CN105369110B - A kind of preparation method of the heat-resisting steel bonded carbide of TiC - Google Patents
A kind of preparation method of the heat-resisting steel bonded carbide of TiC Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of the heat-resisting steel bonded carbide of TiC, it is characterised in that by titanium valve and graphite powder in C/Ti atomic ratios be 0.7~1.1 be configured to needed for ratio in-situ synthesizing TiC powder；By ferrochrome powder, molybdenum-iron powder, ferro-boron 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 the heat-resisting steel bonded carbide of TiC/.Because TiC is in intrinsic silicon fabricated in situ by the reaction in sintering process, enhancing particle size is tiny, and without wedge angle, basal body interface combines preferably and clean interfaces on surface.Prepared steel-bonded carbide method can improve the comprehensive mechanical property of alloy, and cheap, simple process.
Description
Invention field
The present invention relates to a kind of preparation method of the heat-resisting steel bonded carbide of TiC, particularly TiC is produced with reaction sintering
Heat-resisting steel bonded carbide technical field.
Background of invention
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.
At present, the method for preparing TiC steel bonded carbide is mainly powder metallurgy lqiuid phase sintering method.Lqiuid phase sintering method can be with
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 smelting
The hard phase of golden 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 is with gluing
Bad, interface vulnerable to pollution of wetability of phase etc. is tied, therefore the steel bonded carbide prepared by lqiuid phase sintering method has hole
The shortcomings of degree is high, performance is low, cost is high, for requiring that higher application scenario is often needed by forging or hip treatment,
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
It is that one kind designs by alloy, reaction in-situ generation is one or more of thermodynamically stable in parent metal under certain condition
The advanced composite material (ACM) technology of preparing of hard phase.Compared with traditional material preparation method, the technology have preparation technology it is simple,
The features such as enhancing of produced in situ is not mutually contaminated, and interface bond strength is high, it is becoming for steel bonded carbide technology of preparing development
Gesture.
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 preparation method of the heat-resisting steel bonded carbide of TiC, to
Improve the performance of the heat-resisting steel bonded carbide of TiC.
A kind of preparation method of the heat-resisting steel bonded carbide of TiC of the present invention, it uses following technical scheme：
(1) raw material：
Raw materials are titanium valve, ferrochrome powder, molybdenum-iron powder, ferro-boron powder, iron powder, ferrosilicon powder, ferromanganese powder, nickel powder, copper powder, glue
Body graphite, CeO2、Y3O2、La2O3One of them or three 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）Powder and graphite powder are entered by C/Ti atomic ratios for 0.7~1.1
Row 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~
0.5%, Cr4.0~6.0%, Mo1.3~3.0%, V0.5~1.2%, Si0.2~1.0%, Mn0.3~0.6%, B0.4~1.8%,
Cu0.3~1.0%, Ni0.8~2.0%, S≤0.02, P≤0.02, CeO2、Y3O2、La2O3The combination of one of them or more than two kinds
≤ 0.8%, surplus Fe, and inevitable impurity element；
3）The heat-resisting Steel-bonded Cemented Carbides of TiC are prepared：Material chemical composition mass percent is：In-situ synthesizing TiC mixes
Close powder 30~50%, bonding phase matrix alloy powder 70~50%；
(3) step of preparation process is：
1）Material is prepared：By titanium（Ti）Powder and graphite powder are carried out being configured to required ratio by C/Ti atomic ratios for 0.7~1.1
The in-situ synthesizing TiC mixed-powder of example；By ferrochrome powder, molybdenum-iron powder, ferro-boron powder, ferrosilicon powder, ferromanganese powder, according to required chemistry into
Divide mass percent conversion, together with iron powder, nickel powder, copper powder, aquadag, CeO2、Y3O2、La2O3One of them or more than two kinds
Combination raw materials 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, iron powder, ferrochrome powder, molybdenum-iron powder, ferro-boron powder, ferrosilicon powder, ferromanganese 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 carbon
Change titanium volume fraction as 30% one 50% TiC heat resisting steel steel bonded carbide.It is mainly characterized by：1. due to steel bonded carbide
In TiC be and in intrinsic silicon fabricated in situ by the reaction in sintering process, it is possible to obtain Ordinary hardening phase powder
The method of mixing is difficult to reach, or even inaccessiable granular and uniformity coefficient, and basal body interface combines preferably and interface is done
Only.2. fabricated in situ enhancing particle size is tiny, surface is evenly distributed in the base without wedge angle, so as to improve material
Bending strength MPa and properties.3. situ synthesis techniques and liquid phase sintering technology are combined together, simple process, cost
It is low.4. it is cheap due to raw material, cost can be substantially reduced.Simultaneously not only can be in a vacuum in the technique of this powder
Sintering, how can also sinter in the atmosphere such as hydrogen, widen the means approach manufactured.
The present invention improves the activity of powder using high-energy ball milling mode, and reaches titanium carbide and closed with steel matrix powder machinery
The degree of aurification, so as to improve titanium carbide and compatibility of the steel matrix in sintering process, improve the obdurability of final alloy.This
Outside, the relatively low ferro-molybdenum of price is employed in the present invention as raw material, its further improve in sintering process titanium carbide and
The wetability of steel matrix, improve the obdurability of alloy.Therefore, the present invention, which prepares high-performance steel-bonded carbide method, can improve alloy
Comprehensive mechanical property, and process is easy, 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 97. more than 4%.
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 compatibility of the steel matrix in sintering process, improve the obdurability of final alloy.
In addition, employ the relatively low ferroalloy of price in the present invention as raw material, and by add a certain amount of molybdenum with after boron, its
Further improve the wetability of titanium carbide and steel matrix in sintering process, the reaction synthesis of steel bonded carbide situ can be suppressed
Hard phase TiC grow up, make TiC particle sizes reduce, be evenly distributed.Due to adding molybdenum with improving cohesive relative harder after boron
Phase TiC wetability, be advantageous to filling of the liquid phase to hole in sintering process, porosity is low, makes the close of steel bonded carbide
Degree is improved, and crystal grain is tiny, even tissue, so that its hardness and bending strength and obdurability are also improved.Therefore,
The present invention, which prepares high-performance steel-bonded carbide method, can improve the comprehensive mechanical property of alloy, and process is easy, easy to operate,
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 the heat-resisting steel bonded carbide of TiC, it uses following technical scheme：
(1) raw material：
Raw materials are titanium valve, ferrochrome powder, molybdenum-iron powder, ferro-boron powder, ferrosilicon powder, ferromanganese powder, iron powder, nickel powder, copper powder, glue
Body graphite, 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）Powder and graphite powder are matched somebody with somebody by C/Ti atomic ratios for 0.85
In-situ synthesizing TiC mixed-powder is made；
2）Phase matrix alloy powder is bonded to prepare：Bonding phase metal material chemical composition mass percent is：C0.3%,
Cr4.0%, Mo1.5%, V0.6%, Si0.4%, Mn0.3%, B0.6%, Cu0.5%, Ni1.0%, S≤0.02, P≤0.02, CeO2≤
0.8%th, surplus Fe, and inevitable impurity element；
3）The heat-resisting Steel-bonded Cemented Carbides of TiC are prepared：Material chemical composition mass percent is：In-situ synthesizing TiC mixes
Close powder 30%, bonding phase matrix alloy powder 70%；
(3) step of preparation process is：
1）Material is prepared：By titanium（Ti）Powder and graphite powder are carried out being configured to fabricated in situ 30% by C/Ti atomic ratios for 0.85
TiC mixed-powders；By ferrochrome powder, molybdenum-iron powder, ferro-boron powder, ferrosilicon powder, ferromanganese powder, according to required chemical composition mass percent
Conversion, together with iron powder, nickel powder, copper powder, aquadag, CeO2Raw material presses bonding phase metal material chemical composition mass percent
70% ratio is prepared；
2）Two kinds of materials of the fabricated in situ 30%TiC particles needed for Steel-bonded Cemented Carbide and matrix material 70% are entered
Row mixing, is fitted into ball milling bucket, loads steel ball, ratio of grinding media to material 5:1, add absolute ethyl alcohol and make medium and 0.6%PVA as cooling agent
And dispersant, using vibrations ball mill ball milling 55 hours；
3）Sieved after slurry is dried, the product of required size shape is then pressed under 400 MPa pressure；
4）Sinter under vacuum, sintering temperature is 1370 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 the heat-resisting steel bonded carbide of TiC, it uses following technical scheme：
(1) raw material：
Raw materials are titanium valve, ferrochrome powder, molybdenum-iron powder, ferro-boron powder, ferrosilicon powder, ferromanganese powder, iron powder, nickel powder, copper powder, glue
Body graphite, 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）Powder and graphite powder are prepared by C/Ti atomic ratios for 0.9
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：C0.4%,
Cr5.0%, Mo2.3%, V0.9%, Si0.6%, Mn0.5%, B1.2%, Cu0.6%, Ni1.3%, S≤0.02, P≤0.02, CeO2
0.5%, Y3O20.3%th, surplus Fe, and inevitable impurity element；
3）The heat-resisting Steel-bonded Cemented Carbides of TiC are prepared：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 is prepared：By titanium（Ti）Powder and graphite powder are configured to institute's fabricated in situ by C/Ti atomic ratios for 0.9
40%TiC mixed-powders；By ferrochrome powder, molybdenum-iron powder, ferrosilicon powder, ferromanganese powder, ferro-boron powder is according to required chemical composition quality percentage
Than conversion, together with iron powder, nickel powder, copper powder, aquadag, CeO2、Y3O2Raw material presses bonding phase metal material chemical composition quality hundred
Divide and prepared than 60% ratio；
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 7:1, 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 the heat-resisting steel bonded carbide of TiC, it uses following technical scheme：
(1) raw material：
Raw materials are titanium valve, ferrochrome powder, molybdenum-iron powder, ferro-boron powder, ferrosilicon powder, ferromanganese powder, iron powder, nickel powder, copper powder, glue
Body graphite, 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%,
Cr6.0%, Mo3.0%, V1.2%, Si0.9%, Mn0.6%, B1.5%, Cu0.8%, Ni2.0%, S≤0.02, P≤0.02,
CeO20.3%, Y3O20.3%, La2O30.2%th, surplus Fe, and inevitable impurity element；
3）The heat-resisting Steel-bonded Cemented Carbides of TiC are prepared：Material chemical composition mass percent is：In-situ synthesizing TiC mixes
Close powder 50%, bonding phase matrix alloy powder 50%；
(3) step of preparation process is：
1）Material is prepared：By titanium（Ti）Powder and graphite powder are configured to institute's fabricated in situ by C/Ti atomic ratios for 1.0
50%TiC mixed-powders；By ferrochrome powder, molybdenum-iron powder, ferrosilicon powder, ferromanganese powder, ferro-boron powder is according to required chemical composition quality percentage
Than conversion, together with iron powder, nickel powder, copper powder, aquadag, CeO2、Y3O2, La2O3Raw material presses bonding phase metal material chemical composition
The ratio of mass percent 50% is prepared；
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%PVA as cold
But 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)
1. a kind of preparation method of the heat-resisting steel bonded carbide of TiC, it is characterised in that including following technical scheme：
(1) material is prepared：
1）In-situ synthesizing TiC mixed-powder is prepared：By titanium（Ti）Powder and graphite powder are matched somebody with somebody by C/Ti atomic ratios for 0.7~1.1
In-situ synthesizing TiC mixed-powder is made；
2）Phase matrix alloy powder is bonded to prepare：Bonding phase metal material chemical composition mass percent is：C0.3~0.5%,
Cr4.0~6.0%, Mo1.3~3.0%, V0.5~1.2%, Si0.2~1.0%, Mn0.3~0.6%, B0.4~1.8%, Cu0.3~
1.0%, Ni0.8~2.0%, S≤0.02, P≤0.02, CeO2、Y3O2、La2O3The combination of one of them or more than two kinds≤
0.8%, surplus Fe, and inevitable impurity element；
3）The heat-resisting Steel-bonded Cemented Carbides of TiC are prepared：Material chemical composition mass percent is：In-situ synthesizing TiC mixes
Powder 30~50%, bonding phase matrix alloy powder 70~50%；
(2) step of preparation process is：
1）Material is prepared：By titanium（Ti）Powder and graphite powder in C/Ti atomic ratios be 0.7~1.1 be configured to needed for ratio original
Position synthesis TiC mixed-powders；By ferrochrome powder, molybdenum-iron powder, ferro-boron powder, ferrosilicon powder, ferromanganese powder, 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, dress
Enter in 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 cooling 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 350~500MPa pressure；
4）Sinter under vacuum, sintering temperature is 1350 DEG C~1420 DEG C, and sintering process is:10 DEG C/min of firing rate,
Sintering time is 30~40min, after being incubated 1~3 hour, furnace cooling to room temperature, obtains the heat resisting steel knot hard of required composition
Alloy.
A kind of 2. preparation method of the heat-resisting steel bonded carbide of TiC according to claim 1, it is characterised in that：Original used
Material is titanium valve, ferrochrome powder, molybdenum-iron powder, ferro-boron powder, iron powder, ferrosilicon powder, ferromanganese powder, nickel powder, copper powder, aquadag, graphite powder,
CeO2、Y3O2、La2O3One of them or three kinds, PVA, powder size is at 10~50 μm.
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| CN107058901A (en) * | 2017-02-09 | 2017-08-18 | 江苏汇诚机械制造有限公司 | A kind of preparation method of high-toughness heat-resistant TiC/TiN steel bonded carbide |
| CN106591674A (en) * | 2017-02-09 | 2017-04-26 | 江苏汇诚机械制造有限公司 | Preparation method for high-strength high-toughness heat-resistant TiN steel-bonded hard alloy |
| CN106906401A (en) * | 2017-03-04 | 2017-06-30 | 丹阳嘉伟耐磨材料科技有限公司 | A kind of heat-resisting base steel WC40 steel bonded carbide Roll Collar and its manufacture method |
| CN111101047A (en) * | 2018-10-25 | 2020-05-05 | 青海民族大学 | In-situ TiC particle and large-proportion amorphous alloy co-reinforced manganese steel-based composite material and preparation method thereof |
| CN111101074A (en) * | 2018-10-26 | 2020-05-05 | 青海民族大学 | In-situ carbide particle-embedded 3D amorphous alloy network reinforced boron steel-based composite material and preparation method thereof |
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| 《TiC/耐热钢钢结硬质合金原位反应合成研究》;刘均海等;《粉末冶金技术》;20050630;第23卷(第3期);第200页第2部分第1-3段 * |
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