CN106521219A - Preparation method for TiC particle reinforced titanium-based porous material - Google Patents

Preparation method for TiC particle reinforced titanium-based porous material Download PDF

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CN106521219A
CN106521219A CN201710008243.3A CN201710008243A CN106521219A CN 106521219 A CN106521219 A CN 106521219A CN 201710008243 A CN201710008243 A CN 201710008243A CN 106521219 A CN106521219 A CN 106521219A
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tic
preparation
powder
based porous
titanium
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CN106521219B (en
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邱贵宝
卢腾飞
王健
廖益龙
邱淑兴
吕学伟
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Chongqing University
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Chongqing University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/11Making porous workpieces or articles
    • B22F3/1121Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
    • B22F3/1134Inorganic fillers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1017Multiple heating or additional steps
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C14/00Alloys based on titanium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps

Abstract

The invention discloses a preparation method for a TiC particle reinforced titanium-based porous material. The powder metallurgy pore-forming technology is adopted for the preparation method, after TiC powder and titanium powder which are in a certain proportion are used and mixed to be subjected to ball-milling pretreatment under argon gas protection, the TiC powder and the titanium powder, and urea and zinc stearate are subjected to the steps of burden mixing, pressing forming and step-by-step type heat treatment to prepare the titanium-based porous material; the granular urea in the needle-shaped state is preferentially used to serve as a pore-forming agent; and the zinc stearate is adopted as a binding agent, the structure and the components of the titanium-based porous material are made to be easy to control, the raw materials are easy to obtain and low in price, and the preparation period can be shortened and the time cost, the energy consumption, the using loss of equipment and the like can be reduced due to the step-by-step type heat treatment manner. In addition, the characteristics that TiC particles are small in density, high in elastic modulus, high in thermal expansion coefficient, high in abrasion resistant performance, corrosion resistant performance and the like are fully utilized by the preparation method, so that the prepared titanium-based porous material has excellent comprehensive mechanical performance and corrosion resistant performance and has very good application prospect.

Description

A kind of preparation method of TiC granule intensified titaniums based porous materials
Technical field
The present invention relates to foam metal material technical field, more particularly to a kind of TiC granule intensified titaniums based porous materials Preparation method.
Background technology
As a kind of new composite, porous metal material has the advantages that other porous materials are incomparable.Phase Compared with solid material, certain porosity makes it have good compressibility;Compared to foamed polymer, with higher firm Spend and use temperature;Compared to foamed ceramics, with good toughness, heat conductivity, electric conductivity etc..So porous material metal material Material has broad prospects in fields such as auto industry, Aero-Space, field of environment protection, buildings, and on the other hand, the presence of hole makes The yield stress of porous metal material is obtained, the mechanical property such as creep resisting ability and wearability has larger reduction, so improving many The mechanical property of mesoporous metal enjoys the concern of people always.
Titanium or titanium alloy, due to having the advantages that a series of protrusions such as specific strength height, the good, high temperature resistant of corrosion resistance, is a kind of Prepare the excellent matrix of porous metal material.Porous titanium matrix composite is in Titanium base, add the second phase fiber or granule to make To strengthen phase, the biphase composite of titanium and reinforcement is constituted.The introducing for strengthening phase causes the intensity of material, Gao Gang, toughness, resistance to Mill property and the performance such as resisting fatigue increase, and can improve the high temperature resistance of material, the performance such as anticorrosive, greatly extend material Use range.
Early stage is applied to the titanium matrix composite of aerospace industry based on continuous fiber reinforcing titanium matrix composite.It is main The fiber reinforcement wanted mutually has SiC, B, C, Al2O3Fiber etc..It is first-selected in titanium matrix composite of the exploitation with excellent high performance Increasing be mutually SiC fibers.But the preparation method of fibre-reinforced composite is relatively difficult, according to the literature, can only be with admittedly Phase method synthesizes, then with the method molding such as high temperature insostatic pressing (HIP), vacuum hotpressing, forging.It is simultaneously continuous strengthen titanium matrix composite respectively to The opposite sex is stronger.Use range has certain limitation, and complex manufacturing, relatively costly into producing.Therefore discontinuous increasing Strong composite has obtained quick development, is primarily due to a great selection of cheap enhancing phase selected, such as granule, whisker, short fibre Dimension etc., and can free design structure and the features such as composition so that the exploitation of solid metal composite and in producing increasingly Standardization.
Although it should be noted that discontinuous reinforcement body has obtained extensive utilization, Zhu etc. in titanio densification composite People adopts slurry foaming, by the cerium oxide for adding different content in titanium valve, prepares the POROUS TITANIUM of high porosity and grinds Its mechanical property is studied carefully;Xiao etc. are prepared for TiB and Nd by smelting process2O3Enhanced titanium matrix composite, wherein Nd2O3Shape Looks are more complicated, and skewness, have tiny lamellar, lath-shaped and spherical.Preparation process of all and Xiao et al. in composite In be all doped with rare earth oxide, technique is complex, high energy consumption, cost intensive, and structure is wayward with composition.
But in the preparation process of POROUS TITANIUM, it is contemplated that the isotropism of discontinuous reinforcements and porous material with hole wall or Loading characteristic of the hole rib as skeleton, introduces TiC reinforcements and develops and prepare the composite porous related manufacturing processes of titanio It is also less, lack a large amount of systematic researches, be especially a lack of the research to its dynamic mechanical property and characteristic.
The content of the invention
For above-mentioned deficiency present in prior art, it is an object of the invention to provide a kind of TiC granule intensified titanium-bases The preparation method of porous material, to solve the porous titanium material resistance to compression obtained by the POROUS TITANIUM preparation technology of prior art Differ from, corrosion resistance is poor, anti-wear performance is poor, the problem that complex process, high energy consumption, structure and composition hardly possible are controlled.
For achieving the above object, present invention employs following technical scheme:
A kind of preparation method of TiC granule intensified titaniums based porous materials comprises the steps:
1)The titanium valve of the TiC powder and 98 ~ 99.5 weight portions of 0.5 ~ 2 weight portion is weighed, it is 100 weight portions to constitute total weight parts TiC and Ti mixed-powders, load in advance with alcohol washes and in dried high-energy ball milling tank, and ratio of grinding media to material is 10 ~ 20:1;
2)The high-energy ball milling tank good seal of TiC and Ti mixed-powders is will be equipped with, with argon cleaning high-energy ball milling tank body 3 times discharging Air in tank body, then argon is filled with tank body as protective gas;
3)It is filled with tank body after argon, step multiple ball milling is carried out to TiC the and Ti mixed-powders in high-energy ball milling tank Process, each Ball-milling Time is 20 ~ 50min, intermittent time of adjacent ball milling twice is 10 ~ 40min, total effective Ball-milling Time For 1 ~ 4 hour, the prefabricated mixed powders of TiC and Ti after ball-milling treatment, are obtained;
4)The prefabricated mixed powder of TiC and Ti of 100 weight portion obtained above is mixed in grinding body with the carbamide of same volume, Add account for the prefabricated mixed powders of TiC and Ti and carbamide gross mass 0.25% ~ 0.5% zinc stearate in mixed process, then at the uniform velocity 30 ~ 60min of mixing, is obtained mixed material;
5)With steel die by mixed material cold moudling obtained in previous step, unidirectional to suppress, pressing pressure is 180 ~ 250MPa, Dwell time is 45 ~ 60s, and the demoulding afterwards is obtained gives birth to pressed compact;
6)Raw pressed compact is placed in vacuum carbon tube furnace carries out heat treatment, and heat treatment process is divided into low temperature removing carbamide and high temperature sintering Two steps are carried out;In low temperature removing urea process, it is 1 × 10 to control vacuum in vacuum carbon tube furnace-1~1×10-2Pa, control heat up Speed is sintered to 400 DEG C from room temperature for 2 ~ 5 DEG C/min, and 45 ~ 60min is incubated at 400 DEG C;Burn subsequently into high temperature Knot process, temperature are increased to 1180 ~ 1250 DEG C, are 1 × 10 in vacuum-1~1×10-22h is sintered under Pa environment;Sintering is completed Afterwards, furnace cooling takes out to after room temperature and obtains the enhanced titanio porous material of TiC granules.
In the preparation method of above-mentioned TiC granule intensified titanium based porous materials, preferably, the step 1)In, The purity of TiC powder is >=99.8%, and the purity of titanium valve is >=99.8%.
In the preparation method of above-mentioned TiC granule intensified titanium based porous materials, preferably, the step 1)In, The granularity of TiC powder is 2 ~ 10 μm, and the granularity of titanium valve is 38 ~ 48 μm.
In the preparation method of above-mentioned TiC granule intensified titanium based porous materials, preferably, the step 1)In, The ratio of weight and number of TiC powder and titanium valve is preferably 1.5:98.5.
In the preparation method of above-mentioned TiC granule intensified titanium based porous materials, preferably, the step 2)In, The purity of argon being filled with tank body is more than 99.99%.
In the preparation method of above-mentioned TiC granule intensified titanium based porous materials, preferably, the step 3)In, The drum's speed of rotation for carrying out ball milling is 200 ~ 400r/min.
In the preparation method of above-mentioned TiC granule intensified titanium based porous materials, preferably, the step 4)In, For >=99%, the purity of zinc stearate is >=99% to the purity of the carbamide for being adopted.
In the preparation method of above-mentioned TiC granule intensified titanium based porous materials, preferably, the step 4)In, The carbamide for being adopted is acicular morphology granule, and granularity is 0.8 ~ 1.1mm;The granularity of zinc stearate is 25 μm.
Compared to prior art, the present invention has the advantages that:
1st, the preparation method of TiC granule intensified titaniums based porous materials of the present invention, prepares POROUS TITANIUM using powder metallurgy boring technique Based composites, by operations such as ball milling pretreatment, dispensing mixing, compressing, multiple step format heat treatments, TiC granules are used as increasing In Titanium base, in the sintering neck length megastage, TiC fine particles can promote to form non-strong body phase Dispersed precipitate as nucleating agent Homogeneous nucleation carrys out crystal grain thinning, while hindering the coarsening rate of the growth reduction crystal grain of crystal boundary;With above-mentioned easy preparation side Method has been prepared lightweight and has had the composite porous of higher-strength so as to can use as lightweight structural material;Hole is special Levying can make which as materials'uses such as medical science bone alternate material, fluid separating and filtering, fluid distrbution, energy-absorbing dampings;Greatly expand POROUS TITANIUM is opened up and has used field, the reinforcing for porous titanium base material has provided a new effective approach.
2nd, in the preparation method of the TiC granule intensified titanium based porous materials being related in the present invention, ball milling has been carried out to powder Pretreatment, in mechanical milling process, mixed-powder and stainless steel ball continuous impact friction mutually, shock in stainless cylinder of steel, reaches broken With the effect of crystal grain refinement, be conducive to improving the surface energy of powder, while powder have accumulated substantial amounts of lattice in shattering process Defect, such as room, distortion, dislocation etc.;These characteristics both contribute to improve sintering quality, so as to improve gained titanio porous material Mechanical property.
3rd, in the preparation method of the TiC granule intensified titanium based porous materials being related in the present invention, using acicular morphology granule And highly purified carbamide is less than traditional circular carbamide as pore creating material, its surface area and anti-extrusion ability, reduces pore creating material Frictional force with powder in pressing process, the yielding feature of stress increased mobility of the powder in pressing process, make Pressed compact stress must be given birth to and be more uniformly distributed more easy-formation, experiment shows to be more easy to obtain intercommunicating pore structure using needle-like Liao Su;Using Hard Fat Sour zinc can promote molding, the demoulding of raw pressed compact, it is to avoid produce transverse surface cracks during demoulding, improve as binding agent The pick-up rate of raw pressed compact;And the carbamide as pore creating material and the zinc stearate as binding agent are easily removed under high temperature, removing During will not introduce impurity, be conducive to keeping the cleanliness of gained titanio porous material product, and carbamide and zinc stearate Catabolite will not produce pollution environment material.
4th, in the preparation method of TiC granule intensified titanium based porous materials being related in the present invention, using two sections of vacuum not between Disconnected mode opposite pressed compact carries out heat treatment, is divided into low temperature removing two step of carbamide and high-temperature sintering process;Low temperature removes carbamide and hard During fat acid zinc, vacuum environment can will be decomposed generation gas in time and be extracted body of heater out;High-temperature vacuum sintering stage vacuum be 1 × 10-1~1×10-2Sinter under Pa environment, it is ensured that sample is not oxidized;The advantage of this preparation method is that production is with continuous Property, the cycle for obtaining finished products is shortened, energy consumption is reduced, and then is reduced production cost.
Description of the drawings
Fig. 1 is the process chart of TiC granule intensified titaniums based porous materials preparation method of the present invention.
Differential thermal analysis curve figures of the Fig. 2 for carbamide.
Fig. 3 is macro morphology scanning electron microscope (SEM) photograph after TiC in the embodiment of the present invention 1 and Ti powder mixing and ball millings.
Fig. 4 is the physical form figure of gained titanio porous material in the embodiment of the present invention 4.
Fig. 5 is the pore structure scanning electron microscope (SEM) photograph of gained titanio porous material in the embodiment of the present invention 4.
Fig. 6 is the compressive stress strain curve figure of gained titanio porous material in the embodiment of the present invention 4.
Specific embodiment
Be directed to that porous titanium material resistance to compression obtained by the POROUS TITANIUM preparation technology of prior art is poor, corrosion resistance is poor, Anti-wear performance is poor, the problem that complex process, high energy consumption, structure and composition hardly possible are controlled, the invention provides a kind of TiC granule intensified titaniums The preparation method of based porous materials, its method flow is as shown in figure 1, comprise the steps:
1)Raw material is chosen:The titanium valve of the TiC powder and 98 ~ 99.5 weight portions of 0.5 ~ 2 weight portion is weighed, it is 100 to constitute total weight parts TiC the and Ti mixed-powders of weight portion, load in advance with alcohol washes and in dried high-energy ball milling tank, ratio of grinding media to material is 10 ~ 20:1.
Here, in order to ensure prepare TiC granule intensified titanium based porous materials purity and performance, the TiC powder in raw material Purity preferably >=99.8%, the purity preferably >=99.8% of titanium valve.Also, TiC powder preferably selects 2 ~ 10 μm of granularities, so as to Ensure which as the dimensional requirement for strengthening phase, it is meticulous to be susceptible to agglomeration so that prefabricated TiC and Ti blending constituents are uneven It is even;Can slightly make very much reinforced effects not good simultaneously, or even reduce mechanical property of product etc..And the granularity of titanium valve chooses preferably 38 ~ 48 μm, titanium has a great impact to the mobility during powder pressure-like as material matrix, its granule size, Jing test inspections Survey, this particle size range is optimum range.
2)Ball milling prepares:The high-energy ball milling tank good seal of TiC and Ti mixed-powders is will be equipped with, argon cleaning high-energy ball milling is used Tank body 3 times is discharging the air in tank body, then argon is filled with tank body as protective gas.
Using argon cleaning high-energy ball milling tank body 3 times, it is ensured that the discharge that air goes out in tank body, then again in tank body Argon is filled with as protective gas so that mechanical milling process is carried out under an argon atmosphere, can effectively prevent nitride and oxide Formation and oxygen atom solid solution, keep material cleanliness.The purity of argon adopted by this preferably more than 99.99%, keeps away Exempt to introduce impurity, with the cleanliness that material is kept in mechanical milling process preferably.
3)Ball milling pretreatment:It is filled with tank body after argon, TiC the and Ti mixed-powders in high-energy ball milling tank is entered in the ranks The multiple ball-milling treatment of formula of having a rest, each Ball-milling Time are 20 ~ 50min, and the intermittent time of adjacent ball milling twice is 10 ~ 40min, always Effective Ball-milling Time be 1 ~ 4 hour, the prefabricated mixed powders of TiC and Ti are obtained after ball-milling treatment.
In the step, high-energy ball milling cause mixed-powder and stainless steel ball in the stainless cylinder of steel constantly mutually impact friction, Clash into, reach the effect of broken and crystal grain refinement, be conducive to improving the surface energy of powder, while the powder accumulation in shattering process Substantial amounts of lattice defect, such as room, distortion, dislocation etc.;These characteristics both contribute to improve sintering quality, so as to improve gained The mechanical property of titanio porous material.Wherein, the drum's speed of rotation for carrying out ball milling is preferably 200 ~ 400r/min.
4)Dispensing mixes:Carbamide of the prefabricated mixed powder of TiC and Ti of 100 weight portion obtained above with same volume is existed In grinding body mix, in mixed process add account for the prefabricated mixed powders of TiC and Ti with the 0.25% ~ 0.5% of carbamide gross mass it is hard Fat acid zinc, then at the uniform velocity mix 30 ~ 60min, mixed material is obtained.
Here the carbamide for adding is that, used as pore creating material, carbamide preferably adopts acicular morphology granule, its surface area and anti-extrusion Ability is less than traditional circular carbamide, can reduce pore creating material and frictional force of the powder in pressing process so that raw pressed compact is received Power is more uniformly distributed, more easy-formation;Zinc stearate is molding, the demoulding that can promote raw pressed compact as binding agent, it is to avoid in compacting and Surface transversal crack is produced in knockout course.For the selection of urea size scope, it is due in foamed materialss mesoporous character There is conclusive impact on material property, the wherein granularity of carbamide is preferably 0.8 ~ 1.1mm, contributes to sintering finished hole Gap structure is uniform, reduces the frictional force in pressing process, so as to reduce internal flaw.The granularity of zinc stearate is 25 μm, because After ball milling, the granularity of the prefabricated mixed powders of gained TiC and Ti is further refined, and close to 25 μm, therefore is 25 μm from granularity Zinc stearate, the granularity for reducing the prefabricated mixed powders of TiC and Ti and zinc stearate is poor, enhances the prefabricated mixing of TiC and Ti Powder body and the phase separation of zinc stearate, contribute to molding.And blending process at the uniform velocity mixes 30min, it is ensured that mixed material Equal property.Additionally, in order that the follow-up heat treatment pore-creating of the carbamide as pore creating material and the zinc stearate as binding agent In journey easily removing and do not introduce impurity, the purity preferably >=99% of the carbamide for being adopted, the purity of zinc stearate preferably >= 99%。
5)It is compressing:It is with steel die by mixed material cold moudling obtained in previous step, unidirectional to suppress, pressing pressure For 180 ~ 250MPa, the dwell time is 45 ~ 60s, and the demoulding afterwards is obtained gives birth to pressed compact.
During compressing, pressurize is conducive to effective transmission of pressure so that raw pressed compact more densification, increases life The intensity of pressed compact, it is to avoid the generation of arch bridge effect between granule.
6)Multiple step format heat treatment:Raw pressed compact is placed in vacuum carbon tube furnace carries out heat treatment, and heat treatment process is divided into low temperature Removing carbamide and two step of high temperature sintering are carried out;In low temperature removing urea process, it is 1 × 10 to control vacuum in vacuum carbon tube furnace-1~ 1×10-2Pa, controls heating rate and is sintered to 400 DEG C from room temperature for 2 ~ 5 DEG C/min, at 400 DEG C insulation 45 ~ 60min;Subsequently into high-temperature sintering process, temperature is increased to 1180 ~ 1250 DEG C, is 1 × 10 in vacuum-1~1×10-2Pa rings 2h is sintered under border;After the completion of sintering, take out after furnace cooling to room temperature and obtain the enhanced titanio porous material of TiC granules.
The heat treatment of opposite pressed compact of the present invention has been divided into low temperature removing carbamide and two step of high temperature sintering to be carried out.Fig. 2 shows The differential thermal analysis curve figure of carbamide, as shown in Figure 2, when temperature is 400 DEG C, carbamide decomposes substantially and finishes, therefore low temperature is taken off Except the sintering temperature of urea process is determined at 400 DEG C;And in cryogenic vacuum sintering stage, heating rate is preferably relatively slow, control rises Warm speed is optimal in 2 ~ 5 DEG C/min, causes to cave in avoid carbamide from decomposing the too fast raw pressed compact expansion of release;In cryogenic vacuum In sintering process, it is 1 × 10 to control vacuum in vacuum carbon tube furnace-1~1×10-2Pa, purpose is in order that what pore creating material decomposed Gas is extracted into outside body of heater rapidly, it is to avoid pollution sample, 45 ~ 60min is incubated at 400 DEG C, it is therefore an objective to guarantee that carbamide is completely out. In high-temperature sintering process, in the sintering neck length megastage, TiC fine particles can promote to form heterogeneous nucleation as nucleating agent Crystal grain thinning, while hindering the coarsening rate of the growth reduction crystal grain of crystal boundary, in porous titanium matrix composite, crystal grain thinning can Effectively to improve the intensity of material, this is that other intensifying methods can not be compared, under identical external force, in small grains Strain relatively small near portion and crystal boundary, deformation is uniform, and comparatively, stress is concentrated and causes the chance of cracking also less, is made Obtain gained titanio porous material and larger deformation can be born before cracking;On the other hand, as the purer titanium of TiC density is low, For 4.99g.cm-3, contribute to the lighting of titanio porous material, improve its specific strength;Additionally, the elastic modelling quantity of industrially pure titanium is The elastic modelling quantity of 110GPa, TiC is 460GPa, and during material stress and deformation, TiC can bear higher load, to hinder Hinder the extension of crackle or change its extension approach, strengthen cracks can spread energy, so as to improve the intensity and toughness of titanio porous material, The comprehensive mechanical property of TiC granule intensified titanium based porous materials obtained by being lifted.
Below with embodiment further illustrating the inventive method.It should be understood that these embodiments are only used In further illustrating embodiment of the present invention, rather than for limiting the present invention.
Embodiment 1:
The present embodiment from purity is >=99.8%, granularity be 2 ~ 10 μm of TiC powder, and purity is that >=99.8%, granularity is 38 ~ 48 μm of titanium valve, prepares TiC granule intensified titanium based porous materials using the inventive method, and step is as follows:
(1)Raw material ball milling pretreatment:
The titanium valve of the TiC powder and 99.5 weight portions of 0.5 weight portion is weighed, the TiC and Ti mixing that gross weight is 100 weight portions is constituted Powder, loads in advance with alcohol washes and in dried high-energy ball milling tank, and ratio of grinding media to material is 10:1, will be equipped with TiC and Ti mixing The high-energy ball milling tank good seal of powder, with argon cleaning tank body 3 times to discharge the air in tank body, backward tank body in be filled with it is pure The argon for more than 99.99% is spent, step multiple ball milling is carried out to TiC the and Ti mixed-powders in high-energy ball milling tank then Process, this example drum's speed of rotation is 200r/min, and each Ball-milling Time is 20min, per interval time of adjacent ball milling is twice 10min, effective ball milling total time are 1h, then stop ball milling, obtain the prefabricated mixed powders of TiC and Ti.Fig. 3 shows this enforcement Macro morphology scanning electron microscope (SEM) photograph after TiC and Ti powder mixing and ball millings in example, it can be seen that, although effectively Ball-milling Time is only 1h, But can be seen that the powder of the prefabricated mixed powders of gained TiC and Ti has obvious fine-characterization.Then, ball grinder is placed in into vacuum In glove box, prefabricated powder body is taken out from ball grinder, to avoid the prefabricated mixed powders of TiC and Ti from being oxidized.
(2)Dispensing mixes:
The prefabricated mixed powder of 100 weight portion TiC and Ti obtained above is being ground with its volume identical acicular morphology granular urea Mix in body, and addition accounts for the prefabricated mixed powders of TiC and Ti and the 0.25% of carbamide gross mass zinc stearate, at the uniform velocity mixes 30min, obtains mixed material.In the present embodiment, the purity of carbamide used is that >=99%, granularity is 0.8 ~ 1.1mm, zinc stearate Purity be >=99%, granularity be 25 μm.
(3)It is compressing:
Will be the mixed material obtained by back compressing with steel die, unidirectional to suppress, pressing pressure is 180MPa, during pressurize Between be 60s, the demoulding obtains giving birth to pressed compact.
(4)Multiple step format heat treatment:
Raw pressed compact is put in vacuum carbon tube furnace carries out heat treatment, and processing procedure is divided into cryogenic vacuum removing carbamide and high temperature sintering Two steps are carried out.Cryogenic vacuum removes the carbamide stage, and it is 1 × 10 to control vacuum in vacuum carbon tube furnace-1~1×10-2Pa, control rise Warm speed is sintered to 400 DEG C from room temperature for 2 DEG C/min, is incubated 45min at 400 DEG C;Subsequently into high-temperature solid Sintering process, temperature are increased to 1180 DEG C, are 1 × 10 in vacuum-1~1×10-22h is sintered under Pa environment.After the completion of sintering, Furnace cooling takes out to after room temperature and obtains the enhanced titanio porous material of TiC granules.
TiC contents manufactured in the present embodiment are the porous titanium matrix composite of 0.5 weight portion, and its strong stress of surrender is 133.53 Mpa。
Embodiment 2:
The present embodiment from purity is >=99.8%, granularity be 2 ~ 10 μm of TiC powder, and purity is that >=99.8%, granularity is 38 ~ 48 μm of titanium valve, prepares TiC granule intensified titanium based porous materials using the inventive method, and step is as follows:
(1)Raw material ball milling pretreatment:
The titanium valve of the TiC powder and 99 weight portions of 1 weight portion is weighed, TiC the and Ti mixed powders that gross weight is 100 weight portions are constituted End, loads in advance with alcohol washes and in dried high-energy ball milling tank, and ratio of grinding media to material is 10:1, will be equipped with TiC and Ti mixed powders The high-energy ball milling tank good seal at end, with argon cleaning tank body 3 times to discharge the air in tank body, backward tank body in be filled with purity For more than 99.99% argon, then the TiC and Ti mixed-powders in high-energy ball milling tank are carried out at step multiple ball milling Reason, this example drum's speed of rotation are 200r/min, and each Ball-milling Time is 20min, per interval time of adjacent ball milling is twice 10min, effective ball milling total time are 1h, then stop ball milling, obtain the prefabricated mixed powders of TiC and Ti.Then, ball grinder is put In vacuum glove box, prefabricated powder body is taken out from ball grinder, to avoid the prefabricated mixed powders of TiC and Ti from being oxidized.
(2)Dispensing mixes:
The prefabricated mixed powder of 100 weight portion TiC and Ti obtained above is being ground with its volume identical acicular morphology granular urea Mix in body, and addition accounts for the prefabricated mixed powders of TiC and Ti and the 0.25% of carbamide gross mass zinc stearate, at the uniform velocity mixes 30min, obtains mixed material.In the present embodiment, the purity of carbamide used is that >=99%, granularity is 0.8 ~ 1.1mm, zinc stearate Purity be >=99%, granularity be 25 μm.
(3)It is compressing:
Will be the mixed material obtained by back compressing with steel die, unidirectional to suppress, pressing pressure is 180MPa, during pressurize Between be 60s, the demoulding obtains giving birth to pressed compact.
(4)Multiple step format heat treatment:
Raw pressed compact is put in vacuum carbon tube furnace carries out heat treatment, and processing procedure is divided into cryogenic vacuum removing carbamide and high temperature sintering Two steps are carried out.Cryogenic vacuum removes the carbamide stage, and it is 1 × 10 to control vacuum in vacuum carbon tube furnace-1~1×10-2Pa, control rise Warm speed is sintered to 400 DEG C from room temperature for 2 DEG C/min, is incubated 45min at 400 DEG C;Subsequently into high-temperature solid Sintering process, temperature are increased to 1180 DEG C, are 1 × 10 in vacuum-1~1×10-22h is sintered under Pa environment.After the completion of sintering, Furnace cooling takes out to after room temperature and obtains the enhanced titanio porous material of TiC granules.
The present embodiment embodiment compared with, ball milling parameter, zinc stearate addition, heat treatment process all same.This reality The TiC contents for applying example preparation are the titanio porous material of 1 weight portion, and its yield stress is 152.42Mpa.It is possible thereby to can see Go out, the increase of TiC granules can effectively improve yield strength.
Embodiment 3:
The present embodiment from purity is >=99.8%, granularity be 2 ~ 10 μm of TiC powder, and purity is that >=99.8%, granularity is 38 ~ 48 μm of titanium valve, prepares TiC granule intensified titanium based porous materials using the inventive method, and step is as follows:
(1)Raw material ball milling pretreatment:
The titanium valve of the TiC powder and 99 weight portions of 1 weight portion is weighed, TiC the and Ti mixed powders that gross weight is 100 weight portions are constituted End, loads in advance with alcohol washes and in dried high-energy ball milling tank, and ratio of grinding media to material is 15:1, will be equipped with TiC and Ti mixed powders The high-energy ball milling tank good seal at end, with argon cleaning tank body 3 times to discharge the air in tank body, backward tank body in be filled with purity For more than 99.99% argon, then the TiC and Ti mixed-powders in high-energy ball milling tank are carried out at step multiple ball milling Reason, this example drum's speed of rotation are 300r/min, and each Ball-milling Time is 30min, per interval time of adjacent ball milling is twice 20min, effective ball milling total time are 3h, then stop ball milling, obtain the prefabricated mixed powders of TiC and Ti.Then, ball grinder is put In vacuum glove box, prefabricated powder body is taken out from ball grinder, to avoid the prefabricated mixed powders of TiC and Ti from being oxidized.
(2)Dispensing mixes:
The prefabricated mixed powder of 100 weight portion TiC and Ti obtained above is being ground with its volume identical acicular morphology granular urea Mix in body, and addition accounts for the prefabricated mixed powders of TiC and Ti and the 0.4% of carbamide gross mass zinc stearate, at the uniform velocity mixes 45min, obtains mixed material.In the present embodiment, the purity of carbamide used is that >=99%, granularity is 0.8 ~ 1.1mm, zinc stearate Purity be >=99%, granularity be 25 μm.
(3)It is compressing:
Will be the mixed material obtained by back compressing with steel die, unidirectional to suppress, pressing pressure is 200MPa, during pressurize Between be 50s, the demoulding obtains giving birth to pressed compact.
(4)Multiple step format heat treatment:
Raw pressed compact is put in vacuum carbon tube furnace carries out heat treatment, and processing procedure is divided into cryogenic vacuum removing carbamide and high temperature sintering Two steps are carried out.Cryogenic vacuum removes the carbamide stage, and it is 1 × 10 to control vacuum in vacuum carbon tube furnace-1~1×10-2Pa, control rise Warm speed is sintered to 400 DEG C from room temperature for 4 DEG C/min, is incubated 50min at 400 DEG C;Subsequently into high-temperature solid Sintering process, temperature are increased to 1250 DEG C, are 1 × 10 in vacuum-1~1×10-22h is sintered under Pa environment.After the completion of sintering, Furnace cooling takes out to after room temperature and obtains the enhanced titanio porous material of TiC granules.
The present embodiment embodiment 2 compared with, ball milling parameter increase, i.e. milling intensity increase so that manufactured in the present embodiment TiC contents are that the yield stress of the titanio porous material of 1 weight portion reaches 167.42Mpa.Therefore, appropriate increase ball milling is strong Degree, can help improve sintering quality, lift the mechanical property of prepared TiC granule intensified titanium based porous materials.
Embodiment 4:
The present embodiment from purity is >=99.8%, granularity be 2 ~ 10 μm of TiC powder, and purity is that >=99.8%, granularity is 38 ~ 48 μm of titanium valve, prepares TiC granule intensified titanium based porous materials using the inventive method, and step is as follows:
(1)Raw material ball milling pretreatment:
The titanium valve of the TiC powder and 98.5 weight portions of 1.5 weight portions is weighed, the TiC and Ti mixing that gross weight is 100 weight portions is constituted Powder, loads in advance with alcohol washes and in dried high-energy ball milling tank, and ratio of grinding media to material is 20:1, will be equipped with TiC and Ti mixing The high-energy ball milling tank good seal of powder, with argon cleaning tank body 3 times to discharge the air in tank body, backward tank body in be filled with it is pure The argon for more than 99.99% is spent, step multiple ball milling is carried out to TiC the and Ti mixed-powders in high-energy ball milling tank then Process, this example drum's speed of rotation is 400r/min, and each Ball-milling Time is 50min, per interval time of adjacent ball milling is twice 40min, effective ball milling total time are 4h, then stop ball milling, obtain the prefabricated mixed powders of TiC and Ti.Then, ball grinder is put In vacuum glove box, prefabricated powder body is taken out from ball grinder, to avoid the prefabricated mixed powders of TiC and Ti from being oxidized.
(2)Dispensing mixes:
The prefabricated mixed powder of 100 weight portion TiC and Ti obtained above is being ground with its volume identical acicular morphology granular urea Mix in body, and addition accounts for the prefabricated mixed powders of TiC and Ti and the 0.5% of carbamide gross mass zinc stearate, at the uniform velocity mixes 60min, obtains mixed material.In the present embodiment, the purity of carbamide used is that >=99%, granularity is 0.8 ~ 1.1mm, zinc stearate Purity be >=99%, granularity be 25 μm.
(3)It is compressing:
Will be the mixed material obtained by back compressing with steel die, unidirectional to suppress, pressing pressure is 250MPa, during pressurize Between be 45s, the demoulding obtains giving birth to pressed compact.
(4)Multiple step format heat treatment:
Raw pressed compact is put in vacuum carbon tube furnace carries out heat treatment, and processing procedure is divided into cryogenic vacuum removing carbamide and high temperature sintering Two steps are carried out.Cryogenic vacuum removes the carbamide stage, and it is 1 × 10 to control vacuum in vacuum carbon tube furnace-1~1×10-2Pa, control rise Warm speed is sintered to 400 DEG C from room temperature for 5 DEG C/min, is incubated 60min at 400 DEG C;Subsequently into high-temperature solid Sintering process, temperature are increased to 1200 DEG C, are 1 × 10 in vacuum-1~1×10-22h is sintered under Pa environment.After the completion of sintering, Furnace cooling takes out to after room temperature and obtains the enhanced titanio porous material of TiC granules.
Fig. 4, Fig. 5 are respectively the physical form figure and pore structure scanning electron microscope of the titanio porous material prepared by present case Figure, as seen from Figure 4, its complete appearance and have metallic luster, show its prepare link in maintain good cleanliness, from Fig. 5 can be seen that the macro morphology of hole and acicular morphology granular urea match, and even pore distribution has substantial amounts of connection Pore structure, no obvious internal flaw, better overall quality.Compression test is carried out to which, the compression stress-strain of gained is bent Line chart is as shown in Figure 6.Obtained by the present embodiment, the initial yield stress of TiC granule intensified titaniums based porous materials is as seen from Figure 6 233.24Mpa, yield stress are 186.59 Mpa, strain 16.72% or so when reach peak stress for 249.57 Mpa; And from fig. 6 it can be seen that starting compression stage, material is deformed into the linear elasticity stage;When external force continues to increase, enter Plastic period, part hole wall start to cave in, but stress has the trend for continuing to rise and reaches peak value, and this is due to TiC The presence of reinforcement so that the hole process of caving in becomes slow, and failure stress is improved, so as to increased the strong of material Degree.
Embodiment 5:
A kind of preparation method of TiC granule intensified titaniums based porous materials is present embodiments provided, its flow process is with reference to shown in Fig. 1, main Step is wanted to include as follows:
(1)Raw material ball milling pretreatment:
The titanium valve of the TiC powder and 98 weight portions of 2 weight portions is weighed, TiC the and Ti mixed powders that gross weight is 100 weight portions are constituted End, loads in advance with alcohol washes and in dried high-energy ball milling tank, and ratio of grinding media to material is 20:1, will be equipped with TiC and Ti mixed powders The high-energy ball milling tank good seal at end, with argon cleaning tank body 3 times to discharge the air in tank body, backward tank body in be filled with purity For more than 99.99% argon, then the TiC and Ti mixed-powders in high-energy ball milling tank are carried out at step multiple ball milling Reason, this example drum's speed of rotation are 400r/min, and each Ball-milling Time is 50min, per interval time of adjacent ball milling is twice 40min, effective ball milling total time are 4h, then stop ball milling, obtain the prefabricated mixed powders of TiC and Ti.Then, ball grinder is put In vacuum glove box, prefabricated powder body is taken out from ball grinder, to avoid the prefabricated mixed powders of TiC and Ti from being oxidized.
(2)Dispensing mixes:
The prefabricated mixed powder of 100 weight portion TiC and Ti obtained above is being ground with its volume identical acicular morphology granular urea Mix in body, and addition accounts for the prefabricated mixed powders of TiC and Ti and the 0.5% of carbamide gross mass zinc stearate, at the uniform velocity mixes 60min, obtains mixed material.In the present embodiment, the purity of carbamide used is that >=99%, granularity is 0.8 ~ 1.1mm, zinc stearate Purity be >=99%, granularity be 25 μm.
(3)It is compressing:
Will be the mixed material obtained by back compressing with steel die, unidirectional to suppress, pressing pressure is 250MPa, during pressurize Between be 45s, the demoulding obtains giving birth to pressed compact.
(4)Multiple step format heat treatment:
Raw pressed compact is put in vacuum carbon tube furnace carries out heat treatment, and processing procedure is divided into cryogenic vacuum removing carbamide and high temperature sintering Two steps are carried out.Cryogenic vacuum removes the carbamide stage, and it is 1 × 10 to control vacuum in vacuum carbon tube furnace-1~1×10-2Pa, control rise Warm speed is sintered to 400 DEG C from room temperature for 5 DEG C/min, is incubated 60min at 400 DEG C;Subsequently into high-temperature solid Sintering process, temperature are increased to 1200 DEG C, are 1 × 10 in vacuum-1~1×10-22h is sintered under Pa environment.After the completion of sintering, Furnace cooling takes out to after room temperature and obtains the enhanced titanio porous material of TiC granules.
TiC contents manufactured in the present embodiment are the titanio porous material of 2 weight portions, and yield stress is 173.85Mpa.Compare In titanio porous material sample obtained in embodiment 4, yield stress declines.Its reason is, excessive TiC powder with Titanium valve mixes, and can reduce mouldability, so as to, during compressing, form microscopic gaps between some position out-phase, sintering Also retain a part of not closed gap afterwards and then form microfissure, become the stress failure source of material so that reinforced effects It is relative to weaken.The total mechanical property of titanio porous material prepared by present case is higher than 1,2,3 sample of the embodiment of the present invention, reason It is that present case employs higher powder milling intensity, improves sintering quality, reinforcement refinement and Dispersed precipitate is to power The decline for learning performance has the effect of liquidating.Therefore, it is possible to judge that the 100 weight portion mixed powders that TiC powder is mixed to form with titanium valve In end, titanium powder content is no more than 2 weight portions.
In sum, the preparation method of TiC granule intensified titaniums based porous materials of the present invention, with protrusion once a little:The One, process is simple, composition are controllable, with short production cycle, energy consumption is low, the features such as with strong operability, low cost;Second, raw material is easy Obtain and cheap, the decomposable feature of low temperature of carbamide is make use of as pore creating material, and catabolite nontoxic pollution-free, hence it is evident that it is better than The characteristics of pore creating materials such as starch, polymer, magnesium powder and NaCl are difficult to remove and catabolite is harmful substance;3rd, this It is bright make use of TiC can as strengthen phase the characteristics of, be successfully incorporated in the middle of the preparation of POROUS TITANIUM, prepare titanio porous material Material.The high elastic modulus of TiC granules, low-density, high thermal coefficient of expansion, anticorrosive and wearability, improve the comprehensive of POROUS TITANIUM Mechanical property is closed, comprcssive strength is improved, and is provided simultaneously with the performances such as certain Wear-resistant corrosion-resistant, which is extended using neck Domain;4th, the high-energy ball milling pretreatment to powder so that TiC granules can Dispersed precipitate among matrix titanium valve, while so that Powder fining, obtains higher surface energy and distortion of lattice can be waited, with crystal grain thinning and acceleration of sintering effect;The Five, the device simple used by preparation process is easy to industrial mass production.It can be seen that TiC granule intensified titanium-bases porous of the present invention The preparation method of material, solves the titanio porous material corrosion resistance obtained by POROUS TITANIUM preparation technology in prior art well The problems such as difference, material property deterioration, hardly possible control of, complex process short compared with wear life, composition, be to prepare high intensity, porous titanio to be combined Material provides a kind of new technological approaches, with extraordinary application prospect.
Finally illustrate, above example is only unrestricted to illustrate technical scheme, although with reference to compared with Good embodiment has been described in detail to the present invention, it will be understood by those within the art that, can be to the skill of the present invention Art scheme is modified or equivalent, and without deviating from the objective and scope of technical solution of the present invention, which all should be covered at this In the middle of the right of invention.

Claims (8)

1. a kind of preparation method of TiC granule intensified titaniums based porous materials, it is characterised in that comprise the steps:
1)The titanium valve of the TiC powder and 98 ~ 99.5 weight portions of 0.5 ~ 2 weight portion is weighed, it is 100 weight portions to constitute total weight parts TiC and Ti mixed-powders, load in advance with alcohol washes and in dried high-energy ball milling tank, and ratio of grinding media to material is 10 ~ 20:1;
2)The high-energy ball milling tank good seal of TiC and Ti mixed-powders is will be equipped with, with argon cleaning high-energy ball milling tank body 3 times discharging Air in tank body, then argon is filled with tank body as protective gas;
3)It is filled with tank body after argon, step multiple ball milling is carried out to TiC the and Ti mixed-powders in high-energy ball milling tank Process, each Ball-milling Time is 20 ~ 50min, intermittent time of adjacent ball milling twice is 10 ~ 40min, total effective Ball-milling Time For 1 ~ 4 hour, the prefabricated mixed powders of TiC and Ti after ball-milling treatment, are obtained;
4)The prefabricated mixed powder of TiC and Ti of 100 weight portion obtained above is mixed in grinding body with the carbamide of same volume, Add account for the prefabricated mixed powders of TiC and Ti and carbamide gross mass 0.25% ~ 0.5% zinc stearate in mixed process, then at the uniform velocity 30 ~ 60min of mixing, is obtained mixed material;
5)With steel die by mixed material cold moudling obtained in previous step, unidirectional to suppress, pressing pressure is 180 ~ 250MPa, Dwell time is 45 ~ 60s, and the demoulding afterwards is obtained gives birth to pressed compact;
6)Raw pressed compact is placed in vacuum carbon tube furnace carries out heat treatment, and heat treatment process is divided into low temperature removing carbamide and high temperature sintering Two steps are carried out;In low temperature removing urea process, it is 1 × 10 to control vacuum in vacuum carbon tube furnace-1~1×10-2Pa, control heat up Speed is sintered to 400 DEG C from room temperature for 2 ~ 5 DEG C/min, and 45 ~ 60min is incubated at 400 DEG C;Burn subsequently into high temperature Knot process, temperature are increased to 1180 ~ 1250 DEG C, are 1 × 10 in vacuum-1~1×10-22h is sintered under Pa environment;Sintering is completed Afterwards, furnace cooling takes out to after room temperature and obtains the enhanced titanio porous material of TiC granules.
2. the preparation method of TiC granule intensified titaniums based porous materials according to claim 1, it is characterised in that the step Rapid 1)In, the purity of TiC powder is >=99.8%, and the purity of titanium valve is >=99.8%.
3. the preparation method of TiC granule intensified titaniums based porous materials according to claim 1, it is characterised in that the step Rapid 1)In, the granularity of TiC powder is 2 ~ 10 μm, and the granularity of titanium valve is 38 ~ 48 μm.
4. the preparation method of TiC granule intensified titaniums based porous materials according to claim 1, it is characterised in that the step Rapid 1)In, the ratio of weight and number of TiC powder and titanium valve is preferably 1.5:98.5.
5. the preparation method of TiC granule intensified titaniums based porous materials according to claim 1, it is characterised in that the step Rapid 2)In, the purity of argon being filled with tank body is more than 99.99%.
6. the preparation method of TiC granule intensified titaniums based porous materials according to claim 1, it is characterised in that the step Rapid 3)In, the drum's speed of rotation for carrying out ball milling is 200 ~ 400r/min.
7. the preparation method of TiC granule intensified titaniums based porous materials according to claim 1, it is characterised in that the step Rapid 4)In, for >=99%, the purity of zinc stearate is >=99% to the purity of the carbamide for being adopted.
8. the preparation method of TiC granule intensified titaniums based porous materials according to claim 1, it is characterised in that the step Rapid 4)In, the carbamide for being adopted is acicular morphology granule, and granularity is 0.8 ~ 1.1mm;The granularity of zinc stearate is 25 μm.
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106923940A (en) * 2017-03-28 2017-07-07 中奥汇成科技股份有限公司 The preparation method and POROUS TITANIUM Invasive lumbar fusion device of POROUS TITANIUM Invasive lumbar fusion device
CN107287464A (en) * 2017-07-12 2017-10-24 重庆大学 A kind of composite porous preparation method of titanium-based of the ceramics containing nano TiN
CN107321992A (en) * 2017-05-23 2017-11-07 东莞市华航新马金属有限公司 The powder metallurgy molding production technology of metal slide fastener tooth
CN107891152A (en) * 2017-12-05 2018-04-10 重庆大学 Titanium foam preparation method a kind of implantable and with cushion energy absorbing property
CN111063459A (en) * 2019-12-17 2020-04-24 中核四0四有限公司 MOX mixed particle treatment method
CN111822721A (en) * 2020-07-14 2020-10-27 苏州大学 Tungsten-doped titanium-based composite porous material and preparation method thereof
CN113046596A (en) * 2021-03-25 2021-06-29 江南大学 Bone repair titanium-molybdenum-based hydroxyapatite composite material and preparation method thereof
CN114058902A (en) * 2021-11-23 2022-02-18 西安稀有金属材料研究院有限公司 High-hardness titanium-based composite material and preparation method thereof
CN116730740A (en) * 2023-06-25 2023-09-12 兰州理工大学 Preparation method of high-strength TiC-based porous ceramic

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050249625A1 (en) * 2002-06-03 2005-11-10 Martin Bram Method for producing highly porous metallic moulded bodies close to the desired final contours
CN103205592A (en) * 2013-04-12 2013-07-17 重庆大学 Preparation method of titanium foams for cancellous bone
CN103290248A (en) * 2013-05-31 2013-09-11 西华大学 Preparation method of particle-reinforced wearable porous titanium
CN103740964A (en) * 2011-09-29 2014-04-23 重庆润泽医药有限公司 Preparation method of medical porous metal implant material
CN104141063A (en) * 2014-07-31 2014-11-12 重庆大学 Preparing method of in-situ synthesis titanium carbide enhanced titanium-based multi-hole materials
CN104357700A (en) * 2014-11-04 2015-02-18 东北大学 Porous titanium and preparing method thereof
WO2015102026A1 (en) * 2014-01-06 2015-07-09 Council Of Scientific & Industrial Research A process for the preparation of titanium foam
CN105750547A (en) * 2016-03-07 2016-07-13 中国科学院上海硅酸盐研究所 Preparation method of porous metal/ceramic composite material with controllable shape and performance

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050249625A1 (en) * 2002-06-03 2005-11-10 Martin Bram Method for producing highly porous metallic moulded bodies close to the desired final contours
CN103740964A (en) * 2011-09-29 2014-04-23 重庆润泽医药有限公司 Preparation method of medical porous metal implant material
CN103205592A (en) * 2013-04-12 2013-07-17 重庆大学 Preparation method of titanium foams for cancellous bone
CN103290248A (en) * 2013-05-31 2013-09-11 西华大学 Preparation method of particle-reinforced wearable porous titanium
WO2015102026A1 (en) * 2014-01-06 2015-07-09 Council Of Scientific & Industrial Research A process for the preparation of titanium foam
CN104141063A (en) * 2014-07-31 2014-11-12 重庆大学 Preparing method of in-situ synthesis titanium carbide enhanced titanium-based multi-hole materials
CN104357700A (en) * 2014-11-04 2015-02-18 东北大学 Porous titanium and preparing method thereof
CN105750547A (en) * 2016-03-07 2016-07-13 中国科学院上海硅酸盐研究所 Preparation method of porous metal/ceramic composite material with controllable shape and performance

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106923940B (en) * 2017-03-28 2019-04-23 中奥汇成科技股份有限公司 The preparation method and POROUS TITANIUM Invasive lumbar fusion device of POROUS TITANIUM Invasive lumbar fusion device
CN106923940A (en) * 2017-03-28 2017-07-07 中奥汇成科技股份有限公司 The preparation method and POROUS TITANIUM Invasive lumbar fusion device of POROUS TITANIUM Invasive lumbar fusion device
CN107321992A (en) * 2017-05-23 2017-11-07 东莞市华航新马金属有限公司 The powder metallurgy molding production technology of metal slide fastener tooth
CN107287464A (en) * 2017-07-12 2017-10-24 重庆大学 A kind of composite porous preparation method of titanium-based of the ceramics containing nano TiN
CN107891152A (en) * 2017-12-05 2018-04-10 重庆大学 Titanium foam preparation method a kind of implantable and with cushion energy absorbing property
CN111063459B (en) * 2019-12-17 2023-10-20 中核四0四有限公司 MOX mixed particle treatment method
CN111063459A (en) * 2019-12-17 2020-04-24 中核四0四有限公司 MOX mixed particle treatment method
CN111822721A (en) * 2020-07-14 2020-10-27 苏州大学 Tungsten-doped titanium-based composite porous material and preparation method thereof
CN111822721B (en) * 2020-07-14 2022-05-10 苏州大学 Tungsten-doped titanium-based composite porous material and preparation method thereof
CN113046596A (en) * 2021-03-25 2021-06-29 江南大学 Bone repair titanium-molybdenum-based hydroxyapatite composite material and preparation method thereof
CN114058902A (en) * 2021-11-23 2022-02-18 西安稀有金属材料研究院有限公司 High-hardness titanium-based composite material and preparation method thereof
CN116730740A (en) * 2023-06-25 2023-09-12 兰州理工大学 Preparation method of high-strength TiC-based porous ceramic
CN116730740B (en) * 2023-06-25 2023-12-22 兰州理工大学 Preparation method of high-strength TiC-based porous ceramic

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