CN116411275B - Preparation method of laser cladding in-situ authigenic titanium boride-titanium carbide-copper composite coating - Google Patents
Preparation method of laser cladding in-situ authigenic titanium boride-titanium carbide-copper composite coating Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 147
- 239000011248 coating agent Substances 0.000 title claims abstract description 132
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 122
- 239000010949 copper Substances 0.000 title claims abstract description 106
- 239000002131 composite material Substances 0.000 title claims abstract description 72
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 61
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 57
- 238000004372 laser cladding Methods 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 78
- 239000011159 matrix material Substances 0.000 claims abstract description 61
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 57
- 239000010959 steel Substances 0.000 claims abstract description 57
- 238000005253 cladding Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000011219 quaternary composite Substances 0.000 claims abstract description 18
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- 230000001681 protective effect Effects 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 42
- 229910052786 argon Inorganic materials 0.000 claims description 21
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 15
- 239000000758 substrate Substances 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 14
- 239000007795 chemical reaction product Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 244000137852 Petrea volubilis Species 0.000 claims description 8
- 238000005498 polishing Methods 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 19
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000005728 strengthening Methods 0.000 abstract description 2
- 239000000919 ceramic Substances 0.000 description 26
- 230000003014 reinforcing effect Effects 0.000 description 18
- 239000002356 single layer Substances 0.000 description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 11
- 230000009286 beneficial effect Effects 0.000 description 9
- 238000009826 distribution Methods 0.000 description 9
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 8
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
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Classifications
-
- 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
-
- 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
- B22F1/12—Metallic powder containing non-metallic particles
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
A preparation method of a laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating relates to the technical field of laser surface strengthening. The invention aims to solve the problem that the bonding phases Cu and TiO are not utilized at present 2 ‑B 4 Preparation of in-situ authigenic TiB by combining C-C carbothermal reaction system with laser cladding technology 2 -problems of the forming process of TiC-Cu composite coatings. The method comprises the following steps: pretreating the surface of a steel matrix, and preheating to obtain a preheated steel matrix; tiO is mixed with 2 ‑B 4 Drying the C-C-Cu quaternary composite spherical powder to obtain a cladding material; and under the atmosphere of protective gas, adopting a coaxial powder feeding laser cladding mode to carry out in-situ autogenous production on the surface of the preheated steel matrix to obtain the titanium boride-titanium carbide-copper composite coating, wherein the laser power is 1000-1800W. The invention can obtain a preparation method of a laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating.
Description
Technical Field
The invention relates to the technical field of laser surface strengthening, in particular to a preparation method of a laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating.
Background
TiB 2 -TiC complex phaseThe ceramic material has a series of advantages of excellent combination of mechanical and electrical properties, good thermal shock resistance, high-temperature oxidation resistance and the like, and is a material with a very good application prospect. With single-phase TiB 2 TiB, compared to TiC ceramic material 2 The overall performance of the TiC complex-phase ceramic material is greatly improved, especially TiB with the temperature of more than 600 DEG C 2 The hardness of TiC composite ceramics is far higher than TiB 2 And TiC single-phase ceramics are ideal choices as reinforcing phases for high temperature wear-resistant and conductive coatings. At present, there are two main methods for introducing the ceramic reinforcing phase, namely an external addition method and an in-situ autogenous method. The in-situ self-generating method generates ceramic reinforcing phase in situ through high temperature self-propagating reaction, the method overcomes the problems of poor wettability and weak binding force of the ceramic reinforcing phase directly added by an external method, reduces the possibility of generating defects such as air holes and cracks in a cladding layer of the ceramic phase, and the ceramic phase has uniform and fine structure, and the prepared composite coating has better performance than external addition.
The laser in-situ self-generating method combines the advantages of the laser cladding technology and the ceramic reinforcing phase in-situ self-generating method, and is widely applied to the preparation of the metal ceramic composite coating due to the high cooling speed, low dilution rate, high bonding strength and easy realization of automation. Under the irradiation of high-energy density laser beam, the powder is induced to generate high-temperature self-propagating reaction to generate TiB in situ 2 The TiC ceramic reinforcing phase has clean interface between the in-situ self-generated ceramic reinforcing phase and the matrix and the bonding phase, is favorable for obtaining a high-performance coating with uniformly distributed reinforcing phase, and can finish deposition while generating the ceramic reinforcing phase, thereby being favorable for improving the production efficiency and reducing the production cost. At present, the TiO is adopted at home and abroad 2 -B 4 C-Al and Ti-B 4 In-situ generation of TiB by C-system laser cladding 2 The TiC ceramic reinforcing phase has been studied more, but for TiO 2 -B 4 In situ generation of TiB by C-C carbothermal reaction 2 The TiC ceramic reinforcing phase is less studied, and the system is just TiB 2 The industrial production uses more processes, because of TiO 2 Powder, B 4 The price of the C powder and the carbon source powder is lower, and the laser cladding in-situ autogenous reduces TiB 2 And TiC preparation process, can further reduce raw materialsProduction of TiB 2- The cost of TiC ceramic reinforcing phase utilizes bonding phase Cu and TiO 2 -B 4 In-situ authigenic TiB prepared by combining C-C carbothermal reaction system with laser cladding technology 2 The TiC-Cu composite coating is expected to realize the industrialized application of the coating.
Disclosure of Invention
The invention aims to solve the problem that the bonding phases Cu and TiO are not utilized at present 2 -B 4 Preparation of in-situ authigenic TiB by combining C-C carbothermal reaction system with laser cladding technology 2 The problem of the forming process of the TiC-Cu composite coating, and provides a preparation method of the laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating.
The preparation method of the laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating comprises the following steps:
step one: pretreating the surface of a steel matrix, and preheating to obtain a preheated steel matrix;
step two: tiO is mixed with 2 -B 4 Drying the C-C-Cu quaternary composite spherical powder to obtain a cladding material;
step three: and in-situ autogenous production of the cladding material in the second step on the surface of the preheated steel substrate in the first step is carried out in an atmosphere of protective gas by adopting a coaxial powder feeding laser cladding mode, so that the titanium boride-titanium carbide-copper composite coating is obtained, and the laser power is 1000-1800W.
The invention has the beneficial effects that:
the invention adopts TiO 2 -B 4 The C-C carbothermal reaction system combines the advantages of the laser cladding technology, thereby further reducing the preparation of TiB from the perspective of powder raw materials 2 And TiC ceramic phase, reduces TiB 2 And TiC, and avoids the problems of poor wettability with a matrix and a binding phase, easy cracking of a cladding layer and the like caused by adding a ceramic phase.
The method can obtain TiB with higher hardness under the wide laser cladding process parameters of 1000-1800W 2 TiC-Cu composite coating, and the hardness of the cladding layer reaches 800HV 0.2 The depth of the single-layer coating high hard area exceeds 1.2mm, help to improve the wear resistance of the coating; meanwhile, the addition of the pure Cu binding phase is beneficial to improving the plasticity and conductivity of the coating.
The in-situ self-generated TiB prepared by the invention 2 The TiC-Cu coating and the matrix form good metallurgical bonding, the coating hardness is high and the distribution is uniform, the depth of a single-layer coating high-hardness area is large, and the coating is extremely beneficial to the improvement of the wear resistance; and under wider laser cladding process parameters, the coating with ideal performance can be obtained, which is beneficial to the industrialized application of the coating.
The invention can obtain a preparation method of a laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating.
Drawings
FIG. 1 is a diagram of TiO in example 1 2 -B 4 SEM image of C-C-Cu quaternary composite spherical powder;
FIG. 2 is an XRD pattern for the titanium boride-titanium carbide-copper composite coatings of examples 2-6;
FIG. 3 is a graph of the microscopic morphology of the titanium boride-titanium carbide-copper composite coating of example 2;
FIG. 4 is a plot of the distribution of the element Ti for the EDS surface scan of FIG. 3;
FIG. 5 is a plot of the B element profile of the EDS surface scan of FIG. 3;
FIG. 6 is a plot of the distribution of the C element of the EDS surface scan of FIG. 3;
FIG. 7 is a graph showing the distribution of the scanned Cu element on the EDS surface of FIG. 3;
FIG. 8 is a microhardness profile of the titanium boride-titanium carbide-copper composite coatings of examples 2-6.
Detailed Description
The first embodiment is as follows: the preparation method of the laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating comprises the following steps:
step one: pretreating the surface of a steel matrix, and then preheating to obtain a pretreated steel matrix;
step two: tiO is mixed with 2 -B 4 Drying the C-C-Cu quaternary composite spherical powder to obtain a cladding material;
step three: and in-situ autogenous production of the cladding material in the second step on the surface of the preheated steel substrate in the first step is carried out in an atmosphere of protective gas by adopting a coaxial powder feeding laser cladding mode, so that the titanium boride-titanium carbide-copper composite coating is obtained, and the laser power is 1000-1800W.
The second embodiment is as follows: the present embodiment differs from the specific embodiment in that: the steel matrix in the first step is H13 steel.
The other steps are the same as in the first embodiment.
And a third specific embodiment: the present embodiment differs from the first or second embodiment in that: the specific steps of the pretreatment of the surface of the steel matrix are as follows: firstly polishing the surface of a steel matrix by using 400-mesh sand paper, and then performing ultrasonic cleaning to obtain the pretreated steel matrix.
Other steps are the same as those of the first or second embodiment.
The specific embodiment IV is as follows: one difference between this embodiment and the first to third embodiments is that: the ultrasonic cleaning time is 10-30 min.
Other steps are the same as those of the first to third embodiments.
Fifth embodiment: one to four differences between the present embodiment and the specific embodiment are: the medium for ultrasonic cleaning is absolute ethanol or acetone.
Other steps are the same as those of the first to fourth embodiments.
Specific embodiment six: the present embodiment differs from the first to fifth embodiments in that: in the first step, preheating is carried out for 1-2 h under the temperature condition of 150-300 ℃.
Other steps are the same as those of the first to fifth embodiments.
Seventh embodiment: one difference between the present embodiment and the first to sixth embodiments is that: tiO as described in step two 2 -B 4 The C-C-Cu quaternary composite spherical powder is prepared from TiO 2 Powder, B 4 C powder, graphite powder and Cu powder, tiO 2 Powder, B 4 The mass ratio of the C powder to the graphite powder to the Cu powder is (20-21): (7-8): (4.5-6): (18-20).
Other steps are the same as those of embodiments one to six.
Eighth embodiment: one difference between the present embodiment and the first to seventh embodiments is that: and step three, wherein the shielding gas is argon, and the introducing rate of the argon is 18-25L/min.
Other steps are the same as those of embodiments one to seven.
Detailed description nine: one of the differences between this embodiment and the first to eighth embodiments is: the specific parameters of coaxial powder feeding laser cladding in the third step are as follows: the diameter of the laser beam spot is 2-3 mm, the laser scanning speed is 240-600 mm/min, the powder feeding speed is 0.7-1.5 r/min, the powder feeding gas is argon, and the argon feeding rate is 9-15L/min.
Other steps are the same as those of embodiments one to eight.
Detailed description ten: the present embodiment differs from the first to ninth embodiments in that: the titanium boride-titanium carbide-copper composite coating in the third step contains TiB 2 Three phases of TiC and Cu and a small amount of intermediate reaction product Ti 5 O 9 、Ti 4 O 7 、Ti 3 O 5 And B 2 O 3 And (3) phase (C).
Other steps are the same as those of embodiments one to nine.
The following examples are used to verify the benefits of the present invention:
example 1: the preparation method of the quaternary composite powder for reactive thermal spraying comprises the following steps:
step one: tiO is mixed with 2 Powder, B 4 C powder, graphite powder and copper powder are put into a planetary mixer, deionized water, a dispersing agent and a surfactant are added into the uniformly mixed quaternary composite powder after uniform mixing, and the mixture is strongly stirred for 10 to 20 minutes at a rotating speed of 300r/min to obtain suspension, wherein the TiO is 2 Powder, B 4 The mass ratio of the C powder to the graphite powder to the copper powder is 20:8:6:18; deagglomeration and dispersion are carried out on the powder in the suspension by utilizing an ultrasonic nano disperser, ultrasonic dispersion is carried out for 1h, the dispersed suspension is then added with a binder,strongly stirring again at the rotating speed of 500r/min for 2 hours to obtain evenly mixed slurry with good stability and lower viscosity;
step two: spraying and granulating the slurry obtained in the step one to obtain mixed powder; under the protection of argon gas, the temperature of the mixed powder is firstly increased to 500 ℃ at the heating rate of 10 ℃/min, and the mixed powder is preserved for 1h at 500 ℃; heating to 900 ℃ at a heating rate of 10 ℃/min, and preserving heat for 1h at 900 ℃; finally sieving with 800 mesh sieve to remove powder above 800 mesh to obtain TiO 2 -B 4 C-C-Cu quaternary composite spherical powder.
The chemical reaction formula is as follows: 2TiO 2 +B 4 C+3C＝2TiB 2 +4CO；
The dispersing agent is DOLAPIX CE 64, which is purchased from the chemical industry of the German Seamate; the surfactant is 9485 anionic surfactant, and is purchased from Guangzhou wet macro chemical Co., ltd; the binder is polyvinyl alcohol.
TiO in the slurry 2 Powder, B 4 The total mass fraction of the C powder, the graphite powder and the copper powder is 35-40%, and TiO is prepared by the following steps of 2 Powder, B 4 The ratio of the total mass of the C powder, the graphite powder and the copper powder to the volume of deionized water is 0.52:1, the dispersing agent is TiO 2 Powder, B 4 0.75 to 1.25 percent of the total mass of the C powder, the graphite powder, the copper powder and the deionized water, and the surfactant is TiO 2 Powder, B 4 0.06% of the total mass of the C powder, the graphite powder, the copper powder and the deionized water, and the binding agent is TiO 2 Powder, B 4 And 1.5-2% of the total mass of the C powder, the graphite powder, the copper powder and the deionized water.
The TiO 2 Powder, B 4 The mass purity of the C powder, the graphite powder and the copper powder is more than 99.7%, and the mass purity of the TiO is higher than that of the C powder, the graphite powder and the copper powder 2 The average particle diameter of the powder is 25nm, B 4 The average particle diameter of the C powder is 3 mu m, the average particle diameter of the graphite powder is 8000 meshes, the average particle diameter of the copper powder is 500nm, and the TiO is 2 Both the powder and the copper powder are spherical.
In the second step, the slurry is subjected to spray granulation by adopting an airflow type spray dryer, and the operation parameters of the airflow type spray dryer are as follows: the inlet temperature is 180-190 ℃, the outlet temperature is 100-105 ℃, the peristaltic pump efficiency is 15%, the height of the spray air flow meter is 25-30 mm, and the air extractor efficiency is 100%; the inlet pipe is a silicone pipe with an inner diameter of 2mm and an outer diameter of 4mm.
FIG. 1 is a diagram of TiO in example 1 2 -B 4 SEM image of C-C-Cu quaternary composite spherical powder; as shown in fig. 1, tiO 2 -B 4 The C-C-Cu quaternary composite spherical powder has higher density, good sphericity and uniform particle size, and is favorable for the smooth proceeding of subsequent laser cladding and the preparation of high-performance laser cladding coating.
Example 2: the preparation method of the laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating comprises the following steps:
step one: pretreating the surface of the processed H13 steel matrix to obtain a flat clean surface, then placing the flat clean surface in a vacuum drying oven, and preheating for 1H at the temperature of 200 ℃ to obtain a preheated steel matrix;
the specific steps of the pretreatment of the surface of the steel matrix are as follows: firstly polishing the surface of a steel matrix by using 400-mesh sand paper, and then ultrasonically cleaning for 20min by using ultrasonic cleaning equipment to obtain the pretreated steel matrix, wherein the ultrasonic cleaning medium is absolute ethyl alcohol.
Step two: tiO prepared in example 1 2 -B 4 And (5) drying the C-C-Cu quaternary composite spherical powder to obtain the cladding material.
Step three: in-situ autogenous production of the cladding material in the second step on the surface of the preheated steel substrate in the first step is carried out in an argon atmosphere with the feeding rate of 20L/min by adopting a coaxial powder feeding laser cladding mode, so as to obtain a titanium boride-titanium carbide-copper composite coating, wherein the titanium boride-titanium carbide-copper composite coating contains TiB 2 Three phases of TiC and Cu and a small amount of intermediate reaction product Ti 5 O 9 、Ti 4 O 7 、Ti 3 O 5 And B 2 O 3 The depth of the high hard area of the single-layer coating exceeds 1.2mm.
The specific parameters of coaxial powder feeding laser cladding are as follows: the laser power is 1000W, the laser beam spot diameter is 3mm, the laser scanning speed is 240mm/min, the powder feeding speed is 0.9r/min, the powder feeding gas is argon, and the argon feeding rate is 10L/min.
FIG. 2 is an XRD pattern for the titanium boride-titanium carbide-copper composite coatings of examples 2-6; as shown in FIG. 2, it can be seen from the 1000W curve that TiB is generated in situ in the coating 2 And TiC, and at the same time, also generates a small amount of intermediate reaction product Ti 5 O 9 、Ti 4 O 7 、Ti 3 O 5 And B 2 O 3 Phases, each of which is produced by intermediate reactions 1 to 4. Experiments show that when the laser power is lower than 1000W, the prepared coating is thinner and TiB generated in the coating 2 Compared with TiC, the coating hardness is reduced, and the protection of the matrix is not facilitated; when the laser power is higher than 1800W, the prepared coating has poor molding, the dilution ratio of the coating and the matrix is higher, the hardness of the coating is reduced, and the abrasion resistance of the matrix is not improved. In combination with the analysis, the laser cladding power was selected to be 1000-1800W.
2TiO 2 +B 4 C+3C＝2TiB 2 Total +4CO reaction;
20TiO 2 +C＝Ti 20 O 39 +co intermediate reaction 1;
Ti 3 O 5 +3c=3tic+3co intermediate reaction 2;
2TiO 2 +B 4 C+3C＝2/3TiB 2 +4/3TiC+4/3B 2 O 3 +8/3C intermediate reaction 3;
4/3TiC+4/3B 2 O 3 +8/3C＝4/3TiB 2 +4CO intermediate reaction 4.
Fig. 3 is a microscopic morphology diagram of the titanium boride-titanium carbide-copper composite coating of example 2, fig. 4 is an EDS face scan Ti element profile of fig. 3, fig. 5 is an EDS face scan B element profile of fig. 3, fig. 6 is an EDS face scan C element profile of fig. 3, and fig. 7 is an EDS face scan Cu element profile of fig. 3. As shown in FIGS. 3-7, the ceramic reinforcing phase in the coating is distributed more uniformly, tiB 2 The ceramic phase exists mainly in the form of short rod and needle, tiCThe ceramic phase exists mainly in a granular form, and the ceramic phase exist in a symbiotic form.
FIG. 8 is a microhardness profile of the titanium boride-titanium carbide-copper composite coatings of examples 2-6; the hardness of the coating is obviously improved compared with that of the matrix through a 1000W curve, the hardness of the coating is uniformly distributed, the hardness decline trend is gentle along with the increase of the distance from the surface of the coating, and the hardness of the coating declines rapidly until the hardness of the coating reaches the hardness value of the matrix after entering a heat affected zone.
In conclusion, the titanium boride-titanium carbide-copper composite coating prepared in example 1 forms good metallurgical bond with the substrate, and TiB generated in situ by adopting a TiO2-B4C-C carbothermic reaction system 2 And TiC ceramic reinforcing phase are uniformly distributed, so that the hardness of the coating is remarkably improved, the hardness distribution of the whole cladding area is ensured to be uniform, the wear resistance of the coating is improved, and meanwhile, the addition of the pure Cu binding phase is beneficial to improving the plasticity and the conductivity of the coating.
Example 3: the preparation method of the laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating comprises the following steps:
step one: pretreating the surface of the processed H13 steel matrix to obtain a flat clean surface, then placing the flat clean surface in a vacuum drying oven, and preheating for 1H at the temperature of 200 ℃ to obtain a preheated steel matrix;
the specific steps of the pretreatment of the surface of the steel matrix are as follows: firstly polishing the surface of a steel matrix by using 400-mesh sand paper, and then ultrasonically cleaning for 20min by using ultrasonic cleaning equipment to obtain the pretreated steel matrix, wherein the ultrasonic cleaning medium is absolute ethyl alcohol.
Step two: tiO prepared in example 1 2 -B 4 And (5) drying the C-C-Cu quaternary composite spherical powder to obtain the cladding material.
Step three: in the argon atmosphere with the feeding rate of 20L/min, adopting a coaxial powder feeding laser cladding mode to carry out in-situ autogenous production on the surface of the preheated steel substrate in the step two to obtain a titanium boride-titanium carbide-copper composite coating, wherein the titanium boride-titanium carbide-copper composite coating containsTiB 2 Three phases of TiC and Cu and a small amount of intermediate reaction product Ti 5 O 9 、Ti 4 O 7 、Ti 3 O 5 And B 2 O 3 The depth of the high hard area of the single-layer coating exceeds 1.2mm.
The specific parameters of coaxial powder feeding laser cladding are as follows: the laser power is 1200W, the laser beam spot diameter is 3mm, the laser scanning speed is 240mm/min, the powder feeding speed is 0.9r/min, the powder feeding gas is argon, and the argon feeding rate is 10L/min.
FIG. 2 is an XRD pattern for the titanium boride-titanium carbide-copper composite coatings of examples 2-6; as shown in FIG. 2, it can be seen from the 1200W curve that TiB is generated in situ in the coating 2 And TiC, and at the same time, also generates a small amount of intermediate reaction product Ti 5 O 9 、Ti 4 O 7 、Ti 3 O 5 And B 2 O 3 And (3) phase (C).
FIG. 8 is a microhardness profile of the titanium boride-titanium carbide-copper composite coatings of examples 2-6; the hardness of the coating is obviously improved compared with that of the matrix through a 1200W curve, the hardness of the coating is uniformly distributed, the hardness decline trend is gentle along with the increase of the distance from the surface of the coating, and the hardness of the coating declines rapidly until the hardness of the coating reaches the hardness value of the matrix after entering a heat affected zone.
In summary, the titanium boride-titanium carbide-copper composite coating prepared in example 3 forms a good metallurgical bond with the substrate, and adopts TiO 2 -B 4 TiB generated in situ by C-C carbothermal reaction system 2 And TiC ceramic reinforcing phase are uniformly distributed, so that the hardness of the coating is remarkably improved, the hardness distribution of the whole cladding area is ensured to be uniform, the wear resistance of the coating is improved, and meanwhile, the addition of the pure Cu binding phase is beneficial to improving the plasticity and the conductivity of the coating.
Example 4: the preparation method of the laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating comprises the following steps:
step one: pretreating the surface of the processed H13 steel matrix to obtain a flat clean surface, then placing the flat clean surface in a vacuum drying oven, and preheating for 1H at the temperature of 200 ℃ to obtain a preheated steel matrix;
the specific steps of the pretreatment of the surface of the steel matrix are as follows: firstly polishing the surface of a steel matrix by using 400-mesh sand paper, and then ultrasonically cleaning for 20min by using ultrasonic cleaning equipment to obtain the pretreated steel matrix, wherein the ultrasonic cleaning medium is absolute ethyl alcohol.
Step two: tiO prepared in example 1 2 -B 4 And (5) drying the C-C-Cu quaternary composite spherical powder to obtain the cladding material.
Step three: in-situ autogenous production of the cladding material in the second step on the surface of the preheated steel substrate in the first step is carried out in an argon atmosphere with the feeding rate of 20L/min by adopting a coaxial powder feeding laser cladding mode, so as to obtain a titanium boride-titanium carbide-copper composite coating, wherein the titanium boride-titanium carbide-copper composite coating contains TiB 2 Three phases of TiC and Cu and a small amount of intermediate reaction product Ti 5 O 9 、Ti 4 O 7 、Ti 3 O 5 And B 2 O 3 The depth of the high hard area of the single-layer coating exceeds 1.2mm.
The specific parameters of coaxial powder feeding laser cladding are as follows: the laser power is 1400W, the laser beam spot diameter is 3mm, the laser scanning speed is 240mm/min, the powder feeding speed is 0.9r/min, the powder feeding gas is argon, and the argon feeding rate is 10L/min.
FIG. 2 is an XRD pattern for the titanium boride-titanium carbide-copper composite coatings of examples 2-6; as shown in FIG. 2, it can be seen from the 1400W curve that TiB is generated in situ in the coating 2 And TiC, and at the same time, also generates a small amount of intermediate reaction product Ti 5 O 9 、Ti 4 O 7 、Ti 3 O 5 And B 2 O 3 And (3) phase (C).
FIG. 8 is a microhardness profile of the titanium boride-titanium carbide-copper composite coatings of examples 2-6; the 1400W curve can show that the hardness of the coating is obviously improved compared with that of the matrix, the hardness of the coating is uniformly distributed, the hardness decline trend is more gentle along with the increase of the distance from the surface of the coating, and the hardness of the coating is quickly declined until the hardness of the coating reaches the hardness value of the matrix after entering a heat affected zone.
In summary, the titanium boride-titanium carbide-copper composite coating prepared in example 4 forms good metallurgical bond with the substrate, and adopts TiO 2 -B 4 TiB generated in situ by C-C carbothermal reaction system 2 And TiC ceramic reinforcing phase are uniformly distributed, so that the hardness of the coating is remarkably improved, the hardness distribution of the whole cladding area is ensured to be uniform, the wear resistance of the coating is improved, and meanwhile, the addition of the pure Cu binding phase is beneficial to improving the plasticity and the conductivity of the coating.
Example 5: the preparation method of the laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating comprises the following steps:
step one: pretreating the surface of the processed H13 steel matrix to obtain a flat clean surface, then placing the flat clean surface in a vacuum drying oven, and preheating for 1H at the temperature of 200 ℃ to obtain a preheated steel matrix;
the specific steps of the pretreatment of the surface of the steel matrix are as follows: firstly polishing the surface of a steel matrix by using 400-mesh sand paper, and then ultrasonically cleaning for 20min by using ultrasonic cleaning equipment to obtain the pretreated steel matrix, wherein the ultrasonic cleaning medium is absolute ethyl alcohol.
Step two: tiO prepared in example 1 2 -B 4 And (5) drying the C-C-Cu quaternary composite spherical powder to obtain the cladding material.
Step three: in-situ autogenous production of the cladding material in the second step on the surface of the preheated steel substrate in the first step is carried out in an argon atmosphere with the feeding rate of 20L/min by adopting a coaxial powder feeding laser cladding mode, so as to obtain a titanium boride-titanium carbide-copper composite coating, wherein the titanium boride-titanium carbide-copper composite coating contains TiB 2 Three phases of TiC and Cu and a small amount of intermediate reaction product Ti 5 O 9 、Ti 4 O 7 、Ti 3 O 5 And B 2 O 3 The depth of the high hard area of the single-layer coating exceeds 1.2mm.
The specific parameters of coaxial powder feeding laser cladding are as follows: the laser power is 1600W, the laser beam spot diameter is 3mm, the laser scanning speed is 240mm/min, the powder feeding speed is 0.9r/min, the powder feeding gas is argon, and the argon feeding rate is 10L/min.
FIG. 2 is an XRD pattern for the titanium boride-titanium carbide-copper composite coatings of examples 2-6; as shown in FIG. 2, it can be seen from the 1600W curve that TiB was generated in situ in the coating 2 And TiC, and at the same time, also generates a small amount of intermediate reaction product Ti 5 O 9 、Ti 4 O 7 、Ti 3 O 5 And B 2 O 3 And (3) phase (C).
FIG. 8 is a microhardness profile of the titanium boride-titanium carbide-copper composite coatings of examples 2-6; the 1600W curve can show that the hardness of the coating is obviously improved compared with that of the matrix, the hardness of the coating is uniformly distributed, the hardness decline trend is more gentle along with the increase of the distance from the surface of the coating, and the hardness of the coating is quickly declined until the hardness of the coating reaches the hardness value of the matrix after entering a heat affected zone.
In summary, the titanium boride-titanium carbide-copper composite coating prepared in example 5 forms a good metallurgical bond with the substrate, using TiO 2 -B 4 TiB generated in situ by C-C carbothermal reaction system 2 And TiC ceramic reinforcing phase are uniformly distributed, so that the hardness of the coating is remarkably improved, the hardness distribution of the whole cladding area is ensured to be uniform, the wear resistance of the coating is improved, and meanwhile, the addition of the pure Cu binding phase is beneficial to improving the plasticity and the conductivity of the coating.
Example 6: the preparation method of the laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating comprises the following steps:
step one: pretreating the surface of the processed H13 steel matrix to obtain a flat clean surface, then placing the flat clean surface in a vacuum drying oven, and preheating for 1H at the temperature of 200 ℃ to obtain a preheated steel matrix;
the specific steps of the pretreatment of the surface of the steel matrix are as follows: firstly polishing the surface of a steel matrix by using 400-mesh sand paper, and then ultrasonically cleaning for 20min by using ultrasonic cleaning equipment to obtain the pretreated steel matrix, wherein the ultrasonic cleaning medium is absolute ethyl alcohol.
Step two: tiO prepared in example 1 2 -B 4 And (5) drying the C-C-Cu quaternary composite spherical powder to obtain the cladding material.
Step three: in-situ autogenous production of the cladding material in the second step on the surface of the preheated steel substrate in the first step is carried out in an argon atmosphere with the feeding rate of 20L/min by adopting a coaxial powder feeding laser cladding mode, so as to obtain a titanium boride-titanium carbide-copper composite coating, wherein the titanium boride-titanium carbide-copper composite coating contains TiB 2 Three phases of TiC and Cu and a small amount of intermediate reaction product Ti 5 O 9 、Ti 4 O 7 、Ti 3 O 5 And B 2 O 3 The depth of the high hard area of the single-layer coating exceeds 1.2mm.
The specific parameters of coaxial powder feeding laser cladding are as follows: the laser power is 1800W, the laser beam spot diameter is 3mm, the laser scanning speed is 240mm/min, the powder feeding speed is 0.9r/min, the powder feeding gas is argon, and the argon feeding rate is 10L/min.
FIG. 2 is an XRD pattern for the titanium boride-titanium carbide-copper composite coatings of examples 2-6; as shown in FIG. 2, it can be seen from the 1800W curve that TiB was generated in situ in the coating 2 And TiC, and at the same time, also generates a small amount of intermediate reaction product Ti 5 O 9 、Ti 4 O 7 、Ti 3 O 5 And B 2 O 3 And (3) phase (C).
FIG. 8 is a microhardness profile of the titanium boride-titanium carbide-copper composite coatings of examples 2-6; the 1800W curve can show that the hardness of the coating is obviously improved compared with that of the matrix, the hardness of the coating is uniformly distributed, the hardness decline trend is more gentle along with the increase of the distance from the surface of the coating, and the hardness of the coating is quickly declined until the hardness of the coating reaches the hardness value of the matrix after entering a heat affected zone.
In conclusion, the titanium boride-titanium carbide-copper composite coating prepared in example 6 forms good metallurgical bond with the substrate, and adopts TiO 2 -B 4 TiB generated in situ by C-C carbothermal reaction system 2 The TiC ceramic reinforcing phase is uniformly distributed, so that the hardness of the coating is remarkably improved, the hardness distribution of the whole cladding area is ensured to be uniform, the wear resistance of the coating is improved, and the coating is pureThe addition of the Cu binding phase is beneficial to improving the plasticity and conductivity of the coating.
Example 7: the preparation method of the laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating comprises the following steps:
step one: pretreating the surface of the processed H13 steel matrix to obtain a flat clean surface, then placing the flat clean surface in a vacuum drying oven, and preheating for 1H at the temperature of 200 ℃ to obtain a preheated steel matrix;
the specific steps of the pretreatment of the surface of the steel matrix are as follows: firstly polishing the surface of a steel matrix by using 400-mesh sand paper, and then ultrasonically cleaning for 20min by using ultrasonic cleaning equipment to obtain the pretreated steel matrix, wherein the ultrasonic cleaning medium is absolute ethyl alcohol.
Step two: tiO prepared in example 1 2 -B 4 And (5) drying the C-C-Cu quaternary composite spherical powder to obtain the cladding material.
Step three: in-situ autogenous production of the cladding material in the second step on the surface of the preheated steel substrate in the first step is carried out in an argon atmosphere with the feeding rate of 20L/min by adopting a coaxial powder feeding laser cladding mode, so as to obtain a titanium boride-titanium carbide-copper composite coating, wherein the titanium boride-titanium carbide-copper composite coating contains TiB 2 Three phases of TiC and Cu and a small amount of intermediate reaction product Ti 5 O 9 、Ti 4 O 7 、Ti 3 O 5 And B 2 O 3 The depth of the high hard area of the single-layer coating exceeds 1.2mm.
The specific parameters of coaxial powder feeding laser cladding are as follows: the laser power is 1800W, the laser beam spot diameter is 3mm, the laser scanning speed is 360mm/min, the powder feeding speed is 1.2r/min, the powder feeding gas is argon, and the argon feeding rate is 10L/min.
Comparative example 1:
1. guo Xiaoqin, guo Yongchun, gu Linyu laser cladding Cu-TiB 2 Composite coating and its wear resistance [ J]Hot working process, 2004 (11) 22-23+26.
TiB in document 1 2 The hardness of the Cu composite coating is 480-580 HV, and the single-layer high-hardness depth is less than 0.2mm, while the average hardness of the titanium boride-titanium carbide-copper composite coatings in examples 2 to 6 in the present invention is 910 to 961HV0.2, the single-layer high hardness depth exceeds 1.2mm, which is much higher than that of document 1, showing higher hardness and wear resistance.
Comparative example 2:
2. zhou Fang, zhu Tao, he Lianghua in situ synthesis of TiC-TiB by laser cladding 2 Composite coating [ J ]]Chinese surface engineering, 2013,26 (06): 29-34.
In the document 2, the average hardness of the TiC-TiB2 reinforced composite coating is 720-760HV0.2, the high hardness depth of the single-layer coating is less than 0.8mm, and the coating can be prepared only in a narrower laser cladding process range. In the present invention, the average hardness of the titanium boride-titanium carbide-copper composite coating in examples 2 to 6 is 910 to 961HV0.2, and the single-layer high hardness depth exceeds 1.2mm, which is far higher than that of document 2, and the coating exhibits higher hardness and wear resistance.
Claims (7)
1. The preparation method of the laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating is characterized by comprising the following steps of:
step one: pretreating the surface of a steel matrix, and preheating to obtain a preheated steel matrix;
step two: tiO is mixed with 2 -B 4 Drying the C-C-Cu quaternary composite spherical powder to obtain a cladding material;
TiO as described in step two 2 -B 4 The C-C-Cu quaternary composite spherical powder is prepared from TiO 2 Powder, B 4 C powder, graphite powder and Cu powder, tiO 2 Powder, B 4 The mass ratio of the C powder to the graphite powder to the Cu powder is (20-21): (7-8): (4.5-6): (18-20);
step three: in the atmosphere of protective gas, adopting a coaxial powder feeding laser cladding mode to carry out in-situ autogenous production on the surface of the preheated steel substrate in the step two, so as to obtain a titanium boride-titanium carbide-copper composite coating, wherein the laser power is 1000-1800W;
the specific parameters of coaxial powder feeding laser cladding in the third step are as follows: the diameter of the laser beam spot is 2-3 mm, the laser scanning speed is 240-600 mm/min, the powder feeding speed is 0.7-1.5 r/min, the powder feeding gas is argon, and the argon feeding rate is 9-15L/min;
the titanium boride-titanium carbide-copper composite coating in the third step contains TiB 2 Three phases of TiC and Cu and intermediate reaction product Ti 5 O 9 、Ti 4 O 7 、Ti 3 O 5 And B 2 O 3 And (3) phase (C).
2. The method for preparing a laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating according to claim 1, wherein the steel substrate in the step one is H13 steel.
3. The method for preparing the laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating according to claim 1, which is characterized by comprising the following specific steps of: firstly polishing the surface of a steel matrix by using 400-mesh sand paper, and then performing ultrasonic cleaning to obtain the pretreated steel matrix.
4. The method for preparing the laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating according to claim 3, wherein the ultrasonic cleaning time is 10-30 min.
5. The method for preparing the laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating according to claim 3 or 4, wherein the medium for ultrasonic cleaning is absolute ethyl alcohol or acetone.
6. The method for preparing the laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating according to claim 1, wherein the method is characterized in that in the first step, the coating is preheated for 1-2 hours at the temperature of 150-300 ℃.
7. The method for preparing the laser cladding in-situ self-generated titanium boride-titanium carbide-copper composite coating according to claim 1, wherein the shielding gas in the step three is argon, and the introducing rate of the argon is 18-25L/min.
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