Background technology
Structure refinement is the effective way that improves metal strength and comprehensive mechanical property.When material grains refine to nanocrystalline yardstick, not only comprehensive mechanical performance can improve, and physics-chem characteristic also significant change can take place.The large plastometric set technology has the intensive grain refining capability, can directly material inside organization be refine to submicron and even nano level, and being known as by material supply section educational circles is the most promising method of preparation nanometer and high-strength material.Equal-diameter bending passage deformation is a kind of violent plastic deformation method that can directly obtain block sub-micron crystal or nanocrystalline material.At present, many cubic structure pure metal and alloys (as Al, Cu, Ni, carbon steel etc.) thereof that possess good room temperature processibility are successfully realized multi-pass ECAP distortion in room temperature, obtain the high strength tissue.And the difficult deformable metal (as: close-packed hexagonal structure metal) with less slip system is when room temperature ECAP is out of shape, and sample often ruptures and can not successfully realize the ECAP distortion.
Through the prior art literature search is found, S.L.Semiatin, V.M.Segal, R.E.Goforth etc. have once delivered one piece and have been entitled as the paper of " Workability of Commerical-Purity Titanium and 4340 Steelduring Equal Channel Angular Extrusion at Cold-Working Temperatures " on " Metallurgicals and Materials Transactions " (30A (1999) 1425-1435), this article has carried out the ECAP distortion to difficult deformable metals such as pure titanium with close-packed hexagonal structure and 4340 steel.The die channel angle Ф that is adopted in the literature=90 °, lubricant is a graphite treated lubricant, respectively under 25 ℃~325 ℃ temperature, adopt 0.0025
-1~2S
-1Strain rate pure titanium has been carried out the ECAP distortion, the result adopts 0.002S in room temperature (25 ℃)
-1~2S
-1Between any one strain rate carry out ECAP distortion and all fail and obtain ganoid industrially pure titanium sample, all distortion samples all are cut into fragment after deformation process; And this article author attempts pure titanium is carried out the ECAP distortion in other temperature (125 ℃~325 ℃), because the influence of factors such as extrusion temperature, strain rate, lubricating condition are inappropriate, fracture has in various degree also appearred in the pure titanium after the ECAP distortion, thereby fails to obtain ganoid industrially pure titanium grained material.
After this, the people such as Yuntian T.Zhu of Muscovite Vladimir V.Stolyarov, the U.S. have implemented the ECAP distortion at 200 ℃~500 ℃ to industrially pure titanium, have finally obtained ganoid block grained material.(application number is the Chinese patent application that is proposed by Shanghai Communications University: 200510029663.7, the applying date: on September 15th, 2005, open day: on March 15th, 2006), denomination of invention is: the isometrical bent angle extruding production of the brilliant industrially pure titanium bulk of micro-/ nano, this invention prepares the industrially pure titanium bulk with isometrical bent angle extruding, but it has implemented the ECAP distortion at 400 ℃~500 ℃ to industrially pure titanium.Carry out isometrical bent angle extruding preparation industrially pure titanium bulk with high temperature, although finally obtained ganoid block grained material, but during owing to employing high temperature ECAP distortion, will produce and reply and the recrystallize phenomenon, influence grain refining effect, reach desirable strength, then must carry out the more distortion of multi-pass; And high temperature ECAP distortion, required preparation equipment are relatively complicated, and operation is also relatively complicated.
Chinese patent application (application number: 200810017288.8 by Xi'an University of Architecture and Technology's proposition, the applying date: on January 14th, 2008, open day: on July 16th, 2008), denomination of invention is: the pure titanium bulk of high strength industrial room temperature equal-diameter bending passage deformation preparation method, it is 100 °~135 ° mould that the passage angle is at room temperature adopted in this invention, realized the ECAP distortion of industrially pure titanium bulk, but it needs to anneal at the two-phase neighboring trace.
Summary of the invention
Defective or deficiency at above-mentioned prior art existence, the objective of the invention is to, a kind of difficult-to-deformation metal block material room temperature equal-diameter bending passage deformation production method is provided, this method at room temperature to difficulty distortion (room temperature ECAP distortion plasticity is poor) the equal-diameter bending passage deformation technology that material adopts 90 °~110 ° moulds and do not carry out the process annealing operation, has obtained the high-strength metal bulk.Owing at room temperature adopt smaller channels angle mould to carry out the ECAP distortion, so can improve grain refining effect; When carrying out multi-pass deformation, need not carry out the process annealing operation, thereby simplify preparation process.And this method uses equipment simple, easy to operate.
In order to realize above-mentioned task, the present invention takes following technical scheme:
A kind of difficult-to-deformation metal block material room temperature equal-diameter bending passage deformation production method is characterized in that it comprises the steps:
1. select for use the industrially pure titanium hot rolled plate as raw material, hot rolled plate need be annealed;
2. the industrially pure titanium hot rolled plate after will annealing cuts into blank, and grinding process is carried out on its surface;
3. at blank surface coating lubricant;
4. in the equal-diameter bending passage deformation mold cavity, apply lubricant;
5. the blank of surface applied lubricant is put into the equal-diameter bending passage deformation die channel that has applied lubricant, on pressing machine or extrusion machine, blank is carried out room temperature equal-diameter bending passage deformation crimp then;
6. after extruding is finished, repeated for above the 3.~5. step, through 2~8 B
CAfter the equal-diameter bending passage crimp of mode, can obtain the pure titanium of ganoid high strength industrial.
3. above-mentioned steps is the compounded lubricant that molybdenumdisulphide and graphite are formed with the lubricant that 4. step adopts, and it consists of: MoS
2: 10~20%; Graphite: 80~90%.
Step 1. in, the industrially pure titanium bulk is incubated 1~2 hour 650 ℃~750 ℃ annealing.
Step 2. in, the industrially pure titanium bulk cuts into the square cross-section blank, the blank cross dimensions is 15mm * 15mm~50mm * 50mm, length dimension is 60mm~300mm, head is cut into 20 °~60 ° arcuation angles of wedge, and arc radius is determined according to die channel angle, the difficult deformation coefficient of work material and billet size; Grinding process is carried out on the surface, surface working roughness Ra≤3.2 μ m.
The die channel angle that described equal-diameter bending passage deformation adopts is Ф=90 °~110 °, bullnose Ψ=10 °~45 °;
Step 3. with step 4. in blank surface and mold cavity coating molybdenumdisulphide and compound lubricant of graphite be molybdenumdisulphide and Graphite Powder 99 are mixed after, the adding oil-based solvent applies behind the furnishing pasty state.
Step is 0.05~0.1mm with lubricant applying to the coat-thickness of blank surface in 3..
Step is wanted evenly at the lubricant of mold cavity internal surface coating in 4., and coat-thickness is 0.05mm~0.1mm.
Compare with existing technology, difficult-to-deformation metal block material room temperature equal-diameter bending passage deformation production method of the present invention brings following technique effect:
1. at room temperature,, obtain the pure titanium bulk of ganoid high strength industrial by repeatedly ECAP distortion;
2. at room temperature carry out the ECAP distortion, the tool and mould and the equipment of use are simple, easy and simple to handle;
3. at room temperature adopting the passage angle is 90 °~110 °, and single pass ECAP deformation extent is increased, and improves refinement efficient;
4. at room temperature carry out ECAP distortion, crystal grain does not produce when refinement replys and the recrystallize ruckbildung, thereby can make grain refining effect obvious, only need seldom passage just can to obtain high strength industrial pure;
5. when at room temperature carrying out repeatedly the ECAP distortion, do not adopt process annealing, simplified technical process, improved efficient, saved the energy.
Embodiment
Below by specific embodiment technical scheme of the present invention is further described, the experimental result that will implement people such as test result and Muscovite Vladimir V.Stolyarov simultaneously compares.
According to technical scheme of the present invention, difficult-to-deformation metal block material room temperature equal-diameter bending passage deformation production method of the present invention comprises the steps:
1. selecting the room temperature difficult-to-deformation material for use---industrially pure titanium TA1, TA2 hot rolled plate are as raw material, and hot rolled plate will be annealed;
2. industrially pure titanium TA1, TA2 hot rolled plate after will annealing cut into blank, and head cutter becomes certain angle of wedge, and grinding process is carried out on its surface;
3. at blank surface coating lubricant;
4. in the equal-diameter bending passage deformation mold cavity, apply lubricant;
5. the blank of surface applied lubricant is put into the equal-diameter bending passage deformation die channel that has applied lubricant, on pressing machine or extrusion machine, blank is carried out room temperature equal-diameter bending passage deformation crimp then, thereby realize the ECAP distortion of difficult deformable metal (industrially pure titanium, close-packed hexagonal structure) in room temperature;
6. after extruding is finished, repeated for above the 2.~6. step, through 2~8 B
CAfter the equal-diameter bending passage crimp of mode, can obtain the pure titanium of ganoid high strength industrial;
3. above-mentioned steps is the compounded lubricant that molybdenumdisulphide and graphite are formed with the lubricant that 4. step adopts, and it consists of: MoS
2: 10~20%; Graphite: 80~90%.
Step 1. in, the industrially pure titanium bulk is incubated 1~2 hour 650 ℃~750 ℃ annealing.
Step 2. in, the industrially pure titanium bulk cuts into the square cross-section blank, the blank cross dimensions is 5mm * 5mm~60mm * 60mm, length dimension is 60mm~300mm; Grinding process is carried out on the surface, surface working roughness Ra≤3.2 μ m.
The die channel angle that above-mentioned equal-diameter bending passage deformation adopts is Ф=90 °~110 °, bullnose Ψ=10 °~45 °.
Step 3. with step 4. in, blank surface and mold cavity coating molybdenumdisulphide and compound lubricant of graphite are that Graphite Powder 99 is added organic solvent, apply behind the furnishing pasty state.
Step 3. in, be 0.05~0.1mm with lubricant applying to the coat-thickness of blank surface.
Want evenly at the lubricant of mold cavity internal surface coating in 4. in step, coat-thickness is 0.05mm~0.1mm.
The theoretical explanation that the present invention is achieved is:
Adopt the equal-diameter bending passage deformation extrusion process at room temperature to prepare high strength difficult-to-deformation material (is example with the industrially pure titanium), be characterized in that equipment and preparation technology are simple.Adopt molybdenumdisulphide and compound lubricant of graphite that distortion sample and distortion mold cavity are handled during extruding, effectively the friction during controlled deformation improves and is out of shape the interior stress distribution situation of sample.When carrying out the ECAP distortion, by changing the shape of blank head, velocity of flow homogeneity with control each several part metal, can effectively improve the distribution of the additional internal stress that when ECAP is out of shape, produces because of each several part metal flow inequality, thereby guarantee the distortion sample in the ECAP deformation process not by squeeze crack, and finally obtain the high-intensity industrially pure titanium sample of ganoid bulk.The measure of using and controlling each several part metal flow speed of molybdenumdisulphide and compound lubricant of graphite has ensured carrying out smoothly of ECAP deformation technique effectively, guarantee to strengthen efficient simultaneously effectively, make under less extruding passage, obtain high-intensity ganoid industrially pure titanium sample.
It below is the specific embodiment that the contriver provides, need to prove, these embodiment are some more excellent examples, be mainly used in the further the present invention of understanding, the invention is not restricted to these embodiment, select for use different trade mark industrially pure titanium hot rolled plates as raw material through experiment showed, of applicant, all can at room temperature carry out the ECAP distortion according to method of the present invention, obtain high-intensity ganoid industrially pure titanium sample.
Embodiment 1:
Present embodiment adopts industrially pure titanium (TA2) hot rolled plate as raw material, with hot rolled plate 700 ℃ of annealing, be incubated 1 hour, it is 15mm * 15mm that industrially pure titanium TA2 hot-rolled sheet after the employing WEDM will be annealed cuts into cross dimensions, length is the 70mm blank, with the radius is 23.3mm processing head wedge shape, and grinding process is carried out on its surface, requires processing roughness Ra≤3.2 μ m.Then blank surface and passage angle Ф=110 °, mold cavity (distortion passage) internal surface of the ECAP distortion mould of bullnose Ψ=20 ° evenly applies molybdenumdisulphide and compound lubricant of graphite (10% molybdenumdisulphide and 90% graphite), after molybdenumdisulphide and Graphite Powder 99 mixed, add oil-based solvent, be coated to behind the furnishing pasty state in the mold cavity of blank surface and ECAP distortion mould.Coat-thickness is advisable with 0.05~0.1mm.The blank of surface applied lubricant is put into the ECAP distortion die channel that has applied lubricant.On extrusion machine, carry out room temperature ECAP crimp with the speed of 1mm/s.Obtain the pure titanium of ganoid high strength industrial, average grain size can be refined as below the 0.5 μ m by 28 initial μ m, and tensile strength is brought up to 760MPa by initial 475MPa.
Embodiment 2:
Present embodiment adopts industrially pure titanium (TA1) hot rolled plate as raw material, with hot rolled plate 700 ℃ of annealing, be incubated 1 hour, it is 15mm * 15mm that industrially pure titanium TA1 hot-rolled sheet after the employing WEDM will be annealed cuts into cross dimensions, length is the 70mm blank, with the radius is 25.5mm processing head wedge shape, and grinding process is carried out on its surface, requires processing roughness Ra≤3.2 μ m.Then blank surface and passage angle Ф=110 °, mold cavity (distortion passage) internal surface of the ECAP distortion mould of bullnose Ψ=20 ° evenly applies molybdenumdisulphide and compound lubricant of graphite (10% molybdenumdisulphide and 90% graphite), after molybdenumdisulphide and Graphite Powder 99 mixed, add oil-based solvent, be coated to behind the furnishing pasty state in the mold cavity of blank surface and ECAP distortion mould.Coat-thickness is advisable with 0.05~0.1mm.The blank of surface applied lubricant is put into the ECAP distortion die channel that has applied lubricant.On extrusion machine, carry out room temperature ECAP crimp with the speed of 2mm/s.After distortion is finished, sample is carried out surface treatment, and the coating lubricant, will be out of shape sample simultaneously and be rotated counterclockwise 90 °, and put into the ECAP distortion mould that has applied lubricating oil along its vertical symmetry axis, industrially pure titanium is carried out B
CFollowing a time ECAP distortion of mode after the extruding of 8 passages, obtains the pure titanium of ganoid high strength industrial, and average grain size can be refined as below the 0.25 μ m by 23 initial μ m, and tensile strength is brought up to 801MPa by initial 407MPa.
Embodiment 3:
Present embodiment adopts industrially pure titanium (TA1) hot rolled plate as raw material, with hot rolled plate 700 ℃ of annealing, be incubated 1 hour, it is 25mm * 25mm that industrially pure titanium TA1 hot-rolled sheet after the employing WEDM will be annealed cuts into cross dimensions, length is the 100mm blank, with the radius is 28.9mm processing head wedge shape, and grinding process is carried out on its surface, requires processing roughness Ra≤3.2 μ m.Then blank surface and passage angle Ф=90 °, mold cavity (distortion passage) internal surface of the ECAP distortion mould of bullnose Ψ=20 ° evenly applies molybdenumdisulphide+compound lubricant of graphite (20% molybdenumdisulphide and 80% graphite), after molybdenumdisulphide and Graphite Powder 99 mixed, add oil-based solvent, be coated to behind the furnishing pasty state in the mold cavity of blank surface and ECAP distortion mould.Coat-thickness is advisable with 0.05~0.1mm.The blank of surface applied lubricant is put into the ECAP distortion die channel that has applied lubricant.On pressing machine, carry out room temperature ECAP crimp with 26mm/s speed.After extruding is finished, sample is carried out surface treatment, and the coating lubricant, will be out of shape sample simultaneously and be rotated counterclockwise 90 °, and put into the ECAP distortion mould that has applied lubricating oil along its vertical symmetry axis, industrially pure titanium is carried out B
CFollowing a time ECAP distortion of mode after ECAP is out of shape 2 passages, obtains the pure titanium of ganoid high strength industrial, and average grain size can be refined as below the 0.4 μ m by 23 initial μ m, and tensile strength is brought up to 738MPa by initial 407MPa.
The example comparative analysis:
The average true strain amount of the ECAP of present embodiment 2 distortion a time be~0.635, after 8 passage ECAP were out of shape, accumulated deformation reached~and 5.08.The pure titanium average grain size of high strength industrial that obtains is refine to below the 0.25 μ m by 23 initial μ m.And the average true strain amount of the ECAP of embodiment 3 distortion a time be~1.05, after 2 passage ECAP were out of shape, accumulation strain reached~and 2.1.The pure titanium tensile strength of high strength industrial that obtains is brought up to 738MPa by initial 407MPa.Thereby industrially pure titanium intensity and over-all properties at normal temperatures improved.
Russia scholar Vladimir V.Stolyarov and American scholar Yuntian T.Zhu adopt the ECAP distortion mould of passage angle Ф=90 ° that industrially pure titanium is carried out the ECAP distortion at 450 ℃~350 ℃, have finally obtained the pure titanium of high strength industrial.The pure titanium performance of gained high strength industrial of the present invention and its comparing result are as shown in table 1.
Table 1: the present invention obtains to compare with Russian scholar's experiment and result
Annotate: V V Stolyarov, Y T Zhu, I V Alexandrov, et al.Materials Seience and Engineering, 2001, A299:59-67.
B that the present invention adopts
CMode is meant: sample rotates 90 ° around the longitudinal axis along same direction and descends a time extruding between twice extruding passage.