CN106862573B - A kind of WC-Co and CBN-Co graded composite cutter material and preparation method - Google Patents
A kind of WC-Co and CBN-Co graded composite cutter material and preparation method Download PDFInfo
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- CN106862573B CN106862573B CN201710177691.6A CN201710177691A CN106862573B CN 106862573 B CN106862573 B CN 106862573B CN 201710177691 A CN201710177691 A CN 201710177691A CN 106862573 B CN106862573 B CN 106862573B
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- 229910009043 WC-Co Inorganic materials 0.000 title claims abstract description 101
- 239000000463 material Substances 0.000 title claims abstract description 56
- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 114
- 238000007747 plating Methods 0.000 claims abstract description 54
- 230000007704 transition Effects 0.000 claims abstract description 46
- 239000000126 substance Substances 0.000 claims abstract description 31
- 239000011812 mixed powder Substances 0.000 claims abstract description 24
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 7
- 239000010439 graphite Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 59
- 239000008367 deionised water Substances 0.000 claims description 55
- 229910021641 deionized water Inorganic materials 0.000 claims description 55
- 239000000203 mixture Substances 0.000 claims description 55
- 238000003756 stirring Methods 0.000 claims description 37
- 238000000034 method Methods 0.000 claims description 34
- 206010070834 Sensitisation Diseases 0.000 claims description 25
- 230000008313 sensitization Effects 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 150000003839 salts Chemical class 0.000 claims description 15
- 230000003213 activating effect Effects 0.000 claims description 13
- 239000011248 coating agent Substances 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000002202 Polyethylene glycol Substances 0.000 claims description 11
- 229920001223 polyethylene glycol Polymers 0.000 claims description 11
- 238000004062 sedimentation Methods 0.000 claims description 11
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 238000001994 activation Methods 0.000 claims description 10
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 10
- 239000004327 boric acid Substances 0.000 claims description 10
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 10
- 238000007788 roughening Methods 0.000 claims description 9
- 239000001509 sodium citrate Substances 0.000 claims description 9
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 9
- 229940038773 trisodium citrate Drugs 0.000 claims description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 8
- 230000004913 activation Effects 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 8
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 7
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 6
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 6
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 6
- 239000001119 stannous chloride Substances 0.000 claims description 6
- 235000011150 stannous chloride Nutrition 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims description 5
- 239000008139 complexing agent Substances 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 230000010355 oscillation Effects 0.000 claims description 4
- 241000972773 Aulopiformes Species 0.000 claims description 3
- 230000007613 environmental effect Effects 0.000 claims description 3
- 230000013016 learning Effects 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 235000019515 salmon Nutrition 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 abstract description 14
- 239000010410 layer Substances 0.000 description 80
- 238000005520 cutting process Methods 0.000 description 13
- 230000008569 process Effects 0.000 description 12
- 239000002245 particle Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000013461 design Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 238000003475 lamination Methods 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 208000037656 Respiratory Sounds Diseases 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000005253 cladding Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000005728 strengthening Methods 0.000 description 3
- 239000002344 surface layer Substances 0.000 description 3
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 description 2
- 206010020843 Hyperthermia Diseases 0.000 description 2
- 229910033181 TiB2 Inorganic materials 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 230000036031 hyperthermia Effects 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000011017 operating method Methods 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 238000007781 pre-processing Methods 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 208000032170 Congenital Abnormalities Diseases 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007698 birth defect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002648 laminated material Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- SOBHUZYZLFQYFK-UHFFFAOYSA-K trisodium;hydroxy-[[phosphonatomethyl(phosphonomethyl)amino]methyl]phosphinate Chemical compound [Na+].[Na+].[Na+].OP(O)(=O)CN(CP(O)([O-])=O)CP([O-])([O-])=O SOBHUZYZLFQYFK-UHFFFAOYSA-K 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/68—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous solutions with pH between 6 and 8
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2207/00—Aspects of the compositions, gradients
- B22F2207/01—Composition gradients
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Optics & Photonics (AREA)
- Composite Materials (AREA)
- Physics & Mathematics (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemically Coating (AREA)
- Polishing Bodies And Polishing Tools (AREA)
Abstract
A kind of WC-Co and CBN-Co graded composite cutter material, it is made of base layer, articulamentum, First Transition layer, the second transition zone and outer wear layer, base layer is WC-Co, articulamentum, First Transition layer, the second transition zone and outer wear layer are the mixed powder of WC-Co and CBN-Co, and from articulamentum to outer wear layer, the mass fraction of WC-Co is reduced in gradient；Metal Co is coated in two kinds of powder surfaces of WC and CBN by chemical plating, obtain two kinds of powders of WC-Co and CBN-Co, and using WC-Co as base layer, the mixed powder of WC-Co and CBN-Co is using different mixing proportion as articulamentum, First Transition layer, the second transition zone and outer wear layer, after the powder of preparation is successively seated in graphite jig, uniform pressurization carries out discharge plasma sintering under vacuum condition, powers off cooled to room temperature, obtains graded composite cutter material；The material has fabulous hardness, wearability and low coefficient of friction, solves " hardness and the implacable contradiction of toughness " of ceramic composite to a certain extent.
Description
Technical field
The invention belongs to cutter material and the technical fields of processing, and in particular to a kind of WC-Co and CBN-Co graded composite
Cutter material and preparation method.
Background technique
In machining process, cutter is as the main direct executor of cutting process, in the cutting process of workpiece
In be inevitably present abrasion, damaged phenomena such as being even broken, especially in high-speed cutting, the abrasion of cutter is especially tight
Weight；After there is wear phenomenon, the service life of cutter can sharply decline, and the workpiece surface roughness processed rises, and easily lead to workpiece
Size exceed design tolerance, although in time tool changing tool can solve the problems, such as to a certain extent workpiece accuracy deficiency, for
Process aerospace, the relatively high utensil of difficulty of processing such as novel die, be related specifically to national defense requirement heavy parts or
Precision component, the tool changing of overfrequency will increase the resetting error of part, design requirement are not achieved.
Cutting tool surface-coating technology is the material surface modifying skill to grow up that meets the market requirement in recent decades
Art.The service life that can effectively improve cutting tool using coating technology makes cutter obtain excellent comprehensive performance, thus greatly
Amplitude improves machining efficiency.Therefore, coating technology, cutter material, cutting technology are called bite by insider
Have three big key technologies of manufacturing field.
Although CVD coating tool has good wearability, CVD technique also has its birth defect: first is that process temperature
Height easily causes cutter material bending strength to decline；Second is that being in tensile stress state inside film, generated when easily leading to cutter use micro-
Crackle；Third is that exhaust gas, the waste liquid of the discharge of CVD technique will cause larger environmental pollution.Equally, although there are many PVD process advantage,
Certain problem is still had at present.For example, PVD process treatment temperature is lower, therefore coating and tool matrix, coating and coating
Between interface bond strength it is lower, be on the one hand restricted coating layer thickness, while making coating in the effect of cutting load
Under fail quickly because cracking and flaking off, the performance difference of coating and tool matrix is larger, and biggish remnants are easily formed in coating
Stress causes cutter under the action of cutting (especially interrupted cut) load, is also easy to produce micro-crack.
Laminated construction designs the method for enriching ceramic material Strengthening and Toughening, has been developed in recent years Material reinforcement increasing
Tough new technology, this structure are by imitating shell come the nacre of shell is a kind of natural layer structure in nature
Material, fracture toughness are but higher by 3000 times or more than common single homogeneous texture.This kind design have Strengthening and Toughening significant effect,
The advantages that material system is more, flexible design, are one of the effective ways of current composite material Strengthening and Toughening.For grinding for multi-layered ceramic
Study carefully major part also to rest in the building of material system, and for lamination compound tool, it studies both at home and abroad at present less.Lamination knot
The appearance of structure, fixes a cutting tool if be reasonably applied in, and the bond strength with matrix not only can be improved, but also can have a variety of coating materials
Comprehensive physical mechanical performance, to meet requirement (the novel laminated composite ceramic of section development of different materials, different processing conditions
The development of porcelain cutter and its Study on Cutting Performance [D] Shandong University, 2009).
Chinese patent discloses gradient multiple coating tool and preparation method thereof (ZL 201110214393.2), made
Standby ZrTiN composite coating layer cutter has higher hardness and strength, excellent wear-resistant and corrosion resistance, but has in cutting
Its skin-friction coefficient is higher when non-ferrous metal material, and cutter life, which is unable to satisfy, uses needs.Chinese patent discloses one
Kind novel laminated self-lubrication ceramic cutter material and preparation method thereof (ZL 201610232992.X), it be related to it is a kind of novel
Lamination self-lubrication ceramic cutter material TiC/TiN+TiB2/ TiN and preparation method thereof.Using TiC/30wt%TiN as matrix, TiB2/
15wt%TiN is lamination, is formed using each layer thermal expansion coefficient difference in surface layer generation residual compressive stress and surface layer reaction in-situ
Lubricating film improves composite material combination property, but due to the difference of thermal expansion coefficients of layers of material itself, cutter is difficult in cutting
When rapidoprint, laminated material is still easy to produce crackle at its interface, and cutter life is lower.
Cubic boron nitride (CBN) belongs to covalent key compound, have high chemical stabilization ' property, thermal stability and resistivity and
It is only second to the hardness of diamond.CBN is added in hard alloy in the form of micron particles, is not only mentioned to wear-resisting property
Height, and due to the inhibition of CBN On Crack Propagation, the toughness of composite material can be significantly improved.Therefore, WC-Co-cBN
Composite material has great potential to become solution Cemented Carbide Hardness and the contradictory composite material of toughness.
Chinese patent discloses a kind of preparation method (ZL 201610232992.X) of WC-Co-CBN composite material, it is
Using the method for hot pressed sintering, sintering temperature is low, and sintering time is shorter, that is, can guarantee CBN not phase transformation, material can also be made to have greatly
Shrinking percentage and high bulk density.Due to WC and CBN unusual hard-to-sinter, at the same exist during the sintering process WC particle with
The direct contact of CBN particle, so that it is extremely difficult to prepare high performance WC-Co-CBN composite material under this condition.
Summary of the invention
It is an object of the invention to overcome above-mentioned the deficiencies in the prior art, a kind of WC-Co and CBN-Co graded composite are provided
Cutter material and preparation method are plated one layer of Co metal on WC and CBN superfine powder surface, are obtained WC- using the method for chemical plating
Co and CBN-Co powder is seated in graphite jig with sequence according to certain gradient proportion and carries out discharge plasma sintering, obtains
To graded composite cutter material, which has fabulous hardness, wearability and low coefficient of friction, solves to a certain extent
" hardness and the implacable contradiction of toughness " of ceramic composite.
The technical proposal adopted by the invention to solve the above technical problems is that: a kind of WC-Co and CBN-Co graded composite knife
Have material, the material successively base layer as made of being sintered, articulamentum, First Transition layer, the second transition zone and outer wear layer
Composition, from outer wear layer to base layer, the mass fraction that each layer accounts for material gross mass is respectively 15%, 12.5%, 10%, 7.5%
With 55%, base layer WC-Co, articulamentum, First Transition layer, the second transition zone and outer wear layer are WC-Co and CBN-Co
Mixed powder, and from articulamentum to outer wear layer, the mass fraction of WC-Co is reduced in gradient.
A method of the WC-Co and CBN-Co graded composite cutter material being prepared, by chemical plating in WC and CBN
Two kinds of powder surfaces coat metal Co, obtain two kinds of powders of WC-Co and CBN-Co, and using WC-Co as base layer, WC-Co with
The mixed powder of CBN-Co using different mixing proportion as articulamentum, First Transition layer, the second transition zone and outer wear layer,
According to the sequence of base layer, articulamentum, First Transition layer, the second transition zone and outer wear layer, successively it is seated in graphite jig
Afterwards, uniform pressurization carries out discharge plasma sintering under vacuum condition, powers off cooled to room temperature then to get multiple to gradient
Close cutter material；
Main salt is the cobaltous sulfate of 15 ~ 40 g/l, the citric acid that complexing agent is 50 g/l in plating solution used in the chemical plating
Trisodium, reducing agent are the sodium hypophosphite of 20 ~ 60 g/l, buffer is 25 g/l boric acid, the method for preparing plating solution are as follows:
(1) deionized water dissolving cobaltous sulfate is used, solution is obtaineda；
(2) deionized water dissolving trisodium citrate is used, clear solution is obtainedb；
(3) by solutionaSolution is addedbIn, it is stirred solution, obtains main salt complex solutionc；
(4) it under room temperature, with deionized water dissolving sodium hypophosphite, stirs evenly, obtains solutiond；
(5) solution d is added in main salt complex solution c, it is stirring while adding, obtain solution e；
(6) deionized water dissolving boric acid is used, stirs evenly, obtains clear solutionf；
(7) solution is added in solution feIn, it is stirring while adding, obtain plating solution；
It then plus deionized water constant volume (8) is 8 ~ 11 with the pH value of sodium hydroxide adjustment plating solution,；
In articulamentum, First Transition layer, the second transition zone and outer wear layer, the mixed powder of each layer of WC-Co and CBN-Co
The preparation method of body are as follows:
According to WC-Co and CBN-Co place layer in mass fraction, the WC-Co powder for chemical plating of learning from else's experience respectively and
CBN-Co powder pours into the container equipped with deionized water, is uniformly mixed so as to obtain mixture I, and the quality of deionized water is WC-Co powder
With 7 ~ 8 times of CBN-Co powder gross mass；Mixture I is stirred by ultrasonic, keeping the temperature of mixture I is 105 DEG C；Ultrasound
It is 1:80 according to the mass ratio of polyethylene glycol and mixture I after stirring 35min, taking polyethylene glycol is added in mixture I, after
Continuous ultrasonic agitation, obtains mixture II；It is sieved after gained mixture II is dried in vacuo, obtains the mixing of WC-Co and CBN-Co
Powder；
During the discharge plasma sintering, the base layer, articulamentum, the First Transition that are seated in graphite jig
The mass fraction that layer, the second transition zone and outer wear layer account for graded composite cutter material is followed successively by 55%, 7.5%, 10%, 12.5% and
15%。
Preferably, the WC powder purity is greater than 99.1%, average grain diameter 400nm, theoretical density 14.83g/cm3；
CBN powder purity is greater than 99.0%, average grain diameter 500nm.
Preferably, it before carrying out chemical plating to two kinds of powders of WC and CBN, is pre-processed respectively, pretreatment includes thick
Change, sensitization activates and drying.
Preferably, the roughening is that powder to be processed is added in coarsening solution, at room temperature supersonic oscillations；Then quiet
It sets to powder sedimentation, powder is taken out from coarsening solution, the powder of sedimentation is cleaned with deionized water, isolates powder；It is described
Coarsening solution composition including 20ml/l hydrofluoric acid and 2g/l ammonium fluoride.
Preferably, sensitization activation is will to be roughened that treated powder is added in sensitization activating solution, is surpassed at room temperature
Sonication is then allowed to stand to powder sedimentation, takes out the powder of sedimentation, after being cleaned with deionized water, isolated by centrifuge
Powder；The composition of the sensitization activating solution includes the sodium chloride of the palladium chloride of 0.5 g/l, the stannous chloride of 30 g/l, 160 g/l
With the hydrochloric acid of 60ml/l.
Preferably, before the chemical plating, it is pre-dispersed that pretreated powder is carried out to magnetic agitation respectively.
Preferably, in the discharge plasma sintering, during rising to 1800 DEG C from room temperature, environmental pressure is steadily equal
Even adds to 50MPa, keeps the temperature 20 ~ 30min under the conditions of temperature is 1800 DEG C, pressure 50MPa later, then powers off natural cooling
To room temperature.
Preferably, the preparation method of the sensitization activating solution is:
(1) stirring and dissolving in 30ml concentrated hydrochloric acid is added in the palladium chloride for weighing 0.25g, becomes transparent salmon after being completely dissolved
Solution adds deionized water until 50ml is to get to solutionA；(2) sodium chloride for weighing 80g is dissolved in 250ml deionized water
In, obtain solutionB；
(3) by solutionAWith solutionBIt mixes, stirs evenly, obtain solutionC;
(4) stannous chloride for weighing 15g is dissolved in the deionized water of 150ml, obtains the solution of whiteD；
(5) solutionDSolution is added while stirringCIn, obtain dark green solutionE；
(6) to solutionEDeionized water is added and is settled to 500ml, obtains bottle-green sensitization activating solution.
Compared with prior art, the beneficial effects of the present invention are:
1, according to the design concept of difficult-to-machine material cutter, this graded composite cutter material, matrix is that WC-Co has pole
Good toughness, surface layer are that WC-Co/CBN-Co has fabulous hardness, wearability and low coefficient of friction, are solved to a certain extent
" hardness and the implacable contradiction of toughness " of ceramic composite；Meanwhile the graded composite cutter material be on the whole by
Co metal is associated with wherein, is solved gradient composites to a certain extent and is easy to produce crackle at its interface, the service life is lower
Problem；
2, since the outer layer of every kind of ceramic powders during the sintering process has wrapped up Co metal, so that they will not directly connect
Touching, the difficulty of the sintering thus reduced, while ensure that the consistency of agglomerated material；
3, during discharge plasma sintering, since Co is conductive powder body, by applying electric field, the contact site Co of cladding
Electric discharge phenomena can occur, generate localized hyperthermia, promote Co metal molten, under acting on while big pressure, the cobalt of melting is filled
Into the gap of ceramic particle, fine and close lamination cutting tool composite material is formed.
4, multiple decentralized processing during the preparation process, is carried out to powder, biggish reunion can be generated to avoid powder granule,
To guarantee that final products have preferable mechanical property after sintering.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of WC-Co Yu CBN-Co graded composite cutter material；
Fig. 2 is the structural schematic diagram of chemical plating metal Co equipment therefor；
Fig. 3 is the discharge plasma sintering process schematic of graded composite cutter material；
Fig. 4 is the TEM figure of WC-Co powder；
Fig. 5 is the TEM figure of CBN-Co powder；
Marked in the figure: 1, ultrasonic oscillator, 2, sink, 3, beaker, 4, blender.
Specific embodiment
With reference to the accompanying drawing, further description of the technical solution of the present invention by specific embodiment.
Following example 1 ~ 3 are the further instructions to WC-Co and CBN-Co graded composite cutter material.
Embodiment 1
A kind of WC-Co and CBN-Co graded composite cutter material, as shown in Figure 1, the material is to be sintered 5 layers obtained knot
Structure, is followed successively by base layer, articulamentum, First Transition layer, the second transition zone and outer wear layer, and each layer accounts for the ratio of material gross mass
Example is respectively 55%, 7.5%, 10%, 12.5% and 15%, the base layer WC-Co；Articulamentum, First Transition layer, the second transition
Layer and outer wear layer are the mixture of WC-Co and CBN-Co, wherein in articulamentum, WC-Co accounts for the mass fraction of this layer
It is 5% for 95%, the CBN-Co mass fraction for accounting for this layer；In First Transition layer, WC-Co account for this layer mass fraction be 90%,
The mass fraction that CBN-Co accounts for this layer is 10%；In the second transition zone, the mass fraction that WC-Co accounts for this layer is 85%, CBN-Co
The mass fraction for accounting for this layer is 15%；In outer wear layer, the mass fraction that WC-Co accounts for this layer is that 80%, CBN-Co accounts for this layer
Mass fraction is 20%.
Embodiment 2
On the basis of embodiment 1, in articulamentum, the mass fraction that WC-Co accounts for this layer is that 93%, CBN-Co accounts for the layer
Mass fraction be 7%；In First Transition layer, WC-Co accounts for the quality point that the mass fraction of this layer accounts for this layer for 88%, CBN-Co
Number is 12%；In the second transition zone, WC-Co accounts for that the mass fraction of this layer is 83%, CBN-Co accounts for the mass fraction of this layer and is
17%；In outer wear layer, WC-Co accounts for that the mass fraction of this layer is 78%, to account for the mass fraction of this layer be 22% to CBN-Co.
Embodiment 3
On the basis of embodiment 1, in articulamentum, the mass fraction that WC-Co accounts for this layer is that 90%, CBN-Co accounts for the layer
Mass fraction be 10%；In First Transition layer, WC-Co accounts for the quality that the mass fraction of this layer accounts for this layer for 85%, CBN-Co
Score is 15%；In the second transition zone, WC-Co accounts for that the mass fraction of this layer is 80%, CBN-Co accounts for the mass fraction of this layer and is
20%；In outer wear layer, WC-Co accounts for that the mass fraction of this layer is 75%, to account for the mass fraction of this layer be 25% to CBN-Co.
Following example 4 ~ 6 are the preparation methods for preparing WC-Co and CBN-Co the graded composite cutter material of embodiment 1.
Embodiment 4
A method of WC-Co and CBN-Co graded composite cutter material being prepared, the pre- place of selection, powder including raw material
Reason, chemical plating metal Co and discharge plasma sintering, specific steps are as follows:
1, the selection of raw material
The superfine ceramic powder that this method uses is: (a) WC powder, purity be greater than 99.1%, average grain diameter 400nm,
Random cerioid particle, theoretical density 14.83g/cm3；(b) CBN powder, purity is greater than 99.0%, average grain diameter
500nm。
2, it pre-processes
Chemical plating must could occur on the surface with catalytic activity, and WC and CBN powder surface does not have this urge
Change activity, so surface preparation must be carried out to it, depositing one layer of noble metal with catalytic performance on its surface can just make
Obtaining chemical plating can go on smoothly.Pretreatment generally comprises following steps: roughening, sensitization, activation, drying；Superfine powder
Pretreatment have a great impact to plating process, especially sensitization, activation process.
In the present invention, ceramic powder is handled using sensitization activation one-step method, to shorten pretreatment time.
2.1 roughening treatment
Roughening treatment is carried out to above-mentioned raw materials powder respectively.The purpose of roughening is that form powder granule surface countless micro-
Small concave surface, increase absorption surface power is big, is adsorbed on precious metal ion at this, convenient for the progress of reduction process.
Coarsening process:
(a) WC and CBN powder to be pre-treated is separately added into coarsening solution, ultrasonic oscillation 30 minutes at room temperature；
(b) stand to powder sedimentation, powder is taken out, then three times with deionized water cleaning powder body.
Powder settling ratio after roughening is very fast, and about or so half an hour can settle completely, since coarsening solution contains hydrogen fluorine
Acid, it is necessary to be carried out in plastic containers.
The composition of coarsening solution used in roughening treatment are as follows: the ammonium fluoride of the hydrofluoric acid of 20ml/l and 2 g/l；To configure 100ml
For coarsening solution, preparation method are as follows: 0.2g ammonium fluoride is dissolved in 50ml deionized water, then in the ammonium fluoride being completely dissolved
The middle hydrofluoric acid that 2ml concentration about 40% is added, is settled to 100ml after mixing evenly.
2.2 sensitizations are activated
Sensitized treatment, which makes to be roughened treated ceramic grain surface, adsorbs one layer of colloidal substance with reducing power,
When subsequent activation processing, these substances make activator be reduced to form catalysis nucleus, and later chemical plating can be in these tables
Face carries out.
The present invention is aided with ultrasonic wave and is dispersed to powder using sensitization activation one-step method.
It is sensitized activation process: at room temperature, WC the and CBN powder being roughened being separately added into sensitization activating solution, ultrasound
It wave concussion reaction 30 minutes, is then allowed to stand to powder sedimentation, powder is taken out from sensitization activating solution, is cleaned with deionized water
3 times, and powder is isolated with centrifuge.
The composition of sensitization activating solution used are as follows: the chlorination of the palladium chloride of 0.5 g/l, the stannous chloride of 30 g/l, 160 g/l
The hydrochloric acid of sodium and 60ml/l；For configuring 500ml sensitization activating solution, preparation method are as follows:
(a) stirring and dissolving in palladium chloride addition 30ml concentrated hydrochloric acid (concentration 37%) of 0.25g is weighed, become after being completely dissolved
For transparent salmon solution, deionized water is added until 50ml is to get to solutionA；
(b) sodium chloride that weighs 80g is dissolved in 250ml deionized water, obtain solutionB；
(c) by solutionAWith solutionBIt mixes, stirs evenly, obtain solutionC;
(d) stannous chloride that weighs 15g is dissolved in the deionized water of 150ml, obtain the solution of whiteD；
(e) solutionDSolution is added while stirringCIn, obtain dark green solutionE；
(f) deionized water is added is settled to 500ml to get to bottle-green sensitization activating solution.
2.3 drying
WC the and CBN powder after sensitization activation is dried using 101A-1 type drying box (heating power 3kw), temperature
It is 80oC。
3, chemical plating metal Co
Using the method for chemical plating, respectively to pretreated WC and CBN powder surface plating one in device shown in Fig. 2
Layer Co metal.
Plating solution composition used are as follows: using the cobaltous sulfate of 15 g/l as the trisodium citrate of main salt, 50 g/l be complexing agent, 20
The sodium hypophosphite of g/l is reducing agent, 25 g/l boric acid are buffer；For configuring 500ml plating solution, preparation method is such as
Under:
(a) deionized water dissolving main salt is used, obtain solutiona；
(b) deionized water dissolving trisodium citrate is used, obtain clear solutionb；
(c) by solutionaSolution is addedbIn, it is stirred solution, obtains main salt complex solutionc；
(d) under room temperature, with deionized water dissolving sodium hypophosphite, stir evenly, obtain solutiond；
(e) by solutiondSolution is addedcIn, it is stirring while adding, obtain solutione；
(f) deionized water dissolving boric acid is used, it stirs evenly, obtains clear solutionf；
(g) solution f is addedeIn, it is stirring while adding, obtain plating solution；
(h) it with sodium hydroxide adjustment PH is 8, then plus water volumetric flask constant volume.
As shown in Fig. 2, the reaction vessel beaker for carrying out chemical plating is placed in the sink of ultrasonic oscillator, and it is equipped with stirring
Device；Before plating, the stirring that powder to be plated is carried out 10min with magnetic stirring apparatus is pre-dispersed, to ensure not having in powder
With the presence of bulky grain, ultrasonic wave dispersion and auxiliary humidification are improved；Then weigh it is a certain amount of it is pre-dispersed after powder to be plated
Be placed in a beaker, then measure a certain amount of prepared plating solution and pour into beaker, then place the beaker in device shown in Fig. 2 into
Row cladding.When work, blender stirring is started, so that powder granule is suspended in the plating solution, and guarantee that bath concentration is uniform, keeps anti-
Answer temperature less than 70 DEG C.
A large amount of bubbles will be generated after electroless plating reaction starts, in plating solution, and (this is also the mark that observing response carries out in experiment
It is quasi-), after reaction carries out a period of time, with the disappearance of bubble in plating solution, reaction stops.After standing, the WC-Co of metal Co has been coated
Powder and CBN-Co powder deposit to beaker bottom, plating solution lighter.
4, the post-processing of powder
WC-Co powder, the CBN-Co powder of chemical plating acquisition are deposited on container bottom, separate plating solution and WC- with centrifuge
After Co powder and CBN-Co powder, clean WC-Co powder and CBN-Co powder 3-4 times with deionized water, until cleaning go from
Sub- water is transparent, the WC-Co powder cleaned up and CBN-Co powder can be placed in 101A-1 type drying box and dried, kept away
Exempt from influence of the remaining plating solution composition to powder, the WC-Co powder and CBN-Co powder after drying can be used to subsequent preparation and answer
With.
5, the preparation of mixed powder
As shown in Figure 1, base layer is WC-Co, articulamentum, First Transition layer, the second transition in graded composite cutter material
Layer and outer wear layer are the mixed powder of WC-Co and CBN-Co, since WC-Co powder has been obtained through abovementioned steps, because
This, below mainly prepares the mixed powder of WC-Co used in each layer and CBN-Co.
(1) in articulamentum 95%WC-Co and 5%CBN-Co mixed powder preparation
Mass percent according to WC-Co is 95%, the mass percent of CBN-Co is that 5% chemical plating of learning from else's experience respectively is resulting
WC-Co powder and CBN-Co powder, are poured into the container equipped with deionized water, are uniformly mixed so as to obtain mixture A, the quality of deionized water
It is 7 ~ 8 times of WC-Co powder and CBN-Co powder gross mass；Mixture A is stirred by ultrasonic, ultrasonic wave 120-170Hz,
Stirring rate is 180 ~ 220r/min, and keeping the temperature of mixture A is 105 DEG C；After 35min is stirred by ultrasonic, according to poly- second two
The mass ratio of pure and mild mixture A is 1:80, and taking polyethylene glycol is added in mixture A, continues 15 ~ 20min of ultrasonic agitation, obtain
Mixture B；Gained mixture B is dried in vacuo 24 ~ 25h under the conditions of 140 ~ 160 DEG C, is sieved, obtains 95%WC-Co and 5%
The mixed powder of CBN-Co.
(2) in First Transition layer 90%WC-Co and 10%CBN-Co mixed powder preparation
Mass percent according to WC-Co is 90%, the mass percent of CBN-Co is 10% to be learnt from else's experience obtained by chemical plating respectively
WC-Co powder and CBN-Co powder, pour into the container equipped with deionized water, be uniformly mixed so as to obtain mixture C, the matter of deionized water
Amount is 7 ~ 8 times of WC-Co powder and CBN-Co powder gross mass；Mixture C is stirred by ultrasonic, ultrasonic wave 120-
170Hz, stirring rate are 180 ~ 220r/min, and keeping the temperature of mixture C is 105 DEG C；After 35min is stirred by ultrasonic, according to
Polyethylene glycol and the mass ratio of mixture C are 1:80, and taking polyethylene glycol is added in mixture C, continue ultrasonic agitation 15 ~
20min obtains mixture D；Gained mixture D is dried in vacuo 24 ~ 25h under the conditions of 140 ~ 160 DEG C, is sieved, obtains 90%
The mixed powder of WC-Co and 10%CBN-Co.
The preparation of 85%WC-Co and 15%CBN-Co mixed powder in (3) second transition zones
Mass percent according to WC-Co is 85%, the mass percent of CBN-Co is 15% to be learnt from else's experience obtained by chemical plating respectively
WC-Co powder and CBN-Co powder, pour into the container equipped with deionized water, be uniformly mixed so as to obtain mixture E, the matter of deionized water
Amount is 7 ~ 8 times of WC-Co powder and CBN-Co powder gross mass；Mixture E is stirred by ultrasonic, ultrasonic wave 120-
170Hz, stirring rate are 180 ~ 220r/min, and keeping the temperature of mixture E is 105 DEG C；After 35min is stirred by ultrasonic, according to
Polyethylene glycol and the mass ratio of mixture E are 1:80, and taking polyethylene glycol is added in mixture E, continue ultrasonic agitation 15 ~
20min obtains mixture F；Gained mixture F is dried in vacuo 24 ~ 25h under the conditions of 140 ~ 160 DEG C, is sieved, obtains 85%
The mixed powder of WC-Co and 15%CBN-Co.
(4) in outer wear layer 80%WC-Co and 20%CBN-Co mixed powder preparation
Mass percent according to WC-Co is 80%, the mass percent of CBN-Co is 20% to be learnt from else's experience obtained by chemical plating respectively
WC-Co powder and CBN-Co powder, pour into the container equipped with deionized water, be uniformly mixed so as to obtain mixture G, the matter of deionized water
Amount is 7 ~ 8 times of WC-Co powder and CBN-Co powder gross mass；Mixture G is stirred by ultrasonic, ultrasonic wave 120-
170Hz, stirring rate are 180 ~ 220r/min, and keeping the temperature of mixture G is 105 DEG C；After 35min is stirred by ultrasonic, according to
The mass ratio of polyethylene glycol and mixture G are 1:80, and taking polyethylene glycol is added in mixture G, continue ultrasonic agitation 15 ~
20min obtains mixture F；Gained mixture H is dried in vacuo 24 ~ 25h under the conditions of 140 ~ 160 DEG C, is sieved, obtains 80%
The mixed powder of WC-Co and 20%CBN-Co.
6, discharge plasma sintering
By above-mentioned resulting WC-Co powder, 95%WC-Co and 5%CBN-Co mixed powder, 90%WC-Co and 10%CBN-Co
Mixed powder, 85%WC-Co and 15%CBN-Co mixed powder and 80%WC-Co and 10%CBN-Co mixed powder, according to shown in Fig. 1
Material sequence be respectively charged into (i.e. according to the sequence of base layer, articulamentum, First Transition layer, the second transition zone and outer wear layer)
Graphite jig is placed in vacuum environment, and then uniform pressurization carries out discharge plasma sintering；When sintering, risen to from room temperature
During 1800 DEG C, environmental pressure even adds to 50MPa, later under the conditions of temperature is 1800 DEG C, pressure 50MPa
30 ~ 40min is kept the temperature, powers off cooled to room temperature then to get WC-Co and CBN-Co graded composite cutter material is arrived.
During Fig. 3 is the discharge plasma sintering of WC-Co and CBN-Co graded composite cutter material, in particle contact position
Generate the schematic diagram of electric discharge phenomena.Since Co is conductive powder body, by applying electric field, the contact site Co of cladding can discharge
Phenomenon generates localized hyperthermia, promotes Co metal molten, and under acting on while big pressure, the cobalt of melting is filled into ceramic particle
Gap in, form fine and close gradient cutter composite material.
Embodiment 5
On the basis of embodiment 4, the composition of plating solution used in chemical plating are as follows: using the cobaltous sulfate of 40g/l as main salt, 50 g/l
Trisodium citrate be complexing agent, 60 g/l sodium hypophosphite be reducing agent, 25 g/l boric acid are buffer；To configure 500ml
For plating solution, preparation method is as follows:
(a) deionized water dissolving main salt is used, obtain solutiona；
(b) deionized water dissolving trisodium citrate is used, obtain clear solutionb；
(c) by solutionaSolution is addedbIn, it is stirred solution, obtains main salt complex solutionc；
(d) under room temperature, with deionized water dissolving sodium hypophosphite, stir evenly, obtain solutiond；
(e) by solutiondSolution is addedcIn, it is stirring while adding, obtain solutione；
(f) deionized water dissolving boric acid is used, it stirs evenly, obtains clear solutionf；
(g) solution f is addedeIn, it is stirring while adding, obtain plating solution；
(h) it with sodium hydroxide adjustment PH is 11, then plus water volumetric flask constant volume.
The operating method of remaining step is same as Example 1.
Embodiment 6
On the basis of embodiment 4, the composition of plating solution used in chemical plating are as follows: using the cobaltous sulfate of 25g/l as main salt, 50 g/l
Trisodium citrate be complexing agent, 40 g/l sodium hypophosphite be reducing agent, 25 g/l boric acid are buffer；To configure 500ml
For plating solution, preparation method is as follows:
(a) deionized water dissolving main salt is used, obtain solutiona；
(b) deionized water dissolving trisodium citrate is used, obtain clear solutionb；
(c) by solutionaSolution is addedbIn, it is stirred solution, obtains main salt complex solutionc；
(d) under room temperature, with deionized water dissolving sodium hypophosphite, stir evenly, obtain solutiond；
(e) by solutiondSolution is addedcIn, it is stirring while adding, obtain solutione；
(f) deionized water dissolving boric acid is used, it stirs evenly, obtains clear solutionf；
(g) solution f is addedeIn, it is stirring while adding, obtain plating solution；
(h) it with sodium hydroxide adjustment PH is 9, then plus water volumetric flask constant volume.
The operating method of remaining step is same as Example 1.
In preparation method of the present invention, it should be noted that:
(1) the ceramic powder sinking speed after sensitization is activated is very slow, and settling 4-5 hours in activating solution could settle
Completely；When deionized water cleaning is added, sinking speed is substantially reduced, or even is difficult to settle completely, and sedimentation will reach after cleaning
15 hours or more；Second, third time cleaning is even wanted 24 hours or more to be all difficult to settle completely.This may be since sensitization is lived
Nano powder surface after change has adsorbed a large amount of charged ion, so that there is certain repulsive interaction between particle, improves pottery
The dispersibility of porcelain powder causes to settle slack-off, it is therefore desirable to separate powder using centrifuge.
(2) pretreated powder appearance changes less compared with before processing, and scale is suitable, but passes through pretreated powder
Dispersibility preferably.The result is consistent with phenomenon what is observed in preprocessing process, it is believed that preprocessing process is not
Only powder is activated, and plays ideal dispersion effect.
(3) it can generate heat during applying due to ultrasonic wave, so that the water in sink heats up, in order to which reaction temperature control exists
Within a certain range, palpus circulating water, temperature excessively high (70 oCMore than) supersonic generator can be damaged, and can reduce
Bath stability occurs selfdecomposition, generates free metal simple-substance.
Claims (8)
1. a kind of method for preparing WC-Co Yu CBN-Co graded composite cutter material, the material successively base as made of being sintered
Body layer, articulamentum, First Transition layer, the second transition zone and outer wear layer composition, from outer wear layer to base layer, each layer accounts for material
The mass fraction for expecting gross mass is respectively 15%, 12.5%, 10%, 7.5% and 55%, base layer WC-Co, articulamentum, First Transition
Layer, the second transition zone and outer wear layer are the mixed powder of WC-Co and CBN-Co, and from articulamentum to outer wear layer,
The mass fraction of WC-Co is reduced in gradient；It is characterized by: coating metal in two kinds of powder surfaces of WC and CBN by chemical plating
Co obtains two kinds of powders of WC-Co and CBN-Co, and using WC-Co as base layer, the mixed powder of WC-Co and CBN-Co is not with
With mixed proportion respectively as articulamentum, First Transition layer, the second transition zone and outer wear layer, according to base layer, articulamentum,
The sequence of one transition zone, the second transition zone and outer wear layer after being successively seated in graphite jig, uniformly adds under vacuum condition
Pressure carries out discharge plasma sintering, powers off cooled to room temperature then to get graded composite cutter material is arrived；
Main salt is the cobaltous sulfate of 15 ~ 40 g/l in plating solution used in the chemical plating, complexing agent is 50 g/l trisodium citrate,
Reducing agent is the sodium hypophosphite of 20 ~ 60 g/l, buffer is 25 g/l boric acid, the method for preparing plating solution are as follows:
(1) deionized water dissolving cobaltous sulfate is used, solution is obtaineda；
(2) deionized water dissolving trisodium citrate is used, clear solution is obtainedb；
(3) by solutionaSolution is addedbIn, it is stirred solution, obtains main salt complex solutionc；
(4) it under room temperature, with deionized water dissolving sodium hypophosphite, stirs evenly, obtains solutiond；
(5) solution d is added in main salt complex solution c, it is stirring while adding, obtain solution e；
(6) deionized water dissolving boric acid is used, stirs evenly, obtains clear solutionf；
(7) solution is added in solution feIn, it is stirring while adding, obtain plating solution；
It then plus deionized water constant volume (8) is 8 ~ 11 with the pH value of sodium hydroxide adjustment plating solution,；
In articulamentum, First Transition layer, the second transition zone and outer wear layer, the mixed powder of each layer of WC-Co and CBN-Co
Preparation method are as follows:
According to mass fraction of the WC-Co and CBN-Co in the layer of place, the WC-Co powder and CBN- of chemical plating of learning from else's experience respectively
Co powder pours into the container equipped with deionized water, is uniformly mixed so as to obtain mixture I, the quality of deionized water be WC-Co powder and
7 ~ 8 times of CBN-Co powder gross mass；Mixture I is stirred by ultrasonic, keeping the temperature of mixture I is 105 DEG C；Ultrasound is stirred
It is 1:80 according to the mass ratio of polyethylene glycol and mixture I after mixing 35min, taking polyethylene glycol is added in mixture I, is continued
Ultrasonic agitation, obtains mixture II；It is sieved after gained mixture II is dried in vacuo, obtains the mixed powder of WC-Co and CBN-Co
Body；
During the discharge plasma sintering, the base layer, articulamentum, the First Transition layer, that are seated in graphite jig
The mass fraction that two transition zones and outer wear layer account for graded composite cutter material is followed successively by 55%, 7.5%, 10%, 12.5% and 15%.
2. the method according to claim 1 for preparing WC-Co Yu CBN-Co graded composite cutter material, it is characterised in that:
The WC powder purity is greater than 99.1%, average grain diameter 400nm, theoretical density 14.83g/cm3；CBN powder purity is big
In 99.0%, average grain diameter 500nm.
3. the method according to claim 1 for preparing WC-Co Yu CBN-Co graded composite cutter material, it is characterised in that:
It before carrying out chemical plating to two kinds of powders of WC and CBN, is pre-processed respectively, pretreatment includes roughening, sensitization activation and dries
It is dry.
4. the method according to claim 3 for preparing WC-Co Yu CBN-Co graded composite cutter material, it is characterised in that:
The roughening is that powder to be processed is added in coarsening solution, at room temperature supersonic oscillations；It is then allowed to stand to powder sedimentation,
Powder is taken out from coarsening solution, the powder of sedimentation is cleaned with deionized water, isolates powder；The composition packet of the coarsening solution
Include the hydrofluoric acid of 20ml/l and the ammonium fluoride of 2g/l.
5. the method according to claim 3 for preparing WC-Co Yu CBN-Co graded composite cutter material, it is characterised in that:
Sensitization activation is will to be roughened that treated powder is added in sensitization activating solution, and supersonic oscillations, then quiet at room temperature
It sets to powder sedimentation, takes out the powder of sedimentation, after being cleaned with deionized water, powder is isolated by centrifuge；The sensitization is lived
The composition for changing liquid includes the palladium chloride of 0.5 g/l, the stannous chloride of 30 g/l, the sodium chloride of 160 g/l and the hydrochloric acid of 60ml/l.
6. the method according to claim 3 for preparing WC-Co Yu CBN-Co graded composite cutter material, it is characterised in that:
Before the chemical plating, it is pre-dispersed that pretreated powder is carried out to magnetic agitation respectively.
7. the method according to claim 1 for preparing WC-Co Yu CBN-Co graded composite cutter material, it is characterised in that:
In the discharge plasma sintering, during rising to 1800 DEG C from room temperature, environmental pressure even adds to 50MPa,
20 ~ 30min is kept the temperature under the conditions of temperature is 1800 DEG C, pressure 50MPa later, then powers off cooled to room temperature.
8. the method according to claim 5 for preparing WC-Co Yu CBN-Co graded composite cutter material, it is characterised in that:
The preparation method of the sensitization activating solution is:
(1) stirring and dissolving in 30ml concentrated hydrochloric acid is added in the palladium chloride for weighing 0.25g, and it is molten to become transparent salmon after being completely dissolved
Liquid adds deionized water until 50ml is to get to solutionA；
(2) sodium chloride for weighing 80g is dissolved in 250ml deionized water, obtains solutionB；
(3) by solutionAWith solutionBIt mixes, stirs evenly, obtain solutionC;
(4) stannous chloride for weighing 15g is dissolved in the deionized water of 150ml, obtains the solution of whiteD；
(5) solutionDSolution is added while stirringCIn, obtain dark green solutionE；
(6) to solutionEDeionized water is added and is settled to 500ml, obtains bottle-green sensitization activating solution.
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