CN106521219B - A kind of preparation method of TiC granule intensified titaniums based porous materials - Google Patents
A kind of preparation method of TiC granule intensified titaniums based porous materials Download PDFInfo
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- CN106521219B CN106521219B CN201710008243.3A CN201710008243A CN106521219B CN 106521219 B CN106521219 B CN 106521219B CN 201710008243 A CN201710008243 A CN 201710008243A CN 106521219 B CN106521219 B CN 106521219B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
- B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
- B22F3/1134—Inorganic fillers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
Abstract
The invention discloses a kind of TiC granule intensified titaniums based porous materials preparation methods, it uses powder metallurgy boring technique, after ball milling pretreatment being carried out using a certain proportion of TiC powder and titanium valve mixing under protection of argon gas, again with urea, zinc stearate is mixed by dispensing, compression moulding and multiple step format heat treatment step prepare titanium-based porous material, and it is preferable to use acicular morphology granular urea as pore creating material, using zinc stearate as binding agent, so that the structure and easy control of components of titanium-based porous material, raw material is easy to get and cheap, and multiple step format heat treatment mode can shorten manufacturing cycle, reduce time cost, service wear of energy consumption and equipment etc.；In addition the present invention be also fully utilized by TiC particles density it is small, elasticity modulus is high, coefficient of thermal expansion is high, wearability and it is anticorrosive high the features such as, so that the titanium-based porous material being prepared has excellent comprehensive mechanical property and corrosion resistance, there is extraordinary application prospect.
Description
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
Porous metal material has the advantages that other porous materials are incomparable as a kind of novel composite material.Phase
Compared with solid material, certain porosity makes it have good compressibility；Compared to foamed polymer, have higher firm
Degree and temperature in use；Compared to foamed ceramics, there is good toughness, thermal conductivity, electric conductivity etc..So porous material metal material
Material has broad prospects in fields such as auto industry, aerospace, 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 properties such as creep resisting ability and wearability have larger reduction, so improving more
The mechanical property of mesoporous metal receives the concern of people always.
Titanium or titanium alloy is a series of prominent due to having the advantages that specific strength height, the good, high temperature resistant of corrosion resistance etc., is a kind of
Prepare the excellent matrix of porous metal material.Porous titanium matrix composite is that the second phase fiber or particle work are added in Titanium base
For reinforced phase, titanium and the composite material of reinforcement two-phase are formed.The introducing of reinforced phase is so that the intensity of material, Gao Gang, toughness, resistance to
Mill property and the performances such as antifatigue increase, and can improve the high temperature resistance of material, the performances such as anticorrosive, greatly extend material
Use scope.
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 preferred when exploitation has the titanium matrix composite of excellent high performance
Increasing be mutually SiC fibers.But the preparation method of fibre-reinforced composite material is relatively difficult, according to the literature, can only use solid
Phase method synthesizes, and is then molded with the methods of hot isostatic pressing, vacuum hotpressing, forging.Simultaneously continuous enhancing titanium matrix composite respectively to
The opposite sex is stronger.Use scope has certain limitation, and production technology is complicated, higher into production cost.Therefore discontinuous increasing
Strong composite material has obtained quick development, a great selection of cheap reinforced phase selected is primarily due to, such as particle, whisker, short fibre
Dimension etc. and can free design structure and the features such as ingredient so that in the exploitation and production of solid metal composite material increasingly
Standardization.
It is worth noting that, although discontinuous reinforcement body has obtained extensive utilization, Zhu etc. in titanium-based densification composite material
People uses slurry foaming, by adding in the cerium oxide of 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 process2O3The titanium matrix composite of enhancing, wherein Nd2O3Shape
Looks are more complicated, and are unevenly distributed, have tiny sheet, lath-shaped and spherical.Week and Xiao et al. are in the preparation process of composite material
In be all doped with rare earth oxide, the process is more complicated, high energy consumption, expensive, and structure is difficult to control 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 titanium-based
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.
Invention content
For above-mentioned deficiency in the prior art, the purpose of the present invention is 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 process of the prior art
Difference, corrosion resistance is poor, wear-resisting property is poor, complex process, high energy consumption, structure and the problem of composition difficulty control.
To achieve the above object, present invention employs following technical solutions：
A kind of preparation method of TiC granule intensified titaniums based porous materials includes the following steps：
1）The TiC powder of 0.5 ~ 2 parts by weight and the titanium valve of 98 ~ 99.5 parts by weight are weighed, composition total weight parts are 100 parts by weight
TiC and Ti mixed-powders, be fitted into advance in alcohol washes and dried high-energy ball milling tank, ratio of grinding media to material is 10 ~ 20：1；
2）High-energy ball milling tank equipped with TiC and Ti mixed-powders is sealed, with argon cleaning high-energy ball milling tank body 3 times with
The air in tank body is discharged, then argon gas is filled with as protective gas into tank body；
3）After being filled with argon gas into tank body, intermittent to TiC the and Ti mixed-powders progress in high-energy ball milling tank is multiple
Ball-milling treatment, each Ball-milling Time are 20 ~ 50min, and intermittent time of adjacent ball milling twice is 10 ~ 40min, total effective ball milling
Time is 1 ~ 4 hour, and the prefabricated mixed powders of TiC and Ti are obtained after ball-milling treatment；
4）The prefabricated mixed powder of TiC and Ti of 100 parts by weight obtained above and the urea of same volume are mixed in grinding body
It closes, is added in mixed process and account for the prefabricated mixed powders of TiC and Ti and 0.25% ~ 0.5% zinc stearate of urea gross mass, then
30 ~ 60min is at the uniform velocity mixed, mixed material is made；
5）It is unidirectional to suppress with steel die by mixed material cold moudling made from previous step, pressing pressure for 180 ~
250MPa, dwell time are 45 ~ 60s, and raw green compact is made in demoulding later；
6）Raw green compact is placed in vacuum carbon tube furnace and is heat-treated, heat treatment process is divided into low temperature removing urea and high temperature
It is sintered the progress of two steps；In low temperature removing urea process, it is 1 × 10 to control vacuum degree in vacuum carbon tube furnace-1~1×10-2Pa, control
Heating rate is sintered for 2 ~ 5 DEG C/min from room temperature to 400 DEG C, and 45 ~ 60min is kept the temperature at 400 DEG C；Subsequently into height
Warm sintering process, temperature are increased to 1180 ~ 1250 DEG C, are 1 × 10 in vacuum degree-1~1×10-22h is sintered under Pa environment；Sintering
After the completion, it is taken out after furnace cooling to room temperature and obtains the titanium-based porous material of TiC particles enhancing.
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 into 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,
The purity of used urea is >=99%, and the purity of zinc stearate is >=99%.
In the preparation method of above-mentioned TiC granule intensified titanium based porous materials, preferably, the step 4）In,
Used urea is acicular morphology particle, and granularity is 0.8 ~ 1.1mm；The granularity of zinc stearate is 25 μm.
Compared with the 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 is prepared more using powder metallurgy boring technique
Hole titanium matrix composite is made by processes, TiC particles such as ball milling pretreatment, dispensing mixing, compression moulding, multiple step format heat treatments
It is reinforcement phase Dispersed precipitate in Titanium base, in the sintering neck length big stage, TiC fine particles can be used as nucleating agent, promote shape
Carry out crystal grain thinning into heterogeneous nucleation, while the growth of crystal boundary is hindered to reduce the coarsening rate of crystal grain；With above-mentioned easy system
Preparation Method has prepared lightweight and has had the composite porous of higher-strength, can be used as lightweight structural material；Hole
Gap feature can make it as materials'uses such as medicine bone alternate material, fluid separating and filtering, fluid distrbution, energy-absorbing dampings；Greatly
Extend POROUS TITANIUM using field, the reinforcing for porous titanium base material provides an effective approach newly.
2nd, in the preparation method of the TiC granule intensified titanium based porous materials involved in the present invention, ball milling has been carried out to powder
It pre-processes, mixed-powder constantly impact friction, shock mutually in stainless cylinder of steel with stainless steel ball, reaches broken in mechanical milling process
With the effect of crystal grain refinement, be conducive to improve the surface energy of powder, while powder has accumulated a large amount of lattice in shattering process
Defect, such as vacancy, distortion, dislocation；These characteristics both contribute to improve sintering quality, so as to improve gained titanium-based porous material
Mechanical property.
3rd, in the preparation method of the TiC granule intensified titanium based porous materials involved in the present invention, acicular morphology particle is used
And the urea of high-purity is less than traditional round urea as pore creating material, surface area and anti-extrusion ability, reduces pore creating material
With frictional force of the powder in pressing process, the characteristics of stress is yielding, increases mobility of the powder in pressing process, makes
Must give birth to green compact stress be more uniformly distributed it is more easily molded, experiment show using needle-shaped Liao Su be more easy to acquisition intercommunicating pore structure；Using tristearin
Sour zinc can promote molding, the demoulding of raw green compact, avoid generating transverse surface cracks during demoulding, improve as binding agent
The pick-up rate of raw green compact；And the zinc stearate as the urea of pore creating material under high temperature and as binding agent easily removes, removing
Impurity will not be introduced in the process, be conducive to keep the cleanliness of gained titanium-based porous material product, and urea and zinc stearate
Decomposition product will not generate pollution environment substance.
4th, in the preparation method of the TiC granule intensified titanium based porous materials involved in the present invention, using two sections of vacuum not between
Disconnected mode is heat-treated raw green compact, is divided into low temperature removing two step of urea and high-temperature sintering process；Low temperature removes urea and hard
During resin acid zinc, vacuum environment will can decompose and generate gas extraction furnace body in time；High-temperature vacuum sintering stage vacuum degree for 1 ×
10-1~1×10-2It is sintered under Pa environment, ensure that sample is not oxidized；The advantages of this preparation method, is that production has continuous
Property, the period for obtaining finished product is shortened, reduces energy consumption, thereby reduces production cost.
Description of the drawings
Fig. 1 is the process flow chart of TiC granule intensified titaniums based porous materials preparation method of the present invention.
Fig. 2 is the differential thermal analysis curve figure of urea.
Fig. 3 is TiC and macro morphology scanning electron microscope (SEM) photograph after Ti powder mixing and ball millings in the embodiment of the present invention 1.
Fig. 4 is the physical form figure of gained titanium-based porous material in the embodiment of the present invention 4.
Fig. 5 is the pore structure scanning electron microscope (SEM) photograph of gained titanium-based porous material in the embodiment of the present invention 4.
Fig. 6 is the compressive stress strain curve figure of gained titanium-based porous material in the embodiment of the present invention 4.
Specific embodiment
Be directed to porous titanium material resistance to compression obtained by the POROUS TITANIUM preparation process of the prior art is poor, corrosion resistance is poor,
Wear-resisting property is poor, complex process, high energy consumption, structure and the problem of composition difficulty control, and the present invention provides a kind of TiC granule intensified titaniums
The preparation method of based porous materials, method flow is as shown in Figure 1, include the following steps：
1）Raw material is chosen：The TiC powder of 0.5 ~ 2 parts by weight and the titanium valve of 98 ~ 99.5 parts by weight are weighed, forming total weight parts is
TiC the and Ti mixed-powders of 100 parts by weight are fitted into advance in alcohol washes and dried high-energy ball milling tank, and ratio of grinding media to material is
10~20：1.
Here, in order to ensure the purity and performance of the TiC granule intensified titanium based porous materials prepared, the TiC powder in raw material
Purity be preferably >=99.8%, the purity of titanium valve is preferably >=99.8%.Also, TiC powder preferably selects 2 ~ 10 μm of granularities, so as to
Ensure its requirement of size as reinforced phase, meticulous easy generation agglomeration so that prefabricated TiC and Ti blending constituents are uneven
It is even；It can slightly make very much enhancing effect bad simultaneously or even reduce the mechanical property etc. of product.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, granule size, is examined through experiment
It surveys, this particle size range is optimum range.
2）Ball milling prepares：High-energy ball milling tank equipped with TiC and Ti mixed-powders is sealed, with argon cleaning high-energy ball milling
Tank body 3 times is to discharge the air in tank body, then be filled with argon gas as protective gas into tank body.
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 into tank body
Argon gas is filled with as protective gas so that mechanical milling process carries out under an argon atmosphere, can effectively prevent nitride and oxide
Formation and oxygen atom solid solution, keep the cleanliness of material.This used purity of argon is preferably more than 99.99%, is kept away
Exempt to introduce impurity, preferably to keep the cleanliness of material in mechanical milling process.
3）Ball milling pretreatment：After being filled with argon gas into tank body, to TiC the and Ti mixed-powders in high-energy ball milling tank into the ranks
The multiple ball-milling treatment for 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 for 1 ~ 4 hour, obtain the prefabricated mixed powders of TiC and Ti after ball-milling treatment.
In the step, high-energy ball milling cause mixed-powder and stainless steel ball in stainless cylinder of steel constantly mutually impact friction,
It hits, achievees the effect that broken and crystal grain refinement, be conducive to improve the surface energy of powder, while powder accumulates in shattering process
A large amount of lattice defect, such as vacancy, distortion, dislocation；These characteristics both contribute to improve sintering quality, so as to improve gained
The mechanical property of titanium-based porous material.Wherein, the drum's speed of rotation for carrying out ball milling is preferably 200 ~ 400r/min.
4）Dispensing mixes：The urea of the prefabricated mixed powder of TiC and Ti of 100 parts by weight obtained above and same volume is existed
Mixed in grinding body, in mixed process add in account for the prefabricated mixed powders of TiC and Ti with the 0.25% ~ 0.5% of urea gross mass it is hard
Resin acid zinc, then 30 ~ 60min is at the uniform velocity mixed, mixed material is made.
Here the urea added in is as pore creating material, and urea is preferably using acicular morphology particle, surface area and anti-extrusion
Ability be less than traditional round urea, pore creating material and frictional force of the powder in pressing process can be reduced so that give birth to green compact by
Power is more uniformly distributed, is more easily molded；Zinc stearate is the molding that can promote raw green compact as binding agent, demoulding, avoid in compacting and
Surface transversal crack is generated in knockout course.Selection for urea size range is due in foamed material mesoporous character
There is conclusive influence on material property, the wherein granularity of urea 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
The granularity of the gained prefabricated mixed powders of TiC and Ti further refines after ball milling, and close to 25 μm, therefore it is 25 μm to select 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
The phase separation of powder and zinc stearate helps to be molded.And blending process at the uniform velocity mixes 30min, it is ensured that mixed material
Equal property.In addition, the in order to enable subsequent heat treatment pore-creating of the urea as pore creating material and the zinc stearate as binding agent
Easily removed in journey without introducing impurity, the purity of used urea is preferably >=99%, the purity of zinc stearate preferably >=
99%。
5）Compression moulding：It is unidirectional to suppress with steel die by mixed material cold moudling made from previous step, pressing pressure
For 180 ~ 250MPa, the dwell time is 45 ~ 60s, and raw green compact is made in demoulding later.
During compression moulding, pressurize is conducive to effective transmission of pressure so that raw green compact is more densified, and increases life
The intensity of green compact avoids the generation of arch bridge effect between particle.
6）Multiple step format is heat-treated：Raw green compact is placed in vacuum carbon tube furnace and is heat-treated, heat treatment process is divided into low temperature
It removes urea and two step of high temperature sintering carries out；In low temperature removing urea process, it is 1 × 10 to control vacuum degree in vacuum carbon tube furnace-1~
1×10-2Pa, control heating rate are sintered from room temperature to 400 DEG C for 2 ~ 5 DEG C/min, keep the temperature 45 at 400 DEG C ~
60min；Subsequently into high-temperature sintering process, temperature is increased to 1180 ~ 1250 DEG C, is 1 × 10 in vacuum degree-1~1×10-2Pa rings
2h is sintered under border；It is taken out after the completion of sintering, after furnace cooling to room temperature and obtains the titanium-based porous material of TiC particles enhancing.
The present invention has been divided into low temperature removing urea to the heat treatment of raw green compact and two step of high temperature sintering carries out.Fig. 2 shows
The differential thermal analysis curve figure of urea, as shown in Figure 2, when temperature is 400 DEG C, urea is decomposed and is finished substantially, 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, preferably relatively slowly, control rises heating rate
Warm rate is best in 2 ~ 5 DEG C/min, to avoid urea decomposes the too fast raw green compact expansion of release and causes to cave in；In cryogenic vacuum
In sintering process, it is 1 × 10 to control vacuum degree in vacuum carbon tube furnace-1~1×10-2Pa, purpose is in order to enable what pore creating material decomposed
Gas is extracted into outside furnace body rapidly, is avoided pollution sample, 45 ~ 60min is kept the temperature at 400 DEG C, it is therefore an objective to ensure that urea is completely out.
In high-temperature sintering process, in the sintering neck length big stage, TiC fine particles can be used as nucleating agent, and promotion forms heterogeneous nucleation
Crystal grain thinning, while the growth of crystal boundary is hindered to reduce the coarsening rate of crystal grain, crystal grain thinning can in porous titanium matrix composite
Effectively to improve the intensity of material, this is that other intensifying methods cannot compare, under identical external force, in small grains
Portion and crystal boundary nearby strain relatively small, and deformation is uniform, and comparatively, stress concentration causes the chance of cracking also less, makes
Larger deformation can be born before cracking by obtaining gained titanium-based porous material；On the other hand, since the purer titanium of TiC density is low,
For 4.99g.cm-3, contribute to the lighting of titanium-based porous material, improve its specific strength；In addition, the elasticity modulus of industrially pure titanium is
The elasticity modulus of 110GPa, TiC are 460GPa, and during material stress and deformation, TiC can bear higher load, with resistance
Hinder the extension of crackle or change its extension approach, enhance crack propagation energy, so as to improve the intensity of titanium-based porous material and toughness,
The comprehensive mechanical property of TiC granule intensified titaniums based porous materials obtained by promotion.
Below method is further illustrated the present invention with embodiment.It should be understood that these embodiments are only to use
In the embodiment further illustrated the present invention rather than for limiting the present invention.
Embodiment 1：
It is >=99.8% that the present embodiment, which selects purity, granularity be 2 ~ 10 μm TiC powder and purity be >=99.8%, grain
The titanium valve for 38 ~ 48 μm is spent, TiC granule intensified titanium based porous materials are prepared using the method for the present invention, step is as follows：
（1）Raw material ball milling pretreatment：
The TiC powder of 0.5 parts by weight and the titanium valve of 99.5 parts by weight are weighed, forms TiC and Ti that gross weight is 100 parts by weight
Mixed-powder is fitted into advance in alcohol washes and dried high-energy ball milling tank, ratio of grinding media to material 10：1, TiC and Ti will be housed
The high-energy ball milling tank of mixed-powder is sealed, with argon cleaning tank body 3 times to discharge the air in tank body, backward tank body in fill
Enter the argon gas that purity is more than 99.99%, then the TiC and Ti mixed-powders in high-energy ball milling tank are carried out intermittent multiple
Ball-milling treatment, this example drum's speed of rotation is 200r/min, when each Ball-milling Time is the interval of 20min, often adjacent ball milling twice
Between for 10min, effective ball milling total time is 1h, then stops ball milling, obtains the prefabricated mixed powders of TiC and Ti.Fig. 3 shows this
TiC and macro morphology scanning electron microscope (SEM) photograph after Ti powder mixing and ball millings in embodiment, it can be seen that although effectively Ball-milling Time is only
1h, but can be seen that the powder of the gained prefabricated mixed powders of TiC and Ti has apparent fine-characterization.Then, ball grinder is placed in
In vacuum glove box, prefabricated powder from ball grinder is taken out, is aoxidized to avoid the prefabricated mixed powders of TiC and Ti.
（2）Dispensing mixes：
The prefabricated mixed powders of the 100 parts by weight TiC and Ti obtained above acicular morphology granular urea identical with its volume
It is mixed in grinding body, and adds in and account for the prefabricated mixed powders of TiC and Ti and 0.25% zinc stearate of urea gross mass, it is at the uniform velocity mixed
30min is closed, obtains mixed material.In the present embodiment, the purity of urea used is >=99%, granularity is 0.8 ~ 1.1mm, zinc stearate
Purity for >=99%, granularity be 25 μm.
（3）Compression moulding：
Unidirectional to suppress with steel die by the mixed material compression moulding obtained by back, pressing pressure 180MPa is protected
The pressure time is 60s, and demoulding obtains raw green compact.
（4）Multiple step format is heat-treated：
Raw green compact is put into vacuum carbon tube furnace and is heat-treated, processing procedure is divided into cryogenic vacuum removing urea and high temperature
It is sintered the progress of two steps.Cryogenic vacuum removes the urea stage, and it is 1 × 10 to control vacuum degree in vacuum carbon tube furnace-1~1×10-2Pa, control
Heating rate processed is sintered for 2 DEG C/min from room temperature to 400 DEG C, and 45min is kept the temperature at 400 DEG C；Subsequently into high temperature
Solid state sintering process, temperature are increased to 1180 DEG C, are 1 × 10 in vacuum degree-1~1×10-22h is sintered under Pa environment.Sintering is completed
Afterwards, it is taken out after furnace cooling to room temperature and obtains the titanium-based porous material of TiC particles enhancing.
TiC contents manufactured in the present embodiment are the porous titanium matrix composite of 0.5 parts by weight, surrender strong stress and are
133.53 Mpa。
Embodiment 2：
It is >=99.8% that the present embodiment, which selects purity, granularity be 2 ~ 10 μm TiC powder and purity be >=99.8%, grain
The titanium valve for 38 ~ 48 μm is spent, TiC granule intensified titanium based porous materials are prepared using the method for the present invention, step is as follows：
（1）Raw material ball milling pretreatment：
The TiC powder of 1 parts by weight and the titanium valve of 99 parts by weight are weighed, the TiC and Ti for forming gross weight as 100 parts by weight are mixed
Powder is fitted into advance in alcohol washes and dried high-energy ball milling tank, ratio of grinding media to material 10：1, TiC and Ti will be housed and mixed
The high-energy ball milling tank of powder is sealed, 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 gas for more than 99.99% is spent, intermittent multiple ball milling is then carried out to TiC the and Ti mixed-powders in high-energy ball milling tank
Processing, this example drum's speed of rotation are 200r/min, and each Ball-milling Time is 20min, is per interval time of adjacent ball milling 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 from ball grinder is taken out, is aoxidized to avoid the prefabricated mixed powders of TiC and Ti.
（2）Dispensing mixes：
The prefabricated mixed powders of the 100 parts by weight TiC and Ti obtained above acicular morphology granular urea identical with its volume
It is mixed in grinding body, and adds in and account for the prefabricated mixed powders of TiC and Ti and 0.25% zinc stearate of urea gross mass, it is at the uniform velocity mixed
30min is closed, obtains mixed material.In the present embodiment, the purity of urea used is >=99%, granularity is 0.8 ~ 1.1mm, zinc stearate
Purity for >=99%, granularity be 25 μm.
（3）Compression moulding：
Unidirectional to suppress with steel die by the mixed material compression moulding obtained by back, pressing pressure 180MPa is protected
The pressure time is 60s, and demoulding obtains raw green compact.
（4）Multiple step format is heat-treated：
Raw green compact is put into vacuum carbon tube furnace and is heat-treated, processing procedure is divided into cryogenic vacuum removing urea and high temperature
It is sintered the progress of two steps.Cryogenic vacuum removes the urea stage, and it is 1 × 10 to control vacuum degree in vacuum carbon tube furnace-1~1×10-2Pa, control
Heating rate processed is sintered for 2 DEG C/min from room temperature to 400 DEG C, and 45min is kept the temperature at 400 DEG C；Subsequently into high temperature
Solid state sintering process, temperature are increased to 1180 DEG C, are 1 × 10 in vacuum degree-1~1×10-22h is sintered under Pa environment.Sintering is completed
Afterwards, it is taken out after furnace cooling to room temperature and obtains the titanium-based porous material of TiC particles enhancing.
The present embodiment embodiment compared on, ball milling parameter, zinc stearate additive amount, heat treatment process all same.This reality
Apply titanium-based porous material of the TiC contents of example preparation for 1 parts by weight, yield stress 152.42Mpa.It is possible thereby to it can see
Go out, the increase of TiC particles can effectively improve yield strength.
Embodiment 3：
It is >=99.8% that the present embodiment, which selects purity, granularity be 2 ~ 10 μm TiC powder and purity be >=99.8%, grain
The titanium valve for 38 ~ 48 μm is spent, TiC granule intensified titanium based porous materials are prepared using the method for the present invention, step is as follows：
（1）Raw material ball milling pretreatment：
The TiC powder of 1 parts by weight and the titanium valve of 99 parts by weight are weighed, the TiC and Ti for forming gross weight as 100 parts by weight are mixed
Powder is fitted into advance in alcohol washes and dried high-energy ball milling tank, ratio of grinding media to material 15：1, TiC and Ti will be housed and mixed
The high-energy ball milling tank of powder is sealed, 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 gas for more than 99.99% is spent, intermittent multiple ball milling is then carried out to TiC the and Ti mixed-powders in high-energy ball milling tank
Processing, this example drum's speed of rotation are 300r/min, and each Ball-milling Time is 30min, is per interval time of adjacent ball milling 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 from ball grinder is taken out, is aoxidized to avoid the prefabricated mixed powders of TiC and Ti.
（2）Dispensing mixes：
The prefabricated mixed powders of the 100 parts by weight TiC and Ti obtained above acicular morphology granular urea identical with its volume
It is mixed in grinding body, and adds in and account for the prefabricated mixed powders of TiC and Ti and 0.4% zinc stearate of urea gross mass, at the uniform velocity mixed
45min obtains mixed material.In the present embodiment, the purity of urea used is >=99%, granularity is 0.8 ~ 1.1mm, zinc stearate
Purity for >=99%, granularity be 25 μm.
（3）Compression moulding：
Unidirectional to suppress with steel die by the mixed material compression moulding obtained by back, pressing pressure 200MPa is protected
The pressure time is 50s, and demoulding obtains raw green compact.
（4）Multiple step format is heat-treated：
Raw green compact is put into vacuum carbon tube furnace and is heat-treated, processing procedure is divided into cryogenic vacuum removing urea and high temperature
It is sintered the progress of two steps.Cryogenic vacuum removes the urea stage, and it is 1 × 10 to control vacuum degree in vacuum carbon tube furnace-1~1×10-2Pa, control
Heating rate processed is sintered for 4 DEG C/min from room temperature to 400 DEG C, and 50min is kept the temperature at 400 DEG C；Subsequently into high temperature
Solid state sintering process, temperature are increased to 1250 DEG C, are 1 × 10 in vacuum degree-1~1×10-22h is sintered under Pa environment.Sintering is completed
Afterwards, it is taken out after furnace cooling to room temperature and obtains the titanium-based porous material of TiC particles enhancing.
The present embodiment embodiment 2 compared on, ball milling parameter increase, i.e. milling intensity increase so that manufactured in the present embodiment
TiC contents reach 167.42Mpa for the yield stress of the titanium-based porous material of 1 parts by weight.Therefore, appropriate increase ball milling is strong
Degree, can help to improve sintering quality, promote the mechanical property of prepared TiC granule intensified titanium based porous materials.
Embodiment 4：
It is >=99.8% that the present embodiment, which selects purity, granularity be 2 ~ 10 μm TiC powder and purity be >=99.8%, grain
The titanium valve for 38 ~ 48 μm is spent, TiC granule intensified titanium based porous materials are prepared using the method for the present invention, step is as follows：
（1）Raw material ball milling pretreatment：
The TiC powder of 1.5 parts by weight and the titanium valve of 98.5 parts by weight are weighed, forms TiC and Ti that gross weight is 100 parts by weight
Mixed-powder is fitted into advance in alcohol washes and dried high-energy ball milling tank, ratio of grinding media to material 20：1, TiC and Ti will be housed
The high-energy ball milling tank of mixed-powder is sealed, with argon cleaning tank body 3 times to discharge the air in tank body, backward tank body in fill
Enter the argon gas that purity is more than 99.99%, then the TiC and Ti mixed-powders in high-energy ball milling tank are carried out intermittent multiple
Ball-milling treatment, this example drum's speed of rotation is 400r/min, when each Ball-milling Time is the interval of 50min, often adjacent ball milling twice
Between for 40min, effective ball milling total time is 4h, then stops ball milling, obtains the prefabricated mixed powders of TiC and Ti.Then, by ball milling
Tank is placed in vacuum glove box, and prefabricated powder is taken out from ball grinder, is aoxidized to avoid the prefabricated mixed powders of TiC and Ti.
（2）Dispensing mixes：
The prefabricated mixed powders of the 100 parts by weight TiC and Ti obtained above acicular morphology granular urea identical with its volume
It is mixed in grinding body, and adds in and account for the prefabricated mixed powders of TiC and Ti and 0.5% zinc stearate of urea gross mass, at the uniform velocity mixed
60min obtains mixed material.In the present embodiment, the purity of urea used is >=99%, granularity is 0.8 ~ 1.1mm, zinc stearate
Purity for >=99%, granularity be 25 μm.
（3）Compression moulding：
Unidirectional to suppress with steel die by the mixed material compression moulding obtained by back, pressing pressure 250MPa is protected
The pressure time is 45s, and demoulding obtains raw green compact.
（4）Multiple step format is heat-treated：
Raw green compact is put into vacuum carbon tube furnace and is heat-treated, processing procedure is divided into cryogenic vacuum removing urea and high temperature
It is sintered the progress of two steps.Cryogenic vacuum removes the urea stage, and it is 1 × 10 to control vacuum degree in vacuum carbon tube furnace-1~1×10-2Pa, control
Heating rate processed is sintered for 5 DEG C/min from room temperature to 400 DEG C, and 60min is kept the temperature at 400 DEG C；Subsequently into high temperature
Solid state sintering process, temperature are increased to 1200 DEG C, are 1 × 10 in vacuum degree-1~1×10-22h is sintered under Pa environment.Sintering is completed
Afterwards, it is taken out after furnace cooling to room temperature and obtains the titanium-based porous material of TiC particles enhancing.
Fig. 4, Fig. 5 are respectively the physical form figure of the titanium-based porous material prepared by present case and pore structure scanning electron microscope
Figure, as seen from Figure 4, complete appearance and with metallic luster show that it maintains good cleanliness in link is prepared, from
Fig. 5 can be seen that the macro morphology of hole and acicular morphology granular urea match, and even pore distribution, there are a large amount of connections
Pore structure, without apparent internal flaw, better overall quality.Compression test is carried out to it, compression stress-strain of gained is bent
Line chart is as shown in Figure 6.The initial yield stress of TiC granule intensified titanium based porous materials obtained by the present embodiment 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 tendency that continuing to rise and reaches peak value, this is because TiC
The presence of reinforcement so that the hole process of caving in becomes slow, and failure stress is improved, so as to increase the strong of material
Degree.
Embodiment 5：
A kind of preparation method of TiC granule intensified titaniums based porous materials is present embodiments provided, flow is with reference to Fig. 1 institutes
Show, key step includes as follows：
（1）Raw material ball milling pretreatment：
The TiC powder of 2 parts by weight and the titanium valve of 98 parts by weight are weighed, the TiC and Ti for forming gross weight as 100 parts by weight are mixed
Powder is fitted into advance in alcohol washes and dried high-energy ball milling tank, ratio of grinding media to material 20：1, TiC and Ti will be housed and mixed
The high-energy ball milling tank of powder is sealed, 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 gas for more than 99.99% is spent, intermittent multiple ball milling is then carried out to TiC the and Ti mixed-powders in high-energy ball milling tank
Processing, this example drum's speed of rotation are 400r/min, and each Ball-milling Time is 50min, is per interval time of adjacent ball milling 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 from ball grinder is taken out, is aoxidized to avoid the prefabricated mixed powders of TiC and Ti.
（2）Dispensing mixes：
The prefabricated mixed powders of the 100 parts by weight TiC and Ti obtained above acicular morphology granular urea identical with its volume
It is mixed in grinding body, and adds in and account for the prefabricated mixed powders of TiC and Ti and 0.5% zinc stearate of urea gross mass, at the uniform velocity mixed
60min obtains mixed material.In the present embodiment, the purity of urea used is >=99%, granularity is 0.8 ~ 1.1mm, zinc stearate
Purity for >=99%, granularity be 25 μm.
（3）Compression moulding：
Unidirectional to suppress with steel die by the mixed material compression moulding obtained by back, pressing pressure 250MPa is protected
The pressure time is 45s, and demoulding obtains raw green compact.
（4）Multiple step format is heat-treated：
Raw green compact is put into vacuum carbon tube furnace and is heat-treated, processing procedure is divided into cryogenic vacuum removing urea and high temperature
It is sintered the progress of two steps.Cryogenic vacuum removes the urea stage, and it is 1 × 10 to control vacuum degree in vacuum carbon tube furnace-1~1×10-2Pa, control
Heating rate processed is sintered for 5 DEG C/min from room temperature to 400 DEG C, and 60min is kept the temperature at 400 DEG C；Subsequently into high temperature
Solid state sintering process, temperature are increased to 1200 DEG C, are 1 × 10 in vacuum degree-1~1×10-22h is sintered under Pa environment.Sintering is completed
Afterwards, it is taken out after furnace cooling to room temperature and obtains the titanium-based porous material of TiC particles enhancing.
Titanium-based porous material of the TiC contents manufactured in the present embodiment for 2 parts by weight, yield stress 173.85Mpa.It compares
In titanium-based porous material sample made from embodiment 4, yield stress declines.The reason is that excessive TiC powder with
Titanium valve mixes, and can reduce mouldability, so as to which during compression moulding, microscopic gaps are formed between certain position out-phase, is sintered
Also retain a part of not closed gap later and then form microfissure, become the stress failure source of material so that enhancing effect
It is opposite to weaken.The total mechanical property of titanium-based 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 are to power
The decline for learning performance has the effect that liquidates.Therefore, it is possible to judge that the 100 parts by weight mixed powders that TiC powder is mixed to form with titanium valve
In end, titanium powder content is no more than 2 parts by weight.
In conclusion the preparation method of TiC granule intensified titaniums based porous materials of the present invention, has and protrudes a little：The
One, it is simple for process, ingredient is controllable, with short production cycle, low energy consumption, there is strong operability, at low cost；Second, raw material is easy
It obtains and cheap, the decomposable feature of low temperature of urea is utilized as pore creating material, and decomposition product is nontoxic and pollution-free, hence it is evident that be better than
The pore creating materials such as starch, polymer, magnesium powder and NaCl are not easy the characteristics of removing and decomposition product are harmful substance；Third, this hair
It is bright that the characteristics of TiC can be used as reinforced phase is utilized, it is successfully introduced into the preparation of POROUS TITANIUM, prepares the porous material of titanium-based
Material.The high elastic modulus of TiC particles, low-density, high coefficient of thermal expansion, anticorrosive and wearability, improve the comprehensive of POROUS TITANIUM
Mechanical property is closed, compression strength is improved, and is provided simultaneously with the performances such as certain Wear-resistant corrosion-resistant, extends it and uses neck
Domain；4th, the high-energy ball milling of powder is pre-processed so that TiC particles can Dispersed precipitate among matrix titanium valve, simultaneously so that
Powder fining, obtain higher surface can and distortion of lattice can wait, have the function of crystal grain thinning and acceleration of sintering；The
Five, device simple used in preparation process, convenient for industrial mass production.It can be seen that TiC granule intensified titanium-bases of the present invention are porous
The preparation method of material has well solved the titanium-based porous material corrosion resistance in the prior art obtained by POROUS TITANIUM preparation process
It is the problems such as difference, material property deterioration, complex process short compared with wear life, composition difficulty control, compound to prepare high intensity, porous titanium-based
Material provides a kind of new technological approaches, has extraordinary application prospect.
Finally illustrate, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although with reference to compared with
The present invention is described in detail in good embodiment, it will be understood by those of ordinary skill in the art that, it can be to the skill of the present invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of technical solution of the present invention, should all be covered at this
In the right of invention.
Claims (8)
1. a kind of preparation method of TiC granule intensified titaniums based porous materials, which is characterized in that include the following steps：
1）The TiC powder of 0.5 ~ 2 parts by weight and the titanium valve of 98 ~ 99.5 parts by weight are weighed, forms total weight parts as 100 parts by weight
TiC and Ti mixed-powders are fitted into advance in alcohol washes and dried high-energy ball milling tank, and ratio of grinding media to material is 10 ~ 20：1；
2）High-energy ball milling tank equipped with TiC and Ti mixed-powders is sealed, with argon cleaning high-energy ball milling tank body 3 times with discharge
Air in tank body, then argon gas is filled with as protective gas into tank body；
3）After being filled with argon gas into tank body, intermittent multiple ball milling is carried out to TiC the and Ti mixed-powders in high-energy ball milling tank
Processing, each Ball-milling Time are 20 ~ 50min, and intermittent time of adjacent ball milling twice is 10 ~ 40min, total effective Ball-milling Time
It is 1 ~ 4 hour, the prefabricated mixed powders of TiC and Ti is obtained after ball-milling treatment；
4）The prefabricated mixed powder of TiC and Ti of 100 parts by weight obtained above is mixed with the urea of same volume in grinding body,
It is added in mixed process and accounts for the prefabricated mixed powders of TiC and Ti and 0.25% ~ 0.5% zinc stearate of urea gross mass, then at the uniform velocity
30 ~ 60min is mixed, mixed material is made；
5）Unidirectional to suppress with steel die by mixed material cold moudling made from previous step, pressing pressure is 180 ~ 250MPa,
Dwell time is 45 ~ 60s, and raw green compact is made in demoulding later；
6）Raw green compact is placed in vacuum carbon tube furnace and is heat-treated, heat treatment process is divided into low temperature removing urea and high temperature sintering
Two steps carry out；In low temperature removing urea process, it is 1 × 10 to control vacuum degree in vacuum carbon tube furnace-1~1×10-2Pa, control heating
Rate is sintered for 2 ~ 5 DEG C/min from room temperature to 400 DEG C, and 45 ~ 60min is kept the temperature at 400 DEG C；It is burnt subsequently into high temperature
Knot process, temperature are increased to 1180 ~ 1250 DEG C, are 1 × 10 in vacuum degree-1~1×10-22h is sintered under Pa environment；Sintering is completed
Afterwards, it is taken out after furnace cooling to room temperature and obtains the titanium-based porous material of TiC particles enhancing.
2. the preparation method of TiC granule intensified titaniums based porous materials according to claim 1, which is characterized 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, which is characterized 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, which is characterized 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, which is characterized in that the step
Rapid 2）In, the purity of argon being filled with into tank body is more than 99.99%.
6. the preparation method of TiC granule intensified titaniums based porous materials according to claim 1, which is characterized 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, which is characterized in that the step
Rapid 4）In, the purity of used urea is >=99%, and the purity of zinc stearate is >=99%.
8. the preparation method of TiC granule intensified titaniums based porous materials according to claim 1, which is characterized in that the step
Rapid 4）In, used urea is acicular morphology particle, and granularity is 0.8 ~ 1.1mm；The granularity of zinc stearate is 25 μm.
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| 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 |
| 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 |
| CN111822721B (en) * | 2020-07-14 | 2022-05-10 | 苏州大学 | Tungsten-doped titanium-based composite porous material and preparation method thereof |
| CN113046596B (en) * | 2021-03-25 | 2022-09-23 | 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 |
| 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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