CN105296903B - A kind of ZrTiAlV alloys high pressure turn-knob electric field-assisted is heat-treated fine grain method - Google Patents
A kind of ZrTiAlV alloys high pressure turn-knob electric field-assisted is heat-treated fine grain method Download PDFInfo
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Abstract
A kind of ZrTiAlV alloys high pressure turn-knob electric field heat treatment fine grain method, it is mainly：47Zr 45Ti 5Al 3V sheet alloys are carried out into vacuum electric auxiliary solution treatment on discharging plasma sintering equipment, solid solubility temperature is 600 DEG C, 700 DEG C or 800 DEG C, and is incubated 20min, natural cooling cooling is powered off afterwards；By the sheet material after solution treatment under 4GPa or 5GPa pressure high pressure turn-knob, windup-degree be 360 °；The 47Zr 45Ti 5Al 3V sheet alloys after horizontal high voltage knob that different process solution treatment is gone forward side by side are carrying out vacuum electric field-assisted recrystallization annealing treatment, and 800 DEG C of its temperature, soaking time is 20min, and vacuum is 10‑3Pa.Between 20~120 μm, between 1173MPa~1307MPa, between tensile strength 1325MPa~1484MPa, elongation percentage is between 11.2%~15.7% for yield strength for the final 47Zr 45Ti 5Al 3V alloy grain sizes prepared.
Description
Technical field
The present invention relates to a kind of alloy fine grain treatment method, particularly a kind of fine grain treatment method of ZrTiAlV alloys.
Background technology
Zirconium and that zircaloy anti-radiation performance is excellent, small, corrosion-resistant and antioxygenic property is accumulated in neutron absorption cross-section is good, in core work
It is widely used in industry and acetic acid industry.And ZrTiAlV quaternary zircaloys, not only with preferable plasticity, while having higher
Intensity, be that one of more rapid zircaloy kind is developed in structural material field.
Liu Ping, Liang Shunxing et al. have synthesized 47Zr-45Ti-5Al-3V alloys first, and to forging state, annealed state and
Material property after solution treatment is conducted in-depth research, and specify that the basic mechanical that material possesses under various regimes
Energy and microstructure.But for uniform tinyization of 47Zr-45Ti-5Al-3V alloy grains and shortening zircaloy heat treatment when
Between wait it is not for further study.
The content of the invention
It is an object of the invention to provide the short ZrTiAlV alloy high pressures of a kind of crystallite dimension fine uniform, heat treatment time
Turn-knob-electric field-assisted heat treatment fine grain method, has good comprehensive through the 47Zr-45Ti-5Al-3V alloys after the PROCESS FOR TREATMENT
Mechanical property is closed, application of the 47Zr-45Ti-5Al-3V alloys in engineering field can be met.
Technical scheme is specific as follows：
1st, 1.5~2mm thick 47Zr-45Ti-5Al-3V sheet alloys are loaded in mould first, then by alloy and mould
Being placed in discharge plasma sintering (Spark Plasma Sintering, abbreviation SPS) equipment carries out electric field-assisted solution treatment,
Solid solubility temperature is 600 DEG C, 700 DEG C or 800 DEG C, and seaming chuck is descending to apply 5MPa pressure to sample.Heat treatment process of the present invention is equal
Carried out in vacuum environment, vacuum is 10-3Pa, can prevent 47Zr-45Ti-5Al-3V alloys to be oxidized.Pulse current is loaded
Onto 47Zr-45Ti-5Al-3V sheet alloys, it is brought rapidly up to required temperature, and be incubated 20min, afterwards discharge sintering
Device powers down, natural cooling cooling.
2nd, the 47Zr-45Ti-5Al-3V sheet alloys after step 1 solution treatment are carried out into height under 4GPa or 5GPa pressure
Pressure knob, mould as shown in figure 1, windup-degree be 360 °, make 47Zr-45Ti-5Al- under the collective effect of moment of torsion and pressure
There is compression and detrusion in 3V sheet alloys.
3rd, the 47Zr-45Ti-5Al-3V sheet alloys after step 2 is processed through different process set in discharge plasma sintering
Standby above to carry out electric field-assisted recrystallization annealing treatment, its temperature is 800 DEG C, and vacuum is 10-3Pa, soaking time is 20min.
The present invention has the following advantages that compared with prior art：
1st, the residual of original 47Zr-45Ti-5Al-3V sheet alloys can be eliminated using electric field-assisted solid solution treatment process in advance
Residue stress and its tissue defects, prevent it from producing non-plastic fracture during high pressure turn-knob.
2nd, using high pressure turn-knob technique, severe plastic deformation is produced to 47Zr-45Ti-5Al-3V sheet alloys, makes it brilliant
Grain heavy damage and in a large amount of dislocations of Broken Crystal building up inside, then takes discharge plasma sintering process to carry out electric field-assisted
Recrystallization annealing is processed.The characteristics of technique has low-voltage, high current, can significantly change 47Zr-45Ti-5Al-3V alloys
Microstructure.Under pulse current effect, the free ion electric discharge heat production in ZrTiAlV alloys, and it is rapid to heat up, together
When Broken Crystal inside forming core point increase, homogeneous nucleation is grown up afterwards, ultimately forms uniform tiny equiaxed grain structure.
3rd, the 47Zr-45Ti-5Al-3V alloys after processed by the invention have superior comprehensive mechanical property, and its crystal grain is
Uniform equiax crystal, crystallite dimension between 20~120 μm, yield strength between 1173MPa~1307MPa, tensile strength
Between 1325MPa~1484MPa, elongation percentage is capable of achieving 47Zr-45Ti-5Al-3V alloys and exists between 11.2%~15.7%
The application of engineering field.
Brief description of the drawings
Fig. 1 is the simplified schematic diagram that high pressure knob mould clamps sample.
In figure：1st, mold, 2, sample, 3, lower mould.
Specific embodiment
Embodiment 1
The thick upper/lower terminals of 47Zr-45Ti-5Al-3V sheet specimens 2 of 1.5~2mm are respectively charged into the He of upper graphite jig 1
In lower graphite jig 3, the alloy sample and mould that will be completed are placed in discharge plasma sintering machine, and seaming chuck is descending to examination
Sample applies 5MPa pressure, then vacuum is extracted into 10-3Pa.Using upper and lower pressure head and powered electrode will specifically sinter power supply and
Pressing pressure is put on 47Zr-45Ti-5Al-3V sheet specimens, and the plasma that pulse current is produced makes inside alloy sample
Ionic discharge heat production, alloy is brought rapidly up carrying out solution treatment to 600 DEG C, strict temperature control and is incubated 20min afterwards, finally
Power-off natural cooling.Sheet material after solution treatment is entered into mould under horizontal high voltage turn-knob is rotated under 4GPa pressure, the anglec of rotation is
360 °, 800 DEG C of annealing recrystallization treatment are then carried out in discharge plasma sintering machine, soaking time is 20min.This technique is obtained
The 47Zr-45Ti-5Al-3V sheet alloys thickness for arriving is 1~1.3mm, and die break is serious during high pressure turn-knob, then
Grain structure is still not of uniform size after recrystallization annealing temperature, and crystallite dimension is changed into 80~120 μm from original 350~400 μm.Yield strength
1173MPa, tensile strength 1325MPa, plastic elongation rate are 11.2%.
Embodiment 2
The thick 47Zr-45Ti-5Al-3V sheet specimens upper/lower terminals of 1.5~2mm are respectively charged into upper and lower graphite jig
Interior, the alloy sample and mould that will be completed are placed in discharge plasma sintering machine, and seaming chuck is descending to apply 5MPa to sample
Pressure, then vacuum is extracted into 10-3Pa.Specific sintering power supply and pressing pressure are applied using upper and lower pressure head and powered electrode
It is added on 47Zr-45Ti-5Al-3V sheet specimens, the plasma that pulse current is produced produces the electric discharge of alloy sample inner ion
Heat, alloy is brought rapidly up carrying out solution treatment to 600 DEG C, strict temperature control and is incubated 20min afterwards, finally powers off nature cold
But.Sheet material after solution treatment is entered into mould under horizontal high voltage turn-knob is rotated under 5GPa pressure, the anglec of rotation is 360 °, Ran Hou
800 DEG C of annealing recrystallization treatment are carried out in discharge plasma sintering machine, soaking time is 20min.The 47Zr- that this technique is obtained
45Ti-5Al-3V sheet alloys thickness is 0.9~1.2mm, and die break is even more serious during high pressure turn-knob, recrystallization
Grain structure is still not of uniform size after annealing, and crystallite dimension is changed into 60~100 μm from original 350~400 μm.Yield strength
1237MPa, tensile strength 1397MPa, plastic elongation rate can reach 13.2%.
Embodiment 3
The thick 47Zr-45Ti-5Al-3V sheet specimens upper/lower terminals of 1.5~2mm are respectively charged into upper and lower graphite jig
Interior, the alloy sample and mould that will be completed are placed in discharge plasma sintering machine, and seaming chuck is descending to apply 5MPa to sample
Pressure, then vacuum is extracted into 10-3Pa.Specific sintering power supply and pressing pressure are applied using upper and lower pressure head and powered electrode
It is added on 47Zr-45Ti-5Al-3V sheet specimens, the plasma that pulse current is produced produces the electric discharge of alloy sample inner ion
Heat, alloy is brought rapidly up carrying out solution treatment to 700 DEG C, strict temperature control and is incubated 20min afterwards, finally powers off nature cold
But.Sheet material after solution treatment is entered into mould under horizontal high voltage turn-knob is rotated under 4GPa pressure, the anglec of rotation is 360 °, Ran Hou
800 DEG C of annealing recrystallization treatment are carried out in discharge plasma sintering machine, soaking time is 20min.The 47Zr- that this technique is obtained
45Ti-5Al-3V sheet alloys thickness is 0.9~1.25mm, and alloy grain has been refined after recrystallization annealing, is uniform equiaxial
Crystalline substance, crystallite dimension refine to 60~80 μm by 350~400 μm.Yield strength is 1218MPa, and tensile strength is 1389MPa, is prolonged
The rate of stretching reaches 12.5%.
Embodiment 4
The thick 47Zr-45Ti-5Al-3V sheet specimens upper/lower terminals of 1.5~2mm are respectively charged into upper and lower graphite jig
Interior, the alloy sample and mould that will be completed are placed in discharge plasma sintering machine, and seaming chuck is descending to apply 5MPa to sample
Pressure, then vacuum is extracted into 10-3Pa.Specific sintering power supply and pressing pressure are applied using upper and lower pressure head and powered electrode
It is added on 47Zr-45Ti-5Al-3V sheet specimens, the plasma that pulse current is produced produces the electric discharge of alloy sample inner ion
Heat, alloy is brought rapidly up carrying out solution treatment to 700 DEG C, strict temperature control and is incubated 20min afterwards, finally powers off nature cold
But.Sheet material after solution treatment is entered into mould under horizontal high voltage turn-knob is rotated under 5GPa pressure, the anglec of rotation is 360 °, Ran Hou
800 DEG C of annealing recrystallization treatment are carried out in discharge plasma sintering machine, soaking time is 20min.The 47Zr- that this technique is obtained
45Ti-5Al-3V sheet alloys thickness is 0.8~1mm, and alloy grain refinement, is uniform equiax crystal, crystal grain after recrystallization annealing
Size refine to 40~60 μm or so by original 350~400 μm.Yield strength is 1263MPa, and tensile strength is 1415MPa, is prolonged
Stretch rate up to 14.2%.
Embodiment 5
The thick 47Zr-45Ti-5Al-3V sheet specimens upper/lower terminals of 1.5~2mm are respectively charged into upper and lower graphite jig
Interior, the alloy sample and mould that will be completed are placed in discharge plasma sintering machine, and seaming chuck is descending to apply 5MPa to sample
Pressure, then vacuum is extracted into 10-3Pa.Specific sintering power supply and pressing pressure are applied using upper and lower pressure head and powered electrode
It is added on 47Zr-45Ti-5Al-3V sheet specimens, the plasma that pulse current is produced produces the electric discharge of alloy sample inner ion
Heat, alloy is brought rapidly up carrying out solution treatment to 800 DEG C, strict temperature control and is incubated 20min afterwards, finally powers off nature cold
But.Sheet material after solution treatment is entered into mould under horizontal high voltage turn-knob is rotated under 4GPa pressure, the anglec of rotation is 360 °, Ran Hou
800 DEG C of annealing recrystallization treatment are carried out in discharge plasma sintering machine, soaking time is 20min.The 47Zr- that this technique is obtained
45Ti-5Al-3V sheet alloys thickness is 0.8~1.1mm, and crystal grain is uniformly refined after recrystallization annealing, is equiax crystal, crystal grain
Size is refine at 40 μm or so by original 350~400 μm.Yield strength is 1285MPa, and tensile strength is 1443MPa, is extended
Rate is up to 14.9%.
Embodiment 6
The thick 47Zr-45Ti-5Al-3V sheet specimens upper/lower terminals of 1.5~2mm are respectively charged into upper and lower graphite jig
Interior, the alloy sample and mould that will be completed are placed in discharge plasma sintering machine, and seaming chuck is descending to apply 5MPa to sample
Pressure, then vacuum is extracted into 10-3Pa.Specific sintering power supply and pressing pressure are applied using upper and lower pressure head and powered electrode
It is added on 47Zr-45Ti-5Al-3V sheet specimens, the plasma that pulse current is produced produces the electric discharge of alloy sample inner ion
Heat, alloy is brought rapidly up carrying out solution treatment to 800 DEG C, strict temperature control and is incubated 20min afterwards, finally powers off nature cold
But.Sheet material after solution treatment is entered into mould under horizontal high voltage turn-knob is rotated under 5GPa pressure, the anglec of rotation is 360 °, Ran Hou
800 DEG C of annealing recrystallization treatment are carried out in discharge plasma sintering machine, soaking time is 20min.The 47Zr- that this technique is obtained
45Ti-5Al-3V sheet alloys thickness be 0.7~0.9mm, crystal grain is uniformly refined after recrystallization annealing, be even tissue etc.
Axialite, crystallite dimension is changed into 20 μm from original 350~400 μm.Yield strength is 1307MPa, and tensile strength is 1484MPa, is prolonged
Stretch rate up to 15.7%.
Claims (1)
1. a kind of ZrTiAlV alloys high pressure turn-knob-electric field-assisted is heat-treated fine grain method,
(1) the thick 47Zr-45Ti-5Al-3V sheet alloys of 1.5~2mm are placed in discharging plasma sintering equipment together with mould
On carry out electric field-assisted solution treatment, solid solubility temperature is 600 DEG C, 700 DEG C or 800 DEG C, and seaming chuck is descending to apply 5MPa to sample
Pressure, vacuum is 10-3Pa, pulse current is loaded on 47Zr-45Ti-5Al-3V sheet alloys, it is brought rapidly up to institute
Temperature is needed, and is incubated 20min, Temperature fall is powered off afterwards；
(2) sheet material after step (1) solution treatment is carried out into high pressure torsion under 4GPa or 5GPa pressure, windup-degree is
360°；
It is characterized in that：(3) by step (2) different process treatment after 47Zr-45Ti-5Al-3V sheet alloys electric discharge etc. from
Electric field-assisted recrystallization annealing treatment is carried out on sub- agglomerating plant, 800 DEG C of its temperature, soaking time is 20min, and vacuum is
10-3Pa。
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| CN106381458A (en) * | 2016-10-13 | 2017-02-08 | 南京工程学院 | Amorphous alloy strengthening method based on limited high-pressure torsion |
| CN106925648B (en) * | 2017-04-18 | 2018-09-04 | 燕山大学 | A kind of electric field-assisted high pressure torsion device and high pressure torsion method |
| CN107267790A (en) * | 2017-05-19 | 2017-10-20 | 武汉理工大学 | It is a kind of to consolidate the method that nano-sized powders prepare bulk nanocrystalline metal material |
| CN107764664A (en) * | 2017-10-09 | 2018-03-06 | 燕山大学 | A kind of electric field-assisted high pressure torsion testing machine |
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| CN110205573A (en) * | 2019-06-24 | 2019-09-06 | 合肥工业大学 | The quick annealing process of regulation deformation tungsten material microstructure under a kind of low temperature |
| CN110129701B (en) * | 2019-06-24 | 2021-05-04 | 合肥工业大学 | Method for recrystallization annealing of refractory metal |
| CN111763896B (en) * | 2020-06-15 | 2021-09-03 | 北京航空航天大学 | Method for regulating and controlling mechanical property of magnesium alloy by utilizing crystal boundary stability |
| CN113600729B (en) * | 2021-08-30 | 2022-09-16 | 燕山大学 | Reciprocating pressure-shear coupling upsetting method for cast ingot |
| CN114293120B (en) * | 2021-12-30 | 2023-02-07 | 温州大学 | Pulse electric field auxiliary heat treatment method for improving plasticity and toughness of titanium alloy |
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| CN1332057C (en) * | 2003-01-10 | 2007-08-15 | 西北工业大学 | Prepn of columnar superfine crystal material |
| CN100392373C (en) * | 2005-08-04 | 2008-06-04 | 中国科学院力学研究所 | High pressure torsion test method capable of fining sample grain |
| CN104233143B (en) * | 2014-08-26 | 2016-04-06 | 燕山大学 | A kind of ZrTiAlV sheet alloy electric field-assisted heat treating method |
| CN104889186B (en) * | 2015-06-18 | 2017-09-22 | 燕山大学 | A kind of positive and negative Compound Extrusion manufacturing process of ZrTiAlV alloys electric field-assisted |
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