High mangaenese steel of a kind of Doped nanocrystal corundum Hard Inclusion disperse phase and preparation method thereof
Technical field
The present invention relates to high manganese steel material technical field, be specifically related to high mangaenese steel of a kind of Doped nanocrystal corundum Hard Inclusion disperse phase and preparation method thereof.
Background technology
Owing to having concurrently, wear resisting property is good, toughness is high for high mangaenese steel, therefore, in use not easy fracture, safe and reliable, be widely used in being manufactured on the workpiece used under impact abrasive wear and the hard power of height pulverize abrasive wear operating mode.As ball grinding machine lining board, grinding roller of vertical mill, hammer head of hammer crusher, cone crusher rolled mortar wall and crushing wall, also just like excavator bucket teeth, headwall, railroad turnout, the grip-pad etc. of tractor and tank.
At present, both at home and abroad adopt adds the elements such as rare earth to increase intensity and the hardness of its foundry goods more in high mangaenese steel, reaches the object improving wear resistance, such as CN1924059A be add 0.1 ~ 5% rare earth rhenium element; Alterant again in such as patent application CN103451546A is also containing rare earth rhenium element.In exploring the modification method of high mangaenese steel above, although play obvious active effect to its improved performance, also there is clear and definite shortcoming with not enough.The former adds rare earth and adds dependence to rare earth element, simultaneously still still limited to the raising of performance.
Summary of the invention
The object of this invention is to provide high mangaenese steel of a kind of Doped nanocrystal corundum Hard Inclusion disperse phase and preparation method thereof, stop the dependence to rare earth metal, ensure the uniform and stable of composite system.
The technical scheme that the present invention is adopted for achieving the above object is: a kind of high mangaenese steel of Doped nanocrystal corundum Hard Inclusion disperse phase, is made up of the component of following weight percent: Mn:10.0 ~ 17.0%; C:0 ~ 1.50%; Si:0.3 ~ 1.0%; S:<0.040%; P:<0.070%; Cr:l.5 ~ 2.5%; Ti:0 ~ 2.5%; Mo:0 ~ 1.2%; Nanocrystalline corundum: 0.50 ~ 12.5%; All the other are Fe.
Wherein, the α-Al of nanocrystalline corundum to be particle size be 20 ~ 200nm
2o
3.
A kind of preparation method of high mangaenese steel of Doped nanocrystal corundum Hard Inclusion disperse phase, comprise the following steps: step one, by nanocrystal boehmite pre-burning 10 ~ 60min at 500 ~ 600 DEG C, then room temperature is chilled to the rate of temperature fall of 10 ~ 50 DEG C/min, obtained nanometer first product; Then calcine 10min ~ 3h at nanometer first product being placed in 1100 ~ 1600 DEG C, be then chilled to room temperature with the rate of temperature fall of 40 ~ 50 DEG C/min, obtained nanocrystalline corundum, for subsequent use;
Step 2, according to described weight percent, melting is carried out in smelting furnace Mn, C, Si, S, P, Cr, Ti, Mo and Fe being joined argon atmosphere, after all melting formation liquation, add nanocrystalline corundum, continue heat treated 1 ~ 10h, then, be that the liquation of 1370 ~ 1420 DEG C adds in mold shaping by temperature, obtain ingot casting;
Step 3, ingot casting is placed in 1050 ~ 1100 DEG C at insulation 5 ~ 8h, then at 200 ~ 460 DEG C, be incubated 1h, and be incubated 1h at being warming up to 520 DEG C, then be incubated 1h at 580 ~ 850 DEG C, obtain high mangaenese steel.
Further, the preparation method of nanocrystal boehmite that step one adopts is:
A, by potassium hydroxide solution and Al
2(SO
4)
318H
2o solution mixes, and the Ph to mixing solutions is 7 ~ 10, after stirring at normal temperatures, proceeding to temperature is in the autoclave of 102 ~ 170 DEG C, after reaction 5 ~ 10h, and obtained solid product, by solid product through suction filtration, drip washing circulation 1 ~ 4 time, obtained nanocrystal boehmite solid-liquid mixture, for subsequent use;
B, nanocrystal boehmite solid-liquid mixture is placed in pregnant Bayer process liquor, water bath with thermostatic control heating 1 ~ 5h at 100 DEG C, after naturally cooling to room temperature, by crystallization product through suction filtration, drip washing circulation 1 ~ 3 time, ball milling after drying, and by the powder ultrasonic disperse 1h in deionized water after grinding, static 24h, dry, obtained nanocrystal boehmite.
Further, the melting method of step 2 is: high-frequency vacuum smelting furnace being evacuated to pressure in stove is 0.05Pa, be filled with pressure in argon gas to stove and reach 0.05MPa, add Mo, Si, C, S, P of described proportioning and the Fe of part, roasting material 15min below 100 DEG C, then melting 10min below 1000 DEG C, Ti, Mn, Cr and remaining Fe is added respectively again with the form of Ti-Fe, Mn-Fe and Cr-Fe master alloy, then melting at the temperature of 1200 ~ 1350 DEG C, forms liquation to the whole melting of raw material.
Because the particle of nano material itself is tiny, specific surface area is huge, very easily occurs agglomeration.The nano material that conventional meaning is said is the individual particle shown under scanning electron microscope is the particle diameter of 1 ~ 100nm, but this nano material is but shown as the particle diameter of tens microns on Malvern laser particle analyzer.Trace it to its cause, be that nano material is very easily reunited, after reunion, show the particle diameter having reached tens microns in appearance, even if make like this to add nano level particulate material in existing production, in fact be still micron order, be difficult to the real effect playing nano particle.
In the present invention, also cool rapidly after logical step a pair nano level boehmite sinters, can't agglomeration be there is in nano material obtained like this, that is, the nanocrystalline corundum formed after sintering is in single nanoparticle dispersion state, agglomeration can't be shown, it is so just made still to show the character of nano-scale particle when adding rest materials, because particle presents Nano grade, therefore, can think still to be in single_phase system in heat treatment process, not only dispersivity good, be evenly distributed, and combine also tightr.
Beneficial effect: the present invention is by calcining nano level boehmite, then cool rapidly, thus the nanocrystalline corundum obtained in dispersion state, compared with the micron order aluminium sesquioxide of routine, overcome the defect of brittleness of ceramics and compound system instability, adding of nanocrystalline corundum component, make the microtexture of gained high mangaenese steel there occurs change, add Hard Inclusion, cause the hardness of the casting high mangaenese steel of gained, toughness, intensity, wear resistance greatly to improve, work-ing life extends.The present patent application scheme does not add rare earth element, do not add large-size ceramic particle simultaneously, change into and add the nanocrystalline corundum in granules of size at 20 ~ 200nm, when ensure that Hard Inclusion hardness does not reduce, or composite system is uniform and stable, form homogeneous system, improve use properties, extend work-ing life.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the nanocrystalline corundum that embodiment 1 obtains;
Fig. 2 is the phasor of the high mangaenese steel that embodiment 1 obtains.
Embodiment
Below in conjunction with specific embodiment, high mangaenese steel of Doped nanocrystal corundum Hard Inclusion disperse phase of the present invention and preparation method thereof is described further, but illustrated embodiment is not as a limitation of the invention.
A high mangaenese steel for Doped nanocrystal corundum Hard Inclusion disperse phase, is made up of the component of following weight percent: Mn:10.0 ~ 17.0%; C:0 ~ 1.50%; Si:0.3 ~ 1.0%; S:<0.040%; P:<0.070%; Cr:l.5 ~ 2.5%; Ti:0 ~ 2.5%; Mo:0 ~ 1.2%; Nanocrystalline corundum: 0.50 ~ 12.5%; All the other are Fe.α-the Al of nanocrystalline corundum to be particle size be 20 ~ 200nm
2o
3.
Embodiment 1
A preparation method for the high mangaenese steel of Doped nanocrystal corundum Hard Inclusion disperse phase, comprises the following steps:
Step one, by potassium hydroxide solution and Al
2(SO
4)
318H
2o solution mixes, and the Ph to mixing solutions is 7, after stirring at normal temperatures, proceeding to temperature is in the autoclave of 105 DEG C, after reaction 10h, and obtained solid product, solid product is circulated three times through suction filtration, drip washing, obtained nanocrystal boehmite solid-liquid mixture, for subsequent use;
Step 2, nanocrystal boehmite solid-liquid mixture is placed in pregnant Bayer process liquor, water bath with thermostatic control heating 5h at 100 DEG C, after naturally cooling to room temperature, crystallization product is circulated three times through suction filtration, drip washing, ball milling after drying, and by the powder ultrasonic disperse 1h in deionized water after grinding, static 24h, dry, the obtained nanocrystal boehmite being of a size of 10 ~ 40nm, for subsequent use;
Step 3, the nanocrystal boehmite pre-burning 50min at 550 DEG C step 2 obtained, be then chilled to room temperature with the rate of temperature fall of 50 DEG C/min, obtained nanometer first product; Then calcine 3h at nanometer first product being placed in 1500 DEG C, be then chilled to room temperature with the rate of temperature fall of 50 DEG C/min, obtained nanocrystalline corundum, for subsequent use; The XRD figure of nanocrystalline corundum as shown in Figure 1.
Step 4, according to weight percent, take Mn17.0%, C1.0%, Si0.8%, S0.03%, P0.06%, Cr2.0%, Mo0.6%, nanocrystalline corundum 7% and Fe71.21%, high-frequency vacuum smelting furnace being evacuated to pressure in stove is 0.05Pa, be filled with pressure in argon gas to stove and reach 0.05MPa, add the Mo of described proportioning, Si, C, S, P and Fe52.21%, roasting material 15min below 100 DEG C, then melting 10min below 1000 DEG C, Mn is added respectively again with the form of Mn-Fe and Cr-Fe master alloy, Cr and Fe19%, then melting at the temperature of 1350 DEG C, liquation is formed to the whole melting of raw material, add nanocrystalline corundum, continue heat treated 10h, then, be that the liquation of 1420 DEG C adds in mold shaping by temperature, obtain ingot casting,
Step 5, ingot casting is placed in 1100 DEG C at be incubated 8h, then at 460 DEG C, be incubated 1h, and be incubated 1h at being warming up to 520 DEG C, then be incubated 1h at 580 DEG C, obtain high mangaenese steel, the phasor of obtained high mangaenese steel is as shown in Figure 2.
Embodiment 2
Step one, by nanocrystal boehmite pre-burning 30min at 500 DEG C, be then chilled to room temperature with the rate of temperature fall of 30 DEG C/min, obtained nanometer first product; Then calcine 2h at nanometer first product being placed in 1100 DEG C, be then chilled to room temperature with the rate of temperature fall of 45 DEG C/min, obtained nanocrystalline corundum, for subsequent use;
Step 2, according to weight percent, take Mn14.0%, C1.5%, Si1.0%, S0.02%, P0.05%, Cr1.5%, Ti2.5%, nanocrystalline corundum 12.5% and Fe66.93%, high-frequency vacuum smelting furnace being evacuated to pressure in stove is 0.05Pa, be filled with pressure in argon gas to stove and reach 0.05MPa, add the Si of described proportioning, C, S, P and 48.93%Fe, roasting material 15min below 100 DEG C, then melting 10min below 1000 DEG C, again respectively with Ti-Fe, the form of Mn-Fe and Cr-Fe master alloy adds Ti, Mn, the Fe of Cr and 18%, then melting at the temperature of 1200 DEG C, liquation is formed to the whole melting of raw material, add nanocrystalline corundum, continue heat treated 10h, then, be that the liquation of 1370 DEG C adds in mold shaping by temperature, obtain ingot casting,
Step 3, ingot casting is placed in 1050 DEG C at be incubated 5h, then at 200 DEG C, be incubated 1h, and be incubated 1h at being warming up to 520 DEG C, then be incubated 1h at 850 DEG C, obtain high mangaenese steel.
Nano level boehmite used in the present embodiment is that CN2012103957561 records the nano level boehmite prepared according to the patent No., is of a size of 10 ~ 40nm.
Embodiment 3
Step one, by potassium hydroxide solution and Al
2(SO
4)
318H
2o solution mixes, and the Ph to mixing solutions is 10, after stirring at normal temperatures, proceeding to temperature is in the autoclave of 160 DEG C, after reaction 5h, and obtained solid product, solid product is circulated four times through suction filtration, drip washing, obtained nanocrystal boehmite solid-liquid mixture, for subsequent use;
Step 2, nanocrystal boehmite solid-liquid mixture is placed in pregnant Bayer process liquor, water bath with thermostatic control heating 1h at 100 DEG C, after naturally cooling to room temperature, by crystallization product through suction filtration, drip washing circulation twice, ball milling after drying, and by the powder ultrasonic disperse 1h in deionized water after grinding, static 24h, dry, the obtained nanocrystal boehmite being of a size of 10 ~ 40nm, for subsequent use;
Step 3, the nanocrystal boehmite pre-burning 10min at 600 DEG C step 2 obtained, be then chilled to room temperature with the rate of temperature fall of 10 DEG C/min, obtained nanometer first product; Then calcine 50min at nanometer first product being placed in 1600 DEG C, be then chilled to room temperature with the rate of temperature fall of 40 DEG C/min, obtained nanocrystalline corundum, for subsequent use;
Step 4, according to weight percent, take Mn10.0%, Si0.3%, S0.01%, P0.055%, Cr1.5%, Ti1.7%, Mo1.2%, nanocrystalline corundum 0.5% and Fe84.735%, high-frequency vacuum smelting furnace being evacuated to pressure in stove is 0.05Pa, be filled with pressure in argon gas to stove and reach 0.05MPa, add the Si of described proportioning, S, P, Mo and 71.535%Fe, roasting material 15min below 100 DEG C, then melting 10min below 1000 DEG C, again respectively with Mn-Fe, the form of Ti-Fe and Cr-Fe master alloy adds Mn, Ti, Cr and 13.2%Fe, then melting at the temperature of 1280 DEG C, liquation is formed to the whole melting of raw material, add nanocrystalline corundum, continue heat treated 6h, then, be that the liquation of 1400 DEG C adds in mold shaping by temperature, obtain ingot casting,
Step 5, ingot casting is placed in 1080 DEG C at be incubated 7h, then at 350 DEG C, be incubated 1h, and be incubated 1h at being warming up to 520 DEG C, then be incubated 1h at 600 DEG C, obtain high mangaenese steel.
In the present invention, titanium add the tensile strength that can improve high mangaenese steel, make high mangaenese steel have excellent cold and hot working performance simultaneously; Adding of manganese can fully carry heavy alloyed unit elongation, puies forward heavy alloyed anti-softening temperature; Raw material of the present invention melting under an argon atmosphere, can be down to minimum by the scaling loss amount of trace alloying element, and prior art generally adopts melting under nitrogen atmosphere, and scaling loss amount is larger.