CN103205663B - Method for preparing difficultly-deformed metal block nanocrystalline material at low temperature - Google Patents
Method for preparing difficultly-deformed metal block nanocrystalline material at low temperature Download PDFInfo
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- CN103205663B CN103205663B CN201310127478.6A CN201310127478A CN103205663B CN 103205663 B CN103205663 B CN 103205663B CN 201310127478 A CN201310127478 A CN 201310127478A CN 103205663 B CN103205663 B CN 103205663B
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Abstract
The invention discloses a method for preparing a difficultly-deformed metal block nanocrystalline material at a low temperature. The method comprises the following steps of: soaking a block sample to be deformed in a low-temperature cooling liquid so as to obtain a required low temperature, carrying out low-energy repeated impact loading on the block sample by using a drop-hammer impact testing machine, gradually refining crystal particles of the test sample with the increasing of the impact number of times of a drop hammer and the strain capacity of the test sample, and obtaining the block nanocrystalline material when the strain capacity reaches a certain value. In the whole deformation process, the test sample is always soaked in the low-temperature cooling liquid, so that the required low-temperature environment is ensured. The method is particularly suitable for preparation of the difficultly-deformed metal block nanocrystalline material at a low temperature and simultaneously has the advantages of wide low-temperature application range, simplicity in operation, low manufacturing cost and the like.
Description
Technical field
The invention belongs to Metal Forming technical field, relate to the technology of preparing of bulk nano-crystalline material, especially a kind of be applicable to low temperature under use small capacity hump to prepare the method for difficult-to-deformation metal block body nanocrystalline material.
Background technology
Nano material is different from conventional coarse grain material owing to having, and is usually superior to the physics and chemistry of conventional coarse grain material, mechanical property and to become in current Material Field an important research direction.The nano material of severe plastic deformation technology processing is adopted to have the advantages such as three-dimensional dimension large, clean densification, pore-free gap.This makes it become bulk nanostructured material technology of preparing most with prospects, receives increasing concern.Typical severe plastic deformation technology comprises the methods such as Equal Channel Angular Pressing (ECAP), high pressure torsion (HPT) and laminated rolling (ARB).Apply these methods, people have successfully prepared multiple simple metal, alloy block nanocrystalline material (as Cu, Al, Ni, Fe, carbon steel etc.).
Such as, for difficult deformable metal or alloy, titanium alloy, zircaloy etc., they have higher yield strength, usually reach hundreds of MPa and even go up gpa.At room temperature apply above-mentioned severe plastic deformation method and carry out in the process of being out of shape that they show very high resistance of deformation, be difficult to machining deformation.In order to overcome this high resistance of deformation, increase the plastic fluidity of distortion, people, by improving temperature, carry out machining deformation under middle temperature or high temperature.But raised temperature brings again another problem while increasing machinability.Sample crystal grain is on the one hand out of shape refinement, on the other hand because temperature raises, recrystallization appears in crystal grain, alligatoring of growing up, and partial offset distortion refinement, makes grain refining effect weaken.Make a general survey of the difficult deformable metal material applying the processing of severe plastic deformation technology in recent years under middle temperature or hot conditions, be difficult to find to obtain bulk nano-crystalline.
Visible, difficult deformable metal material is out of shape and is unfavorable for block nanometer under middle and high temperature conditions.In order to strengthen the machinability of these materials under room temperature, people have done some in improvement and innovation severe plastic deformation technical elements and have attempted.Such as, ECAP die channel angle is increased with equivalent strain when reducing every time crimp to increase the room temperature machinability of material.Or the extrusion speed of the ECAP that slows down, makes sample occur fully to reply, easily deformable refinement.In addition, in ECAP extrusion process used for forming, increase hydrostatic pressure can reduce tension additional in material, avoid occurring crackle, the machinability of material is increased greatly.Recently, we have proposed " method that small capacity hump technology prepares bulk nanostructured material " (license number: ZL201010286615.7), by controlling landing impact testing machine running parameter, Repeated Impact Load is applied to sample, the technology such as ECAP, HPT, ARB that overcome adopt static state or quasi-static loads difficult deformable metal to be difficult to the difficulty of being out of shape, and have successfully prepared Ti-10V-2Fe-3Al high strength titanium alloy bulk nano-crystalline., it should be noted that these improvement for severe plastic deformation technology above and the main block nanometer concentrating at room temperature difficult deformable metal of innovation.And the bulk nano-crystalline preparing difficult deformable metal under low temperature is seldom related to, also rarely have report in document.
Summary of the invention
The object of the invention is to the shortcoming overcoming above-mentioned prior art, the method of difficult-to-deformation metal block body nanocrystalline material is prepared under a kind of low temperature is provided, the mode of small capacity hump under which employing low temperature, block sample to be deformed is immersed in all the time in cryogenic liquid to obtain required low temperature, then carry out small capacity hump loading, obtain the bulk nano-crystalline of difficult deformable metal material.
The object of the invention is to solve by the following technical programs:
Prepare the method for difficult-to-deformation metal block body nanocrystalline material under this low temperature, comprise the following steps:
1) obtain difficult-to-deformation metal block body sample to be processed, difficult deformable metal is the metal material of all yield strengths more than hundred MPas;
2) continue to inject cryogenic liquid in the anvil recess of drop hammer impact testing machine by liquid injection port, difficult deformable rock blocks sample to be processed is placed in cooling fluid in groove and soaks;
3) trip rod is inserted in anvil recess, dropped hammer after winching to specified altitude assignment and discharged with shock bar, realize the blastic deformation to difficult-to-deformation metal block body sample by power transmission; Drop hammer and repeat above-mentioned impact process with the frequency of impact of 5 ~ 30 times/min, until difficult-to-deformation metal block body sample reaches the deformation strain amount ε specified,
wherein, ε is deformation strain amount, h
0for thickness before sample deformation, h is thickness after sample deformation; In whole deformation process, continue in groove, inject selected cryogenic liquid by liquid injection port, sample is immersed in cooling fluid all the time.
Further, in step 1), the profile of described metal blocks sample is cylindrical, patty or cuboid.Difficult deformable metal is titanium, titanium alloy or zircaloy.
Further, step 2) in, described cryogenic liquid is the mixing of liquid nitrogen, liquid nitrogen and ethanol or the mixing of liquid nitrogen and acetone.
Further, in step 3), the deformation strain amount ε scope of difficult-to-deformation metal block body sample is 1 ~ 5; The tup that drops hammer is the flat tup in heavy in section, and quality of dropping hammer is 1 ~ 20kg, and effective shock height range of choice is 100 ~ 2000mm.
The present invention has following beneficial effect:
The method preparing difficult-to-deformation metal block body nanocrystalline material under the inventive method low temperature adopts the mode of small capacity hump at low temperatures to prepare difficult-to-deformation metal block body nanocrystalline material, low-temperature growth simple metal, alloy block nanocrystalline material can be widely used in, under being specially adapted to low temperature, prepare the bulk nano-crystalline material of difficult deformable metal, alloy.It has, and applicable low temperature range is wide, low cost of manufacture, simple operation and other advantages.Method of the present invention has very wide prospect in fundamental research and practical engineering application.
Accompanying drawing explanation
The structural representation of landing impact testing machine of Fig. 1 for preparing difficult-to-deformation metal block body nanocrystalline material under low temperature of the present invention and adopting.
Wherein, 1 drop hammer; 2 trip rods; 3 anvil recess; 4 liquid injection ports; 5 samples; 6 slide rails; 7 liquid outlets; 8 cooling fluids; 9 anvil blocks.
Fig. 2 is the metallographic pattern photo of Ti-2Al-2.5Zr alloy after 800 ° of C anneal 16 hours.
Fig. 3 is the metallographic pattern photo utilizing the technology of the present invention differently strained amount of distortion in liquid nitrogen (about-196 ° of C) through the Ti-2Al-2.5Zr alloy of annealing in process: (a) 0.1; (b) 0.35; (c) 1.2.
Fig. 4 is the transmission electron micrograph utilizing the technology of the present invention differently strained amount of distortion in liquid nitrogen (about-196 ° of C) through the Ti-2Al-2.5Zr alloy of annealing in process: (a) 0.1; (b) 0.35; (c) 1.2.
Fig. 5 is the metallographic pattern photo of TA2 industrially pure titanium sample after 800 ° of C anneal 2 hours.
Fig. 6 is that the TA2 industrially pure titanium sample of annealed process utilizes the pattern photo of the technology of the present invention in liquid nitrogen+alcohol mixeding liquid (about-90 ° of C) after distortion 1.6 dependent variables: (a) metallographic pattern; (b) transmission electron microscopy pattern.
Detailed description of the invention
The device that the method preparing difficult-to-deformation metal block body nanocrystalline material under low temperature of the present invention uses is landing impact testing machine, and its apparatus structure as shown in Figure 1.In figure, 1 for dropping hammer, and 2 is trip rod, and 3 is anvil recess, and 4 is liquid injection port, and 5 is sample, and 6 is slide rail, and 7 is liquid outlet, and 8 is cooling fluid, and 9 is anvil block.The method specifically comprises the following steps:
1) obtain difficult-to-deformation metal block body sample to be processed, the profile of this difficult-to-deformation metal block body sample can be cylindrical, patty or cuboid.The difficult deformable metal of indication of the present invention comprises all yield strengths such as titanium or titanium alloy, zircaloy and even goes up the metal material of more than gpa in hundred MPas to hundreds of MPa.
2) continue to inject cryogenic liquid in the anvil recess 3 of drop hammer impact testing machine by liquid injection port, difficult deformable rock blocks sample to be processed is placed in cooling fluid in anvil recess 3 and soaks.Cryogenic liquid can select the mixing of liquid nitrogen, liquid nitrogen and ethanol, liquid nitrogen and acetone any low temperature liquid cooling medium such as to mix.
(3) trip rod 2 is inserted in anvil recess, drop hammer 1 after winching to specified altitude assignment and discharge with shock bar 2, realize the blastic deformation to sample by power transmission.Drop hammer and 1 repeat above-mentioned impact process with the frequency of impact of 5 ~ 30 times/min, until sample deformation reaches the dependent variable ε specified,
wherein, ε is deformation strain amount, h
0for thickness before sample deformation, h is thickness after sample deformation.In whole deformation process, continue in groove, inject selected cryogenic liquid by liquid injection port, sample is immersed in cooling fluid all the time.Here, sample deformation dependent variable ε scope is 1 ~ 5.1 tup that drops hammer is the flat tup in heavy in section, and 1 quality of dropping hammer is 1 ~ 20kg, and effective shock height range of choice is 100 ~ 2000mm.
Below in conjunction with drawings and Examples, content of the present invention is further elaborated, it is pointed out that the present invention is not limited to these embodiments.
Embodiment 1:
Small capacity hump is utilized to load the difficult deformable metal Ti-2Al-2.5Zr bulk nano-crystalline material of preparation in liquid nitrogen (about-196 ° of C):
Equipment: landing impact testing machine (as Fig. 1);
Drop hammer 1 quality: 8kg;
Impact effective depth: 900mm;
Frequency of impact: 8 times/min;
Low temperature liquid cooling fluid: liquid nitrogen (about-196 ° of C);
Sample deformation dependent variable: 1.2;
Ti-2Al-2.5Zr alloy material: alloy actual constituent is Ti-1.59%Al-1.91%Zr (percentage by weight), and specimen size is Ф 16mm × 2mm.After 800 ° of C anneal 16 hours, microstructure forms by waiting axle α phase crystal grain, and its crystallite dimension about 100 μm, metallographic pattern as shown in Figure 2.
The metallographic pattern of sample in liquid nitrogen (about-196 ° of C) after the repeat impact distortion of differently strained amount as shown in Figure 3, after can seeing distortion 0.1 dependent variable, forms numerous tiny, parallel faller gill shape twin in coarse-grain.When dependent variable is increased to 0.35, the fragmentation of faller gill shape twin, but still keep original position to.After dependent variable is increased to 1.2, original coarse-grain disappears completely, the substitute is ultrafine crystal grain.Further amplifying observation through transmission electron microscope can be seen, after being out of shape 0.1 dependent variable, transmission electron microscopy pattern is shown as parallel twin sheet.Along with dependent variable be increased to 0.35 time, twin sheet occurs broken.After dependent variable continues to be increased to 1.2, microstructure is made up of nanocrystalline, and crystallite dimension is about 50nm, and electronic diffraction collection of illustrative plates is diffraction annulus, as shown in Figure 4.
Embodiment 2:
Small capacity hump is utilized to load the difficult deformable metal TA2 industrially pure titanium bulk nano-crystalline material of preparation in liquid nitrogen+alcohol mixeding liquid (about-90 ° of C):
Equipment: landing impact testing machine;
Drop hammer quality: 5kg;
Impact effective depth: 500mm;
Cryogenic liquid: liquid nitrogen+alcohol mixeding liquid (about-90 ° of C);
Frequency of impact: 10 times/min;
Sample deformation dependent variable: 1.6;
TA2 industrially pure titanium material: specimen size is Ф 10mm × 4mm.Coarse grains after 800 ° of C anneal 2 hours, about 150 μm, as shown in Figure 5.
The tissue topography of sample in liquid nitrogen+alcohol mixeding liquid (about-90 ° of C) after the repeat impact distortion of 1.6 dependent variables as shown in Figure 6.Can see, after TA2 industrially pure titanium sample after 800 ° of C anneal 2 hours utilizes the technology of the present invention to be out of shape 1.6 dependent variables in liquid nitrogen+alcohol mixeding liquid (about-90 ° of C), metallographic pattern is shown as original coarse grain and disappears completely, the substitute is ultrafine crystal grain.Transmission electron microscopy pattern is shown as microstructure and is made up of nanocrystalline, and crystallite dimension is about 90nm, and electronic diffraction collection of illustrative plates is interrupted shape diffraction annulus.
Embodiment 3
1) obtain difficult-to-deformation metal block body sample to be processed, the profile of this difficult-to-deformation metal block body sample can be cylindrical; Difficult deformable metal selects titanium.
2) continue to inject cryogenic liquid in the anvil recess 3 of drop hammer impact testing machine by liquid injection port, difficult deformable rock blocks sample to be processed is placed in cooling fluid in anvil recess 3 and soaks.Cryogenic liquid can select the mixing of liquid nitrogen, liquid nitrogen and ethanol, liquid nitrogen and acetone any low temperature liquid cooling medium such as to mix.
(3) trip rod 2 is inserted in anvil recess, drop hammer 1 after winching to specified altitude assignment and discharge with shock bar 2, realize the blastic deformation to sample by power transmission.Drop hammer and 1 repeat above-mentioned impact process with the frequency of impact of 5 times/min, until sample deformation reaches the dependent variable ε specified,
wherein, ε is deformation strain amount, h
0for thickness before sample deformation, h is thickness after sample deformation.In whole deformation process, continue in groove, inject selected cryogenic liquid by liquid injection port, sample is immersed in cooling fluid all the time.Here, sample deformation dependent variable ε scope is 1 ~ 5.1 tup that drops hammer is the flat tup in heavy in section, and 1 quality of dropping hammer is 20kg, and effective shock height range of choice is 100 ~ 2000mm.
Embodiment 4
1) obtain difficult-to-deformation metal block body sample to be processed, the profile of this difficult-to-deformation metal block body sample can be patty; Difficult deformable metal selects titanium alloy.
2) continue to inject cryogenic liquid in the anvil recess 3 of drop hammer impact testing machine by liquid injection port, difficult deformable rock blocks sample to be processed is placed in cooling fluid in anvil recess 3 and soaks.Cryogenic liquid can select the mixing of liquid nitrogen, liquid nitrogen and ethanol, liquid nitrogen and acetone any low temperature liquid cooling medium such as to mix.
(3) trip rod 2 is inserted in anvil recess, drop hammer 1 after winching to specified altitude assignment and discharge with shock bar 2, realize the blastic deformation to sample by power transmission.Drop hammer and 1 repeat above-mentioned impact process with the frequency of impact of 30 times/min, until sample deformation reaches the dependent variable ε specified,
wherein, ε is deformation strain amount, h
0for thickness before sample deformation, h is thickness after sample deformation.In whole deformation process, continue in groove, inject selected cryogenic liquid by liquid injection port, sample is immersed in cooling fluid all the time.Here, sample deformation dependent variable ε scope is 1 ~ 5.1 tup that drops hammer is the flat tup in heavy in section, and 1 quality of dropping hammer is 1kg, and effective shock height range of choice is 100 ~ 2000mm.
Embodiment 5
1) obtain difficult-to-deformation metal block body sample to be processed, the profile of this difficult-to-deformation metal block body sample can be cuboid; Difficult deformable metal selects zircaloy.
2) continue to inject cryogenic liquid in the anvil recess 3 of drop hammer impact testing machine by liquid injection port, difficult deformable rock blocks sample to be processed is placed in cooling fluid in anvil recess 3 and soaks.Cryogenic liquid can select the mixing of liquid nitrogen, liquid nitrogen and ethanol, liquid nitrogen and acetone any low temperature liquid cooling medium such as to mix.
(3) trip rod 2 is inserted in anvil recess, drop hammer 1 after winching to specified altitude assignment and discharge with shock bar 2, realize the blastic deformation to sample by power transmission.Drop hammer and 1 repeat above-mentioned impact process with the frequency of impact of 20 times/min, until sample deformation reaches the dependent variable ε specified,
wherein, ε is deformation strain amount, h
0for thickness before sample deformation, h is thickness after sample deformation.In whole deformation process, continue in groove, inject selected cryogenic liquid by liquid injection port, sample is immersed in cooling fluid all the time.Here, sample deformation dependent variable ε scope is 1 ~ 5.1 tup that drops hammer is the flat tup in heavy in section, and 1 quality of dropping hammer is 15kg, and effective shock height range of choice is 100 ~ 2000mm.
Claims (2)
1. prepare a method for difficult-to-deformation metal block body nanocrystalline material under low temperature, it is characterized in that, comprise the following steps:
1) obtain difficult-to-deformation metal block body sample to be processed, difficult deformable metal is titanium, titanium alloy or zircaloy;
2) continue to inject cryogenic liquid in the anvil recess of drop hammer impact testing machine by liquid injection port, difficult deformable rock blocks sample to be processed is placed in cooling fluid in groove and soaks; Described cryogenic liquid is the mixing of liquid nitrogen, liquid nitrogen and ethanol or the mixing of liquid nitrogen and acetone;
3) trip rod is inserted in anvil recess, dropped hammer after winching to specified altitude assignment and discharged with shock bar, realize the blastic deformation to difficult-to-deformation metal block body sample by power transmission; Drop hammer and repeat above-mentioned impact process with the frequency of impact of 5 ~ 30 times/min, until difficult-to-deformation metal block body sample reaches the deformation strain amount ε specified,
wherein, ε is deformation strain amount, h
0for thickness before sample deformation, h is thickness after sample deformation; In whole deformation process, continue in groove, inject selected cryogenic liquid by liquid injection port, sample is immersed in cooling fluid all the time; The deformation strain amount ε scope of difficult-to-deformation metal block body sample is 1 ~ 1.6; The tup that drops hammer is the flat tup in heavy in section, and quality of dropping hammer is 1 ~ 20kg, and effective shock height range of choice is 100 ~ 2000mm.
2. prepare the method for difficult-to-deformation metal block body nanocrystalline material under low temperature according to claim 1, it is characterized in that, step 1) in, the profile of described metal blocks sample is cylindrical, patty or cuboid.
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| CN104593572B (en) * | 2014-12-22 | 2016-08-24 | 浙江大学 | A kind of full-compact nanometer crystalline pure iron block materials preparation method |
| CN110426298A (en) * | 2019-07-24 | 2019-11-08 | 郑州四维新材料技术研究院有限公司 | A kind of test material low-temperature flexibility combination unit |
| CN112143937B (en) * | 2020-09-29 | 2022-02-15 | 中国科学院金属研究所 | High-thermal-stability equiaxial nanocrystalline Ti-Zr-Co alloy and preparation method thereof |
| CN113073184A (en) * | 2021-03-26 | 2021-07-06 | 兰州理工大学 | Ultralow-temperature impact dynamic-load large-plastic-deformation device and method |
| CN114367867B (en) * | 2021-12-22 | 2022-10-18 | 江苏盛安信息科技有限公司 | Pre-shaped quick-freezing operation micro-forced thin titanium alloy robot arm processing equipment |
| CN115537688B (en) * | 2022-10-24 | 2023-08-25 | 西北工业大学 | Method for realizing nanocrystalline and nano twin crystal heterostructure |
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| CN101948948A (en) * | 2010-09-19 | 2011-01-19 | 西安交通大学 | Method for producing blocky nano material by small energy multiple impact technology |
| CN103014389A (en) * | 2013-01-21 | 2013-04-03 | 湘潭大学 | Preparation method of high-strength nanocrystalline type medical Beta titanium alloy for orthopaedic implanting |
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| CN101948948A (en) * | 2010-09-19 | 2011-01-19 | 西安交通大学 | Method for producing blocky nano material by small energy multiple impact technology |
| CN103014389A (en) * | 2013-01-21 | 2013-04-03 | 湘潭大学 | Preparation method of high-strength nanocrystalline type medical Beta titanium alloy for orthopaedic implanting |
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