CN106591664A - Preparation method of VC-VN matrix steel-based steel bond hard alloy - Google Patents
Preparation method of VC-VN matrix steel-based steel bond hard alloy Download PDFInfo
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Abstract
The invention relates to a preparation method of VC-VN matrix steel-based steel bond hard alloy. The preparation method includes the following steps that titanium carbide powder and matrix steel-based powder are weighed in proportion, alloy powder is put in a ball mill to be mixed and broken, absolute ethyl alcohol is added to serve as a process control agent, wet mixed powder is put in a vacuum drying box to be dried after ball milling is completed, and the dried mixed powder is put aside for use; organic monomers and an initiator are added into a solvent, and a premix solution is prepared; an additive for improving slurry fluidity and dispersity is added; a catalyst and a pH modifier are added, the materials are stirred to be uniform, and slurry is obtained; the slurry is injected into an injection setting mold for vacuumizing or vibrating degassing, after the slurry is cured and molded, a blank is put in the vacuum drying box to be dried, the dried blank is subjected to integrated degumming and sintering in a vacuum sintering furnace, and the steel bond hard alloy is prepared. On the basis of guaranteeing the macro-performance of the steel bond hard alloy, the advantages that the process is simple, cost is low, and large-size and complex-shape parts are easy to prepare are achieved.
Description
Technical field
The present invention relates to a kind of preparation method of VC-VN matrixes base steel steel bonded carbide, belongs to metal-base composites
Preparation field.
Background technology
Steel bonded carbide is a kind of composite with ceramic phase and with steel as bonding matrix, and its performance is between common hard
Between matter alloy and iron and steel, while having a series of other advantages so as to be widely used in many fields.In recent years,
To obtain some particular tissues and performance of steel bonded carbide, and alleviate due to conventional rigid alloy material Main Resources W, Co
Increasingly deficient the problems such as, steel bonded carbide is carried out both at home and abroad more extensively and in-depth study, particularly to addition not
With the research (such as addition A1203, TiN, NbC, TiCN, TiB2, Mo2FeB2, Mo2C, Cr3C2, VC, NV etc.) of New Rigid phase.
In recent years, some new hard phase steel-bonded carbides are continued to bring out.Mitsubishi metal company is relatively low but resistance to using TiCN hardness
The characteristics of mill property is very strong, high speed comminuted steel shot is mixed, is shaped, is dewaxed, with titanium carbonitride additive then by high temperature insostatic pressing (HIP), Re Chu
The TiCN base steel-bonded carbides that reason and method for fine finishing are produced, with the high spy of uniform microstructure, segregation-free, alloying level
Point.Rubbing action is little between TiN and ferrite, and antisticking ability is more higher than TiC, and free energy is less, oxidation resistance temperature scope
Greatly.Sandvik AB of Sweden has developed a kind of new steel-bonded carbide CORONlTE based on TiN.They adopt a kind of special work
Skill, the TiN powder of superfine (about 0.1 micron) is equably added in heat treatable steel matrix, and its volume content can be from
35% to 60%, because TiN powder is thin and performance and its stable, by this method obtained CORONITE alloys have hard concurrently
The wearability of alloy and the toughness of high-speed steel.
TiB2 has heat-resisting quantity good, and density and resistivity are little, and conductivity is good, and metal adhesiveness is low and friction factor
It is low, the features such as non-oxidizability is strong, it is considered to be a kind of preferable steel-bonded carbide hard phase.Because of the solid solubility between Fe and TiB2
Low, wettability is good, and Mo can also improve its wettability, therefore the advantage of synthesis TiB2 and Fe, Mo, has made TiB.FeMo composite woods each
Material.
Japanese certain company develops and a kind of does not contain W, Co but the boride-based composite KMH of the M02FeB2 types containing Cr.
Such polynary boride-based alloy be prepared using water atomization Fe-Cr-B alloy powders, boride powder and Fe, Cr, Mo,
The metal dusts such as Ni make raw material, Jing wet grindings mixing, the manufacture of compressing and vacuum-sintering method.
In addition to above-mentioned new steel bonded carbide, Japanese some companies also utilize a variety of hard compounds (such as
TiC, VC, Cr3C2, SiC, ZrC, AlN etc.) and its mixing cpd make hard phase, make binding agent with various steel or ferrous alloy,
Develop some advanced composite material (ACM)s.
Meanwhile, people also in the combination for constantly seeking new hard phase and new Binder Phase, have most preferably to develop
The MC type particulate reinforced composites of tissue and performance.In steel-bonded carbide, the hard particulate carbide species as wear-resistant phase
Comparison is more, there is the ceramic particles such as WC, TiC, Cr7C3, NbC, VC, SiC and alloy carbide and cementite.MC type carbides
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 is poor with Fe intermiscibilities.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 is bad with Fe intermiscibilities, is easily dissolved in Fe during high temperature, and high high-temp stability, calorific intensity are poor,
Separate out in cooling procedure so as to form bridge joint, deteriorate the mechanical performance of alloy；As carbide V element, with
Ti elements are similar to, and V is also a kind of very active alloying element, first with C, N etc. to have very strong affinity.The parent of V element and C
With power more than Cr elements and the affinity of C, two kinds of stable carbides of VC and V2C are easily formed.In carbide ceramics, VC's is hard
Degree highest, and have good heat stability, it is that a kind of preferable hard strengthens phase.
VC is extremely stable, is generally distributed in alloy substrate with tiny graininess, one side crystal grain thinning, improves matrix
The intensity and wearability of alloy；On the other hand, the creep rupture strength and the drag to creep of matrix are increased.The microhardness of VC
It is very high, more than 2800MPa is reached, it is a kind of wear-resistant phase of preferable alloy carbide.Hard is tied by the Novel steel for strengthening phase of VC
Alloy, VC and Fe has extraordinary intermiscibility, and the two joint interface is good, and high high-temp stability, red hardness are good, is TiC, WC
Reinforcement is substituted well.Also between TiC and WC, vanadium can shape in Hi-Stren steel for the fusing point and thermal coefficient of expansion of VC
Precipitate into tiny vanadium carbide and effectively facilitate the crystal grain refinement of steel and strengthen；Vanadium carbide phase energy pinning dislocation and crystal boundary, hinder position
Wrong and crystal boundary migration, improves the intensity of steel；The simultaneously presence of vanadium carbide phase can also improve the recrystallization temperature of material and high temperatures
Energy.Existing research shows：Adding vanadium carbide in steel can also improve wearability, corrosion resistance, toughness, ductility and the hardness of steel
And the comprehensive mechanical performance such as thermal fatigue resistance, and make steel that there is good solderability, and play elimination field trash and extend etc. and make
With.Therefore, vanadium carbide is used widely in steel.
Meanwhile, this novel hard alloy it is alternative traditional in industries such as automobile, metallurgy, mine, building materials and moulds
High-abrasive material, increases substantially parts service life, economizes on resources, with good economic results in society.Additionally, with work
Wilderness demand and inevitably artificially waste that industry is produced, China or even worldwide W, Co resource are quite lean
Weary, price rises steadily, and each national capital Efforts To Develop seeks the research and development of the substitute material of W, Co.And China V ore resources are abundant,
Replace W that there is very high feasibility in resource with V.Therefore, VC bases steel bonded carbide either engineer applied is researched and developed
Aspect, or be all significant in terms of Technological Economy.
VN is a kind of new microalloying additive, with outstanding alloying performance.V element in vanadium nitride
Work with the carbon and nitrogen in steel, generate hard metal carbides and nitride molecule.These compounds are played in steel
The effect of crystal grain thinning and precipitation hardening, can optimize the performance of steel, can obviously improve the tissue of V-bearing microalloyed steel, carry
The intensity of Gao Gang, toughness and wearability, corrosion resistance and thermal fatigue resistance, and enable steel to possess excellent weldability.
Alloy of vanadium nitride additive is more beneficial for the precipitation of vanadium carbide in steel, vanadium nitride, so as to more effectively strengthen and crystal grain thinning.With
Compared using vanadium iron, alloy of vanadium nitride additive improves the service efficiency of vanadium, allow steel manufacturing enterprise save 20%～
40% vanadium consumption, makes steel user save 10%～15% rolled steel dosage.
The method for preparing this kind of material at present is mainly powder metallurgy process, including compressing, cold isostatic compaction, note
Shaping etc. is penetrated, vacuum-sintering is subsequently carried out as final shaping.Larger part is prepared using compressing and cold isostatic compaction
Required larger pressure and it is helpless, the parts for preparing complicated shape are more difficult, simultaneously for prepare ceramic crystalline grain size compared with
When little and content higher composite, shape more difficult and crystal grain and easily grow up；Produce this kind of using ejection forming method
The little parts of material, but this kind of method is not suitable for the preparation of the parts of large-size, while adulterate in this kind of technique
Colloid is more, and usually time is longer, while the consistency of blank of material is relatively low, is unfavorable for quickly carrying out producing and consistency is carried
It is high；Also such material is prepared using Self- propagating Sintering Synthetic reaction method, but the material for preparing often has relatively low densification
Degree.Some are using HIP sintering etc. as final sintering process, but cost intensive.
The content of the invention
The present invention be directed to existing steel bonded carbide exists in terms of shaping and sintering is difficult to quick, economic preparation
The difficulty of the aspects such as crystallite dimension is less and content is higher, large-size, complicated shape part, there is provided one kind prepare large scale,
Complicated shape and simple production process, the preparation method of lower-cost VC-VN matrixes base steel steel bonded carbide.
The present invention provides a kind of preparation method of VC-VN matrixes base steel steel bonded carbide, including procedure below：
（1）Proportionally weigh 20～50% to be carbonized vanadium powders, 2～10% nitridation vanadium powders and 28～58% matrix steel matrix powders, 0.03
～0.3% Ce, 0.05～0.3% Nb, 0.1～0.8% SiMgRe, 0.2～0.6% graphite powder, 5～10% carbonyl iron dusts,
The powder and rare earth, Nb powder are put in ball mill and are mixed and crushed, wherein addition dehydrated alcohol is process control
Agent, mixed powder is put in vacuum drying oven and is dried, standby after being dried；
（2）Organic monomer and initiator are added in solvent and prepare premixed liquid；
（3）Dry mixed powder is added in premixed liquid and is stirred, percentage by volume is added in whipping process for slurry
The Oleic acid of the 1～3% of material, to improve slurry fluidity and dispersibility；
（4）Add catalyst and pH adjusting agent and stir, obtain slurry；Slurry is injected into mould and with evacuation or vibrations
Method bubble removing, slurry curing shaping, the demoulding after the reaction regular hour obtains final product base substrate；
（5）Base substrate is put in vacuum drying oven and is dried, dried base substrate is carried out into degumming and final sintering；
First, described matrix steel matrix includes 6Cr4W3Mo2VNb, 6W6Mo5Cr4V, 7Cr7Mo3V2Si, 7Cr7Mo2V2Si2
One of plant；
Second, described organic monomer is 2-(Acryloyloxy)ethanol, solvent is toluene, initiator is benzoyl peroxide；Wherein have
The volume ratio of machine monomer and solvent is 1：2～2：1, the content of initiator is 0.6～1.5 g in every 100 ml premixed liquids；
3rd, mixed powder percentage by volume in the slurry is 40～60%；
4th, initiator used is dimethylaniline, and it is 0.1～0.2% that addition accounts for the percentage ratio of slurry volume；
5th, pH adjusting agent used is ammonia, and it is 7～8 to adjust pH value；
6th, degumming carries out integral sintering with sintering using vacuum sintering furnace, and technique is：Base substrate is incubated 1 at 400～500 DEG C
～3 h carry out degumming, are incubated 1～2h at 1400～1450 DEG C and are finally sintered.
Beneficial effect
Beneficial effects of the present invention are：
1st, the invention allows to quick, economic preparation crystallite dimension is less, large-size, the part of complicated shape.
2nd, Gelcasting Technique be in low viscosity, the powder body-solvent concentrate suspension of high solid volume fraction, plus
Enter organic monomer, then make the organic monomer in suspended substance be chemically crosslinked polymerization or physics in the presence of catalyst and initiator
Tridimensional network is cross-linked into, so that suspended substance in-situ solidifying molding, finally discharges in colloid a small amount of in base substrate, then is carried out
Sintering obtains compact components.Gel casting can reduce the quantity of gross blow hole in base substrate, and pore-size distribution is more uniform, improves
The uniformity of base substrate；Gel casting cycle is short, the structure and even density of product are not in the segregation of granule, material
It is stable and reliable for performance.Additionally, gel casting to mould without specific requirement, it is considered to be improve reliability of material, prepare
One of large scale, most effectual way of complicated form part.Because gel casting can efficiently control the reunion of granule, system
For the base substrate for going out structure and even density, so as to obtain high performance sintered body, the use reliability of material is improved.It is simultaneously solidifying
Restriction of the glue casting to ceramic crystalline grain size and content is less so as to which use range is wider.During gel casting
Can also by controlling the parameter of each additive, and then control solidification time and body crack defects etc., so as to meet prepare it is different
The demand of parts.Low pressure sintering process can promote the mobility of liquid phase in liquid sintering process, can shorten sintering time, have
Beneficial to the uniformity and compactness of tissue, moreover it is possible to ceramic phase and binder alloy boundary strength are improved, so as to improve the performance of material.
3rd, the present invention mutually manufactures new steel bonded carbide with VC to strengthen, and VC and Fe has an extraordinary intermiscibility, and two
Person's joint interface is good, and high high-temp stability, red hardness are good, in carbide ceramics, the hardness highest of VC, and have well
Heat stability, is that a kind of preferable hard strengthens phase, is that TiC, WC substitute well reinforcement.Vanadium carbide mutually can pinning dislocation with
Crystal boundary, hinders dislocation and crystal boundary migration, improves the intensity of steel；The presence of vanadium carbide phase simultaneously can also improve the recrystallization temperature of material
Degree and high-temperature behavior.Doing hard phase using vanadium carbide can also improve wearability, corrosion resistance, toughness, ductility and the hardness of steel
And the comprehensive mechanical performance such as thermal fatigue resistance, and make steel that there is good solderability, and play elimination field trash and extend etc. and make
With.Can be widely applied to the adverse circumstances of heavy duty, high speed, dry sliding friction or high temperature and high speed friction.
4th, to prevent serious adhesive wear, more preferably self-lubricating effect is obtained, the present invention is by steel bonded carbide
The middle graphite for adding certain content, makes in materials microstructure containing the micro- graphite-phase of many self-lubricatings, makes the friction of hard alloy
Coefficient is greatly improved, so that friction factor is reduced.
5th, in order to adjust the granularmetric composition of compound, improve suppression performance, greatly improve shaping density, the present invention
Add a certain proportion of carbonyl iron dust in reduced iron powder.Substituting reduced iron powder with carbonyl iron dust can improve powder forming
Can, make green density higher, acceleration of sintering process reduces sintering temperature.The steel knot of the present invention is made by adding carbonyl iron dust
The mechanics of hard alloy is significantly improved, and hardness brings up to 81.8HRA by 77.5HRA, bending strength by 1123MPa or to
1447MPa。
6th, the present invention can more effectively be strengthened and crystal grain thinning by adding VN, and the performance of optimized alloy can substantially change
The tissue of kind steel bonded carbide, carries heavy alloyed intensity, toughness and wearability, corrosion resistance and thermal fatigue resistance, and makes
Steel possess excellent weldability energy.20%～40% vanadium consumption can be saved, makes steel user save 10%～15% steel
Timber-used amount.
7th, the present invention is by adding Ce, SiMgRe, and makes Ce, SiMgRe powder content between 0.2% and 0.5%, can rise
To rare earth reinforced effect.Because Ce, SiMgRe chemical property is active, in ball milling and sintering process, RE has to alloy powder
Significantly deoxidation and carbon effect is protected, contribute to improving for wettability between different constituent elements, so as to be conducive to densification process,
Reach the purpose for reducing porosity so that the porosity in steel bonded carbide is reduced, and the reduction of porosity will be helped
In the raising of plasticity and bending strength.At a sintering temperature, rare earth is gathered in TiC particle surfaces so as to which surface energy is reduced, and hinders
TiC crystallization of the dissolution and precipitation processes in the liquid phase, suppress growing up for TiC crystal grain；Simultaneously Ce, SiMgRe can be with metal dust interfaces
On impurity and oxide-film effect, play a part of to purify interface, S, P, Sb can be suppressed in the segregation of crystal boundary, play deoxidation, de-
Sulfur, crystal grain thinning and improve Liquid phase flowability and wettability etc. effect.So as to improve the performance of alloy material.
And because SiMgRe may also operate as in the alloy inoculation(effect), make the alloying pellet in matrix material obtain ball
Shape, so as to improve the toughness of Steel-bonded Cemented Carbide.Therefore intensity, the toughness of the steel bonded carbide of the present invention
It is improved with consistency, bending strength can reach more than 1700MPa, consistency reaches more than 97.4%.
The present invention is by adding Ce, Nb, SiMgRe, it is suppressed that crystal grain is grown up, and plays a part of dispersion-strengtherning.
Specific embodiment
Embodiment 1：Weighing mass fraction is 50% VC powder, 2%VN powder and 0.10% Ce, 0.05% Nb, 0.1%
SiMgRe, 6Cr4W3Mo2VNb matrix steel matrix material powder, the powder and rare earth, Nb are put in ball mill mixed and
It is broken, wherein addition dehydrated alcohol is process control agent, wet mixed powder is put in vacuum drying oven and is dried, it is dried standby
With；According to volume ratio 1：1 measures organic monomer 2-(Acryloyloxy)ethanol and solvent toluene prepares premixed liquid, adds in premixed liquid
The benzoyl peroxide of 1.2 g/100 ml simultaneously stirs；Dry mixed powder is added in premixed liquid, while Deca 2%
Oleic acid and stir, formed slurry；Add 0.15% dimethylaniline in slurry and add ammonia and adjust PH for 7；With
Vacuumizing method removes that base substrate is put in vacuum sintering furnace after bubble carries out degumming and final sintering, and technique is：In 500 DEG C of guarantors
2 h of temperature carry out degumming, are incubated 2h at 1450 DEG C and are finally sintered；Last furnace cooling obtains steel bonded carbide part.
Embodiment 2：Weighing mass fraction is 60% VC powder, 5%VN powder and 0.2% Ce, 0.2% Nb, 0.25%
SiMgRe, 0.3% graphite powder, 5% carbonyl iron dust, 6W6Mo5Cr4V matrix steel matrix material powder, by the powder and rare earth, Nb
Powder is put in ball mill and is mixed and crushed, wherein addition dehydrated alcohol is process control agent, wet mixed powder is put into very
It is dried in empty drying baker, it is standby after being dried；According to volume ratio 1：2 measure organic monomer 2-(Acryloyloxy)ethanol and solvent toluene
Premixed liquid is prepared, the benzoyl peroxide of 0.6 g/100 ml is added in premixed liquid and is stirred；By dry mixed powder
In being added to premixed liquid, while the Oleic acid of Deca 1% and stirring, slurry is formed；The dimethyl benzene of addition 0.1% in slurry
Amine and add ammonia adjust PH be 7.5；Removed that base substrate is put in vacuum low-pressure sintering furnace after bubble with vacuumizing method and taken off
Glue is sintered with final, and technique is：Being incubated 1 h at 500 DEG C carries out degumming, is incubated 2h at 1400 DEG C and is finally sintered；Finally
Furnace cooling obtains the part of steel bonded carbide.
Embodiment 3：Weighing mass fraction is 40% VC powder, 8%VN powder and 0.25% Ce, 0.25% Nb, 0.3%
SiMgRe, 0.4% graphite powder, 8% carbonyl iron dust, 7Cr7Mo3V2Si matrix steel matrix material powder, by the powder and rare earth,
Nb powder is put in ball mill and is mixed and crushed, wherein addition dehydrated alcohol is process control agent, wet mixed powder is put into
It is dried in vacuum drying oven, it is standby after being dried；According to volume ratio 2：1 measures organic monomer 2-(Acryloyloxy)ethanol and solvent first
Benzene prepares premixed liquid, the benzoyl peroxide of 1.5 g/100 ml is added in premixed liquid and is stirred；By dry mixing
Powder is added in premixed liquid, while the Oleic acid of Deca 3% and stirring, forms slurry；The dimethyl of addition 0.2% in slurry
Aniline and add ammonia adjust PH be 8；Removed that base substrate is put in vacuum low-pressure sintering furnace after bubble with vacuumizing method and taken off
Glue is sintered with final, and technique is：Being incubated 3h at 400 DEG C carries out degumming, is incubated 1h at 1450 DEG C and is finally sintered；It is last with
Stove cooling obtains the part of steel bonded carbide.
Embodiment 4：Weighing mass fraction is 30% VC powder, 10%VN powder and 0.3% Ce, 0.3% Nb, 0.5%
SiMgRe, 0.6% graphite powder, 10% carbonyl iron dust, 7Cr7Mo2V2Si2 matrix steel matrix material powder, by the powder and dilute
Soil, Nb powder are put in ball mill and are mixed and crushed, wherein addition dehydrated alcohol is process control agent, wet mixed powder are put
Enter in vacuum drying oven and be dried, it is standby after being dried；According to volume ratio 2：1 measures organic monomer 2-(Acryloyloxy)ethanol and solvent
Toluene prepares premixed liquid, the benzoyl peroxide of 1.5 g/100 ml is added in premixed liquid and is stirred；Dry is mixed
Close powder to be added in premixed liquid, while the Oleic acid of Deca 3% and stirring, form slurry；The diformazan of addition 0.2% in slurry
Base aniline and add ammonia adjust PH be 8；Being removed that base substrate is put in vacuum low-pressure sintering furnace after bubble with vacuumizing method is carried out
Degumming is sintered with final, and technique is：Being incubated 3h at 400 DEG C carries out degumming, is incubated 1h at 1450 DEG C and is finally sintered；Finally
Furnace cooling obtains the part of steel bonded carbide.
Claims (7)
1. a kind of preparation method of VC-VN matrixes base steel steel bonded carbide, it is characterised in that comprise the steps：
Proportionally weigh 20～50% to be carbonized vanadium powders, 2～10% nitridation vanadium powders and 28～58% matrix steel matrix powders, 0.03～
0.3% Ce, 0.05～0.3% Nb, 0.1～0.8% SiMgRe, 0.2～0.6% graphite powder, 5～10% carbonyl iron dusts will
The powder and rare earth, Nb powder are put in ball mill and are mixed and crushed, wherein addition dehydrated alcohol is process control agent,
Mixed powder is put in vacuum drying oven and is dried, it is standby after being dried；
Organic monomer and initiator are added in solvent and prepare premixed liquid；
Dry mixed powder is added in premixed liquid and is stirred, percentage by volume is added in whipping process for slurry
1～3% Oleic acid, to improve slurry fluidity and dispersibility；
Add catalyst and pH adjusting agent and stir, obtain slurry；By the solidifying mould of slurry injection note and with evacuation or shake
Dynamic method bubble removing, slurry curing shaping, the demoulding after the reaction regular hour obtains final product base substrate；
Base substrate is put in vacuum drying oven and is dried, dried base substrate is carried out into degumming and final sintering.
2. preparation method according to claim 1, it is characterised in that described matrix steel matrix include 6Cr4W3Mo2VNb,
One of 6W6Mo5Cr4V, 7Cr7Mo3V2Si, 7Cr7Mo2V2Si2 are planted.
3. preparation method according to claim 1, it is characterised in that described organic monomer is 2-(Acryloyloxy)ethanol, solvent
It is benzoyl peroxide for toluene, initiator；Wherein the volume ratio of organic monomer and solvent is 1：2～2：1, every 100 ml premixs
The content of initiator is 0.6～1.5 g in liquid.
4. preparation method according to claim 1, it is characterised in that mixed powder percentage by volume in the slurry is 40～
60%。
5. preparation method according to claim 1, it is characterised in that initiator used is dimethylaniline, addition accounts for slurry
The percentage ratio of material volume is 0.1～0.2%.
6. preparation method according to claim 1, it is characterised in that pH adjusting agent used is ammonia, adjust pH value be 7～
8。
7. preparation method according to claim 1, it is characterised in that degumming and sintering carry out one using vacuum sintering furnace
Change sintering, technique is：Base substrate is incubated 1～3 h and carries out degumming at 500 DEG C, and being incubated 1～2h at 1400～1450 DEG C is carried out finally
Sintering.
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