CN102560170A - WC-Fe-Y2O3 (Sc2O3) nano-cladded alloy and preparation method capable of inhibiting Eta phase in mechanical activation process - Google Patents

WC-Fe-Y2O3 (Sc2O3) nano-cladded alloy and preparation method capable of inhibiting Eta phase in mechanical activation process Download PDF

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CN102560170A
CN102560170A CN201210046589XA CN201210046589A CN102560170A CN 102560170 A CN102560170 A CN 102560170A CN 201210046589X A CN201210046589X A CN 201210046589XA CN 201210046589 A CN201210046589 A CN 201210046589A CN 102560170 A CN102560170 A CN 102560170A
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alloy
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mechanical activation
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CN102560170B (en
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徐培全
杨尚磊
卢庆华
任江伟
邓沛然
闫华
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Shanghai University of Engineering Science
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Abstract

The invention discloses a WC-Fe-Y2O3 (Sc2O3) nano-cladded alloy. The WC-Fe-Y2O3 (Sc2O3) nano-cladded alloy is prepared from the mixture of the following materials by weight percent: 48-62 percent of nano-WC powder, 33-49 percent of nano-Fe powder, 2-8 percent of nano-Y2O3 powder, and 1-3 percent of nano-Sc2O3 powder. By adding nano-Y2O3 rare earth and nano-Sc2O3 rare earth, an Eta phase which is easily formed in a high-energy ball milling process of the nano-WC powder and the nano-Fe powder can be inhibited in a combined way. The WC-Fe-Y2O3 (Sc2O3) nano-cladded alloy can be applied to laser repair of surfaces of a thick steel plate and an invar and is applied to production and repair of a ship, a valve and other products.

Description

A kind of WC-Fe-Y 2O 3(Sc 2O 3) the nanometer cladding alloy and the preparation method that can suppress the η phase in the mechanical activation process
Technical field
The present invention relates to a kind of nano surface cladding alloy, specifically, is a kind of WC-Fe-Y 2O 3(Sc 2O 3) the nanometer cladding alloy and the preparation method that can suppress the η phase in the mixed powder mechanical activation process, can be used for the laser repairing on thick plate steel and Invar alloy surface.
Background technology
Slab steel and Invar alloy are to make hull, the isostructural critical material of valve, and destructions such as fatigue, wearing and tearing are taken place in the process under arms, have a strong impact on the use properties of product.On the other hand; In the manufacturing processed of hull, valve; The laser melting coating manufacturing technology is more and more ripe; Can go out one deck in steel or Invar alloy surface preparation and have high temperature resistant, wear-resistant and corrosion resistant structure, make product both had steel or Invar alloy anti-corrosion, be prone to the performance that is shaped, high temperature resistant, the wear-resistant and corrosion resistant performance that has cladding layer simultaneously and possessed.At shipbuilding industry and oil gas carrier, stainless steel, Invar alloy, wimet are the important materials of producing key components and parts.The reparation of key components and parts and to make all be to prolong product service life, energy-saving and cost-reducing key issue again.And one of key issue that laser melting and coating technique is used for the high-end product manufacturing to be exploitation mature and stable and have the cladding alloy of excellent properties.
In various cladding alloys, the alloy that contains transition element (Fe, Co, Ni) is widely applicable a kind of material, particularly Fe base alloy material, owing to have good economy performance, with steel, the Invar alloy fusion character is good and widespread use.Secondly, WC is a kind of strengthening element commonly used, have wear resisting property and corrosion resisting property well, the high-temperature behavior excellent characteristics.The particularly application of nanometer WC is used to develop the cladding alloy with nanometer WC, not only has micron performance that WC had, and significantly improves the fracture property of WC, has important effect for the toughness that improves cladding layer.Therefore, nanometer WC is mixed use with nanometer Fe, the bonding that makes full use of nanometer WC and Fe mutually with the effect of strengthening phase, significant for the high-end cladding alloy of exploitation.In the process of WC-Fe alloy preparation; Because the W-C-Fe system is under activation condition; Competent energy will make WC decompose; Diffusion to WC will take place in active big nanometer Fe, and WC forms the η phase owing to losing carbon and transition element to the matrix diffusion, and the formation of η phase can reduce the over-all properties of cladding alloy.
To micron-sized WC-Fe alloy system, proposed under the equilibrium conditions through regulating C, rare earth, Cr 3C 2, composition means control interface η phases such as the poor Co of poor C/, M/C formation and form; Perhaps suppress the formation that η equates intermediate phase through the control synthesis temperature, experiment proves effective.Through the literature search of prior art is found, W Barona Mercado etc. are at magazine Hyperfine Interact, and 2007, the paper that deliver 175:49～54 " Sythesis and characterization of Fe 6W 6C by mechanical alIoying " in, propose to utilize method mechanical activation W, C, the Fe mixed powder of mechanical alloying, carried out the ball milling of 1h, 3h, 5h, 10h, 15h, 30h respectively; along with the carrying out of time; three kinds of powder mix gradually, but in mixing process, have formed Fe 3W 3C, Fe 6W 6η phases such as C.The generation of these non-equilibrium products reduces the toughness of cladding layer easily, reduces surperficial mechanical property.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, developed a kind of WC-Fe-Y 2O 3(Sc 2O 3) nanometer cladding alloy.
The present invention also provides above-mentioned WC-Fe-Y 2O 3(Sc 2O 3) preparation method of nanometer cladding alloy, and nanometer cladding alloy prepares the η phase control method in the process.
For realizing the foregoing invention purpose, technical scheme of the present invention is following:
A kind of WC-Fe-Y 2O 3(Sc 2O 3) nanometer cladding alloy, prepare the used material of this alloy by nanometer WC powder, nanometer Fe powder, nanometer Y 2O 3Powder, nanometer Sc 2O 3Powder is formed, and each components based on weight percentage is respectively in the mixture: WC powder 48～62%, nanometer Fe powder 33～49%, nanometer Y 2O 3Powder 2～8%, nanometer Sc 2O 3Powder 1～3%.
A kind of preparation method who suppresses the η phase in the mixed powder mechanical activation process prepares this WC-Fe-Y 2O 3(Sc 2O 3) method of nanometer cladding alloy, comprise the steps:
(1) by above-mentioned each raw material of content weighing, with the nanometer WC powder after the weighing, nanometer Fe powder, nanometer Y 2O 3Powder, nanometer Sc 2O 3Powder mixed grinding in mortar is even, and the time is unsuitable long, prevents oxidation of iron powder;
(2) adopt mechanical activation technology, the mixed powder of step (1) through mechanical activation, is obtained WC-Fe-Y 2O 3(Sc 2O 3) nanometer cladding alloy.
Described mechanical activation technology is: ball material weight ratio is that 15: 1, the rotating speed of main shaft are 400 rev/mins, countershaft rotating speed-400 rev/min, ball milling time 15h; Grinding ball material can be selected carbon tungsten alloy (WC), ball radius 5～10mm for use.
For preventing that the metal-powder oxidation takes place in the mechanical milling process, dress appearance and sampling are all carried out in the glove box under the atmosphere protection in the ball grinder; Shielding gas is argon gas or helium.
WC, Sc described in the step (1) 2O 3The particle diameter of powder particle is 100nm, Fe, Y 2O 3The particle diameter of powder particle is 50nm.
The present invention is through adding rare earth nano Y 2O 3, nanometer Sc 2O 3, unite and suppress in nanometer WC and the Fe powder high-energy ball milling process easily the η of formation mutually.
WC-Fe-Y of the present invention 2O 3(Sc 2O 3) nanometer cladding alloy can be applicable to the laser repairing on thick plate steel and Invar alloy surface, is used for the production and the reparation of products such as hull, valve.
Description of drawings
Fig. 1 is WC-Fe-Y behind the mechanical activation 2O 3(Sc 2O 3) nanometer cladding alloy XRD phase composite;
Fig. 2 is WC-Fe-Y 2O 3(Sc 2O 3) the scanning pattern and the back scattering figure of nanometer cladding alloy;
Wherein, (a) SEM phase; (b) become phase-splitting for the corresponding back scattering in this visual field;
Fig. 3 is TEM, SEAD diffraction pattern and the HRTEM figure of nano particle;
Wherein, (a) be nanoparticle transmission electron microscope pattern behind the mechanical activation; (b) be the high resolution shape appearance figure of nanoparticle.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is done further in detail, intactly explains:
Embodiment 1
Described preparation WC-Fe-Y 2O 3(Sc 2O 3) the mechanical activation step of nanometer cladding alloy is following,
(1) at first will be scattered in nanometer WC powder, nanometer Fe powder, nanometer Y in the alcohol 2O 3Powder, nanometer Sc 2O 3Powder is drying for standby in vacuum drying oven, weighs after the taking-up, and weight percent is respectively 57.6%, 33.4%, 8%, 1%; In mortar mixed grinding evenly after, argon gas atmosphere condition lower seal is preserved;
(2) adopt mechanical activation technology, step (1) mixed powder is carried out mechanical activation, obtain WC-Fe-Y 2O 3(Sc 2O 3) nanometer cladding alloy.Mechanical activation technology is: ball material weight ratio is that 15: 1, the rotating speed of main shaft are 400 rev/mins, 400 rev/mins of countershaft rotating speeds, ball milling time 15h; Grinding ball material can be selected carbon tungsten alloy (WC), ball radius 5mm for use;
(3) sampling analysis.Behind the 15h, take out sample in the glove box in the ball grinder under the argon gas atmosphere protection, distributed and saved is subsequent use in alcohol.
WC, Sc described in the step (1) 2O 3The particle diameter of powder particle is 100nm, Fe, Y 2O 3The particle diameter of powder particle is 50nm.
Embodiment 2
Described preparation WC-Fe-Y 2O 3(Sc 2O 3) the mechanical activation step of nanometer cladding alloy is following,
(1) at first will be scattered in nanometer WC powder, nanometer Fe powder, nanometer Y in the alcohol 2O 3Powder, nanometer Sc 2O 3Powder is drying for standby in vacuum drying oven, weighs after the taking-up, and weight percent is respectively: WC powder 58%, nanometer Fe powder 33%, nanometer Y 2O 3Powder 8%, nanometer Sc 2O 3Powder 1%. In mortar mixed grinding evenly after, argon gas atmosphere condition lower seal is preserved;
(2) adopt mechanical activation technology, step (1) mixed powder is carried out mechanical activation, obtain WC-Fe-Y 2O 3(Sc 2O 3) nanometer cladding alloy.Mechanical activation technology is: ball material weight ratio is that 15: 1, the rotating speed of main shaft are 400 rev/mins, 400 rev/mins of countershaft rotating speeds, ball milling time 15h; Grinding ball material can be selected carbon tungsten alloy (WC), ball radius 5mm for use;
(3) sampling analysis.Behind the 15h, take out sample in the glove box in the ball grinder under the argon gas atmosphere protection, distributed and saved is subsequent use in alcohol.
Embodiment 3
Described preparation WC-Fe-Y 2O 3(Sc 2O 3) the mechanical activation step of nanometer cladding alloy is following,
(1) at first will be scattered in nanometer WC powder, nanometer Fe powder, nanometer Y in the alcohol 2O 3Powder, nanometer Sc 2O 3Powder is drying for standby in vacuum drying oven, weighs after the taking-up, and weight percent is respectively: WC powder 62%, nanometer Fe powder 35%, nanometer Y 2O 3Powder 2%, nanometer Sc 2O 3Powder 1%; In mortar mixed grinding evenly after, argon gas atmosphere condition lower seal is preserved;
(2) adopt mechanical activation technology, step (1) mixed powder is carried out mechanical activation, obtain WC-Fe-Y 2O 3(Sc 2O 3) nanometer cladding alloy.Mechanical activation technology is: ball material weight ratio is that 15: 1, the rotating speed of main shaft are 400 rev/mins, 400 rev/mins of countershaft rotating speeds, ball milling time 15h; Grinding ball material can be selected carbon tungsten alloy (WC), ball radius 5mm for use;
(3) sampling analysis.Behind the 15h, take out sample in the glove box in the ball grinder under the argon gas atmosphere protection, distributed and saved is subsequent use in alcohol.
Embodiment 4
Described preparation WC-Fe-Y 2O 3(Sc 2O 3) the mechanical activation step of nanometer cladding alloy is following,
(1) at first will be scattered in nanometer WC powder, nanometer Fe powder, nanometer Y in the alcohol 2O 3Powder, nanometer Sc 2O 3Powder is drying for standby in vacuum drying oven, weighs after the taking-up, and weight percent is respectively WC powder 60%, nanometer Fe powder 34%, nanometer Y 2O 3Powder 4%, nanometer Sc 2O 3Powder 2%; In mortar mixed grinding evenly after, argon gas atmosphere condition lower seal is preserved;
(2) adopt mechanical activation technology, step (1) mixed powder is carried out mechanical activation, obtain WC-Fe-Y 2O 3(Sc 2O 3) nanometer cladding alloy.Mechanical activation technology is: ball material weight ratio is that 15: 1, the rotating speed of main shaft are 400 rev/mins, 400 rev/mins of countershaft rotating speeds, ball milling time 15h; Grinding ball material can be selected carbon tungsten alloy (WC), ball radius 5mm for use;
(3) sampling analysis.Behind the 15h, take out sample in the glove box in the ball grinder under the argon gas atmosphere protection, distributed and saved is subsequent use in alcohol.
Through detection, behind the mixed powder process mechanical activation, WC-Fe-Y 2O 3(Sc 2O 3) nanometer cladding alloy XRD facies analysis result shown in accompanying drawing 1, can know that from the result at mechanical activation after 15 hours, main phase place WC, Fe and a spot of WC-η transition phase mutually do not have η to form mutually, Rare Earth Y 2O 3And Sc 2O 3Adding, suppressed the formation of η phase.
WC-Fe-Y 2O 3(Sc 2O 3) nanometer cladding alloy SEM mutually and backscatter images shown in accompanying drawing 2; Fig. 2 (a) is the SEM phase, and Fig. 2 (b) becomes phase-splitting for the corresponding back scattering in this visual field, the different composition of pixel grey scale representative of black and white; Can know; Staple is the WC and the gray Fe of white, and there is certain transition phase the centre, does not have η to form mutually.
Test-results adopts transmission electron microscope structural characterization verification experimental verification, and shown in accompanying drawing 3, Fig. 3 (a) is the nanoparticle transmission electron microscope pattern behind the mechanical activation; The embedded figure in the upper left corner is that electron diffraction pattern (SAED is chosen in the transmission of nanoparticle; Selected Area Electron Diffraction), show that this nanoparticle structure has not been single WC or Fe structure, but a kind of mixed structure; But do not comprise the η phase structure; Fig. 3 (b) is the high resolution shape appearance figure of nanoparticle, visible significantly lattice (amplifying lattice shown in embedded figure), and the fourier transformation of edge lattice (Fourier Transform) is shown in the embedded figure in the upper right corner.Therefore, according to XRD test-results, SEM and back scattering test and transmission electron microscope high resolution analysis structure, can judge: WC-Fe-Y of the present invention 2O 3(Sc 2O 3) nanometer cladding alloy is that a kind of nanoparticle is reunited on a small quantity with WC and Fe uniform mixing, the alloy that does not have η to form mutually.The Rare Earth Y that proposes 2O 3And Sc 2O 3Adding, suppressed the formation of η phase.

Claims (6)

1. WC-Fe-Y 2O 3(Sc 2O 3) nanometer cladding alloy, it is characterized in that: prepare the used material of this alloy by nanometer WC powder, nanometer Fe powder, nanometer Y 2O 3Powder, nanometer Sc 2O 3Powder is formed, and each components based on weight percentage is respectively in the mixture: WC powder 48～62%, nanometer Fe powder 33～49%, nanometer Y 2O 3Powder 2～8%, nanometer Sc 2O 3Powder 1～3%.
2. the preparation method that can suppress the η phase in the mixed powder mechanical activation process is characterized in that: prepare this WC-Fe-Y 2O 3(Sc 2O 3) method of nanometer cladding alloy, comprise the steps:
(1) by each raw material of proportioning weighing, with the nanometer WC powder after the weighing, nanometer Fe powder, nanometer Y 2O 3Powder, nanometer Sc 2O 3Powder mixed grinding in mortar is even, and the time is unsuitable long, prevents oxidation of iron powder;
(2) adopt mechanical activation technology, the mixed powder of step (1) through mechanical activation, is obtained WC-Fe-Y 2O 3(Sc 2O 3) nanometer cladding alloy.
3. preparation method according to claim 2 is characterized in that: described mechanical activation technology is: ball material weight ratio is that 15: 1, the rotating speed of main shaft are 400 rev/mins, countershaft rotating speed-400 rev/min, ball milling time 15h; Grinding ball material can be selected carbon tungsten alloy (WC), ball radius 5～10mm for use.
4. based on the described preparation method of claim 3, it is characterized in that: dress appearance and sampling are all carried out in the glove box under the atmosphere protection in the ball grinder; Protective gas is argon gas or helium.
5. preparation method according to claim 2 is characterized in that: WC, Sc described in the step (1) 2O 3The particle diameter of powder particle is 100nm, Fe, Y 2O 3The particle diameter of powder particle is 50nm.
6. WC-Fe-Y according to claim 1 2O 3(Sc 2O 3) nanometer cladding alloy, it is characterized in that: the laser repairing that can be applicable to thick plate steel and Invar alloy surface.
CN201210046589.XA 2012-02-27 2012-02-27 WC-Fe-Y2O3 (Sc2O3) nano-cladded alloy and preparation method capable of inhibiting Eta phase in mechanical activation process Expired - Fee Related CN102560170B (en)

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CN106086575A (en) * 2016-08-26 2016-11-09 洛阳金鹭硬质合金工具有限公司 A kind of steel bonded carbide and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN106086575A (en) * 2016-08-26 2016-11-09 洛阳金鹭硬质合金工具有限公司 A kind of steel bonded carbide and preparation method thereof
CN106086575B (en) * 2016-08-26 2017-10-20 洛阳金鹭硬质合金工具有限公司 A kind of steel bonded carbide and preparation method thereof

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