CN105714170A - Hard alloy and preparation method thereof - Google Patents
Hard alloy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a hard alloy and a preparation method thereof. A alloy structure contains an alpha phase, a beta phase and a gamma phase; the alpha phase is WC grains; the beta phase is a (Ti, W, TA)C phase; the gamma phase is Co(Ni, Cr) phase; the average grain size of the alpha phase is 2.0-4.0 [mu]m; the average grain size of the beta phase is 0.5-1.5 [mu]m, and the quantity of beta-phase grains accounts for about 10%-40% of the total quantity of alpha-phase grains and beta-phase grains. The hard alloy finished product with relatively excellent comprehensive performance is obtained. The alloy material has the characteristics of high-temperature resistance, wear resistance, cracking resistance, steel sticking resistance and plastic deformation resistant ability while good strength and toughness properties are ensured.
Description
Technical field
The present invention relates to the novel hard alloy collars material of a kind of hard alloy, particularly a kind of steel rolling, the preparation method that present invention additionally comprises above-mentioned hard alloy.
Background technology
Rolling field at iron and steel, particularly during high-speed wire rolling, carbide roll ring is important consumption spare part, has just become the standard fitting of high-speed wire mill from the 60 to 70's of last century.
Along with the progress of steel rolling technology, rolling shapes get more and more, and the demand of difficult steel rolling kind is increasing, and the requirement of product quality is also more and more higher, and common carbide roll ring material increasingly can not meet instructions for use.Particularly at rolling high-carbon steel, steel alloy etc. is high-strength, high rigidity special steel grade time, roll-force is big, both pick by force, common WC-Co, WC-Co-Ni-Cr material collars is easy to crack, and quick abrasion, life-span are low, increasingly can not meet requirement and the expectation of user.
In recent years, for market to existing collars product existing problems when rolling special steel, this has all been carried out studying energetically by each collars manufacturer, develops some plastics on new materials collars, achieves certain effect, but still suffers from the problem such as cost of material height and technology controlling and process difficulty.
Publication number is the patent " a kind of tungsten carbide roll collar formula " of CN101994051A, adopt low binding agent (2～5wt.%), add TiC (0.2～0.3wt.%), CrC (0.2～0.3wt.%), the method of VC (0.05～0.3wt.%), Y (0.05～0.1wt.%) improves wearability and crack resistance.
Publication number is that to adopt Co+Ni be binding agent for the patent material formula of cold-heading steel carbide roll ring " rolling " of CN102051514A; content 10～20wt.%; Co/Ni=5/5～6/4, twin crystal grain or multiple grain tissue are (WC particle size range by weight: 40～60%3～6 μm；20～30%6～9 μm；20～30%9～25 μm) improve shock resistance and wearability.
The patent " preparation method of WC-Co-Ni-Al-B hard alloy, the collars made with this hard alloy and this collars " that publication number is CN102433488A adopts Co/Ni=6/4～4/6, binding agent total amount is 6～26wt.%, without Cr, WC grain is not less than 4 μm, add that Binder Phase is precipitated by Al, B, dispersion-strengtherning to be to improve crack resistance；CN101648213 " carbide roll ring of finished frame and preparation method thereof " adopts yellow tungsten high temperature reduction, and the method for air current classifying high temperature cabonization again prepares super coarse crystal WC powder raw material, then adopts the method that super coarse-grain hard alloy prepared by this raw material to improve crack resistance.
It is known that, in WC-Co hard alloy, add the high-melting-point carbides such as TiC, TaC, be conducive to improving the high-temperature behavior of alloy and chemical stability, but, numerous TiC of practice have shown that, TaC interpolation can significantly reduce the obdurability of alloy, therefore, the addition of general TiC, TaC etc. not can exceed that 0.3wt.%.For special steel rolling carbide roll ring, the mechanical behavior under high temperature of material and chemical stability are very important, add TiC, TaC etc. on a small quantity, the improvement of collars high-temperature behavior is limited, use expectation can not be met, under the premise significantly reducing obdurability, to significantly improve high-temperature behavior and the chemical stability of collars, be still technological difficulties.
Summary of the invention
Present invention aim at: be the deficiency for prior art existence and difficult point, there is provided a kind of hard alloy and preparation method thereof, the feature that this alloy material has high temperature resistant, wear-resisting, cracking resistance, resisting viscosity steel while ensureing good obdurability, plasticity_resistant deformation ability is good.
1, the hard alloy of the present invention, containing α phase, β phase, γ phase three-phase in alloy structure, described α phase is WC grain；Described β phase is (Ti, W, Ta) C phase；Described γ phase is Co (Ni, Cr) phase, and described α phase average grain size is 2.0～4.0 μm, and described β phase average grain size is 0.5～1.5 μm, and described β phase crystal grain quantity accounts for the 10%～40% of α phase and two kinds of crystal grain total quantitys of β phase.Above-mentioned α phase average grain size is preferably 2.4～4.0 μm；β phase average grain size is preferably 0.8～1.0 μm, and described β phase crystal grain quantity accounts for α phase and two kinds of crystal grain total quantitys of β phase are preferably 13%～36%.
The alloy structure of the present invention is designed to three-phase twin crystal structure.Co+Ni+Cr is adopted to make binding metal γ phase, with WC grain (α phase) and (Ti, W, Ta) C solid solution phase (β phase) is as hard phase, and WC grain (α phase) thick in three-phase structure is conducive to increasing the mean free path of Binder Phase, improve alloy obdurability, and fine grain β phase has good stability at elevated temperature, the effect of dispersion-strengtherning Binder Phase can be played again simultaneously, improve alloy rigidity and plasticity_resistant deformation ability.Therefore so that alloy is while keeping high intensity and good impact resistance, and its high rigidity, high temperature resistant, excellent chemical stability also significantly improve, thus realizing its purpose.
Moreover, the hard alloy of the present invention each element wt component is as follows: W:Co:Ni:Ti:Ta:Cr:C: impurity=(62-86): (6.9-30.1): (0.7-1.73): (0.4-1.1): (0.05-0.21): (0.03-0.11): (4.13-5.6): (0.53-0.96)
The preparation method that present invention additionally comprises above-mentioned alloy, its dispensing and ball milling operation press following technology controlling and process:
Described burden process presses following composition by weight preparation raw material
WC, 54.3～84.7, Fisher particle size 20.0-30.0 μm (being preferably 22.0-28.0)；Joining carbon content is 6.12wt.%～6.16wt.% (being preferably 6.12wt.%～6.15wt.%)；
Co, 7.3～30.7；
βPPowder, 8～15；
Described βPPowder is made up of following components by weight percent:
Ni:8.5
TiC:7, Fisher particle size is less than or equal to 2.5 μm (being preferably less than equal to 2.0 μm)；
TaC:1
Cr:0.5
WC:83, Fisher particle size is less than or equal to 0.8 μm (being preferably less than equal to 0.6 μm)；
The technique of described ball milling operation is: βPPowder is first wet grinding in advance 12～18 hours in ball grinding cylinder, then super coarse-grained WC with Fisher particle size 20.0-30.0 μm, Co wet grinding 16～24 hours in ball grinding cylinder in the lump.
Existing ball-milling technology is all the Ginding process adopting the disposable input of raw material, and the present invention, in order to obtain the hard phase of different grain size, at burden process, have chosen extra-coarse grained WC and the β containing fine grain WC, TiC respectivelyPPowder, then it is aided with the method that segmentation is ground, the raw material ball time consuming forming aplitic texture in hard phase is about 28-42 hour, and the raw material ball time consuming forming coarse structure in hard phase is 16～24 hours.
The super thick WC powder of the present invention, it joins carbon content is 6.10wt.%～6.16wt.% (preferred 6.12wt.%～6.15wt.%), average FSSS granularity is not less than 20 μm, it is preferable that be not less than 22 μm, to obtain the α phase that mean grain size is 2.4～4.0 μm.Because the growth of α phase and the alloying behaviour in Binder Phase such as Ti, Ta have appreciable impact in the mixed carbon comtent alloy sintering process of WC, during mixed carbon comtent too low (lower than 6.10wt.%), the alloy α skew obtained after sintering is thin, and shock resistance reduces.Ti, Ta etc. will dissolve in entrance Binder Phase in a large number, it is impossible to form tiny β phase.
Required alloy designations compound is prepared into by above-mentioned operation, then through conventional powder metallurgical operations such as compressing, sintering, the hart metal product obtained, with conventional rigid alloy phase ratio, when Binder Phase content is identical, there is higher hardness, better more resistant to high temperature, chemical stability and plasticity_resistant deformation ability, the advantages such as longer service life, are more suitable for rolling high rigidity, high strength steel.
Accompanying drawing explanation
Fig. 1 is embodiment 3 alloy microscopic structure × 1500 metallographs, and wherein thick polygon Lycoperdon polymorphum Vitt crystal grain is α phase, and tiny subcircular black particle is β phase, and white tissues is γ phase.
Fig. 2 is microscopic structure × 1500 metallograph of comparative example 3-0 alloy, and wherein irregular polygon Lycoperdon polymorphum Vitt crystal grain is α phase, and the granule that subcircular contains black core is β phase, and white tissues is γ phase.
Fig. 3 is microscopic structure × 1500 metallograph of comparative example 3-2 alloy, wherein irregular polygon Lycoperdon polymorphum Vitt crystal grain is α phase, white tissues is γ phase, in this example, owing to mixed carbon comtent is on the low side, all dissolve entrance γ phase containing Ti phase and be almost wholly absent, only remain the thick phase granule containing Ti (in figure black particle).
Fig. 4 is embodiment 1～5 and comparative example 1～5 alloy high-temp hardness (HV30) comparison diagram
Fig. 5 is embodiment 1～5 and comparative example 1～5 Alloy Anti impact flexibility (Ak) comparison diagram
Fig. 6 is embodiment 1～5 and comparative example 1～5 alloy bending strength (TRS) comparison diagram
Detailed description of the invention
All features disclosed in this specification, or the step in disclosed all methods or process, except mutually exclusive feature and/or step, all can combine by any way.This specification (include any accessory claim, summary and accompanying drawing) disclosed in any feature, unless specifically stated otherwise, all can by other equivalences or there is the alternative features of similar purpose replaced.That is, unless specifically stated otherwise, each feature is an example in a series of equivalence or similar characteristics.
The present invention prepares βPThe technique of powder is as follows:
Commercial production standard material powder WC1, TiC, TaC, Ni, Cr will be met, carry out proportioning by table 1 components by weight percent, mixing, it is thus achieved that required βPPowder, stand-by.
Wherein TiC powder, average Fisher particle size 2.0 μm.WC1 powder, average Fisher particle size 0.6 μm.In order to obtain compact grained β phase, TiC powder and WC1 powder, granularity is more thin more good, in order to realize the purpose of the present invention, and TiC: Fisher particle size should be less than being equal to 2.5 μm；WC, Fisher particle size is less than or equal to 0.8 μm.
| Project | WC1 | TiC | TaC | Ni | Cr |
| βPPowder | 83.0 | 7.0 | 1.0 | 8.5 | 0.5 |
Table 1
Embodiment 1:
The preparation method of a kind of hard alloy, comprises the steps:
1, dispensing: by the composition by weight in table 2 embodiment 1 and technological parameter preparation raw material powder WC2, Co, βPPowder.
2, ball milling, by the β of said ratioPPowder adds WC2, Co wet grinding 24 hours after adding ball grinding cylinder wet grinding 18 hours；And add the forming agent paraffin of 1.5wt%.
3, dry, compound slip complete for wet grinding is dried, obtains compound powder；
4, compressing, adopt conventional mould pressing process molding；
5, sintering, conventional low voltage sintering process, be specifically shown in table 3.Obtain alloy product.
Embodiment 2:
The preparation method of a kind of hard alloy, except step 1, except 2,5, all the other are with embodiment 1.
1, dispensing: by the composition by weight in table 2 embodiment 2 and technological parameter preparation raw material powder WC2, Co, β P powder.
2, ball milling, by the β of said ratioPPowder adds WC2, Co wet grinding 22 hours after adding ball grinding cylinder wet grinding 16 hours；And add the forming agent paraffin of 1.8wt%.
5, sintering, conventional low voltage sintering process, be specifically shown in table 3.Obtain alloy product.
Embodiment 3:
The preparation method of a kind of hard alloy, except step 1, except 2,5, all the other are with embodiment 1.
1, dispensing: by the composition by weight in table 2 embodiment 3 and technological parameter preparation raw material powder WC2, Co, β P powder.
2, ball milling, by the β of said ratioPPowder adds WC2, Co wet grinding 20 hours after adding ball grinding cylinder wet grinding 16 hours；And add the forming agent paraffin of 1.8wt%.
5, sintering, conventional low voltage sintering process, be specifically shown in table 3.Obtain alloy product.
Embodiment 4:
The preparation method of a kind of hard alloy, except step 1, except 2,5, all the other are with embodiment 1.
1, dispensing: by the composition by weight in table 2 embodiment 4 and technological parameter preparation raw material powder WC2, Co, βPPowder.
2, ball milling, by the β of said ratioPPowder adds WC2, Co wet grinding 18 hours after adding ball grinding cylinder wet grinding 14 hours；And add the forming agent paraffin of 1.8wt%.
5, sintering, conventional low voltage sintering process, be specifically shown in table 3.Obtain alloy product.
Embodiment 5:
The preparation method of a kind of hard alloy, except step 1, except 2,5, all the other are with embodiment 1.
1, dispensing: by the composition by weight in table 2 embodiment 2 and technological parameter preparation raw material powder WC2, Co, βPPowder.
2, ball milling, by the β of said ratioPPowder adds WC2, Co wet grinding 16 hours after adding ball grinding cylinder wet grinding 12 hours；And add the forming agent paraffin of 2.0wt%.
5, sintering, conventional low voltage sintering process, be specifically shown in table 3.Obtain alloy product.
In order to obtain contrast test data, the WC-Co-Ni-Cr hard alloy according to existing collars, be produced in conventional fashion comparative example alloy 1,2,3-5,4,5.The Binder Phase content of above-mentioned comparative example respectively with embodiment 1,2,3,4 and 5 identical, be specifically shown in table 2.Its tungsten carbide is the coarse granule tungsten carbide of conventional single grain size.All the other ball millings, dry, pressing process, sintering process employing common process.
In order to obtain contrast test data, being also prepared for comparative example 3-0,3-1,3-2,3-3,3-4, its proportioning is in Table 2.
In comparative example 3-0 preparation method, except ball-milling technology, all the other are with embodiment 3.Its ball-milling technology is the conventional ball-milling process adopting " the disposable input of raw material ", and by table 4 and Fig. 2 it can be seen that this alloy has three-phase contexture, but not in twin crystal Granularity Structure, the mean grain size of α phase and β phase is without significant difference.
In comparative example 3-1 preparation method, except WC2FSSS granularity, all the other are with embodiment 3.It adopts the WC2 raw material of FSSS granularity little (20.1 μm).From correction data it can be seen that the granularity alloy performance of WC2 has impact.FSSS granularity should be not less than 20 μm, it is preferable that is not less than 22 μm.
Comparative example 3-2,3-3,3-4 are respectively adopted the super thick WC2 raw material that total carbon content is 6.08wt.%, 6.10wt.%, 6.12wt.%, and all the other are with embodiment 3.From correction data it can be seen that the mixed carbon comtent alloy performance of WC2 has impact.When carbon amounts is relatively low, such as comparative example 3-2, will be unable to form tiny β phase.
The alloy sample prepared by embodiment of the present invention 1-5 adopts X-ray diffraction analysis, all contains α phase, β phase, γ phase three-phase in alloy structure, and described α phase is WC grain；Described β phase is (Ti, W, Ta) C phase；Described γ phase is Co (Ni, Cr) phase.
By the alloy sample prepared by embodiment of the present invention 1-5 and comparative example 1,2,3-0,3-1,3-2,3-3,3-4,3-5,4,5 alloy sample carry out performance detection contrast, data are in Table 4 and table 5.
By the alloy microstructure of the obtained present invention is detected, described α phase average grain size is preferably 2.4～4.0 μm, and β phase average grain size is preferably 0.8～1.0 μm.β phase crystal grain quantity accounts for the 10%～40% of α phase and two kinds of crystal grain total quantitys of β phase, it is preferred to 13%～36%.
The alloy sample prepared by embodiment of the present invention 1-5 is carried out fluorescence spectrum elementary analysis, and data are in Table 5.
Selecting wherein 4 embodiments prepare into collars product and carry out rolling test, and under equal conditions contrast its single cavity with existing material collars product and cross steel tonnage, through test of many times, average, result of the test is listed in table 6 respectively.
Result shows, embodiment of the present invention alloy to by the corresponding comparative example alloy phase ratio prepared by prior art, when not significantly reducing bending strength (TRS) and toughness, its hardness (HRA) is the high temperature hardness (HV30) considerably higher (Fig. 4) at 600 DEG C especially, therefore, about 2 times of existing collars product can be reached service life by the product of gained of the present invention.
Table 2
The sintering process parameter of table 3 embodiment trade mark alloy
Table 4
| Element | W | Co | Ni | Ti | Ta | Cr | C | Impurity |
| Embodiment 1 | 62.152 | 30.016 | 1.404 | 1.046 | 0.201 | 0.107 | 4.406 | 0.668 |
| Embodiment 2 | 72.543 | 20.423 | 1.176 | 0.789 | 0.167 | 0.063 | 4.134 | 0.705 |
| Embodiment 3 | 74.385 | 18.342 | 1.136 | 0.56 | 0.103 | 0.045 | 4.89 | 0.539 |
| Embodiment 4 | 80.358 | 10.748 | 1.723 | 0.762 | 0.087 | 0.035 | 5.567 | 0.720 |
| Embodiment 5 | 85.879 | 6.934 | 0.712 | 0.419 | 0.051 | 0.038 | 5.014 | 0.953 |
Table 5 fluorescence spectrum elementary analysis
Table 6
When without departing from the spirit of the present invention and basic feature, the embodiment of the present invention can be embodied as the form that other is concrete.Such as βPTiC in powder stock can use Ti (C, N) partly or entirely to replace, and TaC partly or entirely can replace with NbC, βPThe composition of powder stock and proportioning can also make corresponding change according to use, and the applicant is at existing βPOn the composition of powder stock and the basis of proportioning, height has adjusted, i.e. Ni powder: 8.5 ± 0.5 parts；TiC powder: 7.0 ± 1.0 parts；TaC powder: 1.0 ± 0.3 parts；Cr powder: 0.5 ± 0.2 part；Fine grained WC powder: 83 ± 2.0 parts.Hard alloy prepared by the inventive method is taked also to achieve satisfied effect.Additionally, presintering operation can complete in same stove with sintering circuit.Can also adopting ordinary sinter technique during sintering, namely pressure sintering is not necessarily.Therefore the example of the present invention is it is believed that be all illustrative and not restrictive in all respects; the scope of the invention indicated by appended claims is better than the scope of description above, therefore within it contain and claim equivalent scope within all changes be all contained among its scope required for protection.
Claims (5)
1. a hard alloy, it is characterised in that containing α phase, β phase, γ phase three-phase in alloy structure；
Described α phase is WC grain；Described β phase is (Ti, W, Ta) C phase；Described γ phase is Co (Ni, Cr) phase；
Described α phase average grain size is 2.0～4.0 μm；Described β phase average grain size is 0.5～1.5 μm,
Described β phase crystal grain quantity accounts for the 10%～40% of α phase and two kinds of crystal grain total quantitys of β phase.
2. by the hard alloy described in claim 1, it is characterised in that: described α phase average grain size is 2.4～4.0 μm；β phase average grain size is 0.8～1.0 μm, and described β phase crystal grain quantity accounts for the 13%～36% of α phase and two kinds of crystal grain total quantitys of β phase.
3. by the hard alloy described in claim 1 or 2, it is characterised in that: described hard alloy each element wt component is as follows:
W:62-86
Co:6.9-30.1
Ni:0.7-1.73
Ti:0.4-1.1
Ta:0.05-0.21
Cr:0.03-0.11
C:4.13-5.6
Impurity: 0.53-0.96.
4. a preparation method for hard alloy, including dispensing, ball milling operation, it is characterised in that:
Described burden process presses following components by weight percent preparation raw material
WC, 54.3～84.7, Fisher particle size 20.0-30.0 μm；Joining carbon content is 6.12wt.%～6.16wt.%；
Co, 7.3～30.7；
βPPowder, 8～15；
Described βPPowder is made up of following weight:
Ni:8.5
TiC:7, Fisher particle size is less than or equal to 2.5 μm；
TaC:1
Cr:0.5
WC:83, Fisher particle size is less than or equal to 0.8 μm；
The technique of described ball milling operation is: βPPowder is first wet grinding in advance 12～18 hours in ball grinding cylinder, then with WC and Co wet grinding 16～24 hours in ball grinding cylinder in the lump.
5. by the hard alloy preparation method described in claim 4, it is characterised in that: described in
Tungsten carbide, Fisher particle size 22.0-28.0 μm, joining carbon is 6.12wt.%～6.15wt.%；
βPTiC Fisher particle size in powder is less than or equal to 2.0 μm；Fine grained WC Fisher particle size is less than or equal to 0.6 μm.
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