4 0.438 0.8％
5 0.437 1.2％
6 0.449 1.5％
7 0.459 3.9％
8 0.451 2％
9 0.452 2.2％
10 0.432 2.3％
质量平均值 0.442  
参照GBT/1041-2008《塑料压缩性能的测定》，用实施例1方法测得该种材料的弹性模量为0.96GPa，比多孔材料采用的原材料本身的弹性模量值下降68％。
该种多孔聚乳酸的制备方法如下：
(1)将聚乳酸在液氮中冷冻，经高速粉碎机粉碎，筛取20μm粒径的颗粒；
(2)选取20μm粒径的NaCl颗粒；
(3)将聚乳酸颗粒与NaCl颗粒按重量比17/33比例混合，在22℃下用低速搅拌机按60r/min搅拌2小时，使其均匀混合；
(4)将上述混合物放入密闭模具内，在75℃、7MPa下压制成块体；
(5)将上述块体放入双蒸水中浸泡72小时，每6小时换一次水，将NaCl完全去除，既得多孔聚乳酸。
该种材料用于制作医用植入物。
实施例4：
本实施例的多孔材料为多孔铌，具有二级孔结构，以材料孔径大小进行分级，其各级孔及各级孔之间是三维贯通的，总有效孔隙率为94％，大孔平均孔径为122μm，在大孔的腔壁上有平均孔径10μm的贯通的小孔。
用机械加工方法在该多孔材料上任取9件10mm×10mm×10mm的相同尺寸的三维体，用梅特勒-托利多XP26Microbalance天平测试其质量，测量温度及步骤与实施例1相同，结果如表4所示，其中，相对于平均值的偏差绝对值用百分比表示，其值为相对于平均值的偏差绝对值除以质量平均值，由表4可知，其质量偏差不大于4％。
表4
件号 质量(mg) 相对于平均值的偏差绝对值(％)
1 512.845 1.3％
2 513.365 1.2％
3 504.011 3％
4 508.169 2.2％
5 510.247 1.8％
6 498.816 4％
7 532.590 2.5％
8 529.992 2％
9 524.796 1％
质量平均值 519.600  
用实施例1方法测得该种材料的弹性模量为1.05GPa，比多孔材料所采用的原材料本身的弹性模量值下降99％。
该种多孔铌的制备方法是：
(1)材料准备
采用10μm的铌粉和粒径为15μm的尿素作为最小级孔造孔剂，将其均匀混合，并用15μm的淀粉作为粘合剂，按照铌粉：尿素：淀粉：蒸馏水体积比1：1.5：1：7配制成浆料。
将所述浆料用泡沫浸渍法均匀填充入棱直径为160±3μm的聚酯泡沫中，形成坯体并干燥，然后破碎得到颗粒为160±3μm的含有铌粉、造孔剂与聚酯泡沫的混合颗粒。
(2)将混合颗粒、粒径为160±3μm的甲基纤维素按体积比1：8均匀混合放入密闭模具压制成致密坯体。
(3)将致密坯体真空烧结，烧结后的坯体按照铌的常规工艺进行后续处理得到孔级数为二级的本实施例所述多孔铌。
该种材料用于制作医用植入物。
实施例5：
本实施例的多孔材料为多孔铜，孔隙率为45.2％，孔径平均值为180nm，用机械加工方法在该多孔材料上任取10件1mm×1mm×1mm的相同尺寸的三维体，用梅特勒-托利多XP26Microbalance天平测试其质量，测量温度及步骤与实施例1相同，结果如表5所示，其中，相对于平均值的偏差绝对值用百分比表示，其值为相对于平均值的偏差绝对值除以质量平均值，由表5可知，其质量偏差小于2％。
表5
件号 质量(mg) 相对于平均值的偏差绝对值(％)
1 4.730 0.8％
2 4.725 0.9％
3 4.706 1.3％
4 4.692 1.6％
5 4.715 1.1％
6 4.859 1.9％
7 4.820 1.1％
8 4.811 0.9％
9 4.825 1.2％
10 4.801 0.7％
质量平均值 4.768  
用实施例1方法测得该种材料的弹性模量为99GPa，比多孔材料采用的原材料本身的弹性模量值下降10％。
该种多孔铜的制备方法如下：
(1)选取粒径为200±4nm的聚苯乙烯小球；
(2)将上述聚苯乙烯小球组装形成三维有序排列的胶体模板；
(3)制备纳米铜晶溶液；
(4)将纳米铜晶溶液直接引入聚苯乙烯小球制成的三维胶体模板中，溶液渗入到聚苯乙烯小球之间；
(5)将三维胶体模板/纳米铜晶溶液的混合物干燥；
(6)用氯仿溶解聚苯乙烯小球，即制得本实施例所述多孔铜。
上述的制备方法中，纳米铜晶溶液用粒径为30-50nm的纳米晶铜粉与去离子水制备，浓度为0.08g/ml，混合物干燥温度为80℃。
该种材料用于制作靶材。

Claims (13)

  1. 一种多孔材料，其孔呈均匀性分布，其特征在于：该孔的均匀性分布是指各孔在多孔材料上任意单位级体积下均呈均匀性分布；且该多孔材料的弹性模量值比制得该多孔材料所采用的原材料本身的弹性模量值下降10-99％。
  2. 如权利要求1所述的多孔材料，其特征在于：所述单位级体积是指立方厘米级或立方毫米级或更小单位级体积。
  3. 如权利要求1所述的多孔材料，其特征在于：所述孔的均匀性分布是指在该多孔材料上任取的体积不大于1立方厘米且相同大小的各三维体，它们的质量基本相当。
  4. 如权利要求3所述的多孔材料，其特征在于：所述质量基本相当是指在多孔材料上任取的多个体积不大于1立方厘米且相同大小的三维体，分别称其质量，得到它们质量的平均值，而任一三维体质量相对于质量平均值的偏差绝对值不大于三维体质量平均值的4％。
  5. 如权利要求3所述的多孔材料，其特征在于：所述质量基本相当是指在多孔材料上任取的多个体积不大于1立方厘米的相同大小的三维体，分别称其质量，得到它们质量的平均值，而任一三维体质量相对于质量平均值的偏差绝对值不大于三维体质量平均值的2％。
  6. 如权利要求1所述的多孔材料，其特征在于：在该多孔材料上任取的体积不大于1立方毫米的相同大小的三维体，它们质量基本相当。
  7. 如权利要求6所述的多孔材料，其特征在于：所述质量基本相当是指在多孔材料上任取的多个体积不大于1立方毫米的相同大小的三维体，分别称其质量，得到它们质量的平均值，而任一三维体质量相对于质量平均值的偏差绝对值不大于三维体质量平均值的4％。
  8. 如权利要求6所述的多孔材料，其特征在于：所述质量基本相当是指在多孔材料上任取的多个体积不大于1立方毫米的相同大小的三维体，分别称其质量，得到它们质量的平均值，而任一三维体质量相对于质量平均值的偏差绝对值不大于三维体质量平均值的2％。
  9. 如权利要求1至8任一权利要求所述的多孔材料，其特征在于：所述多孔材料是以材料孔径大小进行分级的孔，及围绕形成孔的腔壁构成；呈三维空间围绕构成上级大孔的腔壁上设置下级小孔。
  10. 如权利要求1至8任一权利要求所述的多孔材料，其特征在于：所述多孔材料的弹性模量值下降50-99％。
  11. 如权利要求9所述的多孔材料，其特征在于：所述多孔材料的弹性模量值下降50-99％。
  12. 如权利要求1至8任一权利要求所述的多孔材料，其特征在于：所述多孔材料的弹性模量值下降70-99％。
  13. 如权利要求9所述的多孔材料，其特征在于：所述多孔材料的弹性模量值下降70-99％。
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