CN105714170B - 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 kind of hard alloy and preparation method thereof.Contain α phases, β phases, γ phase three-phases in alloy structure；The α phases are WC grain；The β phases are (Ti, W, Ta) C phases；The γ phases are Co (Ni, Cr) phase；Described α phase averages grain size is 2.0~4.0 μm；Described β phase averages grain size is 0.5~1.5 μm, and the β phases crystal grain quantity accounts for the 10%~40% of two kinds of crystal grain total quantitys of α phases and β phases.Obtain the more excellent hard alloy finished product of combination property.The alloy material has the characteristics of high temperature resistant, wear-resisting, cracking resistance, resisting viscosity steel, good plasticity_resistant deformation ability while good obdurability is ensured.
Description
Technical field
The present invention relates to a kind of hard alloy, the novel hard alloy collars material of particularly a kind of steel rolling, the present invention
Also include the preparation method of above-mentioned hard alloy.
Background technology
When steel rolls field, particularly high-speed wire rolling, carbide roll ring is important consumption spare part, from upper
Just turn into the standard fitting of high-speed wire mill from the 60 to 70's of century.
With the progress of steel rolling technology, rolling shapes are more and more, and the demand of difficult steel rolling kind is increasing, to product matter
Also more and more higher, common carbide roll ring material can not increasingly meet requirement for the requirement of amount.Particularly rolling
High-carbon steel, steel alloy etc. are high-strength, high rigidity special steel grade when, roll-force is big, both pick strong, common WC-Co, WC-Co-Ni-
Cr material collars is easy to crack, and quick abrasion, life-span are low, can not increasingly meet the requirement and expectation of user.
In recent years, when rolling special steel problem be present to existing collars product for market, each collars manufacturer is to this
Studied energetically, develop some plastics on new materials collars, achieve certain effect, but still suffer from cost of material height and technique
Control the problems such as difficult.
Publication No. CN101994051A patent《A kind of tungsten carbide roll collar formula》, using low binding agent (2~
5wt.%), addition TiC (0.2~0.3wt.%), CrC (0.2~0.3wt.%), VC (0.05~0.3wt.%), Y (0.05~
Method 0.1wt.%) improves wearability and crack resistance.
Publication No. CN102051514A patent《Roll the material formula of cold-forging steel timber-used carbide roll ring》Using
Co+Ni is binding agent, and 10~20wt.% of content, Co/Ni=5/5~6/4, (WC particle size ranges are pressed for twin crystal grain or multiple grain tissue
Weight ratio：40~60%3~6 μm；20~30%6~9 μm；20~30%9~25 μm) improve shock resistance and wearability.
Publication No. CN102433488A patent《WC-Co-Ni-Al-B hard alloy, the roller made of the hard alloy
The preparation method of ring and the collars》Using Co/Ni=6/4~4/6, binding agent total amount is 6~26wt.%, without Cr, WC grain
Not less than 4 μm, Al is added, B is precipitated to Binder Phase, dispersion-strengtherning improves crack resistance；CN101648213《Finished frame
Carbide roll ring and preparation method thereof》Using yellow tungsten high temperature reduction, air current classifying again high temperature cabonization method prepare it is super thick
Brilliant WC powder raw material, then crack resistance is improved using the method for the super coarse-grain hard alloy of this raw material preparation.
It is well known that in WC-Co hard alloy, the high-melting-point carbide such as addition TiC, TaC, be advantageous to improve alloy
High-temperature behavior and chemical stability, however, it is numerous practice have shown that TiC, TaC addition can significantly reduce the obdurability of alloy,
Therefore, general TiC, TaC etc. addition are no more than 0.3wt.%.For special steel rolling carbide roll ring, material
The mechanical behavior under high temperature and chemical stability of material are very important, add TiC, TaC etc. on a small quantity, collars high-temperature behavior is changed
It is kind limited, it is impossible to meet using it is expected, on the premise of obdurability is significantly reduced, to significantly improve collars high-temperature behavior and
Chemical stability, it is still a technological difficulties.
The content of the invention
Present invention aims at：It is in view of the shortcomings of the prior art and difficult point, there is provided a kind of hard alloy and its system
There is high temperature resistant, wear-resisting, cracking resistance, resisting viscosity steel, anti-plasticity to become while good obdurability is ensured for Preparation Method, the alloy material
The characteristics of shape ability is good.
1st, hard alloy of the invention, containing α phases, β phases, γ phase three-phases in alloy structure, the α phases are WC grain；Institute
It is (Ti, W, Ta) C phases to state β phases；The γ phases are Co (Ni, Cr) phase, and described α phase averages grain size is 2.0~4.0 μm, institute
The β phase averages grain size stated is 0.5~1.5 μm, and described β phase crystal grain quantity accounts for two kinds of crystal grain total quantitys of α phases and β phases
10%~40%.Above-mentioned α phase averages grain size is preferably 2.4~4.0 μm；β phase average grain sizes are preferably 0.8~1.0 μm, institute
It is preferably 13%~36% that the β phase crystal grain quantity stated, which accounts for two kinds of crystal grain total quantitys of α phases and β phases,.
The alloy structure of the present invention is designed to three-phase twin crystal structure.Binding metal γ phases are made using Co+Ni+Cr, it is brilliant with WC
Grain (α phases) and (Ti, W, Ta) C solid solution phases (β phases) are used as hard phase, and thick WC grain (α phases) is advantageous in three-phase structure
Increase the mean free path of Binder Phase, improve alloy obdurability, and fine grain β phases have good stability at elevated temperature,
Dispersion-strengtherning Binder Phase can be played again simultaneously, improve alloy rigidity and plasticity_resistant deformation ability.Therefore so that alloy is being protected
While holding high intensity and good impact resistance, its high rigidity, high temperature resistant, excellent chemical stability are also significantly changed
It is kind, so as to realize its purpose.
Moreover, hard alloy each element components by weight percent of the invention is as follows：W：Co：Ni：Ti：Ta：Cr：C：It is miscellaneous
Matter=(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)
Present invention additionally comprises the preparation method of above-mentioned alloy, its dispensing and ball milling process press following technology controlling and process：
The burden process presses following composition by weight preparation raw material
WC, 54.3~84.7,20.0-30.0 μm of Fisher particle size (being preferably 22.0-28.0)；It is with carbon content
6.12wt.%~6.16wt.% (being preferably 6.12wt.%~6.15wt.%)；
Co, 7.3~30.7；
βPPowder, 8~15；
The 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 (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 (preferably less than equal to 0.6 μm)；
The technique of the ball milling process is：βPPowder first wet-milling 12~18 hours in advance in ball grinding cylinder, then with Fei Shi grains
The super coarse-grained WC of 20.0-30.0 μm of degree, Co wet-milling 16~24 hours in ball grinding cylinder in the lump.
Existing ball-milling technology is all the Ginding process disposably put into using raw material, and the present invention is in order to obtain different grain sizes
Hard phase, in burden process, have chosen extra-coarse grained WC, and the β containing fine grain WC, TiC respectivelyPPowder, then
It is aided with the method for segmentation grinding, the raw material Ball-milling Time for forming aplitic texture in hard phase is about 28-42 hours, forms hard
The raw material Ball-milling Time of coarse structure is 16~24 hours in phase.
The present invention super thick WC powder, its with carbon content be 6.10wt.%~6.16wt.% (preferably 6.12wt.%~
6.15wt.%), average FSSS granularities are not less than 20 μm, preferably not less than 22 μm, to obtain mean grain size as 2.4~4.0 μm
α phases.Because the alloying behaviour in Binder Phase such as the development and Ti, Ta of WC mixed carbon comtent to α phases in alloy sintering process
Have a significant impact, during mixed carbon comtent too low (being less than 6.10wt.%), the alloy α skews obtained after sintering are thin, shock resistance drop
It is low.Ti, Ta etc. largely will be dissolved into Binder Phase, can not form tiny β phases.
Required alloy designations compound is prepared into by above-mentioned operation, then by conventional powders such as compressing, sintering
Metallurgical process, obtained hart metal product, compared with conventional rigid alloy, in the case of Binder Phase content identical, have more
High hardness, more resistant to high temperature, the advantages that chemical stability and plasticity_resistant deformation ability are more preferable, and service life is longer, be more suitable for
In rolling high rigidity, high strength steel.
Brief description of the drawings
Fig. 1 is the metallograph of the alloy microscopic structure of embodiment 3 × 1500, wherein thick polygon grey crystal grain is α phases,
Tiny subcircular black particle is β phases, and white tissues are γ phases.
Fig. 2 is the metallograph of microscopic structure × 1500 of comparative example 3-0 alloys, and wherein irregular polygon grey crystal grain is
α phases, the particle that subcircular contains black core are β phases, and white tissues are γ phases.
Fig. 3 is the metallograph of microscopic structure × 1500 of comparative example 3-2 alloys, and wherein irregular polygon grey crystal grain is
α phases, white tissues are γ phases, and in this example, because mixed carbon comtent is relatively low, phase containing Ti dissolves into γ phases and is almost wholly absent,
Only remain the thick particle of phase containing Ti (black particle in figure).
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 toughness (Ak) comparison diagram
Fig. 6 is embodiment 1~5 and comparative example 1~5 alloy bending strength (TRS) comparison diagram
Embodiment
All features disclosed in this specification, or disclosed all methods or during the step of, except mutually exclusive
Feature and/or step beyond, can combine in any way.This specification (including any accessory claim, summary and
Accompanying drawing) disclosed in any feature, unless specifically stated otherwise, can alternative features equivalent by other or with similar purpose be subject to
Replace.I.e., unless specifically stated otherwise, each feature is an example in a series of equivalent or similar characteristics.
The present invention prepares βPThe technique of powder is as follows：
Industrial production standard material powder WC1, TiC, TaC, Ni, Cr will be met, matched by the components by weight percent of table 1,
Mixing, obtain required βPPowder, it is stand-by.
Wherein TiC powder, average 2.0 μm of Fisher particle size.WC1 powder, average 0.6 μm of Fisher particle size.In order to obtain fine grain
The β phases of grain, TiC powder and WC1 powder, granularity is more thin better, in order to realize the purpose of the present invention, TiC：Fisher particle size should be less than
Equal to 2.5 μm；WC, Fisher particle size are 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：
A kind of preparation method of hard alloy, comprises the following steps：
1st, dispensing：By the composition by weight in the embodiment 1 of table 2 and technological parameter preparation raw material powder WC2, Co, βPPowder.
2nd, ball milling, by the β of said ratioPAfter powder adds ball grinding cylinder wet-milling 18 hours, it is small to add WC2, Co wet-milling 24
When；And add 1.5wt% forming agent paraffin.
3rd, dry, by compound slurry that wet-milling finishes it is dry, obtain compound powder；
4th, it is compressing, it is molded using conventional mould pressing process；
5th, sinter, conventional low voltage sintering process, be specifically shown in Table 3.Obtain alloy product.
Embodiment 2：
A kind of preparation method of hard alloy, in addition to steps 1 and 2,5, remaining is the same as embodiment 1.
1st, dispensing：By the composition by weight in the embodiment 2 of table 2 and technological parameter preparation raw material powder WC2, Co, β P powder.
2nd, ball milling, by the β of said ratioPAfter powder adds ball grinding cylinder wet-milling 16 hours, it is small to add WC2, Co wet-milling 22
When；And add 1.8wt% forming agent paraffin.
5th, sinter, conventional low voltage sintering process, be specifically shown in Table 3.Obtain alloy product.
Embodiment 3：
A kind of preparation method of hard alloy, in addition to steps 1 and 2,5, remaining is the same as embodiment 1.
1st, dispensing：By the composition by weight in the embodiment 3 of table 2 and technological parameter preparation raw material powder WC2, Co, β P powder.
2nd, ball milling, by the β of said ratioPAfter powder adds ball grinding cylinder wet-milling 16 hours, it is small to add WC2, Co wet-milling 20
When；And add 1.8wt% forming agent paraffin.
5th, sinter, conventional low voltage sintering process, be specifically shown in Table 3.Obtain alloy product.
Embodiment 4：
A kind of preparation method of hard alloy, in addition to steps 1 and 2,5, remaining is the same as embodiment 1.
1st, dispensing：By the composition by weight in the embodiment 4 of table 2 and technological parameter preparation raw material powder WC2, Co, βPPowder.
2nd, ball milling, by the β of said ratioPAfter powder adds ball grinding cylinder wet-milling 14 hours, it is small to add WC2, Co wet-milling 18
When；And add 1.8wt% forming agent paraffin.
5th, sinter, conventional low voltage sintering process, be specifically shown in Table 3.Obtain alloy product.
Embodiment 5：
A kind of preparation method of hard alloy, in addition to steps 1 and 2,5, remaining is the same as embodiment 1.
1st, dispensing：By the composition by weight in the embodiment 2 of table 2 and technological parameter preparation raw material powder WC2, Co, βPPowder.
2nd, ball milling, by the β of said ratioPAfter powder adds ball grinding cylinder wet-milling 12 hours, it is small to add WC2, Co wet-milling 16
When；And add 2.0wt% forming agent paraffin.
5th, sinter, conventional low voltage sintering process, be specifically shown in Table 3.Obtain alloy product.
In order to obtain contrast test data, according to the WC-Co-Ni-Cr hard alloy of existing collars, routinely technique system
For comparative example alloy 1,2,3-5,4,5.The Binder Phase content of above-mentioned comparative example is identical with embodiment 1,2,3,4 and 5 respectively, tool
Body is shown in Table 2.Its tungsten carbide is the coarse granule tungsten carbide of conventional single grain size.Remaining ball milling, drying, pressing process, agglomerant
Skill uses common process.
In order to obtain contrast test data, comparative example 3-0,3-1,3-2,3-3,3-4 are also prepared for, its proportioning is shown in Table 2.
In comparative example 3-0 preparation methods, in addition to ball-milling technology, remaining is the same as embodiment 3.Its ball-milling technology is to use " raw material
The conventional ball-milling process of disposable input ", the alloy has three-phase contexture it can be seen from table 4 and Fig. 2, but is not in twin crystal grain
The mean grain size of degree structure, α phases and β phases is without significant difference.
In comparative example 3-1 preparation methods, in addition to WC2FSSS granularities, remaining is the same as embodiment 3.It uses FSSS granularities small
The WC2 raw materials of (20.1 μm).From correction data as can be seen that WC2 granularity has an impact to alloy property.FSSS granularities should not be small
In 20 μm, preferably not less than 22 μm.
It is the super of 6.08wt.%, 6.10wt.%, 6.12wt.% that total carbon content, which is respectively adopted, in comparative example 3-2,3-3,3-4
Thick WC2 raw materials, remaining is the same as embodiment 3.From correction data as can be seen that WC2 mixed carbon comtent has an impact to alloy property.Work as carbon amounts
When relatively low, such as comparative example 3-2, it will be unable to form tiny β phases.
Alloy sample prepared by 1-5 of the embodiment of the present invention uses X-ray diffraction analysis, in alloy structure containing α phases,
β phases, γ phase three-phases, the α phases are WC grain；The β phases are (Ti, W, Ta) C phases；The γ phases are Co (Ni, Cr) phase.
By the alloy sample prepared by 1-5 of the embodiment of the present invention and comparative example 1,2,3-0,3-1,3-2,3-3,3-4,3-5,
4th, 5 alloy samples carry out performance detection contrast, and data are shown in Table 4 and table 5.
By being detected to obtained alloy microstructure of the invention, described α phase average grain sizes are preferably
2.4~4.0 μm, β phase average grain sizes are preferably 0.8~1.0 μm.β phase crystal grain quantity accounts for two kinds of crystal grain sums of α phases and β phases
The 10%~40% of amount, preferably 13%~36%.
The alloy sample prepared by 1-5 of the embodiment of the present invention is subjected to fluorescence spectrum elementary analysis, data are shown in Table 5.
Selection wherein 4 embodiments are prepared into collars product and carry out rolling experiment, and exist with existing material collars product
Its single groove is contrasted under equal conditions and crosses steel tonnage, by test of many times, is averaged, result of the test is listed in table 6 respectively.
As a result show, alloy of the embodiment of the present invention is compared with the corresponding comparative example alloy as prepared by prior art, not
In the case of significantly reducing bending strength (TRS) and toughness, the high temperature hardness at especially 600 DEG C of its hardness (HRA)
(HV30) considerably higher (Fig. 4), therefore, the product service life as obtained by the present invention can reach 2 times of existing collars product
Left and right.
Table 2
The sintering process parameter of the embodiment trade mark alloy of table 3
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 |
The fluorescence spectrum elementary analysis of table 5
Table 6
In the case where not departing from the spirit and essential characteristics of the present invention, the embodiment of the present invention can be embodied as other tools
The form of body.Such as βPTiC in powder stock can use Ti (C, N) partly or entirely to replace, and TaC can use NbC parts or complete
Portion replaces, βPThe composition and proportioning of powder stock can also make corresponding change according to use, and the applicant is in existing βPPowder
On the basis of the composition and proportioning of powder stock, height is 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.Take this hair
Hard alloy prepared by bright method also achieves satisfied effect.In addition, pre-sintered operation can be with sintering circuit in same stove
Interior completion.Ordinary sinter technique can also be used during sintering, i.e. pressure sintering is not essential.Therefore the example of the present invention can be with
Think it is illustrative and no restricted in all respects, be better than as the scope of the invention indicated by appended claims
The scope of description above, therefore all changes within its intension and claim equivalent scope are all contained in required by it
Among the scope of protection.
Claims (5)
1. a kind of hard alloy, it is characterised in that contain α phases, β phases, γ phase three-phases in alloy structure；
The α phases are WC grain；The β phases are (Ti, W, Ta) C phases；The γ phases are Co (Ni, Cr) phase；
Described α phase averages grain size is 2.0~4.0 μm；Described β phase averages grain size is 0.5~1.5 μm,
The β phases crystal grain quantity accounts for the 10%~40% of two kinds of crystal grain total quantitys of α phases and β phases.
2. the hard alloy as described in claim 1, it is characterised in that：The α phase averages grain size is 2.4~4.0 μm；β phases
Mean grain size be 0.8~1.0 μm, described β phase crystal grain quantity account for two kinds of crystal grain total quantitys of α phases and β phases 13%~
36%.
3. the hard alloy as described in claim 1 or 2, it is characterised in that：The hard alloy each element components by weight percent 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 kind of preparation method of hard alloy, including dispensing, ball milling process, it is characterised in that：
The burden process presses following components by weight percent preparation raw material
WC, 54.3~84.7,20.0-30.0 μm of Fisher particle size；It is 6.12wt.%~6.16wt.% with carbon content；
Co, 7.3~30.7；
βPPowder, 8~15；
The 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 the ball milling process is：βPPowder first wet-milling in advance 12~18 hours, then exist in the lump with WC and Co in ball grinding cylinder
Wet-milling 16~24 hours in ball grinding cylinder.
5. the hard alloy preparation method as described in claim 4, it is characterised in that：It is described
Tungsten carbide, 22.0-28.0 μm of Fisher particle size, it is 6.12wt.%~6.15wt.% with carbon；
βPTiC Fisher particle sizes in powder are less than or equal to 2.0 μm；Fine grained WC Fisher particle sizes are less than or equal to 0.6 μm.
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| CN107630162A (en) * | 2016-07-18 | 2018-01-26 | 自贡硬质合金有限责任公司 | A kind of preparation method of WC alloys pellet |
| CN112195385B (en) * | 2020-10-16 | 2021-07-13 | 内蒙金属材料研究所 | High-temperature-resistant high-toughness molybdenum-based composite material and preparation method thereof |
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| CN102383020A (en) * | 2011-11-16 | 2012-03-21 | 重庆市科学技术研究院 | Ultrathin hard alloy with high hardness and preparation method thereof |
| CN102699330A (en) * | 2012-04-30 | 2012-10-03 | 自贡硬质合金有限责任公司 | Method for producing hard-alloy stud assembled on roll surfaces |
| CN102766796A (en) * | 2012-07-23 | 2012-11-07 | 自贡硬质合金有限责任公司 | Hard alloy and preparation method thereof |
| CN103060652A (en) * | 2013-01-25 | 2013-04-24 | 地质矿产部无锡钻探工具厂 | High-temperature-resistant alloy and production process thereof |
| CN103394690A (en) * | 2013-08-13 | 2013-11-20 | 四川川钨硬质合金有限公司 | Cemented carbide powder used in production of nozzles, and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102383020A (en) * | 2011-11-16 | 2012-03-21 | 重庆市科学技术研究院 | Ultrathin hard alloy with high hardness and preparation method thereof |
| CN102699330A (en) * | 2012-04-30 | 2012-10-03 | 自贡硬质合金有限责任公司 | Method for producing hard-alloy stud assembled on roll surfaces |
| CN102766796A (en) * | 2012-07-23 | 2012-11-07 | 自贡硬质合金有限责任公司 | Hard alloy and preparation method thereof |
| CN103060652A (en) * | 2013-01-25 | 2013-04-24 | 地质矿产部无锡钻探工具厂 | High-temperature-resistant alloy and production process thereof |
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