CN105420587B - A kind of preparation method of TiC high-boron low-alloy high-speed steels base steel bonded carbide - Google Patents
A kind of preparation method of TiC high-boron low-alloy high-speed steels base steel bonded carbide Download PDFInfo
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Abstract
The present invention is a kind of preparation method of TiC high-boron low-alloy high-speed steels base steel bonded carbide, and titanium and graphite powder are carried out being configured to in-situ synthesizing TiC mixed-powder by C/Ti atomic molar ratio for 0.7~1.1；By vanadium iron powder, ferrochrome powder, molybdenum-iron powder, ferro-boron powder, ferrosilicon powder, ferromanganese powder, iron powder, nickel powder, copper powder, aquadag and rare earths material are prepared in ratio needed for bonding phase metal chemical composition mass ratio, load steel ball ball milling, wherein adding absolute ethyl alcohol makees medium and PVA, compressing after slurry is dried after ball milling, sintering obtains steel-bonded carbide.In-situ reactive synthesis technology is combined by the present invention with liquid phase sintering technology, is prepared for TiC high-boron low-alloy high-speed steel base steel bonded carbide.For TiC by the reaction in sintering process in intrinsic silicon fabricated in situ, enhancing particle size is tiny, and basal body interface combines preferably and clean interfaces.Preparation technology is easy, and the comprehensive mechanical property of alloy improves.
Description
Technical field
The present invention relates to a kind of preparation method of TiC high-boron low-alloy high-speed steels base steel bonded carbide, particularly with anti-
Sintering process is answered to produce a kind of preparation method of TiC high-boron low-alloy high-speed steels base steel bonded carbide.
Technical background
Steel bonded carbide（Hereinafter referred to as steel-bonded carbide）It is using steel as matrix, tungsten carbide, titanium carbide etc. are hard phase
The high life mould between hard alloy and alloy tool steel, mould steel and high-speed steel produced using powder metallurgy process
Material and engineering material.The ratio range of steel-bonded carbide steel matrix Binder Phase and hard phase quite it is extensive, this just determines its tool
Standby following excellent properties：1）Extensive processing performance, forgeability and machinable performance and it can mainly be heat-treated
Property and weldability.2）Good physical and mechanical properties, it is mainly manifested in the wearability suitable with high-cobalt hart metal；With steel phase
Compare high rigidity, modulus of elasticity, bending strength and compression strength；The higher toughness compared with hard alloy；And good
Self lubricity and high damping characteristic etc..3）Excellent chemical stability, such as high temperature resistant, it is anti-oxidant, resist various dielectric corrosions.
Due to the above-mentioned excellent combination property of steel-bonded carbide so that it is in tool die material, wear part, high temperature resistant and corrosion-resistant structure
Part material etc. more and more occupies consequence, and in intermetallic composite coating, hardware electronics, automobile, machinery, metallurgy, chemical industry, ship
It is used widely and obtains good result in the field such as oceangoing ship, Aero-Space and nuclear industry.Such as with alloy tool steel, mould steel and
High-speed steel is compared, and steel-bonded carbide can be such that die life number is increased substantially with ten times of ground, and economic benefit is also extremely notable.
Titanium carbide steel bonded carbide compares tungsten carbide steel-bonded carbide, and its cost is low, is adapted to marketing to use.But it is closed
The obdurability of gold is still relatively low, far from meeting that more and more power of withstanding shocks are larger, the situation in the case of impact velocity is higher
Lower use.Therefore Development and Production high-performance, the titanium carbide steel bonded carbide of low cost are necessary.Wherein, titanium carbide is improved
The obdurability of steel-bonded carbide is the research direction of emphasis.
TiC has the excellent physical and chemical performances such as hardness is high, anti-oxidant, corrosion-resistant, proportion is small, heat endurance is good, is
A kind of more satisfactory steel bonded carbide hard phase material.V and Ti belongs to the transition metal of same period, and former ordinal number is only
1, VC of difference also has high-melting-point, high rigidity and high chemical stability, and the research on VC steel bonded carbide is in recent years
Cause the interest of some researchers.
At present, the method for preparing steel bonded carbide is mainly powder metallurgy lqiuid phase sintering method.Lqiuid phase sintering method can root
Need to select appropriate Binder Phase according to practical application and can be in the content of interior adjustment hard phase in a big way, but due to powder metallurgy
The hard phase of lqiuid phase sintering method generally introduces in the way of adding, and the cost of raw material is high, particle is thick, hard phase titanium carbide and bonding
Bad, interface vulnerable to pollution of wetability of phase etc., therefore the steel bonded carbide prepared by lqiuid phase sintering method has porosity
High, the shortcomings of performance is low, cost is high, for requiring that higher application scenario is often needed by forging or hip treatment, material
The cost performance of material further reduces.In recent years, the research that steel bonded carbide is prepared using in-situ synthesis has been carried out both at home and abroad.
Situ synthesis techniques are that one kind designs by alloy, and reaction in-situ generation is one or more of in parent metal under certain condition
The advanced composite material (ACM) technology of preparing of thermodynamically stable hard phase.Compared with traditional material preparation method, the technology has
Enhancing is mutually high with the interface bond strength of matrix, and strengthening species, size, distribution and the quantity of phase can control, preparation technology letter
Single, the enhancing of produced in situ is not mutually contaminated, and interface bond strength is high, and cost is low, the spy such as the intensity of material and modulus of elasticity height
Point, it is the trend of steel bonded carbide technology of preparing development.
But in-situ synthesis also has many deficiencies:Enhancing particle is only limited to the thermodynamically stable grain in particular substrate；
Comparing for generation is more complicated, whard to control；Granular size, shape are by the dynamics Controlling of forming core, growth process, and in-situ particle
After formation, in casting process can often be segregated in dendrite asks gap or grain boundary, and bad shadow is produced to material structure and performance
Ring, and manufacturability is poor, and preparation cost is higher than existing process, is unsuitable for large-scale production.Obviously, situ synthesis techniques realize production
The key of industry is must further to study rational homogenization process, optimum synthesis technique, reduces production cost.
The content of the invention
In view of the shortcomings of the prior art, the invention provides a kind of TiC high-boron low-alloy high-speed steels base steel bonded carbide
Preparation method, to improve the performance of TiC steel bonded carbide.
A kind of preparation method of TiC high-boron low-alloy high-speed steels base steel bonded carbide of the present invention, it uses following skill
Art scheme：
(1) raw materials are titanium valve, vanadium iron powder, ferrochrome powder, ferrotungsten, molybdenum-iron powder, ferro-boron powder, iron powder, ferro-niobium, nickel powder,
Copper powder, ferrosilicon powder, ferromanganese powder, aquadag, CeO2、Y3O2、La2O3One of them or three kinds, PVA, powder size 10~
Less than 50 μm；
(2) material is prepared：
1）In-situ synthesizing TiC mixed-powder is prepared：By titanium（Ti）With graphite powder by C/Ti atomic molar ratio for 0.7~
1.1 carry out being configured to in-situ synthesizing TiC mixed-powder；
2）Phase matrix alloy powder is bonded to prepare：Bonding phase metal material chemical composition mass percent is：C0.2~
0.6%, Cr5.0~7.0%, W2.5~3.0%, Mo1.5~3.0%, V1.5~2.5%, Nb0.5~1.0%, Si0.3~1.0%,
Mn0.3~1.0%, B1.4~2.5%, Cu0.3~1.0%, Ni0.8~2.0%, S≤0.02, P≤0.02, CeO2、Y3O2、La2O3
Combination≤0.8%, the surplus Fe of one of them or more than two kinds, and inevitable impurity element；
3）TiC Steel-bonded Cemented Carbides are prepared：Material chemical composition mass percent is：In-situ synthesizing TiC mixed powder
End 30~50%, bonding phase matrix alloy powder 70~50%；
(3) step of preparation process is：
1）Material is prepared：：By titanium（Ti）Carry out being configured to original for 0.7~1.1 by C/Ti atomic molar ratio with graphite powder
Position synthesis TiC mixed-powders；By ferrochrome powder, molybdenum-iron powder, ferrosilicon powder, ferromanganese powder, ferro-boron powder is according to required chemical composition quality
Percentage converts, together with iron powder, nickel powder, copper powder, aquadag, CeO2、Y3O2、La2O3The combination of one of them or more than two kinds
Raw material is prepared in ratio needed for bonding phase metal material chemical composition mass percent；
2）The ratio of TiC particles and matrix material according to needed for Steel-bonded Cemented Carbide is mixed two kinds of materials
Close, be fitted into ball milling bucket, load steel ball, ratio of grinding media to material 5:1~10:1, add absolute ethyl alcohol and make medium and 0.5~1%PVA as cold
But agent and dispersant, using vibrations ball mill ball milling 48~72 hours；
3）Sieved after slurry is dried, the product of required size shape is then pressed under 350~500 MPa pressure；
4）Sinter under vacuum, sintering temperature is 1350 DEG C~1420 DEG C, and sintering process is:10 DEG C of firing rate/
Min, sintering time are 30~40min, after being incubated 1~3 hour, furnace cooling to room temperature, obtain the heat resisting steel knot of required composition
Hard alloy.
Beneficial effect
Compared with prior art, the invention has the advantages that：
1st, the present invention is with cheap titanium valve, vanadium iron powder, iron powder, ferrochrome powder, molybdenum-iron powder, ferrosilicon powder, ferromanganese powder, ferro-boron
Powder, nickel powder, copper powder, aquadag are raw material, and in-situ reactive synthesis technology is combined with liquid phase sintering technology, is prepared for hard
Phase titanium carbide volume fraction is 30%~50% TiC high-boron low-alloy high-speed steel base steel bonded carbide.It is mainly characterized by：①
Because the TiC in steel bonded carbide is and in intrinsic silicon fabricated in situ by the reaction in sintering process, it is possible to
Method to the mixing of Ordinary hardening phase powder is difficult to reach, or even inaccessiable granular and uniformity coefficient, basal body interface
With reference to preferable and clean interfaces.2. fabricated in situ enhancing particle size is tiny, surface is evenly distributed in the base without wedge angle,
So as to improve the bending strength MPa of material and properties.3. situ synthesis techniques are combined with liquid phase sintering technology
Come, simple process, cost are low.4. it is cheap due to raw material, cost can be substantially reduced.Simultaneously in the technique of this powder
It not only can in a vacuum sinter, how can also sinter in the atmosphere such as hydrogen, widen the means approach manufactured.5. due to
The introducing of vanadium, makes the form of TiC particles strengthen the form more rounding of phase particle than Ti rules, TiC.
The present invention improves the activity of powder using high-energy ball milling mode, and reaches titanium carbide and vanadium and steel matrix powder machine
The degree of tool alloying, so as to improve titanium carbide and vanadium and compatibility of the steel matrix in sintering process, improve final alloy
Obdurability.In addition, employing the relatively low ferro-molybdenum of price in the present invention as raw material, it further improves in sintering process
The wetability of titanium carbide and vanadium and steel matrix, improve the obdurability of alloy.Therefore, the present invention prepares high-performance steel-bonded carbide method
The comprehensive mechanical property of alloy can be improved, and process is easy, it is cost-effective.
2nd, the present invention is by adding CeO2、Y3O2、La2O3Growing up for crystal grain is inhibited, and plays a part of dispersion-strengtherning.By
In CeO2、Y3O2、La2O3Chemical property is active, at a sintering temperature, CeO2、Y3O2、La2O3Can with metal dust interface
Impurity and oxide-film effect, play a part of purifying interface, contribute to the improvement of wetability, so as to be advantageous to entering for densification
Journey, reach the purpose for reducing porosity, and the reduction of porosity will contribute to the raising of bending strength.CeO2、Y3O2、
La2O3Powder content can play rare earth reinforced and act between 0. 2% and 0. 5%, therefore the steel bonded carbide of the present invention
Intensity and consistency are improved, and bending strength can reach more than 1700MPa, and consistency reaches more than 97.4%, and hardness reaches
90HRA or so, wearability are 5 times and 6.5 times of rich chromium cast iron respectively.
3rd, the present invention improves the activity of powder using high-energy ball milling mode, and reaches titanium carbide and steel matrix powder machinery
The degree of alloying, so as to improve titanium carbide and vanadium and compatibility of the steel matrix in sintering process, improve the strong of final alloy
Toughness.In addition, the relatively low ferroalloy of price is employed in the present invention as raw material, and by adding a certain amount of molybdenum and boron
Afterwards, it further improves titanium carbide and the wetability of vanadium and steel matrix in sintering process, can suppress in steel bonded carbide
The hard phase TiC of in-situ reactive synthesis grows up, and reduces TiC particle sizes, is evenly distributed.Due to adding molybdenum with being improved after boron
Binder Phase is advantageous to filling of the liquid phase to hole in sintering process, porosity is low, makes steel knot to hard phase TiC wetability
The density of hard alloy is improved, and crystal grain is tiny, even tissue, so that its hardness and bending strength and obdurability also obtain
Improve.Therefore, the present invention, which prepares high-performance steel-bonded carbide method, can improve the comprehensive mechanical property of alloy, and process letter
Just, it is easy to operate, the sintering period is short, process costs it is low, suitable for industrialized production.
Embodiment
Technical scheme is further illustrated with reference to embodiment：
Embodiment 1
A kind of preparation method of TiC high-boron low-alloy high-speed steels base steel bonded carbide, it uses following technical scheme：
(1) raw materials are titanium valve, vanadium iron powder, ferrochrome powder, molybdenum-iron powder, ferrosilicon powder, ferromanganese powder, ferro-boron powder, iron powder, nickel
Powder, copper powder, aquadag, CeO2, PVA, powder size is below 10~50 μm；
(2) material is prepared：
1）In-situ synthesizing TiC mixed-powder is prepared：By titanium（Ti）Carried out with graphite powder by C/Ti atomic molar ratio for 0.8
It is configured to in-situ synthesizing TiC mixed-powder；
2）Phase matrix alloy powder is bonded to prepare：Bonding phase metal material chemical composition mass percent is：C0.3%,
Cr5.0%, W2.5%, Mo1.8%, V1.7%, Nb0.4%, Si0.5%, Mn0.5 %, B1.6%, Cu0.5%, Ni0.9%, S≤0.02, P
≤ 0.02, CeO20.8%th, surplus Fe, and inevitable impurity element；
3）TiC Steel-bonded Cemented Carbides are prepared：Material chemical composition mass percent is：In-situ synthesizing TiC mixed powder
End 30%, bonding phase matrix alloy powder 70%；
(3) step of preparation process is：
1）Material is prepared：By titanium（Ti）With vanadium iron powder according to titanium：Vanadium is 1:Then and graphite powder 1 ratio is prepared,
Carry out being configured to fabricated in situ 30%TiC mixed-powders for 0.8 by C/Ti atomic molar ratio；By ferrochrome powder, molybdenum-iron powder, ferrosilicon
Powder, ferromanganese powder, ferro-boron powder convert according to required chemical composition mass percent, together with iron powder, nickel powder, copper powder, and aquadag,
CeO2Raw material is prepared in the ratio of bonding phase metal material chemical composition mass percent 70%；
2）The ratio of TiC particles and matrix material according to needed for Steel-bonded Cemented Carbide is mixed two kinds of materials
Close, be fitted into ball milling bucket, load steel ball, ratio of grinding media to material 5:1, add absolute ethyl alcohol and make medium and 0.5%PVA as cooling agent and divide
Powder, using vibrations ball mill ball milling 48 hours；
3）Sieved after slurry is dried, the product of required size shape is then pressed under 380 MPa pressure；
4）Sinter under vacuum, sintering temperature is 1380 DEG C, and sintering process is:10 DEG C/min of firing rate, sintering
Time is 30min, after being incubated 1.5 hours, furnace cooling to room temperature, obtains the heat-resisting steel bonded carbide of required composition.
Embodiment 2
A kind of preparation method of TiC high-boron low-alloy high-speed steels base steel bonded carbide, it uses following technical scheme：
(1) raw materials are titanium valve, vanadium iron powder, ferrochrome powder, molybdenum-iron powder, ferrosilicon powder, ferromanganese powder, ferro-boron powder, iron powder, nickel
Powder, copper powder, aquadag, CeO2、Y3O2Two kinds, PVA, powder size is below 10~50 μm；
(2) material is prepared：
1）In-situ synthesizing TiC mixed-powder is prepared：By titanium（Ti）With vanadium iron powder according to titanium：Vanadium is 1:1 ratio is matched somebody with somebody
System, then carry out being configured to in-situ synthesizing TiC mixed-powder for 0.8 by C/Ti atomic molar ratio with graphite powder；
2）Phase matrix alloy powder is bonded to prepare：Bonding phase metal material chemical composition mass percent is：C0.4%,
Cr6.0%, W2.8%, Mo2.5%, V2.0%, Nb 0.5%, Si0.6%, Mn0.6%, B2.0%, Cu0.6%, Ni1.2%, S≤0.02, P
≤ 0.02, CeO2 0.5%, Y3O 0.3%, surplus Fe, and inevitable impurity element；
3）TiC Steel-bonded Cemented Carbides are prepared：Material chemical composition mass percent is：In-situ synthesizing TiC mixed powder
End 40%, bonding phase matrix alloy powder 60%；
(3) step of preparation process is：
1）Material is prepared：By titanium（Ti）With vanadium iron powder according to titanium：Vanadium is 1:Then and graphite powder 1 ratio is prepared,
Carry out being configured to fabricated in situ 40%TiC mixed-powders for 0.92 by C/Ti atomic molar ratio；By ferrochrome powder, molybdenum-iron powder, ferrosilicon
Powder, ferromanganese powder, ferro-boron powder convert according to required chemical composition mass percent, together with iron powder, nickel powder, copper powder, and aquadag,
CeO2Raw material is prepared in the ratio of bonding phase metal material chemical composition mass percent 60%；
2）By two kinds of the 40%TiC particles of fabricated in situ needed for Steel-bonded Cemented Carbide and the ratio of matrix material 60%
Material is mixed, and is fitted into ball milling bucket, loads steel ball, ratio of grinding media to material 8:1, add absolute ethyl alcohol and make medium and 0.8%PVA conducts
Cooling agent and dispersant, using vibrations ball mill ball milling 62 hours；
3）Sieved after slurry is dried, the product of required size shape is then pressed under 450 MPa pressure；
4）Sinter under vacuum, sintering temperature is 1390 DEG C, and sintering process is:10 DEG C/min of firing rate, sintering
Time is 35min, after being incubated 2.3 hours, furnace cooling to room temperature, obtains the heat-resisting steel bonded carbide of required composition.
Embodiment 3
A kind of preparation method of TiC high-boron low-alloy high-speed steels base steel bonded carbide, it uses following technical scheme：
(1) raw materials are titanium valve, vanadium iron powder, ferrochrome powder, molybdenum-iron powder, ferrosilicon powder, ferromanganese powder, ferro-boron powder, iron powder,
Nickel powder, copper powder, aquadag, CeO2、Y3O2、La2O3, PVA, powder size is below 10~50 μm；
(2) material is prepared：
1）In-situ synthesizing TiC mixed-powder is prepared：By titanium（Ti）Powder and graphite powder are prepared by C/Ti atomic ratios for 1.0
Into in-situ synthesizing TiC mixed-powder；
2）Phase matrix alloy powder is bonded to prepare：Bonding phase metal material chemical composition mass percent is：C0.5%,
Cr7.0%, W3.0%, Mo3.0%, V2.5%, Nb 1.0%, Si 1.0%, Mn0.7%, B2.1%, Cu0.8%, Ni2.0%, S≤
0.02, P≤0.02, CeO20.3%, Y3O20.3%, La2O30.2%th, surplus Fe, and inevitable impurity element；
3）（TiV）C Steel-bonded Cemented Carbides are prepared：Material chemical composition mass percent is：Fabricated in situ（TiV）C
Mixed-powder 50%, bonding phase matrix alloy powder 50%；
(3) step of preparation process is：
1）Material is prepared：By titanium（Ti）With vanadium iron powder according to titanium：Vanadium is 1:Then and graphite powder 1 ratio is prepared,
Carry out being configured to fabricated in situ 50%TiC mixed-powders for 1.05 by C/Ti atomic molar ratio；By ferrochrome powder, molybdenum-iron powder, ferrosilicon
Powder, ferromanganese powder, ferro-boron powder convert according to required chemical composition mass percent, together with iron powder, nickel powder, copper powder, and aquadag,
CeO2Raw material is prepared in the ratio of bonding phase metal material chemical composition mass percent 50%；
2）By two kinds of the 50%TiC particles of fabricated in situ needed for Steel-bonded Cemented Carbide and the ratio of matrix material 50%
Material is mixed, and is fitted into ball milling bucket, loads steel ball, ratio of grinding media to material 10:1, add absolute ethyl alcohol and make medium and 1.0%PVA conducts
Cooling agent and dispersant, using vibrations ball mill ball milling 72 hours；
3）Sieved after slurry is dried, the product of required size shape is then pressed under 500 MPa pressure；
4）Sinter under vacuum, sintering temperature is 1420 DEG C, and sintering process is:10 DEG C/min of firing rate, sintering
Time is 40min, after being incubated 3 hours, furnace cooling to room temperature, obtains the heat-resisting steel bonded carbide of required composition.
Claims (2)
- A kind of 1. preparation method of TiC high-boron low-alloy high-speed steels base steel bonded carbide, it is characterised in that：(1) material is prepared：1）In-situ synthesizing TiC mixed-powder is prepared：By titanium（Ti）The atomic molar ratio that C/Ti is pressed with graphite powder is 0.7 ~1.1 carry out being configured to in-situ synthesizing TiC mixed-powder；2）Phase matrix alloy powder is bonded to prepare：Bonding phase metal material chemical composition mass percent is：C0.2~ 0.6%, Cr5.0~7.0%, W2.5~3.0%, Mo1.5~3.0%, V1.5~2.5%, Nb0.5~1.0%, Si0.3~1.0%, Mn0.3~1.0%, B1.4~2.5%, Cu0.3~1.0%, Ni0.8~2.0%, S≤0.02, P≤0.02, CeO2, Y3O2, One of La2O3 or more than two kinds of combination≤0.8%, surplus are Fe and inevitable impurity element；3）TiC Steel-bonded Cemented Carbides are prepared：Material chemical composition mass percent is：In-situ synthesizing TiC mixed-powder 30~50%, bonding phase matrix alloy powder 70~50%；(2) step of preparation process is：1）Material is prepared：By titanium（Ti）Carry out being configured to original position for 0.7~1.1 by C/Ti atomic molar ratio with graphite powder Synthesize TiC mixed-powders；By ferrochrome powder, molybdenum-iron powder, ferrosilicon powder, ferromanganese powder, ferro-boron powder is according to required chemical composition quality Percentage converts, together with one of iron powder, nickel powder, copper powder, aquadag, CeO2, Y3O2, La2O3 or more than two kinds of group Raw material is closed to prepare in ratio needed for bonding phase matrix alloy powder chemistry ingredient percent；2）The ratio of TiC particles and matrix material according to needed for Steel-bonded Cemented Carbide is mixed two kinds of materials, It is fitted into ball milling bucket, loads steel ball, ratio of grinding media to material 5:1~10:1, add absolute ethyl alcohol and make medium and 0.5~1%PVA as cold But agent and dispersant, using vibrations ball mill ball milling 48~72 hours；3）Sieved after slurry is dried, the product of required size shape is then pressed under 350~500 MPa pressure；4）Sinter under vacuum, sintering temperature is 1350 DEG C~1420 DEG C, and sintering process is:10 DEG C of firing rate/ Min, sintering time are 30~40min, after being incubated 1~3 hour, furnace cooling to room temperature, obtain the heat resisting steel of required composition Bond hard alloy.
- 2. a kind of preparation method of TiC high-boron low-alloy high-speed steels base steel bonded carbide according to claim 1, It is characterized in that：Raw materials are titanium valve, vanadium iron powder, ferrochrome powder, ferrotungsten, molybdenum-iron powder, ferro-boron powder, iron powder, ferro-niobium, nickel powder, One of copper powder, ferrosilicon powder, ferromanganese powder, graphite powder, aquadag, CeO2, Y3O2, La2O3 or three kinds, PVA, powder grain Degree is at 10~50 μm.
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