CN107058901A - A kind of preparation method of high-toughness heat-resistant TiC/TiN steel bonded carbide - Google Patents
A kind of preparation method of high-toughness heat-resistant TiC/TiN steel bonded carbide Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of high-toughness heat-resistant TiC/TiN steel bonded carbide, it is characterized in that by Ti02 powder, TiH2 powder or Ti powder is one kind of and aquadag powder by C/ Ti atomic ratios is 0.7~1.1, by Ti02 powder, TiH2 powder or Ti powder is one kind of and urea ((NH2) 2CO) by N/ Ti atomic ratios is 0.4~1.1 to carry out being configured to fabricated in situ TiN mixed-powders；By molybdenum-iron powder, vanadium iron powder, ferrochrome powder, ferromanganese powder, ferrosilicon powder, iron powder, ferro-boron powder, nickel powder, aquadag and the rare earths material proportions as needed for bonding phase metal chemical composition mass ratio, load steel ball ball milling, wherein add absolute ethyl alcohol make after slurry is dried after medium and PVA, ball milling it is compressing, sintering obtain steel-bonded carbide.In-situ reactive synthesis technology is combined by the present invention with liquid phase sintering technology, and enhancing particle size is tiny, and surface combines preferable and clean interfaces without wedge angle, basal body interface.Prepared steel-bonded carbide method can improve the comprehensive mechanical property of alloy, and cheap, and technique is easy.
Description
Invention field
The present invention relates to a kind of preparation method of high-toughness heat-resistant TiC/TiN steel bonded carbide, particularly burnt with reaction
Connection produces high-toughness heat-resistant TiC/TiN steel bonded carbide technical fields.
Background of invention
Hard alloy (WC-Co alloys) is one of the most frequently used material of cutting tool industry, due to hard alloy material it is high into
This and toxicity, in recent years material worker begin look for its alternative materials, to replace WC-Co hard alloy material, rise to promote and make
One factor is Co costs of material rise, and price fluctuation is big in recent years；Another factor is continuous with modern industry
Hardmetal materials are proposed higher requirement, WC-Co hard alloy material is in high temperature, the use environment of high speed by development
Start to lose ground, or even can not use completely.But certainly, topmost reason is the industrial toxicity of Co powder, especially
It is the permanent injury that WC-Co composite powder is caused to human lung, oneself causes the extensive concern of people.
Steel bonded carbide（Hereinafter referred to as steel-bonded carbide）It is that, 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 that its has
Standby following excellent properties：1）Extensive processing performance, forgeability and machinable performance and can mainly be heat-treated
Property and weldability.2）Good physical and mechanical properties, 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, anti-oxidant, anti-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
Consequence is more and more occupied in terms of part material, 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.
In recent years, to obtain some particular tissues and performance of steel bonded carbide, and alleviate due to conventional rigid alloy
The problems such as material main resource W, Co are increasingly deficient, has carried out to steel bonded carbide ground more extensively with deep both at home and abroad
Study carefully, particularly to add different New Rigid phases research (such as addition A1203, TiN, NbC, TiCN, TiB2, Mo2FeB2,
Mo2C, Cr3C2, VC, NV etc.).In recent years, some new hard phase steel-bonded carbides are continued to bring out.
TiB2 has heat-resisting quantity good, and density and resistivity are small, and conductibility is good, and metal adhesiveness is low and friction factor
It is low, a kind of the features such as inoxidizability is strong, it is considered to be preferable steel-bonded carbide hard phase.Because of the solid solubility between Fe and TiB2
Low, wetability is good, and Mo can also improve its wetability, therefore comprehensive TiB2 and Fe, Mo advantage, has made TiB.FeMo composite woods each
Material.
Certain Japanese company, which develops, a kind of does not contain W, Co but the boride-based composite KMH of M02FeB2 types containing Cr.
Such polynary boride-based alloy be using water atomization prepare Fe-Cr-B alloy powders, boride powder and Fe, Cr, Mo,
The metal dusts such as Ni make raw material, are mixed through wet-milling, compressing and vacuum-sintering method is manufactured.
In addition to above-mentioned new steel bonded carbide, some Japanese companies also utilize a variety of hard compounds (such as
TiC, VC, Cr3C2, SiC, ZrC, AlN etc.) and its mixed compound make hard phase, make binding agent with various steel or ferrous alloy,
Develop some advanced composite material (ACM)s.
Meanwhile, people are also constantly seeking new hard phase and the combination of new Binder Phase, so as to develop have it is optimal
The MC type particulate reinforced composites of tissue and performance.In steel-bonded carbide, the hard particulate carbide species as wear-resistant phase
Compare many, there is the ceramic particles such as WC, TiC, Cr7C3, NbC, VC, SiC and alloy carbide and cementite.MC type carbide
Thermodynamic stability putting in order from high to low be：TiC ＞ NbC ＞ VC ＞ WC, putting in order for its hardness be：TiC ＞ VC
＞ WC ＞ NbC.It is known that TiC and Fe intermiscibilities are poor.Sintering temperature is high, and strength ratio WC is poor, and its advantage is light weight, thermally-stabilised
Property, frictional property are good；WC high temperature and Fe intermiscibilities are bad, are easily dissolved in during high temperature in Fe, high high-temp stability, calorific intensity are poor,
Separate out to form bridge joint in cooling procedure, deteriorate the mechanical performance of alloy；As carbide V element, with
Ti elements are similar, and V is also a kind of very active alloying element, and very strong affinity is have with the member such as C, N.The parent of V element and C
It is more than Cr elements and C affinity with power, easily forms two kinds of stable carbides of VC and V2C.In carbide ceramics, VC's is hard
Highest is spent, and has good heat endurance, is a kind of preferable hard enhancing phase.
Ti base cemented carbides refer to the hard alloy that TiC or Ti (C, N) is matrix.Compared with WC base cemented carbides, Ti bases
The hardness of hard alloy is higher, and density is small, and high temperature resistant, wear-resistant, corrosion resistance are stronger, and has very good anti stick, resists
The ability of diffusive wear.Ti base cemented carbides can be divided into by composition and performance:（1）TiC based alloys；（2）Ti (C, N) based alloy.
Because TiC based alloys toughness is very low, too many concern is never obtained.Until in the 1970s, Kieffer et al. has found
Add in TiN to TiC-Mo-Ni series hard metals, hard phase crystal grain is significantly refined, the room temperature and high temperature power of hard alloy
Learning performance is also substantially improved, and the appropriate TiN of addition, can improve TiC steel bonded carbide into nuclear concentration, refinement is brilliant
The high temperature corrosion-resisting and inoxidizability of hard alloy can be also significantly increased after promoting homogeneous grain size, addition TiN in grain
Can, while improving the hardness and bending strength of material.In addition, TiN addition produces the effect that interfacial effect reduces crystal boundary, suppression
Dislocation motion in fracture process processed, pinning effect is played to breakaway poing can also improve intensity.Therefore, Ti (C, N) bases hard is closed
Gold causes the great interest of researchers.TiN is strong as the small oxidation resistance of hard phase free energy, and it rubs between steel matrix
Effect is small, and the wetability of its Binder Phase is better than TiC, and antisticking ability is more stronger than TiC, and free energy is smaller, oxidation resistance temperature model
Enclose big.
Ai Te Vit of Germany have developed a kind of ITE of steel bonded carbide CORO mono- using TiN as hard phase.
TiN particle sizes in the ITE of hard alloy CORO mono- are about 0.1 um, are evenly distributed in heat treatable steel matrix,
Therefore CORO-ITE is provided simultaneously with the high rigidity of hard alloy and the high tenacity of steel matrix.CORO-ITE hard alloy oneself successfully
Apply in many fields, show excellent performance and the potentiality being improved.The milling cutter manufactured with CORO-ITE hard alloy is cut
The rate of cutting is 3 times of high-speed steel milling cutter, while its use time extends 2 times.
Sandvik AB of Sweden has developed a kind of new steel-bonded carbide CORONlTE based on TiN.They are using a kind of
Special process, the TiN powder of superfine (about 0.1 micron) is equably added in heat treatable steel matrix, its volume content
Can be from 35% to 60%, because TiN powder is thin and performance and its stably, obtained CORONITE alloys have concurrently by this method
The wearability of hard alloy and the toughness of high-speed steel.
Japan also develops being machined and heat treatable steel by hard phase of TiN using water atomization and sintering process
Bond hard alloy H34A.By the way that the water atomization comminuted steel shot of tungsten, aluminium and high carbon content is mixed with 10wt%TiN powder, re-compacted shaping
Sintering obtains H34A afterwards.H34A hardness after annealing reaches 46~48HRc, can be machined, and H34A tempering
Hardness is more up to more than 72HRc, because matrix is hardened and WC due to possessing high-carbon quantity, MoC, the disperse of TiN particles
Reinforcing, therefore the alloy possesses excellent cutting ability.During as such as cutting element of drill bit, end mill(ing) cutter etc, performance is bright
It is aobvious to be better than high-speed steel and ordinary rigid alloy.
Relative to traditional WC base cemented carbides, Ti (C, N) base cemented carbides because with excellent high temperature hardness and compared with
High thermal conductivity, so Ti (C, N) base cemented carbide not only ensures that cutter has high cutting speed but also can provided preferably
Surface Machining, outstanding chip and allowance control, it is ensured that the geometric accuracy of workpiece can also be protected while charging rate is improved
Hold strict fixed dimension.Moreover, Ti (C, N) base cemented carbides are compared with traditional hard alloy, no matter in price or
All there is very big competitiveness in the performance of performance, especially in high-speed cutting and process operation；But relative to traditional W
C-Co hard alloy, the shortcoming that Ti (C, N) base cemented carbides obdurability still flexible is not enough.
To improve the obdurability of TiC based ceramic metals, material supply section scholars have done substantial amounts of research., Austria in 1971
Scientist's R bases Fil etc. is found, the raising that TiN will be helpful to toughness of material and wearability is added in TiC based ceramic metals,
And assert Ti (C, N) based ceramic metals by as the wide hard tool materials of a class development prospect.Then, American scientist
By experimental data prove (Ti, Mo) (C, N)-Ni based ceramic metals of fine grain there is higher hardness, it is good toughness, excellent
The features such as different wearability and plasticity_resistant deformation ability, it is highly suitable for making cutting rolled steel process tool.It can be said that Ti
The appearance of (C, N) based ceramic metal, compensate for the blank in performance between traditional WC-Co alloys and ceramic material.With WC-
Co alloys are compared, Ti (C, N) based ceramic metal have higher red hardness, lower coefficient of friction, more excellent wearability and
Corrosion resistance etc.；Compared with TiC based ceramic metals, Ti (C, N) based ceramic metal possesses higher red hardness, thermal conductivity, laterally broken
Resistance to spalling, more excellent high temperature creep resistance and inoxidizability.Therefore, Ti (C, N) based ceramic metals are in machining field,
Especially the field such as semifinishing, finishing and high-speed milling, can even substitute tradition WC-Co hard completely for part and close
Gold and TiC based ceramic metal class cutter materials.
Since 1980s, the research of Ti (C, N) based ceramic metal achieves significant progress.MO2C, WC, VC,
TaC and NbC etc. is used for increasing the agglutinating property of material as additive and improves microstructure.Ni-Mo, Ni-Co, Ni-Cr, Ni
The Binder Phases such as (Co, Fe) and (Ni, Co)-Ti2AlN also continuously emerge.Japan is that the research of Ti (C, N) based ceramic metal is the deepest
Enter, the country being most widely used, counted according to Japanese sintered carbide tools association, in phase at the beginning of the nineties in last century, Ti (C, N) Base Metal
The occupation rate of market of sintex with regard to oneself up to 27.3%, it is suitable with WC base cemented carbides.And to early 20th century, Ti (C, N) Base Metal
Sintex reaches 33 in the occupation rate of market of Japan, the trend of big substituted conventional rigid alloy.And in the U.S. or European Union, Ti
The occupation rate of market of (C, N) base ceramet tool bit is more than 10%, and it is only 1.2% in China market occupation rate.Sweden
Sandvik AB, the Kennametal Inc. in the U.S., the Iscar company of Israel, Toshiba, the company of Sumitomo Electric Industries of Japan etc.
Foreign well-known cutter manufacturing enterprise is all developing Ti (C, N) base ceramet tool bit energetically, and oneself realizes commodity seriation.China
Research on Ti (C, N) based ceramic metal is started in the early 1990s in last century, Zhuzhou hard alloy group company, Zi Gong
The enterprises such as hard alloy group company, and the institution of higher learning such as Central South University, the Central China University of Science and Technology, HeFei University of Technology carry out
Many correlative studys, and achieve certain achievement.Wherein, Ti (C, N) Base Metal that hard alloy group company in Zhuzhou develops
Function of Ceramic Cutting Tools is suitable with Sandvik AB, more excellent even with performance.
TiN presence can improve alloy eutectic temperature, hinder Ti and Mo to carry out counterdiffusion by liquid phase so that Mo in liquid phase
Content increases and Ti concentration reduces, and while the precipitation for suppressing crystal grain is grown up, also inhibits the formation of brittle interphase, from
And cermet is obtained higher toughness and wearability.Because hard compounds TiN and TiC belong to typical face-centered cubic
Crystal formation, but continuous type solid solution is generated, though the TiCN hardness reduction of generation, wearability is still superior.It is appropriate by addition
TiN, can improve TiC steel bonded carbide into nuclear concentration, crystal grain thinning promotes homogeneous grain size, while improving material
Hardness and bending strength.In addition, TiN addition produces the effect that interfacial effect reduces crystal boundary, suppress in fracture process
Dislocation motion, pinning effect is played to breakaway poing can also improve intensity.Add in TiN to TiC-Mo-Ni series hard metals, hard
Phase crystal grain is significantly refined, and the room temperature and mechanical behavior under high temperature of hard alloy are also substantially improved, and after addition TiN also
The high temperature corrosion-resisting and antioxygenic property of hard alloy can be significantly increased.
Mitsubishi metal company have developed a kind of new steel bonded carbide based on this solid solution, and carry out
Production.This new steel bonded carbide is made up of hard compounds TiCN and Binder Phase high-speed steel, using TiCN hardness compared with
The characteristics of low but very strong wearability, high speed comminuted steel shot is mixed with carbon titanium carbonitride powder and additive, by ball milling, drying, shaping,
Dewaxing, the TiCN base steel-bonded carbides then produced by high temperature insostatic pressing (HIP), heat treatment and method for fine finishing.It is this to be defined as
The novel hard alloy of " Chotaigokin " has uniform microstructure tissue, segregation-free, the characteristics of alloying level is high.
Its Physical and mechanical properties has more excellent performance compared with high-speed steel and WC-24%Co hard alloy.
Ti (C, N) based ceramic metal has density low, and hardness is high, wear-resistant, the excellent physical mechanical such as resistance to high temperature oxidation
Performance, and production cost is low, there is high cost performance, can substitute conventional rigid alloy material, is widely used at a high speed, it is high
On the tool for cutting machining of precision.Meanwhile, this novel hard alloy in industries such as automobile, metallurgy, mine, building materials and moulds
Alternative traditional high-abrasive material, increases substantially parts service life, economizes on resources, and is imitated with good social economy
Benefit.In addition, with industrial wilderness demand and inevitable artificial waste, China or even worldwide W, Co money
Source is quite poor, and price rises steadily, and each national capital Efforts To Develop seeks the research and development of W, Co substitute material.And China
Ti ore resources enrich, and replace W to have very high feasibility in resource with Ti.Therefore, TiC/TiN base steel knot hard is researched and developed
Alloy saves precious alloy resource, improves its industrial value and application value, either work to widening the hard phase of hard alloy
Journey application aspect, or be all significant in terms of Technological Economy.Therefore, new TiC/TiN steel knot is researched and developed hard
Matter alloy has good economic benefit and important meaning.
The obdurability for the alloy manufactured by steel bonded carbide manufacturing process developed at present is still relatively low, far from satisfaction
More and more power of withstanding shocks are larger, the use in the case of impact velocity is higher.Therefore Development and Production high-performance, low cost
Steel bonded carbide is necessary.Wherein, the obdurability for improving steel-bonded carbide is the research direction of emphasis.
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 interior content for adjusting hard phase, but due to powder metallurgy in a big way
The hard phase of lqiuid phase sintering method is generally introduced in the way of adding, cost of raw material height, thick particle, 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
It is 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 is further reduced.
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 is designed by alloy, in 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,
Not contaminated, the features such as interface bond strength is high of enhancing phase of produced in situ, 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, often meeting segregation asks gap or grain boundary in dendrite in casting process, 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, reduction production cost.
The content of the invention
In view of the shortcomings of the prior art, the invention provides a kind of system of high-toughness heat-resistant TiC/TiN steel bonded carbide
Preparation Method, the performance to improve TiC/TiN steel bonded carbide.
A kind of preparation method of high-toughness heat-resistant TiC/TiN steel bonded carbide of the present invention, it uses following technical side
Case：
(1) raw material：Raw materials are that Ti02 powder, TiH2 powder or Ti powder are one kind of or three kinds, vanadium iron powder, vanadium iron powder,
Ferrochrome powder, molybdenum-iron powder, ferro-boron powder, iron powder, nickel powder, copper powder, aquadag, CeO2、Y3O2、La2O3One of them or three kinds, PVA,
Powder size is at 10~50 μm；
(2) material is prepared：
1）Fabricated in situ TiN powder is prepared：By Ti02 powder, TiH2 powder or Ti powder is one kind of or three kinds and urea ((NH2)
It is 2CO) that 0.4~1.1 progress is configured to fabricated in situ TiN mixed-powders by N/ Ti atomic ratios；
2）In-situ synthesizing TiC powder is prepared：By Ti02 powder, TiH2 powder or Ti powder is one kind of or three kinds and aquadag powder are pressed
C/ Ti atomic ratios are that 0.7~1.1 progress is configured to in-situ synthesizing TiC powder；
3）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%th, surplus Fe, and inevitably impurity element；
4）High-toughness heat-resistant TiC/TiN Steel-bonded Cemented Carbides are prepared：Material chemical composition mass percent is：Fabricated in situ
TiC powder 25~40%, fabricated in situ TiN powder 5~20%, bonding phase matrix alloy powder 70~40%；
(3) step of preparation process is：
1）TiN powder material is prepared：By Ti02 powder, TiH2 powder or Ti powder is one kind of and industrial urea ((NH2) 2CO) presses N/
Ti atomic ratios are that 0.4~1.1 progress is configured to fabricated in situ TiN mixed-powders；It is fitted into polyurethane ball milling bucket, loads stainless steel
Steel ball, ratio of grinding media to material 10:1~20:1, add absolute ethyl alcohol and make medium and dispersant, sealing ball milling 48 is carried out using vibrations ball mill
~72 hours, it is prepared into TiN powder；
2）Material is prepared：By Ti02 powder, TiH2 powder or Ti powder is one kind of and aquadag powder by C/ Ti atomic ratios is 0.7
~1.1 carry out being configured to in-situ synthesizing TiC mixed-powder；By the TiN powder prepared and vanadium iron powder, ferrochrome powder, molybdenum-iron powder, boron
Iron powder converts according to required chemical composition mass percent, together with iron powder, nickel powder, copper powder, aquadag, CeO2、Y3O2、
La2O3The combination raw materials of one of them or more than two kinds are matched somebody with somebody in ratio needed for bonding phase metal material chemical composition mass percent
System；
3）Fabricated in situ Ti according to needed for Steel-bonded Cemented Carbide（CN）Mixed-powder and bonding phase matrix alloy powder
Ratio is mixed three kinds of materials, 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 to be situated between
Matter and 0.5~1%PVA add 10~20% industrial ureas or ammoniacal liquor as nitrogen source, using vibrations ball as cooling agent and dispersant
Grinding machine carries out sealing ball milling 48~72 hours；
4）Sieved after slurry is dried, the product of size shape needed for being then pressed under 350~500 MPa pressure；
5）Sinter under vacuum, sintering temperature is 1400 DEG C~1500 DEG C, sintering process is:10 DEG C/min of firing rate,
Reach the Isothermal sinter carried out after sintering temperature 2~5 hours, furnace cooling to room temperature, the high-toughness heat-resistant of composition needed for obtaining
TiC/TiN steel bonded carbide；
Beneficial effect
Compared with prior art, the invention has the advantages that：
1st, the present invention is with cheap Ti02 powder, TiH2 powder or Ti powder, iron powder, ferrochrome powder, molybdenum-iron powder, ferrotungsten powder, vanadium iron powder,
Ferrosilicon powder, ferromanganese powder, aquadag is raw material, and in-situ reactive synthesis technology is combined with liquid phase sintering technology, is prepared for hard
Matter phase vanadium carbide volume fraction is 30%~50% high tough VC high-speed steel-bases steel bonded carbide.It is mainly characterized by：1. by
VC in steel bonded carbide is in intrinsic silicon fabricated in situ by the reaction in sintering process, it is possible to obtain general
The method of logical hardening phase powder mixing is difficult to reach, or even inaccessiable granular and uniformity coefficient, and basal body interface is combined
Preferable and clean interfaces.2. fabricated in situ enhancing particle size is tiny, and surface is evenly distributed without wedge angle, and in the base, so that
Improve the bending strength and properties of material.3. situ synthesis techniques are combined together with liquid phase sintering technology, technique
Easy, cost is low.4. it is cheap due to raw material, cost can be substantially reduced.Not only may be used simultaneously in the technique of this powder
To sinter in a vacuum, 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 that titanium carbide is 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, improves 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 with
The wetability of steel matrix, improves 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 conducive to entering for densification
Journey, reaches 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 vanadium carbide and steel matrix powder mechanical alloy
The degree of change, so as to improve vanadium carbide and compatibility of the steel matrix in sintering process, improves the obdurability of final alloy.This
Outside, the relatively low ferroalloy of price is employed as raw material, and by adding after a certain amount of molybdenum in the present invention, it is sintered
Further improve the wetability of vanadium carbide and steel matrix in journey, the hard of steel bonded carbide situ reaction synthesis can be suppressed
Phase VC grows up, and reduces VC particle sizes, is evenly distributed.Due to improving wetting of the Binder Phase to hard phase VC after adding molybdenum
Property, be conducive to filling of the liquid phase to hole in sintering process, porosity is low, be improved the density of steel bonded carbide,
Crystal grain is tiny, even tissue, so that its hardness and bending strength and obdurability are also improved.Therefore, prepared by the present invention
High-performance steel-bonded carbide method can improve the comprehensive mechanical property of alloy, and process is easy, the easy to operate, sintering period
It is short, process costs it is low, suitable for industrialized production.
3rd, TiC is a kind of with high intensity, the hard phase of good wettability, and TiN addition makes hard alloy not drop
Alloy strength is improved in the case of low-alloy hardness, TiN and TiC belongs to typical face-centered cubic crystal formation, can generate continuous system
Row solid solution, expensive metal Mo, Ni alloying action is replaced with TiN, and the present invention is adding a small amount of Alloy Elements Mo, Ni's
On the basis of, improve TiC/TiN steel bonded carbide wearability and bending strength, manufactured TiC/TiN steel bonded carbide
Bending strength reaches more than 1100MPa, and hardness reaches more than 82HRA, its high comprehensive performance, with higher commercial Application valency
Value and good economic benefit.
4th, TiCN based ceramic metals have that density is low, hardness is high, wear-resistant and high temperature resistance is anti-oxidant, are that one kind is suitably replaced
Conversion materials, but this material nickel that is still and cobalt etc. do Binder Phase, the problem of not solving high cost and toxicity.The present invention
Co will be replaced with the close Fe of atomicity, Ni etc. makees the advantage of Binder Phase except Fe as the Binder Phase of cermet with iron
Resource is more rich, and price is less expensive, outside lower toxicity, also as Fe alloy can improve the property of material by being heat-treated
Can, this is not available for general hard alloy.
4th, titanium carbonitride is a kind of function admirable, and widely used non-oxide ceramic material has the excellent of TiC and TiN concurrently
Point, it has fusing point high, and hardness is big, the characteristics of corrosion-resistant and good in oxidation resistance, and has good thermal conductivity, electric conductivity and change
Learn stability.Ti (C, N) base steel bonded carbide prepared by the present invention has density low, and hardness is high, wear-resistant, high temperature resistance oxygen
The excellent physical and mechanical properties such as change, and production cost is low, there is high cost performance, can substitute conventional rigid alloy material
Material, is widely used at a high speed, the material such as high-precision tool for cutting machining, mould, it is adaptable to machinery, chemical industry, automobile making and
Many fields such as Aero-Space.
Embodiment
Technical scheme is further illustrated with reference to embodiment：
Embodiment 1
A kind of preparation method of high-toughness heat-resistant TiC/TiN steel bonded carbide, it uses following technical scheme：
(1) raw material：
Raw materials be Ti02 powder, vanadium iron powder, ferrochrome powder, molybdenum-iron powder, ferro-boron powder, iron powder, nickel powder, copper powder, aquadag,
CeO2, PVA, powder size is at 10~50 μm；
(2) material is prepared：
1）Fabricated in situ TiN powder is prepared：Ti02 powder and urea ((NH2) 2CO) are prepared by N/ Ti atomic ratios for 0.4
Into fabricated in situ TiN mixed-powders；
2）In-situ synthesizing TiC powder is prepared：Ti02 powder and aquadag powder are carried out being configured to original by C/ Ti atomic ratios for 0.7
Position synthesis TiC powder；
3）Phase matrix alloy powder is bonded to prepare：Bonding phase metal material chemical composition mass percent is：C0.3%,
Cr4.0%, Mo1.5%, V0.5%, Si0.3%, Mn0.35%, B0.4%, Cu0.5%, Ni0.8%, S≤0.02, P≤0.02, CeO2、
Y3O2、La2O3Combination≤0.8% of one of them or more than two kinds, surplus Fe, and inevitable impurity element；
4）High-toughness heat-resistant TiC/TiN Steel-bonded Cemented Carbides are prepared：Material chemical composition mass percent is：Fabricated in situ
TiC powder 25%, fabricated in situ TiN powder 5%, bonding phase matrix alloy powder 70%；
(3) step of preparation process is：
1）TiN powder material is prepared：Ti02 powder and industrial urea ((NH2) 2CO) are prepared by N/ Ti atomic ratios for 0.4
Into fabricated in situ TiN mixed-powders；It is fitted into polyurethane ball milling bucket, loads stainless steel steel ball, ratio of grinding media to material 10:1~20:1, add
Absolute ethyl alcohol makees medium and dispersant, carries out sealing ball milling 48~72 hours using vibrations ball mill, is prepared into TiN powder；
2）Material is prepared：Ti02 powder and aquadag powder are configured into in-situ synthesizing TiC for 0.7 progress by C/ Ti atomic ratios to mix
Close powder；By the TiN powder prepared and vanadium iron powder, ferrochrome powder, molybdenum-iron powder, ferro-boron powder is according to required chemical composition quality hundred
Divide than conversion, together with iron powder, nickel powder, copper powder, aquadag, CeO2Raw material presses bonding phase metal material chemical composition quality percentage
Than 70% proportions；
3）By the in-situ synthesizing TiC powder 25% needed for Steel-bonded Cemented Carbide, fabricated in situ TiN powder 5% and matrix material
70% three kinds of materials are mixed, and are fitted into ball milling bucket, load steel ball, ratio of grinding media to material 5:1, add absolute ethyl alcohol make medium and
0.6%PVA was as cooling agent and dispersant, using vibrations ball mill ball milling 55 hours；
4）Sieved after slurry is dried, the product of size shape needed for being then pressed under 400 MPa pressure；
5）Sinter under vacuum, sintering temperature is 1400 DEG C, sintering process is:10 DEG C/min of firing rate, reaches sintering
The heat preservation sintering of progress 2.5 hours, furnace cooling to room temperature after temperature, the high-toughness heat-resistant TiC/TiN steel of composition needed for obtaining
Bond hard alloy.
Embodiment 2
A kind of preparation method of high-toughness heat-resistant TiC/TiN steel bonded carbide, it uses following technical scheme：
(1) raw material：
Raw materials be TiH2 powder, vanadium iron powder, ferrochrome powder, molybdenum-iron powder, ferro-boron powder, iron powder, nickel powder, copper powder, aquadag,
CeO2、Y3O2Two kinds, PVA, powder size is at 10~50 μm；
(2) material is prepared：
1）Fabricated in situ TiN powder is prepared：TiH2 powder and urea ((NH2) 2CO) are prepared by N/ Ti atomic ratios for 0.6
Into fabricated in situ TiN mixed-powders；
2）In-situ synthesizing TiC powder is prepared：TiH2 powder and aquadag powder are carried out being configured to original by C/ Ti atomic ratios for 0.9
Position synthesis TiC powder；
3）Phase matrix alloy powder is bonded to prepare：Bonding phase metal material chemical composition mass percent is：C0.4%,
Cr5.0%, Mo2.5%, V1.0%, Si0.7%, Mn0.5%, B1.0%, Cu0.7%, Ni1.0%, S≤0.02, P≤0.02, CeO2、
Y3O2、La2O3Combination≤0.8% of one of them or more than two kinds, surplus Fe, and inevitable impurity element；
4）High-toughness heat-resistant TiC/TiN Steel-bonded Cemented Carbides are prepared：Material chemical composition mass percent is：Fabricated in situ
TiC powder 30%, fabricated in situ TiN powder 10%, bonding phase matrix alloy powder 60%；
(3) step of preparation process is：
1）TiN powder material is prepared：TiH2 powder and industrial urea ((NH2) 2CO) are prepared by N/ Ti atomic ratios for 0.6
Into fabricated in situ TiN mixed-powders；It is fitted into polyurethane ball milling bucket, loads stainless steel steel ball, ratio of grinding media to material 10:1~20:1, add
Absolute ethyl alcohol makees medium and dispersant, carries out sealing ball milling 48~72 hours using vibrations ball mill, is prepared into TiN powder；
2）Material is prepared：TiH2 powder and aquadag powder are configured into in-situ synthesizing TiC for 0.9 progress by C/ Ti atomic ratios to mix
Close powder；By the TiN powder prepared and vanadium iron powder, ferrochrome powder, molybdenum-iron powder, ferro-boron powder is according to required chemical composition quality hundred
Divide than conversion, together with iron powder, nickel powder, copper powder, aquadag, CeO2Raw material presses bonding phase metal material chemical composition quality percentage
Than 60% proportions；
3）By the in-situ synthesizing TiC powder 30% needed for Steel-bonded Cemented Carbide, fabricated in situ TiN powder 10% and matrix material
60% three kinds of materials are mixed, and are fitted into ball milling bucket, load steel ball, ratio of grinding media to material 5:1, add absolute ethyl alcohol make medium and
0.6%PVA was as cooling agent and dispersant, using vibrations ball mill ball milling 55 hours；
4）Sieved after slurry is dried, the product of size shape needed for being then pressed under 400 MPa pressure；
5）Sinter under vacuum, sintering temperature is 1400 DEG C, sintering process is:10 DEG C/min of firing rate, reaches sintering
The heat preservation sintering of progress 2.5 hours, furnace cooling to room temperature after temperature, the high-toughness heat-resistant TiC/TiN steel of composition needed for obtaining
Bond hard alloy.
Embodiment 3
A kind of preparation method of high-toughness heat-resistant TiC/TiN steel bonded carbide, it uses following technical scheme：
(1) raw material：
Raw materials be Ti powder, vanadium iron powder, ferrochrome powder, molybdenum-iron powder, ferro-boron powder, iron powder, nickel powder, copper powder, aquadag,
CeO2、Y3O2、La2O3, PVA, powder size is at 10~50 μm；
(2) material is prepared：
1）Fabricated in situ TiN powder is prepared：Ti powder and urea ((NH2) 2CO) are configured to by N/ Ti atomic ratios for 1.0
Fabricated in situ TiN mixed-powders；
2）In-situ synthesizing TiC powder is prepared：Ti powder and aquadag powder are carried out being configured to original position by C/ Ti atomic ratios for 1.1
Synthesize TiC powder；
3）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%, Si1.0%, Mn0.6%, B1.6%, Cu1.0%, Ni2.0%, S≤0.02, P≤0.02, CeO2,
One of Y3O2, La2O3 or more than two kinds of combination≤0.8%, surplus Fe, and inevitably impurity element；
4）High-toughness heat-resistant TiC/TiN Steel-bonded Cemented Carbides are prepared：Material chemical composition mass percent is：Fabricated in situ
TiC powder 35%, fabricated in situ TiN powder 15%, bonding phase matrix alloy powder 50%；
(3) step of preparation process is：
1）TiN powder material is prepared：Ti powder and industrial urea ((NH2) 2CO) are configured to by N/ Ti atomic ratios for 1.0
Fabricated in situ TiN mixed-powders；It is fitted into polyurethane ball milling bucket, loads stainless steel steel ball, ratio of grinding media to material 10:1~20:1, add nothing
Water-ethanol makees medium and dispersant, carries out sealing ball milling 48~72 hours using vibrations ball mill, is prepared into TiN powder；
2）Material is prepared：Ti powder and aquadag powder are carried out being configured to in-situ synthesizing TiC mixing by C/ Ti atomic ratios for 1.1
Powder；By the TiN powder prepared and vanadium iron powder, ferrochrome powder, molybdenum-iron powder, ferro-boron powder is according to required chemical composition quality percentage
Than conversion, together with iron powder, nickel powder, copper powder, aquadag, CeO2Raw material presses bonding phase metal material chemical composition mass percent
50% proportions；
3）By the in-situ synthesizing TiC powder 35% needed for Steel-bonded Cemented Carbide, fabricated in situ TiN powder 15% and matrix material
50% three kinds of materials are mixed, and are fitted into ball milling bucket, load steel ball, ratio of grinding media to material 5:1, add absolute ethyl alcohol make medium and
0.6%PVA was as cooling agent and dispersant, using vibrations ball mill ball milling 55 hours；
4）Sieved after slurry is dried, the product of size shape needed for being then pressed under 400 MPa pressure；
5）Sinter under vacuum, sintering temperature is 1400 DEG C, sintering process is:10 DEG C/min of firing rate, reaches sintering
The heat preservation sintering of progress 2.5 hours, furnace cooling to room temperature after temperature, the high-toughness heat-resistant TiC/TiN steel of composition needed for obtaining
Bond hard alloy.
Claims (2)
1. a kind of preparation method of high-toughness heat-resistant TiC/TiN steel bonded carbide, it is characterised in that including as follows：
(1) material is prepared：
1）Fabricated in situ TiN powder is prepared：By Ti02 powder, TiH2 powder or Ti powder is one kind of or three kinds and urea ((NH2)
It is 2CO) that 0.4~1.1 progress is configured to fabricated in situ TiN mixed-powders by N/ Ti atomic ratios；
2）In-situ synthesizing TiC powder is prepared：By Ti02 powder, TiH2 powder or Ti powder is one kind of or three kinds and aquadag powder are pressed
C/ Ti atomic ratios are that 0.7~1.1 progress is configured to in-situ synthesizing TiC powder；
3）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 inevitably impurity element；
4）High-toughness heat-resistant TiC/TiN Steel-bonded Cemented Carbides are prepared：Material chemical composition mass percent is：Fabricated in situ
TiC powder 25~40%, fabricated in situ TiN powder 5~20%, bonding phase matrix alloy powder 70~40%；
(2) step of preparation process is：
1）TiN powder material is prepared：By Ti02 powder, TiH2 powder or Ti powder is one kind of and industrial urea ((NH2) 2CO) presses N/
Ti atomic ratios are that 0.4~1.1 progress is configured to fabricated in situ TiN mixed-powders；It is fitted into polyurethane ball milling bucket, loads stainless steel
Steel ball, ratio of grinding media to material 10:1~20:1, add absolute ethyl alcohol and make medium and dispersant, sealing ball milling 48 is carried out using vibrations ball mill
~72 hours, it is prepared into TiN powder；
2）Material is prepared：By Ti02 powder, TiH2 powder or Ti powder is one kind of and aquadag powder by C/ Ti atomic ratios is 0.7
~1.1 carry out being configured to in-situ synthesizing TiC mixed-powder；By the TiN powder prepared and vanadium iron powder, ferrochrome powder, molybdenum-iron powder, boron
Iron powder converts according to required chemical composition mass percent, together with iron powder, nickel powder, copper powder, aquadag, CeO2、Y3O2、
La2O3The combination raw materials of one of them or more than two kinds are matched somebody with somebody in ratio needed for bonding phase metal material chemical composition mass percent
System；
3）Fabricated in situ Ti according to needed for Steel-bonded Cemented Carbide（CN）Mixed-powder and bonding phase matrix alloy powder
Ratio is mixed three kinds of materials, 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 to be situated between
Matter and 0.5~1%PVA add 10~20% industrial ureas or ammoniacal liquor as nitrogen source, using vibrations ball as cooling agent and dispersant
Grinding machine carries out sealing ball milling 48~72 hours；
4）Sieved after slurry is dried, the product of size shape needed for being then pressed under 350~500 MPa pressure；
5）Sinter under vacuum, sintering temperature is 1400 DEG C~1500 DEG C, sintering process is:10 DEG C/min of firing rate,
Reach the Isothermal sinter carried out after sintering temperature 2~5 hours, furnace cooling to room temperature, the high-toughness heat-resistant of composition needed for obtaining
TiC/TiN steel bonded carbide.
2. a kind of preparation method of high-toughness heat-resistant TiC/TiN steel bonded carbide according to claim 1, its feature exists
In：Raw materials are that Ti02 powder, TiH2 powder or Ti powder are one kind of or three kinds, vanadium iron powder, ferrochrome powder, molybdenum-iron powder, ferro-boron
Powder, iron powder, nickel powder, copper powder, aquadag, CeO2、Y3O2、La2O3One of them or three kinds, PVA, powder size is 10~50
μm。
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Application publication date: 20170818 |