CN104195407B - A kind of preparation method of TiC high-manganese steel-base Steel Bond Hard Alloy - Google Patents
A kind of preparation method of TiC high-manganese steel-base Steel Bond Hard Alloy Download PDFInfo
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- CN104195407B CN104195407B CN201410488746.1A CN201410488746A CN104195407B CN 104195407 B CN104195407 B CN 104195407B CN 201410488746 A CN201410488746 A CN 201410488746A CN 104195407 B CN104195407 B CN 104195407B
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Abstract
The present invention relates to a kind of preparation method of TiC high-manganese steel-base Steel Bond Hard Alloy, to it is characterized in that titanium valve and Graphite Powder 99 in C/Ti atomic ratio being 0.8 ~ 1.0 in-situ synthesizing TiC powder being mixed with required ratio; By molybdenum-iron powder, vanadium iron powder, ferromanganese powder, ferrosilicon powder, iron powder, nickel powder, oildag and rare earths material press proportions needed for bonding phase metal chemical composition mass ratio, load steel ball ball milling, wherein add dehydrated alcohol and make medium and PVA, after ball milling, press forming, sintering after slip drying are obtained steel-bonded carbide.In-situ reactive synthesis technology combines with liquid phase sintering technology by the present invention, has prepared TiC/ high-manganese steel-base Steel Bond Hard Alloy.<b> due to </b>TiC be at intrinsic silicon fabricated in situ by the reaction in sintering process, enhanced granule size is tiny, surface is without wedge angle, and basal body interface combines better and clean interfaces.Prepared steel-bonded carbide method can carry heavy alloyed comprehensive mechanical property, and cheap, simple process.
Description
Technical field
The present invention relates to a kind of preparation method of TiC high-manganese steel-base Steel Bond Hard Alloy, particularly produce TiC high-manganese steel-base Steel Bond Hard Alloy technical field with reaction sintering.
Background technology
Steel Bond Hard Alloy (hereinafter referred to as steel-bonded carbide) take steel as matrix, wolfram varbide, titanium carbide etc. be hard phase adopt powder metallurgy process to produce between Wimet and the high life moulding stock between alloy tool steel, die steel and rapid steel and engineering materials.The ratio range of steel-bonded carbide steel matrix Binder Phase and hard phase is quite extensive, and this just determines it and possesses following excellent properties: 1) processing performance widely, mainly can forgeability and machinable performance and heat-treatability and weldability.2) good physical and mechanical properties, is mainly manifested in the wear resistance suitable with high-cobalt hart metal; Rigidity high compared with steel, Young's modulus, bending strength and ultimate compression strength; Toughness high compared with Wimet; And good self lubricity and high damping characteristic etc.3) excellent chemical stability, as high temperature resistant, anti-oxidant, anti-various dielectric corrosions etc.Due to the over-all properties of the above-mentioned excellence of steel-bonded carbide, make it in tool die material, wear part, high temperature resistant and corrosion resistant member material etc., more and more occupy consequence, and be used widely in fields such as intermetallic composite coating, five metals electronics, automobile, machinery, metallurgy, chemical industry, boats and ships, aerospace and nuclear industry and obtain good result.As compared with alloy tool steel, die steel and rapid steel, steel-bonded carbide can make die life number increase substantially with ten times of ground, and economic benefit is also very remarkable.
Wolfram varbide steel-bonded carbide compared by titanium carbide Steel Bond Hard Alloy, and its cost is low, is applicable to marketing and uses.But the obdurability of its alloy is still lower, more and more many power that withstands shocks far can not be met comparatively large, the use in the higher situation of impact velocity.Therefore the titanium carbide Steel Bond Hard Alloy of Development and Production high-performance, low cost is necessary.Wherein, the obdurability improving titanium carbide steel-bonded carbide is the research direction of emphasis.
At present, the method mainly powder metallurgy lqiuid phase sintering method of TiC Steel Bond Hard Alloy is prepared.Lqiuid phase sintering method can need to select suitable Binder Phase according to practical application and can adjust the content of hard phase in a big way, but due to the hard phase add mode introducing in addition usually of powder metallurgy lqiuid phase sintering method, material cost is high, particle is thick, the wettability of hard phase titanium carbide and Binder Phase is bad, interface vulnerable to pollution etc., therefore it is high that the Steel Bond Hard Alloy prepared by lqiuid phase sintering method has porosity, performance is low, high in cost of production shortcoming, for requiring that higher application scenario often needs through forging or hip treatment, the cost performance of material reduces further.
In recent years, the research that employing in-situ synthesis prepares Steel Bond Hard Alloy has been carried out both at home and abroad.Situ synthesis techniques is a kind of by alloy designs, and under certain condition, in matrix metal, reaction in－situ generates the advanced composite material technology of preparing of one or more thermodynamically stable hard phases.Compared with traditional material preparation method, this technology has that preparation technology is simple, the wild phase of produced in situ is not contaminated, interface bond strength high, is the trend of Steel Bond Hard Alloy technology of preparing development.
But in-situ synthesis also has many deficiencies: enhanced granule is only limited to the thermodynamically stable grain in particular substrate; Comparing of generating is complicated, wayward; Granular size, shape are by the kinetic control of forming core, growth process; and after in-situ particle formed; often segregation gap or grain boundary can be asked in dendrite in castingprocesses; detrimentally affect is produced to material structure and performance; and manufacturability is poor; preparation cost is higher than existing technique, is unsuitable for large-scale production.Obviously, the key that situ synthesis techniques realizes industrialization must study rational homogenization process further, optimum synthesis technique, reduction production cost.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of preparation method of TiC high-manganese steel-base Steel Bond Hard Alloy, in order to improve the performance of TiC high-manganese steel-base Steel Bond Hard Alloy.
The preparation method of a kind of TiC high-manganese steel-base Steel Bond Hard Alloy of the present invention, its by the following technical solutions:
(1) starting material:
Raw materials is titanium valve, molybdenum-iron powder, vanadium iron powder, ferromanganese powder, ferrosilicon powder, iron powder, nickel powder, oildag, CeO
2, Y
3o
2, La
2o
3one of them or three kinds, PVA, powder size is all below 10 ~ 50 μm;
(2) material formulation:
1) in-situ synthesizing TiC mixed powder preparation: be 0.8 ~ 1.0 carry out being mixed with in-situ synthesizing TiC mixed powder by C/Ti atomic ratio by titanium (Ti) powder and Graphite Powder 99;
2) bonding phase matrix alloy powder preparation: bonding phase metal material chemical composition mass percent is: C0.7 ~ 1.5%, Mo0.5 ~ 2.2%, V0.1 ~ 0.3%, Si0.3 ~ 0.6%, Mn8 ~ 14%, Ni0.5 ~ 2.0%, S≤0.02, P≤0.02, CeO
2, Y
3o
2, La
2o
3combination≤0.8% of one of them or more than two kinds, surplus Fe, and inevitable impurity element;
3) TiC high-manganese steel-base Steel-bonded Cemented Carbide preparation: material chemical composition mass percent is: in-situ synthesizing TiC mixed powder 30 ~ 60%, bonding phase matrix alloy powder 70 ~ 40%;
(3) step of preparation process is:
1) material formulation: be 0.8 ~ 1.0 in-situ synthesizing TiC mixed powder carrying out being mixed with required ratio in C/Ti atomic ratio by titanium (Ti) powder and Graphite Powder 99; By molybdenum-iron powder, vanadium iron powder, ferromanganese powder, ferrosilicon powder, converts according to required chemical composition mass percent, together with iron powder, nickel powder, oildag, CeO
2, Y
3o
2, La
2o
3the combination raw materials of one of them or more than two kinds presses proportions needed for bonding phase metal material chemical composition mass percent;
2) bi-material mixes by the TiC particle needed for Steel-bonded Cemented Carbide and the ratio of body material, load in ball milling bucket, load steel ball, ratio of grinding media to material 5:1 ~ 10:1, add dehydrated alcohol and make medium and 0.5-1%PVA as refrigerant and dispersion agent, adopt vibrations ball mill ball milling 48-72 hour;
3) sieve after slip drying, then make the product of desired size shape at 350 ~ 500MPa pressure;
4) sinter under vacuum, sintering temperature is 1350 DEG C ~ 1400 DEG C, and sintering process is: rate of heating 10 DEG C/min, and sintering time is 30 ~ 40min, is incubated after 1 ~ 3 hour, and furnace cooling, to room temperature, obtains the high-manganese steel-base Steel Bond Hard Alloy of required composition.
beneficial effect
Compared with prior art, tool of the present invention has the following advantages:
1, the present invention is with cheap titanium valve molybdenum-iron powder, vanadium iron powder, ferromanganese powder, ferrosilicon powder, iron powder, nickel powder, oildag is raw material, in-situ reactive synthesis technology is combined with liquid phase sintering technology, has prepared the TiC High wear-resistant steel bond hard alloy that hard phase titanium carbide volume fraction is 30% one 50%.Its principal feature is: 1. because the TiC in Steel Bond Hard Alloy is at intrinsic silicon fabricated in situ by the reaction in sintering process, so the method that can obtain the mixing of Ordinary hardening phase powder is difficult to reach, even inaccessiable granular and degree of uniformity, basal body interface combines better and clean interfaces.2. fabricated in situ enhanced granule size is tiny, and surface without wedge angle, and is evenly distributed in the base, thus improves bending strength and the properties of material.3. situ synthesis techniques and liquid phase sintering technology are combined together, simple process, cost are low.4. due to raw-material cheap, can greatly reduce costs.Not only can sinter in a vacuum in the technique of simultaneously this powder, also how can sinter in the atmosphere such as hydrogen, widen the means approach manufactured.
The present invention adopts high-energy ball milling mode to improve the activity of powder, and reaches the degree of titanium carbide and steel matrix Mechanical Alloying, thus improves titanium carbide and the affinity of steel matrix in sintering process, improves the obdurability of final alloy.In addition, have employed the lower ferro-molybdenum of price in the present invention as raw material, it improves the wettability of titanium carbide and steel matrix further in sintering process, carries heavy alloyed obdurability.Therefore, the present invention prepares high-performance steel-bonded carbide method can carry heavy alloyed comprehensive mechanical property, and process is easy, cost-saving.
2, the present invention is by adding CeO
2, Y
3o
2, La
2o
3inhibit growing up of crystal grain, and play the effect of dispersion-strengthened.Due to CeO
2, Y
3o
2, La
2o
3chemical property is active, at a sintering temperature, and CeO
2, Y
3o
2, La
2o
3can with the impurity on metal-powder interface and oxide film effect, play the effect at purification interface, contribute to the improvement of wettability, thus be conducive to the process of densification, reach the object of reduction holes porosity, and the reduction of porosity will contribute to the raising of bending strength.CeO
2, Y
3o
2, La
2o
3powder content, between 0.2% and 0.5%, can play rare earth reinforced effect, and therefore the intensity of Steel Bond Hard Alloy of the present invention and density are improved, and bending strength can reach more than 1700MPa, and density reaches more than 97.4%.
3, the present invention adopts high-energy ball milling mode to improve the activity of powder, and reaches the degree of titanium carbide and steel matrix Mechanical Alloying, thus improves titanium carbide and the affinity of steel matrix in sintering process, improves the obdurability of final alloy.In addition, the lower iron alloy of price is have employed as raw material in the present invention, and after adding a certain amount of molybdenum, it improves the wettability of titanium carbide and steel matrix further in sintering process, the hard phase TiC of Steel Bond Hard Alloy situ Reactive Synthesis can be suppressed to grow up, TiC particle size is reduced, is evenly distributed.After adding molybdenum, improve the wettability of Binder Phase to hard phase TiC, be conducive to liquid phase filling to hole in sintering process, porosity is low, the density of Steel Bond Hard Alloy is improved, crystal grain is tiny, homogeneous microstructure, thus makes its hardness and bending strength and obdurability have also been obtained raising.Therefore, the present invention prepares high-performance steel-bonded carbide method can carry heavy alloyed comprehensive mechanical property, and process is easy, easy to operate, the sintering period is short, process costs is low, be suitable for suitability for industrialized production.
Embodiment
Technical scheme of the present invention is further illustrated below in conjunction with embodiment:
Embodiment 1
A preparation method for TiC high-manganese steel-base Steel Bond Hard Alloy, its by the following technical solutions:
(1) starting material:
Raw materials is titanium valve, molybdenum-iron powder, vanadium iron powder, ferromanganese powder, ferrosilicon powder, iron powder, nickel powder, oildag, CeO
2, PVA, powder size is all below 10 ~ 50 μm;
(2) material formulation:
1) in-situ synthesizing TiC mixed powder preparation: be 0.85 carry out being mixed with in-situ synthesizing TiC mixed powder by C/Ti atomic ratio by titanium (Ti) powder and Graphite Powder 99;
2) bonding phase matrix alloy powder preparation: bonding phase metal material chemical composition mass percent is: C0.9%, Mo1.5%, V0.1%, Si0.4%, Mn10%, Ni1.5%, S≤0.02, P≤0.02, CeO
2≤ 0.8%, surplus Fe, and inevitable impurity element;
3) TiC high-manganese steel-base Steel-bonded Cemented Carbide preparation: material chemical composition mass percent is: in-situ synthesizing TiC mixed powder 30%, bonding phase matrix alloy powder 70%;
(3) step of preparation process is:
1) material formulation: be 0.85 carry out being mixed with fabricated in situ 30%TiC mixed powder by C/Ti atomic ratio by titanium (Ti) powder and Graphite Powder 99; By molybdenum-iron powder, vanadium iron powder, ferromanganese powder, ferrosilicon powder, converts according to required chemical composition mass percent, together with iron powder, nickel powder, oildag, CeO
2bonding phase metal material chemical composition mass percent 70% proportions pressed by raw material;
2) bi-material of the fabricated in situ 30%TiC particle needed for Steel-bonded Cemented Carbide and body material 70% is mixed, load in ball milling bucket, load steel ball, ratio of grinding media to material 5:1, add dehydrated alcohol and make medium and 0.6%PVA as refrigerant and dispersion agent, adopt vibrations ball mill ball milling 55 hours;
3) sieve after slip drying, then make the product of desired size shape at 400MPa pressure;
4) sinter under vacuum, sintering temperature is 1370 DEG C, and sintering process is: rate of heating 10 DEG C/min, and sintering time is 30min, is incubated after 1.5 hours, and furnace cooling, to room temperature, obtains the high-manganese steel-base Steel Bond Hard Alloy of required composition.
Embodiment 2
A preparation method for TiC high-manganese steel-base Steel Bond Hard Alloy, its by the following technical solutions:
(1) starting material:
Raw materials is titanium valve, molybdenum-iron powder, vanadium iron powder, ferromanganese powder, ferrosilicon powder, iron powder, nickel powder, oildag, CeO
2, Y
3o
2two kinds, PVA, powder size is all below 10 ~ 50 μm;
(2) material formulation:
1) in-situ synthesizing TiC mixed powder preparation: be 0.9 carry out being mixed with in-situ synthesizing TiC mixed powder by C/Ti atomic ratio by titanium (Ti) powder and Graphite Powder 99;
2) bonding phase matrix alloy powder preparation: bonding phase metal material chemical composition mass percent is: C1.2%, Mo1.8%, V0.2%, Si0.5%, Mn12%, Ni1.8%, S≤0.02, P≤0.02, CeO
20.5%, Y
3o
20.3%, surplus Fe, and inevitable impurity element;
3) TiC high-manganese steel-base Steel-bonded Cemented Carbide preparation: material chemical composition mass percent is: fabricated in situ 40%TiC mixed powder, bonding phase matrix alloy powder 60%;
(3) step of preparation process is:
1) material formulation: titanium (Ti) powder and Graphite Powder 99 are carried out being mixed with institute fabricated in situ 40%TiC mixed powder for 0.9 by C/Ti atomic ratio; By molybdenum-iron powder, ferrosilicon powder, ferromanganese powder, vanadium iron powder, converts according to required chemical composition mass percent, together with iron powder, nickel powder, oildag, CeO
2, Y
3o
2bonding phase metal material chemical composition mass percent 60% proportions pressed by raw material;
2) bi-material of the 40%TiC particle of fabricated in situ needed for Steel-bonded Cemented Carbide and the ratio of body material 60% is mixed, load in ball milling bucket, load steel ball, ratio of grinding media to material 7:1, add dehydrated alcohol and make medium and 0.8%PVA as refrigerant and dispersion agent, adopt vibrations ball mill ball milling 62 hours;
3) sieve after slip drying, then make the product of desired size shape at 450MPa pressure;
4) sinter under vacuum, sintering temperature is 1390 DEG C, and sintering process is: rate of heating 10 DEG C/min, and sintering time is 35min, is incubated after 2.3 hours, and furnace cooling, to room temperature, obtains the high-manganese steel-base Steel Bond Hard Alloy of required composition.
Embodiment 3
A preparation method for TiC high-manganese steel-base Steel Bond Hard Alloy, its by the following technical solutions:
(1) starting material:
Raw materials is titanium valve, molybdenum-iron powder, vanadium iron powder, ferromanganese powder, ferrosilicon powder, iron powder, nickel powder, oildag, CeO
2, Y
3o
2, La
2o
3, PVA, powder size is all below 10 ~ 50 μm;
(2) material formulation:
1) in-situ synthesizing TiC mixed powder preparation: be 1.0 carry out being mixed with in-situ synthesizing TiC mixed powder by C/Ti atomic ratio by titanium (Ti) powder and Graphite Powder 99;
2) bonding phase matrix alloy powder preparation: bonding phase metal material chemical composition mass percent is: C1.5%, Mo2.0%, V0.3%, Si0.6%, Mn13%, Ni2.0%, S≤0.02, P≤0.02, CeO
20.3%, Y
3o
20.3%, La
2o
30.2%, surplus Fe, and inevitable impurity element;
3) TiC high-manganese steel-base Steel-bonded Cemented Carbide preparation: material chemical composition mass percent is: in-situ synthesizing TiC mixed powder 48%, bonding phase matrix alloy powder 52%;
(3) step of preparation process is:
1) material formulation: titanium (Ti) powder and Graphite Powder 99 are carried out being mixed with institute fabricated in situ 48%TiC mixed powder for 1.0 by C/Ti atomic ratio; By molybdenum-iron powder, vanadium iron powder, ferromanganese powder, ferrosilicon powder, converts according to required chemical composition mass percent, together with iron powder, nickel powder, oildag, CeO
2, Y
3o
2, La
2o
3bonding phase metal material chemical composition mass percent 52% proportions pressed by raw material;
2) bi-material of the 52%TiC particle of fabricated in situ needed for Steel-bonded Cemented Carbide and the ratio of body material 48% is mixed, load in ball milling bucket, load steel ball, ratio of grinding media to material 10:1, add dehydrated alcohol and make medium and 1%PVA as refrigerant and dispersion agent, adopt vibrations ball mill ball milling 72 hours;
3) sieve after slip drying, then make the product of desired size shape at 500MPa pressure;
4) sinter under vacuum, sintering temperature is 1420 DEG C, and sintering process is: rate of heating 10 DEG C/min, and sintering time is 40min, is incubated after 3 hours, and furnace cooling, to room temperature, obtains the high-manganese steel-base Steel Bond Hard Alloy of required composition.
Claims (2)
1. a preparation method for TiC high-manganese steel-base Steel Bond Hard Alloy, is characterized in that comprising as follows:
(1) material formulation:
1) in-situ synthesizing TiC mixed powder preparation: be 0.8 ~ 1.0 carry out being mixed with in-situ synthesizing TiC mixed powder by C/Ti atomic ratio by titanium (Ti) powder and Graphite Powder 99;
2) bonding phase matrix alloy powder preparation: bonding phase metal material chemical composition mass percent is: C0.7 ~ 1.5%, Mo0.5 ~ 2.2%, V0.1 ~ 0.3%, Si0.3 ~ 0.6%, Mn8 ~ 14%, Ni0.5 ~ 2.0%, S≤0.02, P≤0.02, CeO
2, Y
3o
2, La
2o
3combination≤0.8% of one of them or more than two kinds, surplus Fe, and inevitable impurity element;
3) TiC high-manganese steel-base Steel-bonded Cemented Carbide preparation: material chemical composition mass percent is: in-situ synthesizing TiC mixed powder 30 ~ 60%, bonding phase matrix alloy powder 70 ~ 40%;
(2) step of preparation process is:
1) material formulation: be 0.8 ~ 1.0 in-situ synthesizing TiC mixed powder carrying out being mixed with required ratio in C/Ti atomic ratio by titanium (Ti) powder and Graphite Powder 99; By molybdenum-iron powder, vanadium iron powder, ferromanganese powder, ferrosilicon powder, converts according to required chemical composition mass percent, together with iron powder, nickel powder, oildag, CeO
2, Y
3o
2, La
2o
3the combination raw materials of one of them or more than two kinds presses proportions needed for bonding phase metal material chemical composition mass percent;
2) bi-material mixes by the TiC particle needed for Steel-bonded Cemented Carbide and the ratio of body material, load in ball milling bucket, load steel ball, ratio of grinding media to material 5:1 ~ 10:1, add dehydrated alcohol and make medium and 0.5-1%PVA as refrigerant and dispersion agent, adopt vibrations ball mill ball milling 48-72 hour;
3) sieve after slip drying, then make the product of desired size shape at 350 ~ 500MPa pressure;
4) sinter under vacuum, sintering temperature is 1350 DEG C ~ 1400 DEG C, and sintering process is: rate of heating 10 DEG C/min, and sintering time is 30 ~ 40min, is incubated after 1 ~ 3 hour, and furnace cooling, to room temperature, obtains the high-manganese steel-base Steel Bond Hard Alloy of required composition.
2. the preparation method of a kind of TiC high-manganese steel-base Steel Bond Hard Alloy according to claim 1, is characterized in that: titanium valve in raw materials, molybdenum-iron powder, vanadium iron powder, ferromanganese powder, ferrosilicon powder, iron powder, nickel powder, oildag, CeO
2, Y
3o
2, La
2o
3one of them or three kinds, PVA, powder size is all at 10 ~ 50 μm.
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| CN106868384A (en) * | 2017-02-09 | 2017-06-20 | 江苏汇诚机械制造有限公司 | A kind of preparation method of tough medium managese steel base VC steel bonded carbide high |
| CN106893931A (en) * | 2017-03-04 | 2017-06-27 | 蒋培丽 | A kind of granule enhancement type austenitic steel and its steel plate manufacturing process |
| CN107937789B (en) * | 2017-11-14 | 2019-06-28 | 邯郸史威新材料有限公司 | A kind of manganese steel base steel bonded carbide and preparation method thereof |
| CN107904476B (en) * | 2017-11-14 | 2019-07-19 | 邯郸史威新材料有限公司 | A kind of chrome molybdenum base steel bonded carbide and preparation method thereof |
| CN111185591B (en) * | 2020-02-18 | 2022-05-10 | 北京科技大学广州新材料研究院 | TiC high manganese steel composite material and preparation method thereof |
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| CN1031864A (en) * | 1988-08-01 | 1989-03-22 | 湖南省冷水滩耐火材料厂 | A kind of Steel Bond Hard Alloy and manufacture craft thereof |
| CN1851032A (en) * | 2006-05-31 | 2006-10-25 | 株洲硬质合金集团有限公司 | High manganese steel base hard alloy, and its preparing method |
| CN102828105B (en) * | 2011-06-18 | 2015-01-07 | 无锡鑫群新材料科技有限公司 | Preparation method of titanium-carbide-based steel-bonded cemented carbide material |
| CN102605273B (en) * | 2012-04-11 | 2013-12-25 | 长沙威斯坦冶金制品有限公司 | Steel bonded hard alloy and preparation method thereof |
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