CN106756996B - A kind of rare earth modified laser cladding layer and its preparation process - Google Patents
A kind of rare earth modified laser cladding layer and its preparation process Download PDFInfo
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- CN106756996B CN106756996B CN201611113999.6A CN201611113999A CN106756996B CN 106756996 B CN106756996 B CN 106756996B CN 201611113999 A CN201611113999 A CN 201611113999A CN 106756996 B CN106756996 B CN 106756996B
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- 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
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/058—Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0005—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with at least one oxide and at least one of carbides, nitrides, borides or silicides as the main non-metallic constituents
Abstract
The present invention provides a kind of rare earth modified laser cladding layer and its preparation process.On titanium alloy substrate, with Ni60A Co-based alloy powder, B4C or nickel packet B4C(Ni@B4C), micron or nanometer level RE oxide are that cladding material laser melting coating prepares rare earth modified laser cladding layer.Part R2O3R and O can be decomposed into.Rare-earth element R can be adsorbed on crystal boundary, hinder crystal boundary mobile；The surface tension and Critical nucleation radius of liquid metal can also be reduced, nucleation rate is improved, thus thinning microstructure.Step is simple and convenient to operate, is practical.
Description
Technical field
The invention belongs to metal surface properties modification and reinforcement technique field, in particular to a kind of rare earth modified laser melting coating
Layer and its preparation process.
Background technique
Laser melting and coating technique is to form the material cladding of addition with substrate in substrate surface to be in using high energy laser beam
The cladding layer that existing metallurgy rank combines, improves the surface propertys such as surface hardness, wearability, corrosion resistance, the antioxygenic property of substrate.
Surface peening and modification are carried out to metal materials such as steel, titanium alloy, aluminium alloy, magnesium alloys using laser melting and coating technique,
As current one of research hotspot.
Laser melting and coating technique has the advantage that
(1) by designing reasonable cladding material composition and suitable laser melting coating parameter, fine microstructures can be obtained
Cladding layer fine and close and that metallurgical bonding is presented with matrix, realizes the improvement of substrate performance；
(2) cooling velocity fast (up to 10 when solidifying6DEG C/s), there is rapid solidification structure feature, be easily obtained amorphous Asia
Steady phase, ultra-fine or even nanoscale disperse educt mutually improve coating texture and performance；
(3) coating composition, thickness are controllable, and heat affected area is small, influence on substrate small；
(4) constituency cladding can be carried out, realizes increasing material manufacturing, stock utilization is high；
(5) technical process is easy to automate, high in machining efficiency, it can be achieved that high efficiency manufacture.
In laser cladding process, the design of cladding material is most important, is related to success or failure and the cladding layer of cladding process
Performance.The self-fluxing alloyed powders such as Ni base, Fe base, Co base are golden with majority due to having the function of good deoxidation slag making, while again
Belonging to material has good wetability, being most widely used in laser melting coating.On this basis, it is wanted according to the performance of material
It asks, the ceramic particles such as various dystectic carbide, nitride, boride and oxide is added in self-melting alloy, or logical
The mode for crossing reaction in-situ forms ceramic strengthening phase in cladding layer, forms cermet composite coating, further increases titanium conjunction
The microhardness and wearability of gold, so that the application prospect of laser melting and coating technique is more wide.
Some rare earth oxides are introduced in laser cladding of material, facilitate the microstructure for refining cladding layer, further
Improve coating performance.In recent years, nano material is due to good calorifics, magnetics, optics, superconductivity and chemical catalysis
Many performances different from conventional material such as matter and quantum size effect, skin effect, macro quanta tunnel effect, become
The big research hotspot of the one of functional material research field.Meanwhile while reinforcing to material again material can keep centainly
Therefore the attention for also causing domestic and international researcher is strengthened to material using nano material or be modified to toughness.
Summary of the invention
In order to overcome above-mentioned deficiency, the present invention provides a kind of rare earth modified laser cladding layer.It is molten in titanium alloy surface laser
Cover introducing oxide nano rare earth (nanometer Nd in material system2O3、La2O3), achieve preferable effect.Part R2O3It can decompose
For R and O.Rare-earth element R can be adsorbed on crystal boundary, hinder crystal boundary mobile；The surface tension of liquid metal and critical can also be reduced
Nucleation radius improves nucleation rate, thus thinning microstructure.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of rare earth modified laser cladding layer, on titanium alloy substrate, with Ni60A Co-based alloy powder, B4C or nickel packet B4C
(Ni@B4C), micron or nanometer level RE oxide are that cladding material laser melting coating prepares rare earth modified laser cladding layer.
Preferably, the cladding material middle rare earth is Nd2O3Or La2O3。
Preferably, in the cladding material each component mass percent are as follows: Nd2O31.0~4.0%, B4C or Ni@B4C
10~30%, Yu Wei Ni60A.
Preferably, in the cladding material each component mass percent are as follows: La2O31.0~4.0%, Ni@B4C 10~
30%, Yu Wei Ni60A.
Preferably, the Nd2O3Granularity be 5~20 μm or 40~60nm, be referred to as μ-Nd2O3Or n-Nd2O3。
Preferably, the La2O3The granularity of rare earth oxide is 5~20 μm or 40~60nm, is referred to as μ-La2O3Or
n-La2O3。
Most preferably, the Nd2O3Or La2O3Rare earth oxide is n-Nd2O3Or n-La2O3。
The ingredient for the Ni60A nickel base self-fluxing alloy powder that the present invention uses is as shown in table 1.
The chemical component (wt.%) of 1 Ni60A nickel base self-fluxing alloy powder of table
The present invention also provides a kind of preparation processes of rare earth modified laser cladding layer, comprising:
1) titanium-based material removing surface to be processed is clean, remove surface scale；
2) cladding powder is uniformly mixed, is layered on substrate surface in advance；
3) cladding is carried out to the sample for overlaying cladding powder to test to get rare earth modified laser cladding layer；
The cladding powder includes: Ni60A Co-based alloy powder, B4C or nickel packet B4C(Ni@B4C), micron or nanoscale are dilute
Native oxide.
Preferably, the cladding powder overlays with a thickness of 0.8~1.0mm.
Preferably, the laser melting coating condition are as follows: laser power be 1.0~3.0kW, scanning speed be 200~
600mm/min, spot diameter 3.0mm, argon gas protection molten bath is blowed in cladding process, and argon flow is 5~15L/min.
The present invention also provides Ni60A Co-based alloy powders, B4C or nickel packet B4C(Ni@B4C), micron or nano-scale rare earth
Oxide prepares the application in titanium alloy laser cladding layer in laser melting coating.
Beneficial effects of the present invention
(1) part R2O3R and O can be decomposed into.Rare-earth element R can be adsorbed on crystal boundary, hinder crystal boundary mobile；It can also reduce
The surface tension and Critical nucleation radius of liquid metal improve nucleation rate, thus thinning microstructure.
(2) R that part is not decomposed2O3It can be used as heterogeneous forming core core, improve nucleation rate, the tiny R in part2O3?
Grain can also hinder the growth of crystal.
(3) preparation method of the present invention is simple, practical, easy to spread.
Detailed description of the invention
Fig. 1 wear test schematic diagram；
Fig. 2 embodiment 1 (a), embodiment 2 (b) cladding layer bottom pattern；
Fig. 3 embodiment 1 (a), embodiment 2 (b) cladding layer top microstructure morphology；
The XRD diffraction patterns of Fig. 4 embodiment 1 (a), embodiment 2 (b) cladding layer；
The hardness profile of 2 cladding layer of Fig. 5 embodiment 1 and embodiment；
Fig. 6 Ni60A+10%B4C+1.0wt.%Nd2O3The polishing scratch cross section profile and three-dimensional appearance of cladding layer；
(a) TC4 substrate, (b) (the 1.0wt.% microns of Nd of embodiment 12O3), (c) (1.0wt.% nanometers of embodiment 2
Nd2O3)；
Fig. 7 embodiment 3 (a), embodiment 4 (b) cladding layer bottom pattern；
Fig. 8 embodiment 3 (a), embodiment 4 (b) cladding layer top microstructure morphology；
The hardness profile of 4 cladding layer of Fig. 9 embodiment 3 and embodiment；
The polishing scratch cross section profile and three-dimensional appearance of Figure 10 embodiment 3 (a) and embodiment 4 (b) cladding layer.
Specific embodiment
Feature of present invention and other correlated characteristics are described in further detail by the following examples, in order to the same industry
The understanding of technical staff:
Cladding layer capability test method of the present invention:
(1) micro-hardness testing: using the microhardness of DHV-1000 type microhardness testers test cladding layer, load
200g, load time 10s, it is micro- every 0.1mm measurement by clad layer surface to substrate along the maximum fusion penetration direction of cladding layer
Hardness number, to analyze the microhardness distribution feature at each position of cladding layer.
(2) wear test: carrying out wear test with HT-1000 type abrasion tester, and abrading-ball selects Si3N4Ceramic grinding ball
(Φ 6mm), revolving speed 448r/min, friction radius 4mm, load 1.5kg, wear test time are 30min.Wear test principle
Figure is as shown in Figure 1, cladding layer wear scar volumes can be calculated according to V=S2 π r.Wherein, S is polishing scratch area of section, and r is friction
Radius.Polishing scratch section and three-dimensional appearance are tested by optical profilometer.
It further illustrates combined with specific embodiments below:
Embodiment 1:
The cladding material quality proportioning of the present embodiment designs are as follows: [Ni60A+10wt.%B4C]+1.0% μ-Nd2O3, specifically
Processing step is as follows:
1) substrate surface to be processed is cleaned out, removes surface scale.
2) cladding powder is uniformly mixed, is layered on substrate surface in advance, control it with a thickness of 0.8mm.
3) CO is utilized2Gas laser carries out cladding test to sample ready in step 2), and laser power is
3.0kW, scanning speed 450mm/min, spot diameter 3.0mm blow argon gas protection molten bath, argon flow in cladding process
For 10L/min.
Embodiment 2:
The cladding material quality proportioning of the present embodiment designs are as follows: [Ni60A+10wt.%B4C]+1.0%n-Nd2O3, specifically
Processing step is as follows:
1) substrate surface to be processed is cleaned out, removes surface scale.
2) cladding powder is uniformly mixed, is layered on substrate surface in advance, control it with a thickness of 0.8mm.
3) CO is utilized2Gas laser carries out cladding test to sample ready in step 2), and laser power is
3.0kW, scanning speed 450mm/min, spot diameter 3.0mm blow argon gas protection molten bath, argon flow in cladding process
For 10L/min.
The microstructure morphology of cladding layer is observed and analyzed, as shown in Figures 2 and 3.The result shows that addition nanometer
The cladding layer of rare earth oxide, microstructure are obviously refined, it can be seen that, the effect of nanometer level RE oxide is ten
Divide significant.The object phase composition of cladding layer is analyzed, as a result as shown in Figure 4.The object phase composition of the two is similar, by γ-
Ni、NiTi、TiB2、TiC、Cr2B、CrB、Ni2B、Ni3B、NiTi2Equal objects phase composition.Nd is not marked in XRD diffraction patterns2O3's
On the one hand diffraction maximum is due to Nd2O3Additive amount it is very few；On the other hand, part Nd2O3Nd is resolved into, is played in the form of Nd
Effect.
Fig. 5 is the hardness profile of 2 cladding layer of embodiment 1 and embodiment, the results showed that, with addition micron order Nd2O3Phase
Than adding nanoscale Nd2O3Later, the microhardness of cladding layer further increases.
The abrasion Cross Section Morphology of substrate titanium alloy and cladding layer is as shown in fig. 6, calculate its wear scar volumes, calculated result such as table
Shown in 2.The result shows that the wearability of embodiment 1,2 cladding layer of embodiment is increased to 3.16 times and 4.39 times of titanium alloy substrate.
It can be seen that addition nanoscale Nd2O3Function and effect it is fairly obvious.
2 Ni60A+B of table4C+1.0wt.%Nd2O3Cladding layer abrasion loss
Embodiment 3:
The cladding material quality proportioning of the present embodiment designs are as follows: [Ni60A+10wt.%B4C]+1.0% μ-La2O3, specifically
Processing step is as follows:
1) substrate surface to be processed is cleaned out, removes surface scale.
2) cladding powder is uniformly mixed, is layered on substrate surface in advance, control it with a thickness of 0.8mm.
3) CO is utilized2Gas laser carries out cladding test to sample ready in step 2), and laser power is
3.0kW, scanning speed 450mm/min, spot diameter 3.0mm blow argon gas protection molten bath, argon flow in cladding process
For 10L/min.
Embodiment 4:
The cladding material quality proportioning of the present embodiment designs are as follows: [Ni60A+10wt.%B4C]+1.0%n-La2O3, specifically
Processing step is as follows:
1) substrate surface to be processed is cleaned out, removes surface scale.
2) cladding powder is uniformly mixed, is layered on substrate surface in advance, control it with a thickness of 0.8mm.
3) CO is utilized2Gas laser carries out cladding test to sample ready in step 2), and laser power is
3.0kW, scanning speed 450mm/min, spot diameter 3.0mm blow argon gas protection molten bath, argon flow in cladding process
For 10L/min.
Comparative example 3 and embodiment 4, the results showed that, n-La2O3Modifying function be substantially better than μ-La2O3, microcosmic group
It knits and is obviously refined, as shown in Figure 7, Figure 8.Microhardness significantly improves, as shown in Figure 9.4 cladding of embodiment 3 and embodiment
The polishing scratch section and three-dimensional appearance of layer are as shown in Figure 10, and abrasion loss calculated result is as shown in table 3, the results showed that, cladding layer is resistance to
Mill property is respectively increased 4.05 times and 4.94 times of titanium alloy substrate, cladding layer wearability be improved significantly.
3 Ni60A+B of table4C+1.0wt.%La2O3Cladding layer abrasion loss
Embodiment 5:
The cladding material quality proportioning of the present embodiment designs are as follows: [Ni60A+20wt.%B4C]+2.0%n-La2O3, specifically
Processing step is as follows:
1) substrate surface to be processed is cleaned out, removes surface scale.
2) cladding powder is uniformly mixed, is layered on substrate surface in advance, control it with a thickness of 0.8mm.
3) CO is utilized2Gas laser carries out cladding test to sample ready in step 2), and laser power is
2.0kW, scanning speed 300mm/min, spot diameter 3.0mm blow argon gas protection molten bath, argon flow in cladding process
For 10L/min.
Performance test shows that cladding layer wearability is increased to 14.15 times of titanium alloy substrate.
Embodiment 6:
The cladding material quality proportioning of the present embodiment designs are as follows: [Ni60A+30wt.%B4C]+2.0%n-Nd2O3, specifically
Processing step is as follows:
1) substrate surface to be processed is cleaned out, removes surface scale.
2) cladding powder is uniformly mixed, is layered on substrate surface in advance, control it with a thickness of 0.8mm.
3) CO is utilized2Gas laser carries out cladding test to sample ready in step 2), and laser power is
3.0kW, scanning speed 450mm/min, spot diameter 3.0mm blow argon gas protection molten bath, argon flow in cladding process
For 10L/min.
Performance test shows that cladding layer wearability is increased to 15.07 times of titanium alloy substrate.
Embodiment 7:
The cladding material quality proportioning of the present embodiment designs are as follows: [Ni60A+15wt.%Ni B4C]+2.0%n-Nd2O3, tool
Steps are as follows for body technology:
1) substrate surface to be processed is cleaned out, removes surface scale.
2) cladding powder is uniformly mixed, is layered on substrate surface in advance, control it with a thickness of 0.8mm.
3) CO is utilized2Gas laser carries out cladding test to sample ready in step 2), and laser power is
3.0kW, scanning speed 450mm/min, spot diameter 3.0mm blow argon gas protection molten bath, argon flow in cladding process
For 10L/min.
Performance test shows that cladding layer wearability is increased to 10.15 times of titanium alloy substrate.
Embodiment 8:
The cladding material quality proportioning of the present embodiment designs are as follows: [Ni60A+20wt.%Ni B4C]+2.0%n-Nd2O3, tool
Steps are as follows for body technology:
1) substrate surface to be processed is cleaned out, removes surface scale.
2) cladding powder is uniformly mixed, is layered on substrate surface in advance, control it with a thickness of 0.9mm.
3) CO is utilized2Gas laser carries out cladding test to sample ready in step 2), and laser power is
2.0kW, scanning speed 400mm/min, spot diameter 3.0mm blow argon gas protection molten bath, argon flow in cladding process
For 12L/min.
Performance test shows that cladding layer wearability is increased to 15.73 times of titanium alloy substrate.
Embodiment 9:
The cladding material quality proportioning of the present embodiment designs are as follows: [Ni60A+20wt.%Ni B4C]+2.0%n-La2O3, tool
Steps are as follows for body technology:
1) substrate surface to be processed is cleaned out, removes surface scale.
2) cladding powder is uniformly mixed, is layered on substrate surface in advance, control it with a thickness of 0.8mm.
3) CO is utilized2Gas laser carries out cladding test to sample ready in step 2), and laser power is
3.0kW, scanning speed 300mm/min, spot diameter 3.0mm blow argon gas protection molten bath, argon flow in cladding process
For 10L/min.
Performance test shows that cladding layer wearability is increased to 13.42 times of titanium alloy substrate.
Embodiment 10:
The cladding material quality proportioning of the present embodiment designs are as follows: [Ni60A+30wt.%Ni B4C]+3.0%n-Nd2O3, tool
Steps are as follows for body technology:
1) substrate surface to be processed is cleaned out, removes surface scale.
2) cladding powder is uniformly mixed, is layered on substrate surface in advance, control it with a thickness of 0.9mm.
3) CO is utilized2Gas laser carries out cladding test to sample ready in step 2), and laser power is
3.0kW, scanning speed 450mm/min, spot diameter 3.0mm blow argon gas protection molten bath, argon flow in cladding process
For 15L/min.
Performance test shows that cladding layer wearability is increased to 12.65 times of titanium alloy substrate.
Finally it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not limited to this hair
It is bright, although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still
It can modify to technical solution documented by previous embodiment, or part is equivalently replaced.It is all in this hair
Within bright spirit and principle, any modification, equivalent replacement, improvement and so on should be included in protection scope of the present invention
Within.Above-mentioned, although the foregoing specific embodiments of the present invention is described with reference to the accompanying drawings, not to the scope of the present invention
Limitation, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art are not required to
Make the creative labor the various modifications or changes that can be made still within protection scope of the present invention.
Claims (1)
1. a kind of rare earth modified laser cladding layer, which is characterized in that on titanium alloy substrate, with Ni60A Co-based alloy powder, B4C
Or nickel packet B4C(Ni@B4C), the laser cladding powder of micron or nanometer level RE oxide composition prepares rare earth modified laser melting coating
Layer；
The mass percent of each component in the laser cladding powder are as follows: Nd2O3Or La2O31.0~4.0%, B4C or Ni@B4C10
~30%, Yu Wei Ni60A；
The Nd2O3Granularity be 5~20 μm or 40~60nm；
The La2O3The granularity of rare earth oxide is 5~20 μm or 40~60nm；
The rare earth modified laser cladding layer is prepared using following technique, comprising:
1) titanium-based material removing surface to be processed is clean, remove surface scale；
2) cladding powder is uniformly mixed, is layered on substrate surface in advance；
3) cladding is carried out to the sample for overlaying cladding powder to test to get rare earth modified laser cladding layer；
The cladding powder includes: Ni60A Co-based alloy powder, B4C or nickel packet B4C(Ni@B4C), micron or nano-scale rare earth oxygen
Compound；
The cladding powder overlays with a thickness of 0.8~1.0mm；
The laser melting coating condition are as follows: laser power is 1.0~3.0kW, and scanning speed is 200~600mm/min, and hot spot is straight
Diameter is 3.0mm, and argon gas protection molten bath is blowed in cladding process, and argon flow is 5~15L/min；
The ingredient of Ni60A nickel base self-fluxing alloy powder is as shown in table 1,
The chemical component (wt.%) of 1 Ni60A nickel base self-fluxing alloy powder of table
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| CN107513711B (en) * | 2017-08-31 | 2019-06-18 | 燕山大学 | A kind of preparation method of copper surface laser fabricated in situ rare earth oxide ceramics cladding layer |
| CN107761093A (en) * | 2017-09-22 | 2018-03-06 | 天津工业大学 | A kind of preparation method of titanium alloy grading powder laser cladding layer and the titanium alloy with the cladding layer |
| CN109954885A (en) * | 2017-12-25 | 2019-07-02 | 中国石油化工股份有限公司 | A kind of increasing material manufacturing composite powder and preparation method thereof |
| CN110643993B (en) * | 2019-10-18 | 2023-11-28 | 山东大学 | Steel surface Sm 2 O 3 Modified laser cladding material, composite coating and preparation method thereof |
| CN110756797B (en) * | 2019-10-18 | 2021-12-28 | 山东农业工程学院 | Nano rare earth oxide modified alloying material, alloying layer and preparation method thereof |
| CN115074724B (en) * | 2022-06-23 | 2023-12-15 | 北京工业大学 | V-element reinforced Ni-based wear-resistant laser cladding coating and preparation method thereof |
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