CN108637261A - A kind of preparation method of TiAl/TMCs laminar composites - Google Patents
A kind of preparation method of TiAl/TMCs laminar composites Download PDFInfo
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- CN108637261A CN108637261A CN201810565021.6A CN201810565021A CN108637261A CN 108637261 A CN108637261 A CN 108637261A CN 201810565021 A CN201810565021 A CN 201810565021A CN 108637261 A CN108637261 A CN 108637261A
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- tial
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- laminar composites
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- 239000002131 composite material Substances 0.000 title claims abstract description 64
- 229910010038 TiAl Inorganic materials 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 81
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 43
- 239000000956 alloy Substances 0.000 claims abstract description 43
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 27
- 239000010439 graphite Substances 0.000 claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 239000010936 titanium Substances 0.000 claims abstract description 15
- 238000003892 spreading Methods 0.000 claims abstract description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003475 lamination Methods 0.000 claims abstract description 10
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 10
- 239000011159 matrix material Substances 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 9
- 229910001069 Ti alloy Inorganic materials 0.000 claims abstract description 8
- 239000010410 layer Substances 0.000 claims description 54
- 238000000498 ball milling Methods 0.000 claims description 13
- 229910033181 TiB2 Inorganic materials 0.000 claims description 10
- 239000012528 membrane Substances 0.000 claims description 10
- 239000002356 single layer Substances 0.000 claims description 10
- 239000002808 molecular sieve Substances 0.000 claims description 6
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 6
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical group B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 claims description 5
- 239000000470 constituent Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 230000002787 reinforcement Effects 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000007710 freezing Methods 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 17
- 238000000227 grinding Methods 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 14
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000009977 dual effect Effects 0.000 abstract description 3
- 230000003247 decreasing effect Effects 0.000 abstract description 2
- 239000011812 mixed powder Substances 0.000 description 12
- 239000000203 mixture Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000010406 interfacial reaction Methods 0.000 description 3
- BPJYAXCTOHRFDQ-UHFFFAOYSA-L tetracopper;2,4,6-trioxido-1,3,5,2,4,6-trioxatriarsinane;diacetate Chemical compound [Cu+2].[Cu+2].[Cu+2].[Cu+2].CC([O-])=O.CC([O-])=O.[O-][As]1O[As]([O-])O[As]([O-])O1.[O-][As]1O[As]([O-])O[As]([O-])O1 BPJYAXCTOHRFDQ-UHFFFAOYSA-L 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 206010058155 Heart alternation Diseases 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
Classifications
-
- 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
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
-
- B22F1/0003—
-
- 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
- B22F3/003—Apparatus, e.g. furnaces
-
- 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
- B22F3/004—Filling molds with powder
-
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a kind of preparation methods of TiAl/TMCs laminar composites, belong to field of compound material.For the present invention on the basis of keeping or being decreased slightly as low TiAl-base alloy high-temperature behavior, the room temperature intensity for solving TiAl-base alloy is low with the dual problem of poor toughness.The method of the present invention is specific as follows：One, titanium alloy powder is uniformly mixed first with low energy ball grinding technique with reinforced phase particle and obtains titanium matrix composite (TMCs) powder；Two and then TiAl alloy powder and TMCs powder alternatively layereds are laid down into acquisition stratiform powder blank in graphite jig using homemade lamination power spreading device；Three, TiAl/TMCs laminar composites finally are prepared using discharge plasma sintering (SPS) technology.The present invention provides a kind of high-strength, lightweight, heat-resisting structural material for aerospace.
Description
Technical field
The invention belongs to technical field of composite materials；More particularly to a kind of preparation side of TiAl/TMCs laminar composites
Method.
Background technology
TiAl-base alloy disclosure satisfy that not with the advantages that low-density, high specific stiffness, high specific strength and good high-temperature behavior
Carry out double requirements of the aerospace supersonic vehicle to structural weight reduction and elevated temperature strength, is that 21 century is most potential resistance to
One of hot lightweight structural material.Aviation High Performance Turbine Engine and thermal protection system are for high performance TiAl-base alloy at present
It is in urgent need.However TiAl-base alloy room temperature intensity is low, poor toughness, and it is difficult to deformation processing, significantly limit its functionization
Process.The current room-temperature property method for improving TiAl-base alloy includes mainly alloying and thermomechanical process etc., although one
Determine to improve the room-temperature property of TiAl-base alloy in degree, but complex process, the manufacturing cost high period is long, most importantly
Its intensity-plasticity (toughness) inversion problem can not be still solved, even intensity improves, then plasticity reduces.
Invention content
The present invention will solve existing TiAl-base alloy on the basis of keeping or being decreased slightly as low TiAl-base alloy high-temperature behavior
The low dual problem with poor toughness of room temperature intensity；The present invention provides a kind of preparation methods of TiAl/TMCs laminar composites.
The present invention is compound by titanium matrix composite (TMCs) and TiAl-base alloy progress, while having played TiAl-base alloy
Two big advantage of high-temperature behavior and the room-temperature property of titanium matrix composite realizes the effect of 1+1 ＞ 2.
The present invention obtains titanium matrix composite powder using low energy ball milling, then by titanium matrix composite powder and business
TiAl-base alloy powder alternative stacked powdering obtains TiAl/TMCs stratiform powder blanks, and discharge plasma is recycled to be sintered skill
Art (SPS) prepares TiAl/TMCs laminar composites.
The TiAl-base alloy layer of the present invention is alternately arranged composition layer structure material with titanium matrix composite layer, and TiAl bases close
Layer gold can ensure the high-temperature behavior of TiAl/TMCs laminar composites as refractory layer, and titanium matrix composite layer is as modeling
Property layer can ensure the plasticity and toughness of TiAl/TMCs laminar composites.The present invention TiAl/TMCs laminar composites with
TiAl-base alloy is compared, and under conditions of significantly reducing high-temperature behavior, while it is strong to obtain room temperature more better than TiAl-base alloy
Degree and toughness；SPS sintering, which is realized, to be rapidly heated and cools down, and is conducive to control interface layer reaction and refinement microstructure.
In order to solve the above technical problems, a kind of preparation method of TiAl/TMCs laminar composites of the present invention is specifically
It carries out in the steps below：
Step 1: being uniformly mixed titanium alloy powder with reinforced phase particle first with low energy ball milling, it is compound to obtain titanium-based
Material (TMCs) powder；
Step 2: being then uniformly layed in TiAl alloy powder and TMCs powder alternatively layered in graphite jig, obtain
TiAl/TMCs stratiform powder blanks；
Step 3: finally carrying out discharge plasma sintering (SPS) to the stratiform powder blank that step 2 obtains, obtain
TiAl/TMCs laminar composites.
It further limits, reinforcement described in step 1 is TiB2、C、TiC、B4C, one kind in B, SiC or in which several
It is arbitrary than mixing.
It further limits, TiAl alloy powder described in step 1 is TiAl-base alloy powder, Ti3In Al base alloy powders
It is one or more of arbitrary than mixing.
It further limits, reinforced phase granule content≤5vol.% in TMCs powder described in step 1.
It further limits, the thickness general control of every layer of laying of TiAl alloy powder is in 2mm or less in step 2.
It further limits, the thickness general control of every layer of laying of TMCs powder is in 2mm or less in step 2.
It further limits, according to each constituent element layer (TiAl in the TiAl/TMCs laminar composites of design in step 2
Based alloy layer with TMCs layers) thickness, utilize m=ρ × π r2× h (formula 1) calculates separately out the TiAl-base alloy of thickness in monolayer
The TMCs of required original TiAl bases pre-alloyed powder quality, that is, mono- part of TiAl base pre-alloyed powder quality and thickness in monolayer
Required original TMCs powder qualities, that is, mono- part of TMCs powder quality；
The quality (g) of m-powder in formula 1；Density (the g/cm of ρ-powder3)；R --- mould therefor radius (cm)；
H --- powder layer thickness (cm) can be regulated and controled by adjusting the relative mass of raw material powder type and various raw material powders
The ingredient (including reinforcement content etc.) of TiAl/TMCs laminar composites and constituent element layer thickness, need not be prepared separately in advance
Layers of material, but fine and close TiAl/TMCs laminar composites are directly prepared by SPS sintering.
It further limits, discharge plasma sintering is specifically to be carried out by operations described below in step 3：It will be equipped with
The graphite jig of TiAl/TMCs stratiform powder blanks is placed in SPS sintering furnaces, and closed furnace body vacuumizes simultaneously, true when furnace body
Reciprocal of duty cycle reaches 10-2When Pa, starts to apply the progress precompressed of 10MPa pressure, be then warming up to the rate of 50~100 DEG C/min
1000 DEG C, start to gradually rise pressure at this time, when it is 1000~1300 DEG C that in-furnace temperature, which reaches sintering temperature, by pressure rise
To 30~70MPa, then simultaneously 10~50min of heat-insulation pressure keeping；At the end of heat preservations, 500 DEG C are quickly cooled to, pressure is removed,
Cool to room temperature with the furnace.
Further limit, in step 2 be laid with powder lamination power spreading device include end cap 1, end 2, telescopic rod 3,
Fixed plate 4, upper connecting rod 5, lower connecting rod 6, sub-sieve 7, L-shaped baffle 8, straight baffle 9, x are to vibrator 10 and y to vibrator
11；
The longitudinal section of the end cap 1 is in convex shape, and 1 upper end edge axis direction of axis line of end cap is equipped with through-hole, and 1 lower end of end cap is set
Inner groovy is set, is connected at the top of via bottoms and inner groovy；
The end 2 is inserted into the inner groovy of end cap 1 and is fixedly connected with end cap 1, is equipped with and leads to along direction of axis line in end 2
Hole；
The bottom end of the telescopic rod 3 passes through the through-hole of end cap 1 and end 2 and stretches out the bottom of end 2, telescopic rod 3 and end
Cap 1 is limited by bolt, and bottom end and the fixed plate 4 of telescopic rod 3 are detachably connected；
2 outer wall top of the end is evenly arranged with 6 upper connecting rods 5, and top and the end 2 of each upper connecting rod 5 are cut with scissors
It connects, the upper articulation of the bottom end of upper connecting rod 5 and spaced straight baffle 9 and L-shaped baffle 8；
Each 5 underface of upper connecting rod of 2 outer wall of the end is hinged with lower connecting rod 6, lower connecting rod 6 and upper connecting rod 5
Be arranged in parallel, the bottom end of each lower connecting rod 6 passes through the limit hole in fixed plate 4, the bottom end of lower connecting rod 6 with it is spaced
The middle part of straight baffle 9 and L-shaped baffle 8 is hinged,
The lower part of the straight baffle 9 is equipped with x to vibrator 10 (horizontal direction vibration), the top surface of 8 horizontal component of L-shaped baffle
Y is provided with to vibrator 11 (vertical vibration),
The x can be against to vibrator 10 on the outer wall of molecular sieve 7, and y can be against the bottom of molecular sieve 7 to vibrator 11；
Symmetrical position is fixedly connected with transverse support bar 12 on 1 outer wall of the end cap, and transverse support bar 12 is in addition
One end is fixedly connected with the top of retractable support column 13, and 13 bottom of retractable support column is fixedly connected with support base 14；
The diameter of the sub-sieve 7 is more than the outer diameter of graphite jig 15, and sub-sieve 7 is placed on graphite jig 15, divides sample
7 bottoms are sieved along direction of axis line setting lower limit circle 72, the diameter of the diameter of lower limit circle 72 than the membrane cavity 151 of graphite jig 15
The bottom inside of big 2~4mm, sub-sieve 7 are provided with upper limit circle 71,71 a diameter of stone of upper limit circle along direction of axis line
The diameter of 15 membrane cavity 151 of black mold is equal.
The present invention carries out machinery using above-mentioned lamination power spreading device and is laid with powder process：It is weighed with photoelectric analytical balance
TiB2/ TC4 mixed-powders spreading is in the upper limit circle 71 of sub-sieve 7, and start whole X keeps mixed-powder equal to vibrator 10
It is even to be distributed on sieve；It is last to open whole X simultaneously to vibrator 10 and Y-direction vibrator 11, drive sub-sieve 7 in vertical direction
Upper vibrations ensure that powder is drained to by sieve in graphite jig 15.All shakes are closed after powder all leaks into graphite jig 15
Dynamic device, single layer TiB2/ TC4 mixed-powder powderings terminate.Again Ti-46Al-2Cr-2Nb prealloy powder is weighed with photoelectric analytical balance
Last spreading is in the upper limit circle 71 of sub-sieve 7, and start whole X makes mixed-powder be evenly distributed on sieve to vibrator 10
On；It is last to open whole X simultaneously to vibrator 10 and Y-direction vibrator 11, it drives sub-sieve 7 to shake in the vertical direction, ensures
Powder is drained to by sieve in graphite jig 15.All vibrators, single layer Ti- are closed after powder all leaks into die cavity 151
46Al-2Cr-2Nb pre-alloyed powder powderings terminate.It repeats the above process, obtains Layering powder green body；Using mechanical laminated powdering
Compared with traditional manual powdering, the thickness in monolayer size of powder, layer thickness uniformity significantly improve device, and powdering efficiency is significantly
It improves.
The method of the present invention realization is rapidly heated and cools down, and can effectively inhibit the microcosmic of TiAl/TMCs laminar composites
Microstructure coarsening reduces the interface layer reaction of each constituent element, is conducive to control interface layer and react that TMCs can be retained to greatest extent
Layer be used as ductile bed, while rapid temperature rise and drop be conducive to obtain fine microstructures TiAl-base alloy layer with TMCs layers, in unobvious
Under conditions of reducing high-temperature behavior, while obtaining room temperature intensity more better than TiAl-base alloy and toughness.
The present invention prepares TiAl/TMCs layers in such a way that low energy ball milling mixes powder-alternative stacked powdering-SPS sintering
Shape composite material, TMCs layers and the brittle TiAl-base alloy layer of plasticity are sintered by mechanical alternans lamination powdering combination SPS
Mode directly obtain, do not need previously prepared layers of material, simplify preparation process path, saved process costs.
Ductile bed of the present invention and brittle layer material category range of choice are wide, by adjust brittle layer, ductile bed type with
The type and content of reinforcement in Thickness ratio, ductile bed realize the structural constituent and mechanical property of TiAl/TMCs laminar composites
Can it is controllable.
Description of the drawings
Fig. 1 is the structural schematic diagram for the lamination power spreading device for being laid with powder；
Fig. 2 is sub-sieve and graphite jig assembling schematic diagram；
Fig. 3 is discharge plasma sintering (SPS) process schematic；
Fig. 4 is the pictorial diagram of 400 (2vol.%TiB/TC4) -400TiAl laminar composites；
Fig. 5 is the microstructure morphology of 400 (2vol.%TiB/TC4) -400TiAl laminar composites, (a) allusion quotation in figure
(TiB/TC4)-TiAl scanned photographs of type layer structure, (b) interfacial reaction situation (Ti35 μm of Al conversion zones ＜)；
Fig. 6 is the crack propagation path of 400 (2vol.%TiB/TC4) -400TiAl laminar composites；
Fig. 7 is 800 (2vol.%TiB/TC4) -400TiAl laminar composite microstructure morphologies；
In Fig. 1 and 2,1 --- end cap, 2 --- end, 3 --- telescopic rods, 4 --- fixed plate, 5 --- upper connecting rod,
6 --- lower connecting rod, 7 --- sub-sieve, 71 --- upper limit circle, 72 --- lower limit circle, 8 --- L-shaped baffle, 9 --- it is straight
Baffle, 10 --- x is to vibrator, and 11 --- y is to vibrator, and 12 --- supporting rod, 13 --- retractable support column, 14 --- support
Seat, 15 --- graphite jig, 151 --- membrane cavity, 16 --- pressure head, 17 --- sample.
Specific implementation mode
Embodiment 1：The present embodiment prepares 400 (2vol.%TiB/TC4) -400TiAl laminar composites.
Titanium matrix composite (the 2vol.%TiB/ for the TiB enhancings that the ductile bed that this example selects is 2% for volume content
Ti), brittle layer is Ti-46Al-2Cr-2Nb dual alloy billets (TiAl-base alloy), and powder-friendship is mixed using low energy ball milling
Excellent (the 2vol.%TiB/TC4)-TiAl laminar composites of comprehensive mechanical property are prepared for lamination powdering-SPS sintering process,
Powdering is carried out using lamination power spreading device, is illustrated in conjunction with Fig. 1 and 2, two the step of the present embodiment in be laid with the dress of powder
It includes end cap 1, end 2, telescopic rod 3, fixed plate 4, upper connecting rod 5, lower connecting rod 6, sub-sieve 7, L to set (as illustrated in fig. 1 and 2)
Shape baffle 8, straight baffle 9, x are to vibrator 10 and y to vibrator 11；
The vibrator is by vibrations motor, shell, power supply composition, and vibrations motor power is 0.8w, voltage 3V, outside vibrator
Shell is plastic shell, and power supply is two section 1.5V lithium ion button shape cells；
The aperture size of the sub-sieve is equal to the maximum particle diameter of ductile bed powder and brittle layer powder；
The longitudinal section of the end cap 1 is in convex shape, and 1 upper end edge axis direction of axis line of end cap is equipped with through-hole, and 1 lower end of end cap is set
Inner groovy is set, is connected at the top of via bottoms and inner groovy；
The end 2 is inserted into the inner groovy of end cap 1 and is fixedly connected by welding with end cap 1, along axial line side in end 2
To equipped with through-hole；
The end 2 is regular hexagonal prism shape, and indent groove shape is corresponding with end 2, and the end and end cap are stainless
Steel material；
The bottom end of the telescopic rod 3 passes through the through-hole of end cap 1 and end 2 and stretches out the bottom of end 2, telescopic rod 3 and end
Cap 1 is limited by bolt, and bottom end and the fixed plate 4 of telescopic rod 3 are bolted；
2 outer wall top of the end is evenly arranged with 6 upper connecting rods 5, and top and the end 2 of each upper connecting rod 5 are cut with scissors
It connects, the upper articulation of the bottom end of upper connecting rod 5 and spaced straight baffle 9 and L-shaped baffle 8；
Each 5 underface of upper connecting rod of 2 outer wall of the end is hinged with lower connecting rod 6, lower connecting rod 6 and upper connecting rod 5
Be arranged in parallel, the bottom end of each lower connecting rod 6 passes through the limit hole in fixed plate 4, the bottom end of lower connecting rod 6 with it is spaced
The middle part of straight baffle 9 and L-shaped baffle 8 is hinged；
The lower part of the straight baffle 9 is equipped with x to vibrator 10 (horizontal direction vibration), the top surface of 8 horizontal component of L-shaped baffle
Y is provided with to vibrator 11 (vertical vibration)；
The baffle is with vibrator by being adhesively fixed；The L-shaped baffle 8, straight baffle 9, upper connecting rod 5 and lower connecting rod
6 be aluminium alloy；
The x can be against to vibrator 10 on the outer wall of molecular sieve 7, and y can be against the bottom of molecular sieve 7 to vibrator 11；
Symmetrical position, which is fixedly connected by welding, on 1 outer wall of the end cap transverse support bar 12 (stainless steel tube), cross-brace
The other end of bar 12 and the top of retractable support column 13 are fixedly connected by welding, 13 bottom of retractable support column and support base 14
(stainless steel hollow base) is fixedly connected with the retractable support column 13；The retractable support column 13 is made of stainless steel tube to be formed；
The diameter of the sub-sieve 7 is more than the outer diameter of graphite jig 15, and lower limit is arranged along direction of axis line in 7 bottom of sub-sieve
Position 72 (material is aluminium alloy) of circle, the diameter of lower limit circle 72 is bigger 2mm than the diameter of the membrane cavity 151 of graphite jig 15, sub-sieve 7
It is placed on graphite jig 15 and lower limit circle 72 is contacted with the top of graphite jig 15, the bottom inside of sub-sieve 7 is along axle center
Line direction is provided with upper limit circle 71 (material is plastics), 71 a diameter of graphite jig of upper limit circle, 15 membrane cavity 151 it is straight
Diameter is equal.
The specific preparation process of the present embodiment is as described below：
Step 1: low energy ball milling mixes powder：2vol.%TiB/Ti composite layers are to pass through TiB in this example2Particle and quotient
Industry TC4 titanium alloy powders first pass through low energy ball milling and mix the powder original position in-situ reaction acquisition in subsequent SPS sintering processes again.Cause
This first has to TiB2Particle and business TC4 titanium alloy powders are uniform by ball milling mixing, and detailed process is as follows：Due to design
Finally TiB/TC4 composite material powder layer thickness is 400 μm in (2vol.%TiB/TC4)-TiAl laminar composites, and TiB
Volume content is 2%, therefore can calculate the original TiB to obtain needed for the TiB/TC4 composite layers of 400 μ m-thicks2/
TC4 mixed-powder quality is 5.11g, by calculating TiB2The mass fraction of particle is 1.2wt.%, thus to obtain TC4 titanium alloys
Powder quality is 5.049g, TiB2The quality of particle is 0.061g (wherein ρTC4=4.52g/cm3, ρTiB2=4.45g/cm3).By
It it is 12 layers in the number of plies of the TiB/TC4 composite materials of design, therefore, TC4 titanium alloy powder gross masses are 60.588g, TiB2
The quality of grain is 0.732g.The TiB of the TC4 titanium alloy powders and 0.732g of 60.588g is weighed with photoelectric analytical balance2Particle,
It is put into QM-1SP4 type planetary type ball-milling tanks simultaneously, adds the GCr15 bearing steel balls of 245.280g as ball-milling medium, argon
Ball milling is carried out in gas atmosphere.Ball-milling technology is：Rotating speed is that 150rpm Ball-milling Times are 5h, ratio of grinding media to material 4:1.Uniformly mixed
TiB2The taking-up of/TC4 mixed-powders is placed in vacuum glove box for use.
Step 2: alternative stacked powdering：The graphite jig internal diameter d=60mm that SPS sintering uses, TiAl-base alloy layer thickness
H=400 μm, TiAl-base alloy density is ρTiAl=3.8g/cm3, therefore calculate single layer TiAl-base alloy institute according to formula (1)
Single part of quality m of the Ti-46Al-2Cr-2Nb pre-alloyed powders neededTiAlFor 4.30g.And by step 1 it is found that obtain 400 μm
Original TiB needed for thick TiB/TC4 composite layers2Single part of quality of/TC4 mixed-powders is 5.11g.
First, according to the operation of step 2 in invention content by SPS sintering graphites mold and homemade lamination power spreading device
According to Fig. 1 assemble for use；Secondly, the TiB of 5.11g is weighed with photoelectric analytical balance2/ TC4 mixed-powders spreading is dividing
In the upper limit circle 71 of sample sieve 7, and start whole X makes mixed-powder be evenly distributed on sieve to vibrator 10；Simultaneously finally
Whole X is opened to vibrator 10 and Y-direction vibrator 11, drives sub-sieve 7 to shake in the vertical direction, ensures that powder passes through sieve
It drains in the membrane cavity 151 of graphite jig 15.All vibrators, single layer TiB are closed after powder all leaks into membrane cavity 1512/TC4
Mixed-powder powdering terminates.The Ti-46Al-2Cr-2Nb pre-alloyed powders spreading for weighing 4.30g with photoelectric analytical balance again is dividing
In the upper limit circle of sample sieve, and start whole X makes mixed-powder be evenly distributed on sieve to vibrator 10；Finally open simultaneously
Whole X drive sub-sieve 7 to shake in the vertical direction to vibrator 10 and Y-direction vibrator 11, ensure that powder is drained to by sieve
In the membrane cavity 151 of graphite jig 15.All vibrators, single layer Ti-46Al- are closed after the membrane cavity 151 that powder is all leak into
2Cr-2Nb pre-alloyed powder powderings terminate.It repeats the above process, obtains (2vol.%TiB/TC4)-TiAl Layering powder green bodies.
Step 3: SPS is sintered：The same graphite of (2vol.%TiB/TC4)-TiAl Layering powder green bodies that program two is obtained
Mold is placed in SPS freezings of a furnace (as shown in Figure 3) and closed furnace body while vacuumizing together, when the vacuum degree of furnace body reaches 10-2Pa
When, start to apply the progress precompressed of 10MPa pressure, it is therefore an objective to which the consistency for improving stratiform powder blank is convenient for follow-up sintering；Then
It is rapidly heated to 1000 DEG C with the rate of 100 DEG C/min, starts to gradually rise pressure at this time, when in-furnace temperature reaches sintering
When temperature (1250 DEG C), by pressure rise to 50MPa, while heat-insulation pressure keeping 10min；At the end of heat preservation, it is quickly cooled to 500
DEG C, pressure is removed, cools to room temperature with the furnace, finally prepares fully dense 400 (2vol.%TiB/TC4) -400TiAl stratiforms
Composite material, it is in kind as shown in Figure 4.Microstructure is as shown in Figure 5.By Fig. 5 a it is found that (2vol.%TiB/TC4)-TiAl is compound
Typical layer structure feature is presented in material, by (2vol.%TiB/TC4) composite layer and 400 μ m-thicks of 400 μ m-thicks
TiAl-base alloy layer is alternately arranged composition, and TiB/TC4 composite layers are reacted with TiAl-base alloy bed boundary and controlled very well
System, only occurs slight interfacial reaction, interfacial reaction layer thickness is about 5 μm, as shown in Figure 5 b.400 (2vol.%TiB/TC4)-
The Mechanics Performance Testing of 400TiAl laminar composites shows：Its tensile strength reaches 580MPa, bending strength 988MPa,
Fracture Toughness is up to 36.2MPam1/2, the TiB/TC4 composite materials of plasticity are introduced in brittle TiAl-base alloy,
Toughness and intensity significantly improve, and have reached desired effect.Its fracture process crack propagation path is as shown in Figure 6.
Embodiment 2：The present embodiment prepares 800 (2vol.%TiB/TC4) -400TiAl laminar composites, in this example,
Difference lies in the thickness of ductile bed 2vol.%TiB/TC4 composite layers to become 800 μm by 400 μm with example 1, therefore
Single part of quality of 2vol.%TiB/TC4 mixed-powders increases to 10.22g, and the thickness of brittle TiAl-base alloy layer is constant.
Other steps and parameter are same as Example 1.
Microstructure such as Fig. 7 of 800 (2vol.%TiB/TC4) -400TiAl laminar composites manufactured in the present embodiment
It is shown.As shown in Figure 7, typical layer structure feature is presented in (2vol.%TiB/TC4)-TiAl composite materials, by 800 μ m-thicks
(2vol.%TiB/TC4) composite layer and the TiAl-base alloy layers of 400 μ m-thicks be alternately arranged composition.800 (2vol.%
TiB/TC4) Mechanics Performance Testing of -400TiAl laminar composites shows：Its tensile strength is 647MPa, and bending strength is high
Up to 1460MPa, Fracture Toughness is up to 53MPam1/2, it can be seen that, by the TiB/TC4 composite layers for adjusting plasticity
Thickness, Toughness and intensity can be significantly improved further, therefore, the lamination powdering combination SPS developed using the present invention
Sintering technology can prepare the excellent TiAl/TMCs laminar composites of comprehensive mechanical property, can provide one for aerospace
High-strength, lightweight, heat-resisting structural material are planted, desired effect has been reached.
Claims (9)
1. a kind of preparation method of TiAl/TMCs laminar composites, it is characterised in that the preparation method is in the steps below
It carries out：
Step 1: being uniformly mixed titanium alloy powder with reinforced phase particle first with low energy ball milling, titanium matrix composite is obtained
(TMCs) powder；
Step 2: being then uniformly layed in TiAl alloy powder and TMCs powder alternatively layered in graphite jig, TiAl/ is obtained
TMCs stratiform powder blanks；
Step 3: finally obtaining stratiform powder blank to step 2 carries out discharge plasma sintering (SPS), TiAl/ is obtained
TMCs laminar composites.
2. a kind of preparation method of TiAl/TMCs laminar composites according to claim 1, it is characterised in that step 1
The reinforcement is TiB2、C、TiC、B4C, one kind in B, SiC or in which several arbitrary ratio mixing.
3. a kind of preparation method of TiAl/TMCs laminar composites according to claim 1, it is characterised in that step 1
The TiAl alloy powder is TiAl-base alloy powder, Ti3The arbitrary ratio mixing of one or more of Al base alloy powders.
4. a kind of preparation method of TiAl/TMCs laminar composites according to claim 1, it is characterised in that step 1
Reinforced phase granule content≤5vol.% in the TMCs powder.
5. a kind of preparation method of TiAl/TMCs laminar composites according to claim 1, it is characterised in that step 2
The thickness general control of every layer of laying of middle TiAl alloy powder is in 2mm or less.
6. a kind of preparation method of TiAl/TMCs laminar composites according to claim 1, it is characterised in that step 2
The thickness general control of every layer of laying of middle TMCs powder is in 2mm or less.
7. a kind of preparation method of TiAl/TMCs laminar composites according to claim 1, it is characterised in that step 2
The thickness of each constituent element layer (TiAl-base alloy layer and TMCs layers), profit in the middle TiAl/TMCs laminar composites according to design
With m=ρ × π r2× h (formula 1) calculates separately out the required original TiAl bases prealloy powder of TiAl-base alloy of thickness in monolayer
The required original TMCs powder qualities of TMCs of last quality, that is, mono- part of TiAl base pre-alloyed powder quality and thickness in monolayer are
Single part of TMCs powder quality；
The quality (g) of m-powder in formula 1；
Density (the g/cm of ρ-powder3)；
R --- mould therefor radius (cm)；
H --- powder layer thickness (cm).
8. a kind of preparation method of TiAl/TMCs laminar composites according to claim 1, it is characterised in that step 3
Middle discharge plasma sintering is specifically to be carried out by operations described below：By the graphite mo(u)ld equipped with TiAl/TMCs stratiform powder blanks
Tool is placed in SPS freezings of a furnace, and closed furnace body vacuumizes simultaneously, when the vacuum degree of furnace body reaches 10-2When Pa, start to apply 10MPa pressures
Power carries out precompressed, then carries out being warming up to 1000 DEG C with the rate of 50~100 DEG C/min, starts to gradually rise pressure at this time, when
In-furnace temperature reach sintering temperature be 1000~1300 DEG C when, by pressure rise to 30~70MPa, then simultaneously heat-insulation pressure keeping 10
~50min；At the end of heat preservation, 500 DEG C are quickly cooled to, pressure is removed, cools to room temperature with the furnace.
9. a kind of preparation method of TiAl/TMCs laminar composites according to claim 1, it is characterised in that step 2
The middle lamination power spreading device for being laid with powder includes end cap (1), end (2), telescopic rod (3), fixed plate (4), upper connecting rod
(5), lower connecting rod (6), sub-sieve (7), L-shaped baffle (8), straight baffle (9), x are to vibrator (10) and y to vibrator (11)；
The longitudinal section of the end cap (1) is in convex shape, and end cap (1) upper end edge axis direction of axis line is equipped with through-hole, end cap (1) lower end
Inner groovy is set, is connected at the top of via bottoms and inner groovy；
The end (2) is inserted into the inner groovy of end cap (1) and is fixedly connected with end cap (1), is set along direction of axis line in end (2)
There is through-hole；
The bottom end of the telescopic rod (3) passes through the through-hole of end cap (1) and end (2) and stretches out the bottom of end (2), telescopic rod
(3) it is limited by bolt with end cap (1), bottom end and the fixed plate (4) of telescopic rod (3) are bolted；
End (2) the outer wall top is evenly arranged with 6 upper connecting rods (5), the top and end of each upper connecting rod (5)
(2) hinged, the upper articulation of the bottom end of upper connecting rod (5) and spaced straight baffle (9) and L-shaped baffle (8)；
Lower connecting rod (6), lower connecting rod (6) and upper connection are hinged with immediately below each upper connecting rod of end (2) outer wall (5)
Bar (5) is arranged in parallel, and the bottom end of each lower connecting rod (6) passes through the limit hole in fixed plate (4), the bottom end of lower connecting rod (6)
It is hinged with the middle part of spaced straight baffle (9) and L-shaped baffle (8)；
The lower part of the straight baffle (9) is equipped with x to vibrator (10), and the top surface of L-shaped baffle (8) horizontal component is provided with y to shake
Dynamic device (11)；
The x can be against to vibrator (10) on the outer wall of molecular sieve (7), and y can be against the bottom of molecular sieve (7) to vibrator (11)
Portion；
Symmetrical position is fixedly connected with transverse support bar (12) on end cap (1) outer wall, transverse support bar (12) it is another
Outer one end is fixedly connected with the top of retractable support column (13), and retractable support column (13) bottom is fixedly connected with support base (14)；
The diameter of the sub-sieve (7) is more than the outer diameter of graphite jig (15), and sub-sieve (7) bottom is under direction of axis line setting
The diameter of spacing collar (72), lower limit circle (72) is bigger 2~4mm than the diameter of the membrane cavity (151) of graphite jig (15), sub-sieve
(7) bottom inside is provided with upper limit circle (71), upper limit circle (71) a diameter of graphite jig (15) film along direction of axis line
The diameter of chamber is equal, and sub-sieve (7) is placed on graphite jig (15) and the top of lower limit circle (72) and graphite jig (15)
Contact.
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