CN102357652B - Multi-scale ceramic/metal composite abrasion-resistant material and preparation method thereof - Google Patents
Multi-scale ceramic/metal composite abrasion-resistant material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a preparation technology of a high-performance and abrasion-resistant material, in particular to a multi-scale ceramic/metal composite abrasion-resistant material and a preparation method thereof. The resource-saving high-performance and abrasion-resistant material is obtained by using a high-performance foamed ceramic/metal double continuous phase composite material as an abrasion-resistant matrix, using a high-toughness metal as a constraint framework and using a casting method. The abrasion-resistant material has multi-scale composite structural characteristics, the abrasion-resistant unit is compounded in micron and millimeter scales, and the abrasion-resistant unit and the constraint framework are compounded in a centimeter scale. The structure can well realize reasonable matching of high abrasion resistance and high strength and toughness of the material, the abrasion resistance and the impact toughness of the material are respectively over 7 times and 10 times those of high-chromium cast iron, and meanwhile, scarce alloy elements (Cr, Ni, Mo and the like) are not used. The material is applied to large engineering equipment of crushing, excavating, transporting and the like, is excellent in abrasion resistance, low in cost and convenient to use, greatly prolongs the service life, greatly improves the production efficiency, and has good social benefit and economic benefit.
Description
Technical field
The present invention relates to the technology of preparing of high-performance abrasion-proof material, specifically a kind of Multi-scale ceramic/metal composite abrasion-resistant material and preparation method thereof.
Background technology
Wearing and tearing are one of principal modes of workpiece inefficacy, have caused the energy and raw-material a large amount of consumption.According to incompletely statistics, consumed every year on average the iron and steel of each industrial country 3% left and right, the world, the energy of 20-30%.China consumes every year on average abrasion-resistant stee and is approximately ten thousand tons of 300-400, is worth more than 60,000,000,000 yuan.Abrasion-resistant stee, as the effective means that reduces wearing and tearing, is widely used in the fields such as the energy, building materials, metallurgy, mine, traffic, equipment manufacture, environmental protection and national defence.For example, abrading-ball, the liner plate of grinding roller, mill and the ball mill of a large amount of grinding machines that use of the industries such as thermoelectricity, cement, mine, metallurgy, the bucket tooth of excavator, scraper bowl, the beater plate of the crushing wall of various disintegrating machines, tooth plate, fan grinding machine etc. all needs to use the high-performance abrasion-proof steel.
Along with the fast development of China's industry, to basic industry, as the production capacity demand of the industries such as electric power, building materials, mine constantly enlarges, annual hundred million tons of raw coal of mill 14-15, hundred million tons of cement raw materials of 40-50, hundred million tons of ores of 6-8 of needing.Grinding machine, as the capital equipment of all kinds of ore powder process, has ball milling, Vertical Mill and roll squeezer etc., and the annual electric power that consumes abrasion-resistant stee more than 1,000,000 tons, consumes accounts for enterprise's more than 60% of total amount of power consumption.
Abrasion-resistant stee is the general name of the ferrous materials that abrasion resistance properties is strong, is a kind of of consumption maximum in current high-abrasive material.The development experience of abrasion-resistant stee from potassium steel, ordinary white cast iron, ni-hard cast iron, rich chromium cast iron and several stages such as Property of High Alloy White Cast Iron, wear-resisting alloy steel.At present, potassium steel, rich chromium cast iron, middle-low alloy steel etc. are to pulverize the maximum a few class abrasion-resistant stees of consumption in equipment.
There is high-wearing feature and the high-strength tenacity standard problem with high unity in the wear-resisting steel capital such as potassium steel, rich chromium cast iron, middle-low alloy steel that are widely used in pulverizing equipment.Although the effort through decades, people are by alloyage process and in conjunction with means such as smelting, casting, deformation processing, heat treatments, the combination property of above-mentioned abrasion-resistant stee is significantly improved, but the contradiction between high-wearing feature and high-strength tenacity fundamentally is not resolved yet.Simultaneously, utilize alloyage process to improve the abrasion-resistant stee combination property, all need to use a large amount of rare metallic elements, in view of abrasion-resistant stee, wearing and tearing cause the characteristics that resource can not recycling, a large amount of consumption of rare metals resources, become the new problem that the restriction abrasion-resistant stee develops.
Therefore, develop the resource-conserving high-performance abrasion-proof steel that high-wearing feature and high-strength tenacity are unified, use no or little rare alloying element, become the development trend of wear-resistant steel material.Except continuing to explore new alloying process, utilize composite technology can realize the characteristics that the multiple material best performer group is closed, adapt to the effort of abrasion-resistant stee technology trends by the composite technology of research and development abrasion-resistant stee, just day by day be subject to the attention of academia and industrial circle.
At present, the composite technology of abrasion-resistant stee relates generally to homogeneous steel base wearable composite material preparation, stratiform and inserted composite construction abrasion-resistant stee, the original three kinds of technological approaches such as Multi-scale ceramic/metal composite abrasion-resistant material based on material and structure multistage composite of China in the world.
The homogeneous steel base wearable composite material preparation now developed, be to take steel as binding metal, makes the bond material of hard phase with refractory carbide, at some, in harsh wear working condition, obtained commercial Application.Its tissue characteristic is that fine hard uniform crystal particles is scattered in steel matrix, has hardness, the wearability of hard compounds concurrently, and the intensity of steel and toughness, in the middle status of ordinary rigid alloy and steel.But the interpolation unit that binding agent is the most often used have the rare metals such as nickel, chromium, and need the processing method preparations such as powder metallurgy process, infusion process, pressure sintering, hot isostatic pressing method, spray-up method, mix and blend casting and plasma melting powder method, cause existing steel-based wearing composite material not possess obvious superiority of effectiveness, it is applied and is subject to larger restriction.
Stratiform and inserted composite construction abrasion-resistant stee, the material different with obdurability obtaining by fusion, pressing, sintering, the method such as spray, inlay with two or more wearabilities, structure composite is its basic characteristics.With the homogeneous steel base wearable composite material preparation, compare, this class wear-resistant composite steel can obtain better serviceability, but also has many problem demanding prompt solutions.For the layered composite structure abrasion-resistant stee, inner high tough structural steel and the marked difference of outer high abrasion steel aspect the coefficient of expansion and plasticity, often cause outer high abrasion steel occur to ftracture in preparation and use procedure and unstable wear makes its high-wearing feature advantage not obtain fine performance.For inserted composite construction abrasion-resistant stee, be embedded in the column in high-ductility steel, spherical pottery or carbide alloy and there is very strong wearability, can significantly improve the anti-wear performance of material, but still face a series of problems that it is applied that limit aspect preparation, use and cost.When adopting carbide alloy as wear-resisting primitive, because carbide alloy self price is high, the reliable connection of carbide alloy and metallic matrix often needs to utilize the soldering means in addition, and large-scale promotion application will be restricted because of too high cost pressure.When adopting the ceramic wear-resisting primitive, how in recombination process, to guarantee the reliable connection of pottery and steel and don't produce excessive internal stress, how in use to prevent that ceramic fragmentation from coming off, do not obtain so far fine solution yet.
Summary of the invention:
The invention provides a kind of Multi-scale ceramic/metal composite abrasion-resistant material and preparation method thereof, efficiently solve due to the phenomenon of pottery with the excessive Interface Cracking caused of expansion of metal difference of coefficients, realized good interface combination, the bulk peeling phenomenon of having avoided ceramic block and metal composite to exist, and then the service life of obviously having improved Multi-scale ceramic/metal composite abrasion-resistant material.
Technical scheme of the present invention is:
A kind of Multi-scale ceramic/metal composite abrasion-resistant material, take foamed ceramics/metal bicontinuous phase compound material as wear-resisting primitive, take high-toughness metal as the constraint framework, foamed ceramics/metal bicontinuous phase compound material and high-toughness metal are combined into high-abrasive material by casting method.
Described Multi-scale ceramic/metal composite abrasion-resistant material, foamed ceramics/metal bicontinuous phase compound material is foamed ceramics and the Material cladding of metal on micron and two yardsticks of millimeter, foamed ceramics/metal bicontinuous phase compound material and high-toughness metal retrain the compound of frame, are the structure composite of bi-material on centimeter scale of simultaneously realizing when carrying out foamed ceramics and metal composite.
Described Multi-scale ceramic/metal composite abrasion-resistant material, foamed ceramics/metal bicontinuous phase compound material is foamed ceramics and the Material cladding of metal on mm-scale, foamed ceramics/metal bicontinuous phase compound material and high-toughness metal retrain the compound of frame, are the structure composite of bi-material on centimeter scale of simultaneously realizing when carrying out foamed ceramics and metal composite.
The preparation method of described Multi-scale ceramic/metal composite abrasion-resistant material, foamed ceramics is mounted in high-toughness metal constraint frame, utilize normal pressure casting, extrusion casint, vacuum pressing and casting or negative pressure suction casting method, the metal of melting is entered in the three-dimensional communication mesh of foamed ceramics, realize foamed ceramics and metal compound to centimetre three yardsticks again from the micron to the millimeter, or realize compound from millimeter to centimetre two yardsticks of foamed ceramics and metal.
The preparation method of described Multi-scale ceramic/metal composite abrasion-resistant material, described foamed ceramics is foam silicon carbon, foam silicon nitride, foamed alumina, foam zirconia or foam glass, the average-size of mesh is: 0.5mm-5mm, the volume fraction of foamed ceramics is: 5%-70%, and average grain size is at 10nm-300 μ m; Foamed ceramics is foamed ceramics skeleton fine and close or porous.
The preparation method of described Multi-scale ceramic/metal composite abrasion-resistant material, the metal of described melting is cast iron, cast steel, copper alloy, aluminium alloy or cast magnesium alloy.
The preparation method of described Multi-scale ceramic/metal composite abrasion-resistant material, cast iron is spheroidal graphite cast-iron or gray iron, cast steel is casting carbon steel or cast alloy steel, and copper alloy is cast tin bronze, aluminium bronze or Allen's metal, and aluminium alloy is alusil alloy, aluminium copper, almag or alumin(i)um zinc alloy.
The preparation method of described Multi-scale ceramic/metal composite abrasion-resistant material, high-toughness metal constraint frame is single hole or loose structure, and hole shape is square, circular, hexagon or other polygon, and it is through hole or half through hole that high-toughness metal retrains frame; For half through hole, there are one or several back taper aperture in the bottom surface, hole; Constraint frame wall thickness or the thick 1/100-1/2 that is designed to as required the foamed ceramics maximum transverse size of hole wall; The material of constraint frame is steel, copper alloy or aluminium alloy; The constraint frame adopts hot investment casting, area of computer aided rapid shaping and machine-tooled method to obtain.
The preparation method of described Multi-scale ceramic/metal composite abrasion-resistant material, the steel framework material is 16Mn steel, 20# steel, 35# steel, 45# steel or other structural steel; Copper alloy frame material is tin bronze, aluminium bronze or Allen's metal frame; The aluminum alloy frame material is alusil alloy, aluminium copper or almag.
The preparation method of described Multi-scale ceramic/metal composite abrasion-resistant material doses ceramic powder in the foamed ceramics mesh, and ceramic powder is SiC, SiO
2or Al
2o
3, granularity is: 200nm-1mm, the 0wt%-50wt% that addition is foamed ceramics weight adds method to be: ceramic powder is poured in the foamed ceramics mesh, and the method by mechanical oscillation is by ceramic powder jolt ramming.
The present invention has following beneficial effect:
1. Multi-scale ceramic/metal composite abrasion-resistant material is a kind of resource-conserving abrasion-resistant stee.
Take the high-performance foam ceramic/metallic double continuous phase composite material as wear-resisting primitive, take high-toughness metal as constraint framework, the resource-conserving high-performance abrasion-proof material that utilizes casting method to obtain.Multi-scale ceramic/metal composite abrasion-resistant material is not used rare metallic element (Cr, Ni, Mo), can save a large amount of rare metallic elements.Therefore, can realize that on the one hand basic industry is energy-conservation, lower consumption, reduce discharging, promote the high-abrasive material technological progress, realize sustainable development; Use resource-conserving high-performance abrasion-proof steel at the energy-conservation pulverizing equipment of Large Efficient on the other hand, there is significantly exemplary and drive property.
2. Multi-scale ceramic/metal composite abrasion-resistant material has good anti-wear performance and good obdurability.
Carborundum, aluminium oxide, zirconia etc. being prepared into to foamed ceramics, can keeping the advantage of ceramic anti-wear performance, can bring into play again the overall enhanced characteristic of three-dimensional network simultaneously, is a kind of ceramic material with structural reinforcing.By the molten metal pressure injection or be filled in the foamed ceramics mesh and obtain ceramic/metallic double continuous phase composite material, become the wear-resisting unit of Multi-scale ceramic/metal composite abrasion-resistant material.This wear-resisting unit has very strong abrasive resistance, high compression strength and fracture toughness.The combination of this wear-resisting unit and high-toughness metal constraint frame makes Multi-scale ceramic/metal composite abrasion-resistant material possess good anti-wear performance and good obdurability simultaneously.
Test result shows: the anti-wear performance that No. 35 steel of take are constraint frame, the foam silicon carbon/spheroidal graphite cast-iron bicontinuous phase compound material multiple dimensioned complex abrasion-proof steel that is wear-resisting unit is 7 times of rich chromium cast iron, 30 times of potassium steel, and impact flexibility is 10 times of rich chromium cast irons.Therefore, at some, important application substitutes rich chromium cast iron and will produce considerable economic benefit and and social benefit.
For example, China's thermoelectricity, cement, mine are the use rich anies influential family of abrasion-resistant stee.The large-scale grinding equipment used at present is just towards efficient, energy-saving future development, and Vertical Mill, roll mill have progressively occupied leading position, are badly in need of the high-performance abrasion-proof steel and are supported.The crucial wear members such as the grinding roller of existing Vertical Mill, roll squeezer, mill adopt the good rich chromium cast iron of anti-wear performance in steel mostly, and are used with foundry goods or built-up welding mode.High-wearing feature and high-strength tenacity contradiction, the large common problem of the outspent abrasion-resistant stee two of scarce resource show particularly outstandingly on rich chromium cast iron, and 2009, use the grinding roller of rich chromium cast iron, the consumption of mill to reach more than 300,000 tons, be worth more than 7,000,000,000 yuan.Along with the large-scale popularization of Vertical Mill, roll mill, rich chromium cast iron is by the great market pressure faced.There is the alternative rich chromium cast iron of the good wear-resisting multiple dimensioned complex abrasion-proof steel with impact property and will produce considerable society and economic benefit.
3. adopt multiple dimensioned complex technique, improved the service life of Multi-scale ceramic/metal composite abrasion-resistant material.
Foamed ceramics and metal and high tenacity constraint frame is compound in micron, millimeter and centimeter scale, efficiently solve due to the phenomenon of pottery with the excessive Interface Cracking caused of expansion of metal difference of coefficients, realized good interface combination, the bulk peeling phenomenon of having avoided ceramic block and metal composite to exist, and then the service life of obviously having improved Multi-scale ceramic/metal composite abrasion-resistant material.
4. cost is low, easy to use
Adopt the foamed ceramicses such as carborundum that in reaction sintering technology and air atmosphere, sintering process produces, aluminium oxide, zirconia, can take full advantage of the useful space of sintering furnace, can realize mass production; The Extrution casting technique of utilization in air atmosphere has that combination process is simple, shaping speed is fast and can the near-net-shape manufacture etc. characteristics, can carry out the serialization low cost fabrication.Multi-scale ceramic/metal composite abrasion-resistant material can be produced multiple dimensioned wear-resisting integrated member and a minute body component according to needs of production, adopts bolt, rivet or welding manner to install, easy for installation and be convenient to change.
In a word, the present invention proposes a kind of preparation method of Multi-scale ceramic/metal composite abrasion-resistant material.The Multi-scale ceramic/metal composite abrasion-resistant material prepared by the method has the characteristics such as good anti-wear performance and shock resistance, cost be low, easy to use.
The accompanying drawing explanation
Fig. 1 (a) is multiple dimensioned complex abrasion-proof steel exemplar schematic diagram.
The weight-loss ratio that Fig. 1 (b) is not same piece and wearing and tearing distance relation figure.
Fig. 2 is Multi-scale ceramic/metal composite abrasion-resistant material preparation technology flow chart.
Fig. 3 (a)-(b) is 35# steel constraint frame schematic diagram; Wherein, Fig. 3 (a) is top view; Fig. 3 (b) is upward view.In figure, 1 constraint frame; 2 reverse taper holes; 3 square holes; 4 horizontal bars.
Fig. 4 is properties of SiC foam ceramics piece schematic diagram.
Fig. 5 is the constraint frame schematic diagram of inlaying the properties of SiC foam ceramics piece.
Fig. 6 is medium-speed pulverizer grinding roller member front schematic view.
Fig. 7 is medium-speed pulverizer grinding roller member side schematic view.
The 35# steel constraint frame top view that Fig. 8 is embodiment 7; In figure, 1 constraint frame; 2 reverse taper holes; 3 square holes; 4 horizontal bars.
The 16 manganese steel constraint frame schematic diagrames that Fig. 9 is embodiment 8; In figure, 1 constraint frame; 2 reverse taper holes; 3 square holes; 4 horizontal bars.
Figure 10 is properties of SiC foam ceramics piece schematic diagram.
Figure 11 is the constraint frame schematic diagram of inlaying the properties of SiC foam ceramics piece.
Figure 12 is multiple dimensioned complex abrasion-proof steel member-front schematic view.
The specific embodiment
Metal Inst., Chinese Academy of Sciences utilizes it in high-performance foam ceramic/metal co-continuous phase material technology (Chinese patent application, application number 200610046242.X) experience accumulation of aspect and technical advantage, take the lead in the world proposing " to utilize the multiple dimensioned complex technique of material, development does not rely on Cr, Mo, Ni and other rare metal, can be fine realize the abrasion resistance material that high-wearing feature and high-strength tenacity are unified " imagination, and develop and take foamed ceramics/metal bicontinuous phase compound material as the high-strength wearable primitive, take high-toughness metal as retraining the multiple dimensioned composite abrasion resistance material of framework.
In Multi-scale ceramic/metal composite abrasion-resistant material, foamed ceramics/metal bicontinuous phase compound material is foamed ceramics and the Material cladding of metal on micron and two yardsticks of millimeter, there is very high compression strength and wearability, and foamed ceramics/metal bicontinuous phase compound material and high-toughness metal retrain the compound of frame, be the structure composite of bi-material on centimeter scale of simultaneously realizing when carrying out foamed ceramics and metal composite.
In the present invention, micro-meter scale refers to 0.1-100 micron (not containing 100 microns), and mm-scale refers to 0.1-10 millimeter (not containing 10 millimeters), and centimeter scale refers to 1-10 centimetre.
Foamed ceramics and the metal Material cladding on micron and two yardsticks of millimeter, making between bi-material has very strong mutual effect of contraction, significantly reduced the internal stress of composite simultaneously, thereby can give full play under the prerequisite of ceramic abrasive resistance, avoid well the problem that in inserted composite construction high-abrasive material, the fragmentation of ceramic wear-resisting unit comes off.The high-toughness metal framework makes multiple dimensioned composite abrasion resistance material possess good shock resistance to the constraint of bicontinuous phase compound material.Test result shows: the multiple dimensioned complex abrasion-proof steel that properties of SiC foam ceramics/cast iron wherein (cast steel)/high-ductility steel three-phase forms is than potassium steel and rich chromium cast iron has respectively more than thirtyfold and wearability more than seven times, its impact flexibility also reaches more than 10 times of rich chromium cast iron, has also confirmed that multiple dimensioned complex abrasion-proof steel can realize the advantage of high-wearing feature and high-strength tenacity desired combination under the prerequisite of not utilizing Cr, Mo, Ni and other rare metal simultaneously.
The performance test results shows: the compression strength of the multiple dimensioned complex abrasion-proof steel that properties of SiC foam ceramics/cast iron wherein (cast steel)/high-ductility steel three-phase forms surpasses 650MPa, and impact flexibility surpasses 50J/cm
2, anti-wear performance reaches 7 times of rich chromium cast iron, demonstrates and realizes the desirable advantage coordinated of material high-wearing feature and high-strength tenacity, as shown in Fig. 1 (a)-(b).The present invention also provides the preparation method of Multi-scale ceramic/metal composite abrasion-resistant material, preparation technology's flow process as shown in Figure 2, mainly comprise: foamed ceramics piece preparation, the manufacture of high tenacity constraint frame, foamed ceramics piece are inlayed, preheating, Metal Melting, compound, machined finishing etc., form Multi-scale ceramic/metal composite abrasion-resistant material.
Preparation process is as follows:
(1) high tenacity constraint frame manufacture
Adopt the method casting (processing) of hot investment casting (machined) to go out to need the high-ductility steel of shape and size to retrain frame.The material of high tenacity constraint frame can be steel framework, as 16Mn steel, 20# steel, 35# steel, 45# steel or other structural steel etc.; Can be the copper alloy frame, as tin bronze, aluminium bronze or Allen's metal frame etc.; Can be aluminum alloy frame, as alusil alloy, aluminium copper, almag etc.Open reverse taper holes in constraint frame bottom surface, so that in recombination process, the metal liquid of melting, under the effect of pressure, fills type to reverse taper holes, solidifies the effect of rear formation rivet, improves bicontinuous phase compound material and the bond strength that retrains frame.
(2) foamed ceramics piece preparation
Prepared referring to patent by the properties of SiC foam ceramics piece:
1. high-strength foam silicon carbide ceramics and preparation method thereof (patent No. ZL00110479.9), take after pyrolysis that to keep the macromolecular material of high carbon residue rate be raw material, take the polyaminoresin foam plastics as skeleton, through hanging, solidify, pyrolysis, siliconising process, and obtains dense foam silicon carbide ceramics piece.
The average-size of described foamed ceramics mesh is: 0.5mm-5mm; The volume fraction of foamed ceramics is: 5%-70%, and average grain size is at 10nm-300 μ m, and the relative density of foamed ceramics muscle is greater than 98%.
2. two yardstick silicon carbide foam ceramic materials and preparation method thereof (application number 200910248558.0), foam silicon carbide ceramics has the three-dimensional networks structure, have the mesh that the grade yardstick is interconnected on macroscopic view, pore diameter range is 0.5mm-5mm; Ceramic skeleton muscle inside has the mesh that the micron order yardstick is interconnected, and pore diameter range is 5~100 μ m.Described foam silicon carbide ceramics be take polygonal closed-loop as elementary cell, and each elementary cell is interconnected to form three-dimensional networks, and the volume fraction of foamed ceramics is: 5%-70%, the carborundum average grain size is at 10nm-300 μ m.
Utilize above-mentioned two patents to prepare the properties of SiC foam ceramics piece of required size and shape.At first, cut out the polyurethane foam of corresponding size, after soaking the extension silicon carbide slurry and extruding unnecessary slip, put into baking oven heating cure typing, repeat after taking-up to soak and hang silicon carbide slurry until reach the volume fraction needed, then through pyrolysis, machined cuts into needs the foamed ceramics of shape and size carbon piece, then processes through reaction-sintered siliconising, high temperature silica removal, obtains porous foam silicon carbide ceramics piece.
The preparation method of other foamed ceramics: the same with the properties of SiC foam ceramics forming method aspect moulding, adopt equally slip to soak the method preparation of extension, preparation process is as follows:
The first step, the slip preparation
By weight percentage, after ceramic A (wt%) 30-50, stabilizing agent B (wt%) 2-10, sintering aid C (wt%) 2-10, solvent D (wt%) 66-30 are mixed, ball milling after mechanical agitation, filter, obtain slip, the 5-60% that described slurry solution is the solute gross weight; Wherein:
Ceramic A: ceramic is silicon nitride, aluminium oxide, zirconia or glass micro mist etc., and granularity is 200nm-1mm;
Stabilizing agent B: magnesia, cerium oxide or rare earth etc., granularity is 10nm-10 μ m;
Sintering aid C: titanium oxide or yittrium oxide etc., granularity is 10nm-10 μ m;
Solvent D: Ludox, ethyl silicate or waterglass etc.
Second step, soak extension
The polyurethane foam is cut into to required form and size, immerse equably in slip, take out rear squeeze and remove unnecessary slip, adopt air-blowing or centrifugal mode to remove unnecessary slip, the heating semi-solid preparation, repeatedly, to reaching needed volume fraction, obtain the foamed ceramics presoma.
Wherein, semi-solid preparation is heat cure at 100-250 ℃ of temperature, 10 minutes-2 hours time.
The 3rd step, pyrolysis
By the pyrolysis under the protection of argon gas, nitrogen or other inert gas of foamed ceramics presoma, foam generated ceramic skeleton; Wherein, heating rate 1-5 ℃ per minute, be warming up to 800-1200 ℃, insulation 0.5-2 hour.
The 4th step, sinter molding
In air atmosphere, to foamed ceramics skeleton sinter molding, heating rate is 5-15 ℃ per minute, and sintering temperature is: 1400 ℃-1750 ℃, temperature retention time is 0.5-8 hour, obtains foam ceramic material.
Described foamed ceramics be take polygonal closed-loop as elementary cell, and each elementary cell is interconnected to form three-dimensional networks, and the average-size of foamed ceramics mesh is: 0.5mm-5mm; The volume fraction of foamed ceramics is: 5%-70%, average grain size is at 10nm-300 μ m.
Can have the mesh that the grade yardstick is interconnected on its macroscopic view, pore diameter range is 0.5mm-5mm; Ceramic skeleton muscle inside can have the mesh that the micron order yardstick is interconnected, and pore diameter range is 5~100 μ m.
In the present invention, in the foamed ceramics mesh, can dose ceramic powder, add method to be: ceramic powder is poured in the foamed ceramics mesh, and the method by mechanical oscillation is by ceramic powder jolt ramming.Ceramic powder is SiC, SiO
2or Al
2o
3, granularity is: 200nm-1mm, the 0wt%-50wt% that addition is foamed ceramics weight.
(3) inlay
At first, high-toughness metal is retrained to the texturing of frame table face and process, as sandblast texturing etc., the surface-treated purpose is to improve interface quality.Then, the foamed ceramics piece is mounted in high-toughness metal constraint frame.
(4) Metal Melting
Cast iron or cast steel or copper alloy or aluminium alloy are put into to medium frequency induction melting furnace or crucible for smelting stove, according to corresponding specification requirement melting.
For example, smelting nodular cast iron, adopt lid to water the method melting.At first, the pig iron is carried out to melting, smelting temperature is 1300 ℃-1400 ℃; Then, quantitative nodulizer (RE-Mg-ferrosilicon alloy) and inovulant (ferrosilicon) are joined to the cast crucible bottom; Then, pour pig iron liquid into, be poured in mould after waiting abundant reaction again, the spheroidal graphite cast-iron composition is in Table 2.
Table 2 spheroidal graphite cast-iron composition
(5) complex method 1-extrusion casint
The capital equipment of extrusion casint comprises forcing press, batch-type furnace and medium frequency induction melting furnace etc.
The high-toughness metal constraint frame that at first will be inlaid with the foamed ceramics piece is put into the batch-type furnace preheating, and preheat temperature is 300 ℃-900 ℃.Simultaneously, composite die is utilized acetylene flame or blowtorch etc. are preheated to 200 ℃-400 ℃.
Then will put into composite die through the high-toughness metal constraint frame of preheating, and utilize crucible that melting is poured in mould to the relevant temperature molten metal simultaneously, type is filled in pressurization.Institute's plus-pressure is 50MPa-120MPa, and be 5S-120S pressing time, and the dwell time is 10S-120S.
After depanning, be machined to the size needed and can obtain Multi-scale ceramic/metal composite abrasion-resistant material.
(6) complex method 2-negative pressure casting
The capital equipment of negative pressure casting comprises composite die, batch-type furnace, medium frequency induction melting furnace and vavuum pump etc.
Composite die bottom surface or lateral opening hole, connect with steel pipe and vacuum chamber, and the middle butterfly valve of installing is controlled break-make, and steel pipe and the water flowing of mould junction are cooling, prevent that molten metal from entering butterfly valve or vacuum chamber, and the vacuum of vacuum chamber is 200-2000Pa.
The high-toughness metal constraint frame that at first will be inlaid with the foamed ceramics piece is put into the batch-type furnace preheating, and preheat temperature is 300 ℃-900 ℃.Simultaneously, composite die is utilized acetylene flame or blowtorch etc. are preheated to 200 ℃-400 ℃.
Then will put in composite die through the high-toughness metal constraint frame of preheating, utilize crucible that melting is poured in mould to the relevant temperature molten metal simultaneously, open butterfly valve and make the high-toughness metal constraint frame that is inlaid with the foamed ceramics piece form rapidly vacuum, utilize atmospheric pressure that molten metal is pressed onto in the foamed ceramics mesh.
After depanning, be machined to the size needed and can obtain Multi-scale ceramic/metal composite abrasion-resistant material.
Below by embodiment in detail the present invention is described in detail.
Embodiment 1
1. high-ductility steel constraint frame casting
Adopt casting method, cast out 35# steel constraint frame, constraint frame 1 bottom surface has: top being of a size of
below be of a size of
reverse taper holes 2, surface uniform 21 * 21 * 20mm that distributes
3square hole 3, middle horizontal bar 4 width are 3mm, as shown in Figure 3.Then utilize the method for sandblast, will retrain the processing of frame rough inner surface.
2. properties of SiC foam ceramics piece preparation
According to patent: a kind of high-strength foam silicon carbide ceramics and preparation method thereof (ZL00110479.9) is prepared the foam silicon carbide ceramics piece, the average-size of mesh is: 1.0mm, volume fraction is: 60%, and average grain size, at 5 μ m, is of a size of 21 * 21 * 20mm
3, the foamed ceramics piece, through high-temperature process, is removed remaining silicon, as shown in Figure 4.
3. inlay
To prepare the properties of SiC foam ceramics piece is mounted in high-ductility steel constraint frame, as shown in Figure 5.
4. spheroidal graphite cast-iron melting
Select 14# foundry iron, put into medium frequency induction melting furnace, smelting temperature is 1350 ℃.Then quantitative nodulizer and inovulant (in Table 3) are joined to the cast crucible bottom, then pour pig iron liquid into, after waiting after abundant reaction and obtaining spheroidal graphite cast-iron, then be poured in mould.
Table 3 spheroidal graphite cast-iron composition
5. extrusion casint
The high-ductility steel constraint frame that at first will be inlaid with the foam silicon carbide ceramics piece is put into the batch-type furnace preheating, and preheat temperature is 800 ℃.
Simultaneously, composite die is utilized acetylene flame or blowtorch etc. are preheated to 300 ℃.
Then will put into composite die through the high-ductility steel of preheating constraint frame, simultaneously by the spheroidal graphite cast-iron solution casting that obtains after reaction in mould, pressurize and fill type.Institute's plus-pressure is 100MPa; Be 10S pressing time; Dwell time is 10S.
6. repair type
After depanning, be machined to the size needed and can obtain multiple dimensioned complex abrasion-proof steel member, as shown in Figure 6,7.
In Multi-scale ceramic/metal composite abrasion-resistant material, foamed ceramics and the metal Material cladding on mm-scale, there is very high compression strength and wearability, and foamed ceramics/metal bicontinuous phase compound material and high-toughness metal retrain the compound of frame, be the structure composite of bi-material on centimeter scale of simultaneously realizing when carrying out foamed ceramics and metal composite.In the present embodiment, properties of SiC foam ceramics/spheroidal graphite cast-iron/35# steel three-phase has formed multiple dimensioned complex abrasion-proof steel, demonstrates the desirable advantage coordinated of material high-wearing feature and high-strength tenacity that realizes.
Be that with the difference of embodiment 1 high-ductility steel retrains the preparation of frame.
Adopt casting method, cast out 16 manganese steel constraint frames.Then utilize the method for sandblast, will retrain the processing of frame rough inner surface.
In the present embodiment, properties of SiC foam ceramics/spheroidal graphite cast-iron/16 manganese steel three-phases have formed multiple dimensioned complex abrasion-proof steel, demonstrate the desirable advantage coordinated of material high-wearing feature and high-strength tenacity that realizes.
Embodiment 3
Be the preparation of properties of SiC foam ceramics piece with the difference of embodiment 1.According to patent: a kind of high-strength foam silicon carbide ceramics and preparation method thereof (ZL00110479.9) is prepared the foam silicon carbide ceramics piece, and the average-size of mesh is: 1.5mm, and volume fraction is: 70%, average grain size is at 20 μ m.
In the present embodiment, properties of SiC foam ceramics/spheroidal graphite cast-iron/35# steel three-phase has formed multiple dimensioned complex abrasion-proof steel, demonstrates the desirable advantage coordinated of material high-wearing feature and high-strength tenacity that realizes.
Embodiment 4
Be the selection of the molten steel of extrusion casint with the difference of embodiment 1.
The molten steel of extrusion casint is selected the 45# steel, and smelting temperature is 1520 ℃.
In the present embodiment, properties of SiC foam ceramics/45# steel/35# steel three-phase has formed multiple dimensioned complex abrasion-proof steel, demonstrates the desirable advantage coordinated of material high-wearing feature and high-strength tenacity that realizes.
Embodiment 5
Be the selection of foamed ceramics piece with the difference of embodiment 1.The foamed ceramics piece is the foamed alumina ceramic block, and the average-size of mesh is: 1.5mm, and volume fraction is: 40%, average grain size is at 50nm.
In the present embodiment, foamed alumina pottery/spheroidal graphite cast-iron/35# steel three-phase has formed multiple dimensioned complex abrasion-proof steel, demonstrates the desirable advantage coordinated of material high-wearing feature and high-strength tenacity that realizes.
Embodiment 6
Be the selection of high-toughness metal constraint frame and the selection of compound tense metal bath with the difference of embodiment 1.
Adopt casting method, cast out 663 tin bronze constraint frames, be of a size of above constraint frame bottom surface has
below be of a size of
reverse taper holes, surface uniform 25 * 25 * 15mm that distributes
3square hole, middle horizontal bar width is 3mm.Then utilize the method for sandblast, will retrain the processing of frame rough inner surface.The cast alloy is the ZL101 Birmasil, and pouring temperature is 780 ℃.
In the present embodiment, properties of SiC foam ceramics/spheroidal graphite cast-iron/663 tin bronze three-phases have formed multiple dimensioned composite abrasion resistance material, demonstrate the desirable advantage coordinated of material high-wearing feature and high-strength tenacity that realizes.
Embodiment 7
Be high-ductility steel constraint frame size with the difference of embodiment 1.
Adopt casting method, cast out 35# steel constraint frame, constraint frame gross thickness is 20mm, and constraint frame 1 bottom surface has: top being of a size of
below be of a size of
reverse taper holes 2, surface uniform 21 * 21 * 20mm that distributes
3square hole 3, between the square hole 3 of constraint in frame 1, the horizontal bar width is 3mm, as shown in Figure 8.Then utilize the method for sandblast, will retrain the processing of frame rough inner surface.
In the present embodiment, properties of SiC foam ceramics/spheroidal graphite cast-iron/35# steel three-phase has formed multiple dimensioned complex abrasion-proof steel, demonstrates the desirable advantage coordinated of material high-wearing feature and high-strength tenacity that realizes.
Embodiment 8
1. high-ductility steel constraint frame casting
Adopt mach method, prepare 16 manganese steel constraint frames, constraint frame gross thickness is 20mm, and constraint frame 1 bottom surface has: top being of a size of
below be of a size of
reverse taper holes 2, surface uniform 30 * 30 * 10mm that distributes
3square hole 3, between the square hole 3 of constraint in frame 1, the horizontal bar width is 2mm, as shown in Figure 9.Then utilize the method for sandblast, will retrain the processing of frame rough inner surface.
2. properties of SiC foam ceramics piece preparation
According to patent: a kind of pair of yardstick silicon carbide foam ceramic material and preparation method thereof (200910248558.0) prepared the foam silicon carbide ceramics piece, the properties of SiC foam ceramics piece, for remove the porous foam silicon carbide ceramics piece of remaining silicon through high-temperature process, is of a size of 30 * 30 * 10mm
3;
In the present embodiment, foam silicon carbide ceramics has the three-dimensional networks structure, and volume fraction is: 70%, and the carborundum average grain size is at 8 μ m.Described foam silicon carbide ceramics be take polygonal closed-loop as elementary cell, and each elementary cell is interconnected to form three-dimensional networks.Have the mesh that the grade yardstick is interconnected on macroscopic view, the average-size of mesh is: 2.0mm; Ceramic skeleton muscle inside has the mesh that the micron order yardstick is interconnected, and the average-size of mesh is: 20 μ m, as shown in figure 10.
3. inlay
As shown in figure 11, will prepare the properties of SiC foam ceramics piece is mounted in high-ductility steel constraint frame.
4. spheroidal graphite cast-iron melting
Select 14# foundry iron, put into medium frequency induction melting furnace, smelting temperature is 1350 ℃.Then quantitative nodulizer and inovulant are joined to cast crucible bottom (in Table 4), then pour pig iron liquid into, after waiting after abundant reaction and obtaining spheroidal graphite cast-iron, then be poured in mould.
Table 4 spheroidal graphite cast-iron composition
5. extrusion casint
The high-ductility steel constraint frame that at first will be inlaid with the properties of SiC foam ceramics piece is put into the batch-type furnace preheating, and preheat temperature is 800 ℃.
Composite die is utilized acetylene flame or blowtorch etc. to be preheated to 250 ℃ simultaneously.
Then will put into composite die through the high-ductility steel of preheating constraint frame, simultaneously by the spheroidal graphite cast-iron solution casting that obtains after reaction in mould, pressurize and fill type.Institute's plus-pressure is 80MPa; Be 5S pressing time; Dwell time is 10S.
6. repair type
After depanning, be machined to the size needed and can obtain multiple dimensioned complex abrasion-proof steel member, as shown in figure 12.
In the present embodiment, in Multi-scale ceramic/metal composite abrasion-resistant material, foamed ceramics and the metal Material cladding on micron and two yardsticks of millimeter, there is very high compression strength and wearability, and foamed ceramics/metal bicontinuous phase compound material and high-toughness metal retrain the compound of frame, be the structure composite of bi-material on centimeter scale of simultaneously realizing when carrying out foamed ceramics and metal composite.The performance test results of properties of SiC foam ceramics/spheroidal graphite cast-iron/multiple dimensioned complex abrasion-proof steel that 16 manganese steel three-phases form is as follows:
Compression strength 620MPa, impact flexibility 71J/cm
2, anti-wear performance is 7 times of rich chromium cast iron, 30 times (Fig. 1 (b)) of potassium steel, demonstrates material high-wearing feature and the desirable advantage coordinated of high-strength tenacity of realizing.
Embodiment 9
Be the preparation of properties of SiC foam ceramics piece with the difference of embodiment 8.
According to patent: a kind of pair of yardstick silicon carbide foam ceramic material and preparation method thereof (200910248558.0) prepared the properties of SiC foam ceramics piece, and the properties of SiC foam ceramics piece is for removing the porous foam silicon carbide ceramics piece of remaining silicon through high-temperature process.In the present embodiment, foam silicon carbide ceramics has the three-dimensional networks structure, and volume fraction is: 50%, and the carborundum average grain size is at 50nm.Described foam silicon carbide ceramics be take polygonal closed-loop as elementary cell, and each elementary cell is interconnected to form three-dimensional networks.Have the mesh that the grade yardstick is interconnected on macroscopic view, the average-size of mesh is: 2.5mm; Ceramic skeleton muscle inside has the mesh that the micron order yardstick is interconnected, and the average-size of mesh is: 50 μ m.
In the present embodiment, properties of SiC foam ceramics/spheroidal graphite cast-iron/16 manganese steel three-phases have formed multiple dimensioned complex abrasion-proof steel, demonstrate the desirable advantage coordinated of material high-wearing feature and high-strength tenacity that realizes.
Embodiment 10
Be to adopt the method for negative pressure casting with the difference of embodiment 8.
The high-ductility steel constraint frame that at first will be inlaid with the properties of SiC foam ceramics piece is put into the batch-type furnace preheating, and preheat temperature is 850 ℃.Composite die is utilized acetylene flame or blowtorch etc. to be preheated to 200 ℃ simultaneously.
The vacuum of vacuum chamber is 2000Pa.
Then will put in composite die through the high-ductility steel constraint frame of preheating, utilize crucible that melting is poured in mould to relevant temperature cast iron liquid simultaneously, open butterfly valve and make the high-ductility steel constraint frame that is inlaid with the properties of SiC foam ceramics piece form rapidly vacuum, utilize atmospheric pressure that iron liquid or molten steel are pressed onto in the foamed ceramics mesh.
In the present embodiment, properties of SiC foam ceramics/spheroidal graphite cast-iron/16 manganese steel three-phases have formed multiple dimensioned complex abrasion-proof steel, demonstrate the desirable advantage coordinated of material high-wearing feature and high-strength tenacity that realizes.
Embodiment 11
Be the selection of foamed ceramics piece with the difference of embodiment 8.The foamed ceramics piece is the foam glass ceramic block, and the preparation process of foam glass ceramic block is as follows:
The first step, the slip preparation
By weight percentage, after glass micro mist 45wt% (granularity is 10 μ m), stabilizing agent cerium oxide 2wt% (granularity is 5 μ m), sintering aid titanium oxide 2wt% (granularity is 5 μ m), solvent Ludox 51wt% are mixed, ball milling after mechanical agitation, filter, and obtains slip.
Second step, soak extension
The polyurethane foam is cut into to required form and size, immerse equably in slip, take out rear squeeze and remove unnecessary slip, adopt air-blowing or centrifugal mode to remove unnecessary slip, the heating semi-solid preparation, repeatedly, to reaching needed volume fraction 50%, obtain the foamed ceramics presoma.
Wherein, semi-solid preparation is heat cure at 100 ℃ of temperature, 10 minutes time.
The 3rd step, pyrolysis
By the pyrolysis under argon shield of foamed ceramics presoma, foam generated ceramic skeleton; Wherein, 1 ℃ per minute of heating rate, be warming up to 800 ℃, is incubated 0.5 hour.
The 4th step, sinter molding
In air atmosphere, to foamed ceramics skeleton sinter molding, heating rate is 5 ℃ per minute, and sintering temperature is 1500 ℃, and temperature retention time is 0.5 hour, obtains the foam glass ceramic material.
In the present embodiment, the foam glass ceramic material be take polygonal closed-loop as elementary cell, and each elementary cell is interconnected to form three-dimensional networks, and foam glass ceramic material volume integral number is: 50%.Have the mesh that the grade yardstick is interconnected on macroscopic view, the average-size of mesh is: 3.0mm; Ceramic skeleton muscle inside has the mesh that the micron order yardstick is interconnected, and the average-size of mesh is: 60 μ m.
Add the silicon carbide micro-powder that granularity is 20 μ m in foam glass ceramic material mesh, to add weight be foamed ceramics 30%, add method to be: ceramic powder is poured in the foamed ceramics mesh, method by mechanical oscillation is by ceramic powder jolt ramming, silicon carbide micro-powder is filled in the micrometer grade hole of foam glass ceramic material, with rigidity and the wearability that further improves composite abrasion resistance material.
In the present embodiment, foam glass pottery/spheroidal graphite cast-iron/16 manganese steel three-phases have formed multiple dimensioned composite abrasion resistance material, demonstrate the desirable advantage coordinated of material high-wearing feature and high-strength tenacity that realizes.
Embodiment 12
Be the selection of high-toughness metal constraint frame and the selection of compound tense metal bath with the difference of embodiment 8.
Adopt casting method, cast out ZL301 aluminium constraint frame, be of a size of above constraint frame bottom surface has
below be of a size of
reverse taper holes, surface uniform 15 * 15 * 10mm that distributes
3square hole, middle horizontal bar width is 2mm.Then utilize the method for sandblast, will retrain the processing of frame rough inner surface.The casting metal melt is the ZL101 Birmasil, and pouring temperature is 670 ℃.
In the present embodiment, properties of SiC foam ceramics/spheroidal graphite cast-iron/ZL301 aluminium three-phase has formed multiple dimensioned composite abrasion resistance material, demonstrates the desirable advantage coordinated of material high-wearing feature and high-strength tenacity that realizes.
Embodiment 13
Be the selection of the metal bath of extrusion casint with the difference of embodiment 8.
The metal bath of extrusion casint is selected cast stainless steel 1Cr18Ni9Ti, and smelting temperature is 1520 ℃, in fusion process, logical as the protection of Ar gas, in case the alloying element oxidation ablation.
In the present embodiment, properties of SiC foam ceramics/stainless steel 1Cr18Ni9Ti/16 manganese steel three-phase has formed multiple dimensioned complex abrasion-proof steel, demonstrates the desirable advantage coordinated of material high-wearing feature and high-strength tenacity that realizes.
The embodiment result shows, the heavy constructions such as Multi-scale ceramic/metal composite abrasion-resistant material of the present invention can be widely used in pulverizing, excavate, transport equipment, there are the characteristics such as anti-wear performance is good, cost is low, easy to use, service life and the production efficiency of the heavy construction equipment such as can increase substantially pulverizing, excavate, transport, can produce good Social benefit and economic benefit.
Claims (7)
1. the preparation method of a Multi-scale ceramic/metal composite abrasion-resistant material, it is characterized in that: take foamed ceramics/metal bicontinuous phase compound material as wear-resisting primitive, take high-toughness metal as the constraint framework, foamed ceramics/metal bicontinuous phase compound material and high-toughness metal are combined into high-abrasive material by casting method;
Foamed ceramics/metal bicontinuous phase compound material is foamed ceramics and the Material cladding of metal on micron and two yardsticks of millimeter, foamed ceramics/metal bicontinuous phase compound material and high-toughness metal retrain the compound of frame, are the wear-resisting primitives and the structure composite of constraint framework bi-material on centimeter scale of simultaneously realizing when carrying out foamed ceramics and metal composite;
Perhaps; foamed ceramics/metal bicontinuous phase compound material is foamed ceramics and the Material cladding of metal on mm-scale; foamed ceramics/metal bicontinuous phase compound material and high-toughness metal retrain the compound of frame, are the wear-resisting primitives and the structure composite of constraint framework bi-material on centimeter scale of simultaneously realizing when carrying out foamed ceramics and metal composite;
Foamed ceramics is mounted in high-toughness metal constraint frame, utilize normal pressure casting, extrusion casint, vacuum pressing and casting or negative pressure suction casting method, the metal of melting is entered in the three-dimensional communication mesh of foamed ceramics, when realizing foamed ceramics and the metal Material cladding on micron and two yardsticks of millimeter, wear-resisting primitive and constraint framework are compound centimeter scale, when perhaps realizing foamed ceramics and the metal Material cladding on mm-scale, wear-resisting primitive and constraint framework are compound centimeter scale.
2. press the preparation method of Multi-scale ceramic/metal composite abrasion-resistant material claimed in claim 1, it is characterized in that: described foamed ceramics is foam silicon carbon, foam silicon nitride, foamed alumina, foam zirconia or foam glass, the average-size of mesh is: 0.5mm-5mm, the volume fraction of foamed ceramics is: 5%-70%, and average grain size is at 10nm-300 μ m; Foamed ceramics is foamed ceramics skeleton fine and close or porous.
3. by the preparation method of Multi-scale ceramic/metal composite abrasion-resistant material claimed in claim 1, it is characterized in that: the metal of described melting is cast iron, cast steel, copper alloy, aluminium alloy or cast magnesium alloy.
4. press the preparation method of Multi-scale ceramic/metal composite abrasion-resistant material claimed in claim 3, it is characterized in that: cast iron is spheroidal graphite cast-iron or gray iron, cast steel is casting carbon steel or cast alloy steel, copper alloy is cast tin bronze, aluminium bronze or Allen's metal, and aluminium alloy is alusil alloy, aluminium copper, almag or alumin(i)um zinc alloy.
5. press the preparation method of Multi-scale ceramic/metal composite abrasion-resistant material claimed in claim 1, it is characterized in that: high-toughness metal constraint frame is single hole or loose structure, hole shape is square, circular, hexagon or other polygon, and high-toughness metal constraint frame is through hole or half through hole; For half through hole, there are one or several back taper aperture in the bottom surface, hole; Constraint frame wall thickness or the thick 1/100-1/2 that is designed to as required the foamed ceramics maximum transverse size of hole wall; The material of constraint frame is steel, copper alloy or aluminium alloy; The constraint frame adopts hot investment casting, area of computer aided rapid shaping and machine-tooled method to obtain.
6. by the preparation method of Multi-scale ceramic/metal composite abrasion-resistant material claimed in claim 5, it is characterized in that: the steel framework material is 16Mn steel, 20# steel, 35# steel, 45# steel or other structural steel; Copper alloy frame material is tin bronze, aluminium bronze or Allen's metal; The aluminum alloy frame material is alusil alloy, aluminium copper or almag.
7. by the preparation method of Multi-scale ceramic/metal composite abrasion-resistant material claimed in claim 1, it is characterized in that: dose ceramic powder in the foamed ceramics mesh, ceramic powder is SiC, SiO
2or Al
2o
3, granularity is: 200nm-1mm, the 0wt%-50wt% that addition is foamed ceramics weight adds method to be: ceramic powder is poured in the foamed ceramics mesh, and the method by mechanical oscillation is by ceramic powder jolt ramming.
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TWI586461B (en) * | 2012-08-29 | 2017-06-11 | Ngk Spark Plug Co | An alumina sintered body and a method for producing the same |
CN103710562B (en) * | 2013-12-23 | 2015-09-30 | 上海应用技术学院 | The preparation method of a kind of porous ceramics/metal bicontinuous phase compound material |
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