CN100361756C - Process for preparing laminar composite of Ti-TiAl3 metal/intermetallic compound - Google Patents
Process for preparing laminar composite of Ti-TiAl3 metal/intermetallic compound Download PDFInfo
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- CN100361756C CN100361756C CNB2005100467289A CN200510046728A CN100361756C CN 100361756 C CN100361756 C CN 100361756C CN B2005100467289 A CNB2005100467289 A CN B2005100467289A CN 200510046728 A CN200510046728 A CN 200510046728A CN 100361756 C CN100361756 C CN 100361756C
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- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 229910000765 intermetallic Inorganic materials 0.000 title claims abstract description 34
- 239000002184 metal Substances 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title abstract description 5
- 229910010039 TiAl3 Inorganic materials 0.000 title abstract description 4
- 239000010936 titanium Substances 0.000 claims abstract description 72
- 238000005098 hot rolling Methods 0.000 claims abstract description 21
- 238000002360 preparation method Methods 0.000 claims abstract description 20
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 14
- 229910010038 TiAl Inorganic materials 0.000 claims description 19
- 238000005096 rolling process Methods 0.000 claims description 16
- 239000003513 alkali Substances 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 11
- 238000003466 welding Methods 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000005554 pickling Methods 0.000 claims description 8
- 238000004381 surface treatment Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 230000014759 maintenance of location Effects 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 14
- 239000011888 foil Substances 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000003475 lamination Methods 0.000 abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 150000001875 compounds Chemical class 0.000 description 10
- 229910052751 metal Inorganic materials 0.000 description 10
- 239000000243 solution Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000003801 milling Methods 0.000 description 6
- 239000002360 explosive Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000002905 metal composite material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 2
- 239000011157 advanced composite material Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Natural products CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
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- 229910000679 solder Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- Pressure Welding/Diffusion-Bonding (AREA)
Abstract
The present invention relates to a preparation technique of a composite material, more specifically a preparation method of Ti-TiAl3 metal / intermetallic compound laminar composite material. After the surfaces of Ti foil and AL foil are processed, the Ti foil and the AL foil are alternatively placed in the mode of lamination, and a hot rolling test sample is made. The test sample is wrapped and milled by a pure titanium plate, and is thermally milled after being thermally preserved for 5 to 15 minutes at the temperature of 750 to 950 DEG C, and the Ti-TiAl3 metal / intermetallic compound laminar composite material is obtained. The present invention can complete the preparation of the composite material in a one-step way and has the advantages of simplicity and easy operation of production process, low cost, no pollution in the preparation process of the present invention, and good interface combination of the composite material. The laminar composite materials of the present invention with different thicknesses can be conveniently obtained by the adjustment of the number of the alternative lamination of the Ti foil and the Al foil or the thicknesses of raw materials.
Description
Technical field
The present invention relates to the Composite Preparation technology, specifically a kind of Ti-TiAl
3The preparation method of metal/intermetallic compound laminar composite.
Background technology
Along with the appearance of the development of modern industrial technology and various new technology, new industry, people increase day by day to the requirement of material property, and the performance of single group element material has been difficult to meet the demands under some working condition.Therefore, research has become important developing direction in the Materials Science and Engineering field with the preparation advanced composite material (ACM).Layer metal composite plate is to be composited by special preparation for processing by two kinds of different metallic plates of performance, compare with single metal constituent element, combine two kinds of metal constituent elements advantage separately through the laminated composite plate after the appropriate design combination, can obtain physics and chemical property that single metal does not have.In recent decades, the development of layer metal composite plate, production and application more and more cause people's attention, the new material that has become countries in the world competitively to develop.Up to the present, this composite has obtained application in fields such as Aero-Space, oil, chemical industry, metallurgy, machinery, automobile, steamer, building, nuclear energy and electric power and electronics.The manufacturing process of laminated-metal composite mainly contains following two kinds of methods:
1. explosive welding composite algorithm.The metallic explosive welding is to drive compound plate high velocity impact substrate by the high-strength chemical energy that explosive charge produces, the instantaneous pressure that the point of impingement produces has not only destroyed the oxide film on metallic plate top layer, exposed fresh surface, and formed skim on the fresh metal surface and have the welding transition district of plastic deformation, fusing, diffusion and wave character exposing, thereby realize the new technology and the new technology of a kind of metal solder of strong combination.Different with the substrate installation form according to compound plate, explosive welding can be divided into parallel method and preset angle configuration.When parallel method was installed, it is parallel that compound plate and substrate are in, and the gap remains unchanged; The angle rule is angled installation between compound plate and the substrate.The difference of explosive welding composite algorithm and other method is: (1) high pressure; (2) high strain rate; (3) locality of used load and mobility; (4) the composite plate compound interface presents wavy combination; (5) restriction that not differed greatly by material melting point, plasticity, and compound dimensions flexibility is very big.
2, roll-bonding method.The basic principle of roll-bonding method is meant that metallic plate is being subjected under the effect that milling train is applied thereto crunch, double layer of metal treat composite surface generation plastic deformation, surface metal-layer is broken.Subsequently, clean and metal level activation exposes from the metal surface of breaking, under the crunch effect, form plane metallurgical binding.Faying face continues to enlarge in follow-up heat treatment process, forms firm combination.Rolling fundamental difference compound and that the monometallic plate is rolling is, must impose big initial reduction in pass, impels the physics contact of composite surface.
Summary of the invention
The present invention designs the laminar composite that preparation is formed by connecting by ductile metal and hard crisp intermetallic compound alternative stacked, and utilizes the effect of reaction diffusion to reach the good interface combination.Occur in the cold-rolled process in order to solve: the Ti/Al interface is in conjunction with the problem of the composite board delamination splitting that occurs in bad and subsequently the vacuum heat process.It is compound to the present invention proposes new combination process-accumulation hot rolling, and this new method has excellent mechanical property, for example high strength and high tenacity with respect to traditional coarse grained metal material.Accumulation ply rolling method has practical significance, and it just can be realized by the common operation of rolling.
To achieve these goals, technical scheme of the present invention is:
A kind of Ti-TiAl
3The preparation method of metal/intermetallic compound laminar composite, Ti paper tinsel and Al paper tinsel are made the hot rolling sample through alternative stacked placement after the surface treatment, and sample adopts pure titanium plate pack rolling, and sample is under 750-950 ℃, carry out hot rolling after temperature retention time 5-15 minute, obtain Ti-TiAl
3The metal/intermetallic compound laminar composite.
Described surface treatment is to clean Ti paper tinsel and Al paper tinsel surface with organic solvent earlier, again Ti paper tinsel and Al paper tinsel is carried out pickling or alkali cleaning respectively.
Surface treated Ti paper tinsel and Al paper tinsel are cut into small pieces, and alternative stacked is placed then, amounts to the 11-31 layer, wherein: and be all Ti paper tinsel or Al paper tinsel bottom, wrap up one deck Al paper tinsel or Ti paper tinsel more outside topmost, standby.
After sample adopted pure titanium plate jacket, jacket adopted the argon arc welding sealing.
750-950 ℃ of described hot-rolled temperature scope, rate of heat addition 10-20 ℃/min, mill speed 0.2-0.5m/s, air cooling after the hot rolling.
The thickness of described Ti paper tinsel and Al paper tinsel is respectively 220 μ m and 210 μ m, and under the alternative stacked 11-31 layer situation, the thickness of Ti layer and TiAl3 layer is respectively 80 μ m-100 μ m and 70 μ m-90 μ m.
The present invention has following advantage:
1. adopt the present invention can disposablely finish the preparation of composite, production technology is simple, and cost is low.
2. preparation process of the present invention is pollution-free, and composite material interface is in conjunction with good.
The thickness of laminar composite of the present invention can be easily the thickness of number by adjusting Ti paper tinsel and Al paper tinsel alternative stacked or raw material itself obtain the laminar composite of different-thickness.
Description of drawings
Fig. 1 (a)-(b) is the schematic diagram of hot rolling combination process.Wherein, be that Ti paper tinsel and Al paper tinsel alternative stacked are placed (a), and with pure titanium jacket; (b) be Ti paper tinsel and Al paper tinsel behind jacket, it is compound to carry out hot rolling.Among the figure, 1, jacket; 2, Ti layer; 3, Al layer; 4, heating furnace; 5, Ti/Al alternative stacked; 6, roll.
Fig. 2 is the photograph in kind of rolling preceding jacket.
Fig. 3 is the ESEM back reflection photo of preparation sample among the embodiment 1.
Fig. 4 is the photograph in kind of rolling back jacket among the embodiment 3.
The specific embodiment
The present invention adopts the hot rolling composite algorithm to prepare Ti-TiAl
3The metal/intermetallic compound laminar composite, the experiment raw material are Ti paper tinsel (TAl) and Al paper tinsel (L3), after handling through cleaning surfaces Ti paper tinsel and Al paper tinsel alternative stacked placed and amount to the 11-31 layer and make the hot rolling sample, sample adopts pure titanium plate pack rolling, and the hot-rolled temperature scope is 750-950 ℃.The sample that temperature retention time is different can obtain Ti-TiAl through after the hot rolling
3The metal/intermetallic compound laminar composite.Specifically can carry out as follows:
1) raw-material surface (cleaning) handled.At first getting raw material is Ti paper tinsel and Al paper tinsel, cleans Ti paper tinsel and Al paper tinsel surface with organic solvent (as benzinum, acetone or methyl alcohol etc.); Again Ti paper tinsel and Al paper tinsel are carried out pickling or alkali cleaning respectively;
Described pickling is to be 5-15%HNO to Ti paper tinsel working concentration
3Solution acid pickling 10-20min rinses well with clear water again, dries up.
Described alkali cleaning is to be that 30-50 ℃, concentration are to take out behind the NaOH aqueous solution alkali cleaning 10-30min of 5-20% to Al paper tinsel serviceability temperature, rinse well with clear water, place the dilute nitric acid solution of 20-40% to carry out the photochemical processing of 5-10min again with the surplus alkali that neutralizes, avoid alkali lye to continue corrosion Al matrix, rinse well with clear water then, dry up.
2) described Ti paper tinsel and Al paper tinsel are cut into small pieces, alternative stacked is placed then, and wherein: topmost and be all Ti paper tinsel or Al paper tinsel bottom, (scattering for preventing paillon foil) can wrap up one deck Al paper tinsel or Ti paper tinsel more outside, and be standby;
3) with 2) in ready sample adopt pure titanium plate jacket, jacket adopts the argon arc welding sealing.
4) will seal jacket and be heated to the temperature required pack rolling that on milling train, carries out.
5) after 750-950 ℃ of sample process hot rolling that is incubated 5-15 minute down, obtain composite.
Ti paper tinsel that the present invention is surface-treated and Al paper tinsel are sealed in the pure titanium jacket immediately, adopt the cold, hot two-purpose milling train to carry out the jacket hot rolling, arrive and begin feeding when setting rolling temperature, rolling temperature 750-950 ℃, 10-20 ℃/min of the rate of heat addition (being programming rate), mill speed 0.2-0.5m/s, air cooling after the hot rolling.
Below in conjunction with embodiment and accompanying drawing in detail the present invention is described in detail.
As Fig. 1 (a), shown in Figure 2, Ti layer 2, Al layer 3 that pure titanium jacket is placed by alternative stacked in jacket 1 and the jacket 1 constitute; Shown in Fig. 1 (b), equipment of hot rolling mainly comprises heating furnace 4, roll 6 etc., and Ti/Al alternative stacked 5 places in the heating furnace 4.
Embodiment 1
Getting Ti paper tinsel and Al paper tinsel is raw material, handles through surface (cleaning) earlier, Ti paper tinsel and Al paper tinsel alternative stacked is placed again, and is sealed in the pure titanium jacket with argon arc welding.Specifically can carry out as follows:
1) raw-material surface treatment: raw material are Ti paper tinsel (TAl) and Al paper tinsel (L3), and original thickness is respectively 220 μ m and 210 μ m, at first, clean the greasy dirt on Ti paper tinsel and Al paper tinsel surface with benzinum; Be 50 ℃ to Al paper tinsel temperature again, concentration is to take out behind 10% the NaOH aqueous solution alkali cleaning 10min, washes 5min with clear water, place 30% dilute nitric acid solution to carry out the photochemical processing of 5min again with the surplus alkali that neutralizes, avoid alkali lye to continue corrosion Al matrix, rinse well with clear water again, dry up; To Ti paper tinsel 10%HNO
3-HF solution acid pickling 15min washes 5min with clear water, dries up; Ti paper tinsel thickness after surface treatment is about 210 μ m, and Al paper tinsel thickness is about 200 μ m;
2) surface-treated tinsel is cut into the rectangular-shaped pieces of 75mm * 40mm, the Ti paper tinsel and the Al paper tinsel alternative stacked of well cutting are placed totally 21 layers,, can wrap up one deck Al paper tinsel outside for preventing that paillon foil from scattering wherein topmost and be all the Ti paper tinsel bottom, it is standby to make sample;
3) surface-treated Ti paper tinsel and Al paper tinsel are sealed in the pure titanium jacket immediately, adopt the cold, hot two-purpose milling train to carry out the jacket hot rolling, arrive when setting rolling temperature, are incubated 5 minutes, the beginning feeding.The present embodiment hot-rolled temperature is set at 950 ℃, and programming rate is 15 ℃/min, mill speed 0.5m/s.
Its result as can see from Figure 3, through preparing the laminar composite Ti-TiAl that is formed by connecting by ductile metal and hard crisp intermetallic compound alternative stacked after 950 ℃ of hot rollings
3Grey is Ti among the figure, and the grey black particle is TiAl
3Phase, a spot of black are residual toughness Al matrix.Ti layer and TiAl
3The thickness of layer is respectively 100 μ m and 90 μ m.
Difference from Example 1 is:
1) cleans the greasy dirt on Ti paper tinsel and Al paper tinsel surface with benzinum; To Al paper tinsel temperature is 30 ℃, and concentration is to take out behind 20% the NaOH aqueous solution alkali cleaning 20min, washes 5min with clear water, places 20% dilute nitric acid solution to carry out photochemical processing 10min again, rinses well with clear water again, dries up; To Ti paper tinsel 15%HNO
3-HF solution acid pickling 10min washes 5min with clear water, dries up;
2) surface-treated tinsel alternative stacked is placed totally 17 layers, wherein be all the Al paper tinsel topmost and bottom; Can wrap up one deck Ti paper tinsel outside for preventing that paillon foil from scattering, it is standby to make sample;
3) surface-treated Ti paper tinsel and Al paper tinsel are sealed in the pure titanium jacket immediately, adopt the cold, hot two-purpose milling train to carry out the jacket hot rolling, arrive when setting rolling temperature, are incubated 15 minutes, the beginning feeding.The present embodiment hot-rolled temperature is set at 750 ℃, 10 ℃/min of the rate of heat addition, mill speed 0.2m/s.Ti layer and TiAl
3The thickness of layer is respectively 80 μ m and 70 μ m.
Difference from Example 1 is:
1) cleans the greasy dirt on Ti paper tinsel and Al paper tinsel surface with acetone; Al paper tinsel temperature is 30 ℃, and concentration is to take out behind 20% the NaOH aqueous solution alkali cleaning 20min, washes 5min with clear water, places 20% dilute nitric acid solution to carry out photochemical processing 10min again, rinses well with clear water again, dries up; Ti paper tinsel 15%HNO
3-HF solution acid pickling 10min washes 5min with clear water, dries up;
2) surface-treated tinsel alternative stacked is placed totally 31 layers, wherein be all the Al paper tinsel topmost and bottom; Can wrap up one deck Ti paper tinsel outside for preventing that paillon foil from scattering, it is standby to make sample;
3) surface-treated Ti paper tinsel and Al paper tinsel are sealed in the pure titanium jacket immediately, adopt the cold, hot two-purpose milling train to carry out the jacket hot rolling, arrive when setting rolling temperature, are incubated 10 minutes, the beginning feeding.The present embodiment hot-rolled temperature is set at 850 ℃, 20 ℃/min of the rate of heat addition, mill speed 0.3m/s.Ti layer and TiAl
3The thickness of layer is respectively 90 μ m and 80 μ m.
Fig. 4 is the photograph in kind of rolling back jacket among the embodiment 3, and the plate shape of jacket is smooth as we can see from the figure, and distortion is even, and material is compound good.
Claims (6)
1. Ti-TiAl
3The preparation method of metal/intermetallic compound laminar composite, it is characterized in that: Ti paper tinsel and Al paper tinsel are made the hot rolling sample through alternative stacked placement after the surface treatment, sample adopts pure titanium plate pack rolling, sample is under 750-950 ℃, carry out hot rolling after temperature retention time 5-15 minute, obtain Ti-TiAl
3The metal/intermetallic compound laminar composite.
2. according to the described Ti-TiAl of claim 1
3The preparation method of metal/intermetallic compound laminar composite is characterized in that: surface treatment is to clean Ti paper tinsel and Al paper tinsel surface with organic solvent earlier, again the Ti paper tinsel is carried out pickling, and the Al paper tinsel is carried out alkali cleaning.
3. according to the described Ti-TiAl of claim 1
3The preparation method of metal/intermetallic compound laminar composite, it is characterized in that: surface treated Ti paper tinsel and Al paper tinsel are cut into small pieces, alternative stacked is placed then, amount to the 11-31 layer, wherein: be all Ti paper tinsel or Al paper tinsel topmost and bottom, wrap up one deck Al paper tinsel or Ti paper tinsel more outside, standby.
4. according to the described Ti-TiAl of claim 1
3The preparation method of metal/intermetallic compound laminar composite is characterized in that: after sample adopted pure titanium plate jacket, jacket adopted the argon arc welding sealing.
5. according to the described Ti-TiAl of claim 1
3The preparation method of metal/intermetallic compound laminar composite is characterized in that: 750-950 ℃ of hot-rolled temperature scope, rate of heat addition 10-20 ℃/min, mill speed 0.2-0.5m/s, air cooling after the hot rolling.
6. according to the described Ti-TiAl of claim 1
3The preparation method of metal/intermetallic compound laminar composite is characterized in that: the thickness of Ti paper tinsel and Al paper tinsel is respectively 220 μ m and 210 μ m, under the alternative stacked 11-31 layer situation, and Ti layer and TiAl
3The thickness of layer is respectively 80 μ m-100 μ m and 70 μ m-90 μ m.
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| CN101811137A (en) * | 2010-04-13 | 2010-08-25 | 中南大学 | Preparation method of TiAl-based alloy rolled sheet |
| CN103639235B (en) * | 2013-12-16 | 2015-06-03 | 中国航空工业集团公司北京航空制造工程研究所 | Ti-Al intermetallic compound laminated composite material tube and preparation method thereof |
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| CN109706415A (en) * | 2019-01-25 | 2019-05-03 | 北京工业大学 | A kind of memory alloy-based nano lamellar composite material and preparation method |
| CN110170527B (en) * | 2019-06-06 | 2020-08-18 | 哈尔滨理工大学 | Preparation method of high-niobium porous layered titanium-aluminum alloy plate |
| CN111261594A (en) * | 2020-03-12 | 2020-06-09 | 哈尔滨铸鼎工大新材料科技有限公司 | Copper-molybdenum-copper carrier substrate with heat conduction channel and manufacturing method thereof |
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| CN1883834A (en) | 2006-12-27 |
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