CN110315083A - A method of quickly preparing fibre reinforced titanium alloy laminar composite - Google Patents
A method of quickly preparing fibre reinforced titanium alloy laminar composite Download PDFInfo
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- CN110315083A CN110315083A CN201910675352.XA CN201910675352A CN110315083A CN 110315083 A CN110315083 A CN 110315083A CN 201910675352 A CN201910675352 A CN 201910675352A CN 110315083 A CN110315083 A CN 110315083A
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- titanium alloy
- nickel
- cloth
- fibre reinforced
- laminar composite
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 136
- 239000002131 composite material Substances 0.000 title claims abstract description 62
- 239000000835 fiber Substances 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 48
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 186
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 99
- 239000004917 carbon fiber Substances 0.000 claims abstract description 99
- 239000004744 fabric Substances 0.000 claims abstract description 96
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 93
- 238000005245 sintering Methods 0.000 claims abstract description 56
- 229910002114 biscuit porcelain Inorganic materials 0.000 claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 35
- 238000007747 plating Methods 0.000 claims abstract description 34
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 32
- 230000008569 process Effects 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 21
- 238000007599 discharging Methods 0.000 claims abstract description 15
- 238000002791 soaking Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 67
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 30
- 230000001235 sensitizing effect Effects 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000012153 distilled water Substances 0.000 claims description 17
- 230000003213 activating effect Effects 0.000 claims description 14
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 13
- 229910002666 PdCl2 Inorganic materials 0.000 claims description 10
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 8
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 8
- 230000009467 reduction Effects 0.000 claims description 8
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 7
- 239000001632 sodium acetate Substances 0.000 claims description 7
- 235000017281 sodium acetate Nutrition 0.000 claims description 7
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 229960004756 ethanol Drugs 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 239000001509 sodium citrate Substances 0.000 claims description 6
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 6
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 244000248349 Citrus limon Species 0.000 claims description 2
- 235000005979 Citrus limon Nutrition 0.000 claims description 2
- 101150003085 Pdcl gene Proteins 0.000 claims 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 43
- 239000010410 layer Substances 0.000 abstract description 37
- 239000000843 powder Substances 0.000 abstract description 18
- 230000000694 effects Effects 0.000 abstract description 5
- 239000002344 surface layer Substances 0.000 abstract description 4
- 238000004140 cleaning Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 20
- 239000000463 material Substances 0.000 description 14
- 230000008859 change Effects 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 9
- 239000010936 titanium Substances 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- 229910052719 titanium Inorganic materials 0.000 description 8
- 239000000956 alloy Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000004321 preservation Methods 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- VMWYVTOHEQQZHQ-UHFFFAOYSA-N methylidynenickel Chemical compound [Ni]#[C] VMWYVTOHEQQZHQ-UHFFFAOYSA-N 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 229910000906 Bronze Inorganic materials 0.000 description 1
- 229910001339 C alloy Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000010974 bronze Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- GQZXNSPRSGFJLY-UHFFFAOYSA-N hydroxyphosphanone Chemical compound OP=O GQZXNSPRSGFJLY-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002023 wood 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
- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- 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
- B22F7/04—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 with one or more layers not made from powder, e.g. made from solid metal
-
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
The invention discloses a kind of method for quickly preparing fibre reinforced titanium alloy laminar composite, this method comprises: one, will be dry after carbon cloth ultrasonic cleaning；Two, carbon cloth after drying is successively sensitized, is activated and is restored simultaneously cleaning, drying；Three, carbon cloth nickel plating after drying is obtained into nickel-coated carbon fibers cloth；Four, it is laid with nickel-coated carbon fibers layer of cloth after Titanium Powder to be laid on to the mold of plasma hot pressed sintering, titanium alloy bisque is re-layed, is repeated in above-mentioned bisque and layer of cloth laying process, obtain fibre reinforced titanium alloy laminar composite through plasma discharging hot pressed sintering.The present invention is using heating rate is fast, soaking time is short and pressure is high during plasma discharging hot pressed sintering, and nickel-coated carbon fibers cloth plating nickel on surface layer quickly prepares fibre reinforced titanium alloy laminar composite to the insulating effect of carbon fiber and titanium alloy powder, the integrality that ensure that carbon fiber improves the mechanical property of fibre reinforced titanium alloy laminar composite.
Description
Technical field
The invention belongs to technical field of material, and in particular to it is multiple that one kind quickly prepares fibre reinforced titanium alloy stratiform
The method of condensation material.
Background technique
Titanium or titanium alloy possesses higher specific strength, specific stiffness and good as the lightweight structure material haveing excellent performance
Processability, corrosion resistance and high temperature resistance, therefore it is in space flight and aviation, ship automobile, weapons engineering, medical instrument and chemical industry energy
The various fields such as source have a extensive future.But titanium or titanium alloy wears no resistance, the more low weakness of hardness hinders it in engineering
Application.Adjoint various demands are developed rapidly to meet high and new technology, are badly in need of research and development new titanium alloy composite material to meet
The demand of aerospace career development.
Fibre reinforced titanium alloy composite material has many advantages, such as that density is low, specific strength is high, stretch-proof and specific modulus are high, is
A kind of high performance lightweight structural material.Since titanium alloy under hot environment and most toughened fibers easily react and generate interface
Product influences the performance of material, causes fibre reinforced titanium and composite materials property to reduce, therefore prepare fiber reinforced titanium
The technique of alloy composite materials require it is more stringent and complicated, it is general using solid phase the preparation method, still, its boundary under the high temperature conditions
Face reaction is still relatively more violent.Therefore, it is intended that being modified by process for modifying surface carbon fiber surface, effective control interface
The extent of reaction, thus the structure feature of effective protection carbon fiber.
Summary of the invention
Technical problem to be solved by the present invention lies in view of the above shortcomings of the prior art, provide one kind quickly to prepare carbon
The method of fiber reinforcement titanium alloy laminar composite.This method utilizes heating faster during plasma discharging hot pressed sintering
Rate, shorter soaking time and higher pressure and nickel-coated carbon fibers cloth plating nickel on surface layer are to carbon fiber and Titanium Powder
The insulating effect at end quickly prepares fibre reinforced titanium alloy laminar composite, effectively prevent in hot environment carbon fiber with
Titanium alloy powder, which reacts, generates boundary material, ensure that the complete of carbon fiber in fibre reinforced titanium alloy laminar composite
Whole property is conducive to the mechanical property for improving fibre reinforced titanium alloy laminar composite.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: it is a kind of quickly to prepare the conjunction of fibre reinforced titanium
The method of golden laminar composite, which is characterized in that method includes the following steps:
It is then 100 in temperature Step 1: carbon cloth is put into ultrasonic cleaning 10min~30min in dehydrated alcohol
Dry 10h~20h under conditions of DEG C；
Step 2: the carbon cloth in step 1 after drying is carried out sensitized treatment using sensitizing solution, then using work
Change and be activated in liquid, then reduction treatment is carried out using sodium hypophosphite aqueous solution, dries after washing with distilled water；It is described quick
Change liquid by SnCl2, mass concentration be 37% hydrochloric acid solution and distilled water composition, the activating solution is by PdCl2, ethyl alcohol and distillation
Water composition；
Step 3: carbon cloth after drying in step 2 is put into nickel plating solution, it is then heated to 60 DEG C~90
DEG C heat preservation 10min~120min, take out drying after obtain nickel-coated carbon fibers cloth；The nickel plating layer thick of the nickel-coated carbon fibers cloth is
200nm~500nm；
It is formed Step 4: Titanium Powder is uniformly laid in the mold of plasma hot pressed sintering with a thickness of 0.5mm~2mm
The first titanium alloy bisque, then by nickel-coated carbon fibers cloth obtained in one layer of step 3 be laid on titanium alloy bisque formed plate
Nickel carbon fibre cloth layer, then Titanium Powder is uniformly laid on nickel-coated carbon fibers layer of cloth and forms thickness and the first titanium alloy bisque phase
Deng the second titanium alloy bisque, be repeated in the forming process of the first titanium alloy bisque, the forming process of nickel-coated carbon fibers layer of cloth
With the forming process of the second titanium alloy bisque, until the total height of titanium alloy bisque and nickel-coated carbon fibers layer of cloth is plasma hot pressing
The 60%~70% of the mold height of sintering is sent into plasma hot-pressed sintering furnace and carries out plasma discharging hot pressed sintering, cooling
After obtain fibre reinforced titanium alloy laminar composite；The technological parameter of the plasma hot pressed sintering are as follows: vacuum degree 1.0 ×
10-3Pa~3.0 × 10-3Pa, heating rate be 50 DEG C/min~100 DEG C/min, 800 DEG C~1100 DEG C of sintering temperature, pressure
40MPa~180MPa, soaking time 5min~10min；The granularity of the Titanium Powder is 15 μm~45 μm.
The present invention first by carbon cloth successively it is preprocessed remove carbon cloth surface impurity, make carbon fiber through sensitized treatment
The substance that dimension cloth adsorption is easily oxidized, activated processing makes carbon cloth Surface Creation catalytic active layer, through reduction treatment
The palladium chloride reduction on carbon cloth surface will be remained in, then carries out nickel plating on carbon cloth surface and obtain nickel-coated carbon fibers cloth,
Titanium alloy powder is successively spread with nickel-coated carbon fibers cloth according to titanium alloy powder-nickel-coated carbon fibers cloth-titanium alloy powder sequence
It is located at mold and forms multilayered structure, carry out plasma discharging hot pressed sintering and prepare fibre reinforced titanium alloy laminar composite,
Utilize heating rate faster during plasma discharging hot pressed sintering, shorter soaking time and higher pressure, and plating
Nickel carbon cloth plating nickel on surface layer effectively prevents carbon fiber in hot environment to the insulating effect of carbon fiber and titanium alloy powder
It reacts with titanium alloy powder and generates boundary material, ensure that carbon fiber in fibre reinforced titanium alloy laminar composite
Integrality is conducive to the mechanical property for improving fibre reinforced titanium alloy laminar composite.
The method that above-mentioned one kind quickly prepares fibre reinforced titanium alloy laminar composite, which is characterized in that step
SnCl in sensitizing solution described in two2Concentration be 1g/L~20g/L.The sensitizing solution further improves carbon cloth surface to easy
The suction-operated for the substance being oxidized is conducive to going on smoothly for subsequent nickel plating technology.
The method that above-mentioned one kind quickly prepares fibre reinforced titanium alloy laminar composite, which is characterized in that step
The mass concentration of hydrochloric acid solution is 37% in sensitizing solution described in two, and the mass percent of hydrochloric acid solution is 1%~5%.This is quick
The mass concentration and mass percent for changing hydrochloric acid solution in liquid are to prepare the most common parameter of sensitizing solution.
The method that above-mentioned one kind quickly prepares fibre reinforced titanium alloy laminar composite, which is characterized in that step
PdCl in activating solution described in two2Concentration be 0.1g/L~0.6g/L.The activating solution promotes carbon cloth Surface Creation and urges
Change active layer.
The method that above-mentioned one kind quickly prepares fibre reinforced titanium alloy laminar composite, which is characterized in that step
The concentration of sodium hypophosphite is 5g/L~50g/L in nickel plating solution described in three, and the concentration of nickel sulfate is 5g/L~50g/L, lemon
The concentration of sour sodium is 1g/L~20g/L, and the concentration of sodium acetate is 1g/L~30g/L.The nickel plating of said components and concentration composition is molten
Liquid provides enough reducing agents, nickel element and complexing agent for nickel plating technology, is conducive to the nickel-coated carbon fibers cloth for obtaining high quality, from
And it avoids during plasma discharging hot pressed sintering carbon fiber and titanium alloy powder in hot environment and reacts and generate interface
Substance.
Compared with the prior art, the present invention has the following advantages:
1, the present invention using heating rate faster during plasma discharging hot pressed sintering, shorter soaking time and compared with
High pressure and nickel-coated carbon fibers cloth plating nickel on surface layer quickly prepares carbon fiber to the insulating effect of carbon fiber and titanium alloy powder
Dimension enhancing titanium alloy laminar composite effectively prevents carbon fiber and titanium alloy powder in hot environment and reacts to generate boundary
Face substance ensure that the integrality of carbon fiber in fibre reinforced titanium alloy laminar composite, be conducive to improve carbon fiber increasing
The mechanical property of strength titanium alloy laminar composite.
2, the present invention forms the nickel coating with a thickness of 200nm~500nm on carbon cloth surface using nickel chemical plating technology,
It avoids carbon fiber in sintering process and is contacted with titanium alloy powder and chemically reacted, so that the structure of effective protection carbon fiber is special
Sign, advantageously ensures that the stable mechanical property of fibre reinforced titanium alloy laminar composite, while nickel-coated carbon fibers cloth can
The extent of reaction for controlling nickel coating and titanium alloy powder interface, improves preparation speed of the invention.
3, the present invention combines cloth lamination with powdering technique and discharge plasma sintering process, is prepared for layered titanium
Based composites, compared with conventional titanium base material, mechanical property can be improved 25%~30%.
Technical solution of the present invention is described in further detail below by drawings and examples.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Fig. 2 a is the SEM figure (2000 ×) of nickel-coated carbon fibers cloth prepared by the embodiment of the present invention 1.
Fig. 2 b is the SEM figure (5000 ×) of nickel-coated carbon fibers cloth prepared by the embodiment of the present invention 1.
Fig. 3 a is the Cross Section Morphology figure (50 of fibre reinforced titanium alloy laminar composite prepared by the embodiment of the present invention 1
×)。
Fig. 3 b is the Cross Section Morphology figure of fibre reinforced titanium alloy laminar composite prepared by the embodiment of the present invention 1
(5000×)。
Fig. 4 is the Cross Section Morphology figure (2000 ×) of titanium alloy prepared by comparative example 1 of the present invention.
Fig. 5 a is the Cross Section Morphology figure (50 of fibre reinforced titanium alloy laminar composite prepared by comparative example 2 of the present invention
×)。
Fig. 5 b is the Cross Section Morphology figure of fibre reinforced titanium alloy laminar composite prepared by comparative example 2 of the present invention
(2000×)。
Specific embodiment
As shown in Figure 1, the present invention quickly prepares the process flow of fibre reinforced titanium alloy laminar composite are as follows: by carbon
Fiber cloth nickel plating after processing, obtains nickel-coated carbon fibers cloth, then by titanium alloy powder and the laying of nickel-coated carbon fibers cloth and mold
Middle progress plasma hot pressed sintering, obtains fibre reinforced titanium alloy laminar composite.
Embodiment 1
The present embodiment the following steps are included:
Step 1: carbon cloth is put into ultrasonic cleaning 10min in dehydrated alcohol, the item for being then 100 DEG C in temperature
Dry 10h under part；
Step 2: the carbon cloth in step 1 after drying is carried out sensitized treatment using sensitizing solution, then using work
Change and be activated in liquid, then reduction treatment is carried out using the sodium hypophosphite aqueous solution of 10g/L, dries after washing with distilled water
It is dry；The sensitizing solution is by SnCl2, hydrochloric acid solution and distilled water composition that mass concentration is 37%, SnCl in sensitizing solution2Concentration
For 1g/L, the mass percent of hydrochloric acid solution is 1%, and the activating solution is by PdCl2, ethyl alcohol and distilled water composition, in activating solution
PdCl2Concentration be 0.1g/L；
Step 3: carbon cloth after drying in step 2 is put into nickel plating solution, it is then heated to 60 DEG C of heat preservations
10min obtains nickel-coated carbon fibers cloth after taking out drying；The concentration of sodium hypophosphite is 5g/L in the nickel plating solution, nickel sulfate
Concentration is 5g/L, and the concentration of sodium citrate is 1g/L, and the concentration of sodium acetate is 1g/L；The nickel plating thickness of the nickel-coated carbon fibers cloth
Degree is 200nm；
It is formed Step 4: Titanium Powder is uniformly laid in the mold of plasma hot pressed sintering with a thickness of the of 0.5mm
Then nickel-coated carbon fibers cloth obtained in one layer of step 3 is laid on titanium alloy bisque and forms nickel-plated carbon by one titanium alloy bisque
Scrim cloth, then Titanium Powder is uniformly laid on to the second Titanium Powder formed on nickel-coated carbon fibers layer of cloth with a thickness of 0.5mm
Layer, is repeated in the forming process of the first titanium alloy bisque, the forming process of nickel-coated carbon fibers layer of cloth and the second titanium alloy bisque
Forming process, until the total height of titanium alloy bisque and nickel-coated carbon fibers layer of cloth is the mold height of plasma hot pressed sintering
60%, it is sent into plasma hot-pressed sintering furnace and carries out plasma discharging hot pressed sintering, obtain fibre reinforced titanium alloy after cooling
Laminar composite；The technological parameter of the plasma hot pressed sintering are as follows: vacuum degree 1.0 × 10-3Pa, heating rate be 50 DEG C/
Min, 1100 DEG C of sintering temperature, pressure 40MPa, soaking time 5min；The granularity of the Titanium Powder is 15 μm~45 μm.
Fig. 2 a is the SEM figure (2000 ×) of nickel-coated carbon fibers cloth manufactured in the present embodiment, and Fig. 2 b is manufactured in the present embodiment
The SEM of nickel-coated carbon fibers cloth schemes (5000 ×), can be seen that from Fig. 2 a and Fig. 2 b, in nickel-coated carbon fibers cloth manufactured in the present embodiment
Carbon cloth surface is coated with one layer of metal nickel particle, and is tightly combined between the two, and no obscission occurs.
Fig. 3 a is the Cross Section Morphology figure (50 ×) of fibre reinforced titanium alloy laminar composite manufactured in the present embodiment, figure
3b is the Cross Section Morphology figure (5000 ×) of fibre reinforced titanium alloy laminar composite manufactured in the present embodiment, can from Fig. 3 a
Out, carbon fiber is evenly distributed in fibre reinforced titanium alloy stratiform composite inner, can be seen that from Fig. 3 b, due to carbon fiber surface
Face is there are one layer of metallic nickel, carbon fiber and titanium alloy circle in fibre reinforced titanium alloy laminar composite manufactured in the present embodiment
There is no vigorous reaction and a large amount of carbide to generate at face, illustrate the present invention using nickel-coated carbon fibers cloth prevent carbon fiber with
The contact of titanium alloy powder, the discharge plasma sintering process fast in combination with heating rate, soaking time is short and pressure is high, has
Effect avoids carbon fiber in hot environment and reacts generation boundary material with titanium alloy powder.
Comparative example 1
This comparative example the following steps are included:
Step 1: the Titanium Powder that granularity is 15 μm~45 μm is uniformly laid on shape in the mold of plasma hot pressed sintering
At titanium alloy bisque, and the height of titanium alloy bisque is the 60% of the mold height of plasma hot pressed sintering, obtains closing equipped with titanium
The mold of bronze layer；
It is carried out Step 2: the mold that titanium alloy bisque is housed obtained in step 2 is put into plasma hot-pressed sintering furnace
Plasma discharging hot pressed sintering obtains titanium alloy material after cooling；The technological parameter of the plasma hot pressed sintering are as follows: vacuum degree
1.0×10-3Pa, 1100 DEG C of sintering temperature, pressure 40MPa, soaking time 5min.
Fig. 4 is the Cross Section Morphology figure (2000 × times) of the titanium alloy of this comparative example preparation, from fig. 4, it can be seen that this comparison
Densified sintering product inside the titanium alloy of example preparation, without obvious hole and defect.
Comparative example 2
This comparative example the following steps are included:
Step 1: carbon cloth is put into ultrasonic cleaning 10min in dehydrated alcohol, the item for being then 100 DEG C in temperature
Dry 10h under part；
Step 2: the carbon cloth in step 1 after drying is carried out sensitized treatment using sensitizing solution, then using work
Change and be activated in liquid, then reduction treatment is carried out using the sodium hypophosphite aqueous solution of 10g/L, dries after washing with distilled water
It is dry；The sensitizing solution is by SnCl2, hydrochloric acid solution and distilled water composition that mass concentration is 37%, SnCl in sensitizing solution2Concentration
For 1g/L, the mass percent of hydrochloric acid solution is 1%, and the activating solution is by PdCl2, ethyl alcohol and distilled water composition, in activating solution
PdCl2Concentration be 0.1g/L；
Step 3: carbon cloth after drying in step 2 is put into nickel plating solution, it is then heated to 60 DEG C of heat preservations
10min obtains nickel-coated carbon fibers cloth after taking out drying；Nickel sulfate, sodium hypophosphite, sodium citrate and acetic acid in the nickel plating solution
The mass ratio of sodium is 10:5:1:5；The nickel plating layer thick of the nickel-coated carbon fibers cloth is 200nm；Hypophosphorous acid in the nickel plating solution
The concentration of sodium is 5g/L, and the concentration of nickel sulfate is 5g/L, and the concentration of sodium citrate is 1g/L, and the concentration of sodium acetate is 1g/L；
It is formed Step 4: Titanium Powder is uniformly laid in the mold of plasma hot pressed sintering with a thickness of the of 0.5mm
Then nickel-coated carbon fibers cloth obtained in one layer of step 3 is laid on titanium alloy bisque and forms nickel-plated carbon by one titanium alloy bisque
Scrim cloth, then Titanium Powder is uniformly laid on to the second Titanium Powder formed on nickel-coated carbon fibers layer of cloth with a thickness of 0.5mm
Layer, is repeated in the forming process of the first titanium alloy bisque, the forming process of nickel-coated carbon fibers layer of cloth and the second titanium alloy bisque
Forming process, until the total height of titanium alloy bisque and nickel-coated carbon fibers layer of cloth is the mold height of plasma hot pressed sintering
60%, it is sent into plasma hot-pressed sintering furnace and carries out plasma discharging hot pressed sintering, obtain fibre reinforced titanium alloy after cooling
Laminar composite；The technological parameter of the plasma hot pressed sintering are as follows: vacuum degree 1.0 × 10-3Pa, heating rate be 50 DEG C/
Min, 1100 DEG C of sintering temperature, pressure 40MPa, heating-up time 220min, soaking time 30min；The granularity of the Titanium Powder
It is 15 μm~45 μm.
Fig. 5 a is the Cross Section Morphology figure (50 ×) of the fibre reinforced titanium alloy laminar composite of this comparative example preparation, from
Fig. 5 a can be seen that between each carbon fiber layer of fibre reinforced titanium alloy stratiform composite inner of this comparative example preparation by titanium
Alloy substrate filling, generates without apparent hole and defect.
Fig. 5 b is the Cross Section Morphology figure (2000 ×) of the fibre reinforced titanium alloy laminar composite of this comparative example preparation,
It can be seen that carbon fiber and titanium alloy substrate in fibre reinforced titanium alloy laminar composite prepared by this comparative example from Fig. 5 b
Interface generate a large amount of carbide, part carbon fiber is corroded, and illustrate that the plasma hot pressed sintering for using vacuum hotpressing is led
It causes carbon fiber and titanium alloy powder to react in the high temperature environment and generates boundary material.
Fig. 3 a, Fig. 3 b, Fig. 4, Fig. 5 a and Fig. 5 b are compared it is found that introducing carbon fiber in titanium alloy substrate as increasing
Its pattern tissue can be improved by mutually preparing fibre reinforced titanium alloy laminar composite by force, be conducive to improve the conjunction of fibre reinforced titanium
The mechanical property of golden laminar composite, but carry out lower plasma discharging hot pressed sintering in conventional hot conditions and result in carbon fiber
Dimension generates vigorous reaction with titanium alloy substrate, and the humidification of carbon fiber is caused to significantly reduce；And use nickel-coated carbon fibers cloth every
Exhausted carbon fiber and titanium alloy powder, and faster heating rate, shorter soaking time and higher pressure are combined, effectively avoid
Carbon fiber and titanium alloy powder, which react, in hot environment generates boundary material, ensure that fibre reinforced titanium alloy stratiform
The integrality of carbon fiber in composite material is conducive to the mechanical property for improving fibre reinforced titanium alloy laminar composite.
Embodiment 2
The present embodiment the following steps are included:
Step 1: carbon cloth is put into ultrasonic cleaning 30min in dehydrated alcohol, the item for being then 100 DEG C in temperature
Dry 20h under part；
Step 2: the carbon cloth in step 1 after drying is carried out sensitized treatment using sensitizing solution, then using work
Change and be activated in liquid, then reduction treatment is carried out using the sodium hypophosphite aqueous solution of 10g/L, dries after washing with distilled water
It is dry；The sensitizing solution is by SnCl2, hydrochloric acid solution and distilled water composition that mass concentration is 37%, SnCl in sensitizing solution2Concentration
For 20g/L, the mass percent of hydrochloric acid solution is 5%, and the activating solution is by PdCl2, ethyl alcohol and distilled water composition, in activating solution
PdCl2Concentration be 0.6g/L；
Step 3: carbon cloth after drying in step 2 is put into nickel plating solution, it is then heated to 90 DEG C of heat preservations
120min obtains nickel-coated carbon fibers cloth after taking out drying；The concentration of sodium hypophosphite is 50g/L, nickel sulfate in the nickel plating solution
Concentration be 50g/L, the concentration of sodium citrate is 20g/L, and the concentration of sodium acetate is 30g/L；The plating of the nickel-coated carbon fibers cloth
Nickel layer thickness is 500nm；
It is formed Step 4: Titanium Powder is uniformly laid in the mold of plasma hot pressed sintering with a thickness of the first of 2mm
Then nickel-coated carbon fibers cloth obtained in one layer of step 3 is laid on formation nickel plating carbon fiber on titanium alloy bisque by titanium alloy bisque
Layer of cloth is tieed up, then Titanium Powder is uniformly laid on to the second titanium alloy bisque formed on nickel-coated carbon fibers layer of cloth with a thickness of 2mm, according to
The formation of the forming process, the forming process of nickel-coated carbon fibers layer of cloth and the second titanium alloy bisque of secondary the first titanium alloy of repetition bisque
Process, until the total height of titanium alloy bisque and nickel-coated carbon fibers layer of cloth is the 70% of the mold height of plasma hot pressed sintering,
It is sent into plasma hot-pressed sintering furnace and carries out plasma discharging hot pressed sintering, it is multiple that fibre reinforced titanium alloy stratiform is obtained after cooling
Condensation material；The technological parameter of the plasma hot pressed sintering are as follows: vacuum degree 3.0 × 10-3Pa, heating rate are 100 DEG C/min, are burnt
800 DEG C of junction temperature, pressure 180MPa, soaking time 10min；The granularity of the Titanium Powder is 15 μm~45 μm.
Embodiment 3
The present embodiment the following steps are included:
Step 1: carbon cloth is put into ultrasonic cleaning 20min in dehydrated alcohol, the item for being then 100 DEG C in temperature
Dry 15h under part；
Step 2: the carbon cloth in step 1 after drying is carried out sensitized treatment using sensitizing solution, then using work
Change and be activated in liquid, then reduction treatment is carried out using the sodium hypophosphite aqueous solution of 10g/L, dries after washing with distilled water
It is dry；The sensitizing solution is by SnCl2, hydrochloric acid solution and distilled water composition that mass concentration is 37%, SnCl in sensitizing solution2Concentration
For 10g/L, the mass percent of hydrochloric acid solution is 3%, and the activating solution is by PdCl2, ethyl alcohol and distilled water composition, in activating solution
PdCl2Concentration be 0.3g/L；
Step 3: carbon cloth after drying in step 2 is put into nickel plating solution, it is then heated to 80 DEG C of heat preservations
30min obtains nickel-coated carbon fibers cloth after taking out drying；The concentration of sodium hypophosphite is 20g/L in the nickel plating solution, nickel sulfate
Concentration is 25g/L, and the concentration of sodium citrate is 10g/L, and the concentration of sodium acetate is 20g/L；The nickel plating of the nickel-coated carbon fibers cloth
Layer is with a thickness of 300nm；
It is formed Step 4: Titanium Powder is uniformly laid in the mold of plasma hot pressed sintering with a thickness of the first of 1mm
Then nickel-coated carbon fibers cloth obtained in one layer of step 3 is laid on formation nickel plating carbon fiber on titanium alloy bisque by titanium alloy bisque
Layer of cloth is tieed up, then Titanium Powder is uniformly laid on to the second titanium alloy bisque formed on nickel-coated carbon fibers layer of cloth with a thickness of 1mm, according to
The formation of the forming process, the forming process of nickel-coated carbon fibers layer of cloth and the second titanium alloy bisque of secondary the first titanium alloy of repetition bisque
Process, until the total height of titanium alloy bisque and nickel-coated carbon fibers layer of cloth is the 65% of the mold height of plasma hot pressed sintering,
It is sent into plasma hot-pressed sintering furnace and carries out plasma discharging hot pressed sintering, it is multiple that fibre reinforced titanium alloy stratiform is obtained after cooling
Condensation material；The technological parameter of the plasma hot pressed sintering are as follows: vacuum degree 2.0 × 10-3Pa, heating rate are 80 DEG C/min, are burnt
1000 DEG C of junction temperature, pressure 60MPa, soaking time 6min；The granularity of the Titanium Powder is 15 μm~45 μm.
To 1~embodiment of the embodiment of the present invention 3, comparative example 2 prepare fibre reinforced titanium alloy laminar composite and
Titanium alloy material prepared by comparative example 1 carries out mechanics properties testing, using tensile strength as examination criteria, as a result such as the following table 1 institute
Show.
Fibre reinforced titanium alloy laminar composite and comparison prepared by 1 1~embodiment of embodiment 3 of table, comparative example 2
The tensile strength of titanium alloy material prepared by example 1
| Sample | Tensile strength (MPa) |
| Embodiment 1 | 605~627 |
| Embodiment 2 | 633~664 |
| Embodiment 3 | 662~688 |
| Comparative example 1 | 427~449 |
| Comparative example 2 | 482~518 |
As it can be seen from table 1 fibre reinforced titanium alloy stratiform composite wood prepared by 1~embodiment of the embodiment of the present invention 3
The drawing for the titanium alloy material that the tensile strength of material is all remarkably higher than the titanium alloy material of the preparation of comparative example 1 and prepared by comparative example 2
Intensity is stretched, and the tensile strength of the fibre reinforced titanium alloy laminar composite of the preparation of embodiment 1 is compared with carbon prepared by comparative example 2
Fiber reinforcement titanium alloy laminar composite improves 25%~30%, illustrates that introducing carbon fiber as reinforced phase can be improved carbon fiber
The mechanical property of dimension enhancing titanium alloy laminar composite, using nickel-coated carbon fibers cloth and the fast, soaking time in conjunction with heating rate
Short and high pressure discharge plasma sintering process, avoids carbon alloy powder and chemistry occurs under high temperature environment for carbon fiber instead
It answers, ensure that integrality of the carbon fiber in fibre reinforced titanium alloy laminar composite, be conducive to give full play to carbon fiber
Toughness humidification, pass through the bridging of carbon fiber, extraction and titanium alloy substrate micro-crack etc. and enhance mechanism and absorb a large amount of energy
Amount, to further increase the mechanical property of fibre reinforced titanium alloy laminar composite.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way.It is all according to invention skill
Art any simple modification, change and equivalence change substantially to the above embodiments, still fall within technical solution of the present invention
Protection scope in.
Claims (5)
1. a kind of method for quickly preparing fibre reinforced titanium alloy laminar composite, which is characterized in that this method include with
Lower step:
It is then 100 DEG C in temperature Step 1: carbon cloth is put into ultrasonic cleaning 10min~30min in dehydrated alcohol
Under the conditions of dry 10h~20h；
Step 2: the carbon cloth in step 1 after drying is carried out sensitized treatment using sensitizing solution, activating solution is then used
In be activated, then using sodium hypophosphite aqueous solution carry out reduction treatment, dry after washing with distilled water；The sensitizing solution
By SnCl2, hydrochloric acid solution and distilled water composition, the activating solution is by PdCl2, ethyl alcohol and distilled water composition；
Step 3: carbon cloth after drying in step 2 is put into nickel plating solution, it is then heated to 60 DEG C~90 DEG C guarantors
Warm 10min~120min obtains nickel-coated carbon fibers cloth after taking out drying；Nickel sulfate, sodium hypophosphite, lemon in the nickel plating solution
The mass ratio of sour sodium and sodium acetate is (10~50): (5~30): (1~20): (5~30)；The nickel plating of the nickel-coated carbon fibers cloth
Layer is with a thickness of 200nm~500nm；
It is formed Step 4: Titanium Powder is uniformly laid in the mold of plasma hot pressed sintering with a thickness of the of 0.5mm~2mm
Then nickel-coated carbon fibers cloth obtained in one layer of step 3 is laid on titanium alloy bisque and forms nickel-plated carbon by one titanium alloy bisque
Scrim cloth, then Titanium Powder is uniformly laid on on nickel-coated carbon fibers layer of cloth to form thickness equal with the first titanium alloy bisque
Second titanium alloy bisque is repeated in the forming process of the first titanium alloy bisque, the forming process of nickel-coated carbon fibers layer of cloth and
The forming process of two titanium alloy bisques, until the total height of titanium alloy bisque and nickel-coated carbon fibers layer of cloth is plasma hot pressed sintering
Mold height 60%~70%, be sent into plasma hot-pressed sintering furnace and carry out plasma discharging hot pressed sintering, it is cooling after
To fibre reinforced titanium alloy laminar composite；The technological parameter of the plasma hot pressed sintering are as follows: vacuum degree 1.0 × 10- 3Pa~3.0 × 10-3Pa, heating rate be 50 DEG C/min~100 DEG C/min, 800 DEG C~1100 DEG C of sintering temperature, pressure 40MPa
~180MPa, soaking time 5min~10min；The granularity of the Titanium Powder is 15 μm~45 μm.
2. a kind of method for quickly preparing fibre reinforced titanium alloy laminar composite according to claim 1, special
Sign is, SnCl in sensitizing solution described in step 22Concentration be 1g/L~20g/L.
3. a kind of method for quickly preparing fibre reinforced titanium alloy laminar composite according to claim 1, special
Sign is that the mass concentration of hydrochloric acid solution is 37% in sensitizing solution described in step 2, and the mass percent of hydrochloric acid solution is 1%
~5%.
4. a kind of method for quickly preparing fibre reinforced titanium alloy laminar composite according to claim 1, special
Sign is, PdCl in activating solution described in step 22Concentration be 0.1g/L~0.6g/L.
5. a kind of method for quickly preparing fibre reinforced titanium alloy laminar composite according to claim 1, special
Sign is, the concentration of sodium hypophosphite is 5g/L~50g/L in nickel plating solution described in step 3, the concentration of nickel sulfate be 5g/L~
50g/L, the concentration of sodium citrate are 1g/L~20g/L, and the concentration of sodium acetate is 1g/L~30g/L.
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