CN109338285B - Method for forming Si-Co composite infiltration gradient coating on titanium alloy surface - Google Patents
Method for forming Si-Co composite infiltration gradient coating on titanium alloy surface Download PDFInfo
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- CN109338285B CN109338285B CN201811315234.XA CN201811315234A CN109338285B CN 109338285 B CN109338285 B CN 109338285B CN 201811315234 A CN201811315234 A CN 201811315234A CN 109338285 B CN109338285 B CN 109338285B
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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
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
- C23C10/34—Embedding in a powder mixture, i.e. pack cementation
- C23C10/52—Embedding in a powder mixture, i.e. pack cementation more than one element being diffused in one step
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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
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/02—Pretreatment of the material to be coated
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Abstract
The application discloses a method for forming a Si-Co composite infiltration gradient coating on the surface of a titanium alloy, which comprises the following steps: pretreating the surface of the titanium alloy; and then immersing the titanium alloy in a penetrating agent, sealing, heating to 1050-1200 ℃, preserving heat for 2-20 hours, cooling, cleaning and drying. The invention adopts a surface activation process, a penetrating agent formula and a diffusion Co-penetration process to prepare the Si-Co composite gradient coating with uniform and compact structure and close combination with a matrix on the surface of the titanium alloy. The method can improve the wear resistance and high-temperature oxidation resistance of the surface of the titanium alloy, expands the engineering application of the titanium alloy and has very important significance.
Description
Technical Field
The application relates to the technical field of material preparation, in particular to a method for forming a Si-Co composite infiltration gradient coating on the surface of a titanium alloy.
Background
The titanium alloy has a series of excellent comprehensive properties of low density, higher melting point, high specific strength and good corrosion resistance, thereby being widely applied in the fields of aerospace, automobile energy, biomedical treatment and the like. However, the titanium alloy has low hardness, high viscosity and poor friction and abrasion resistance, so that the surface of the connecting piece prepared from the titanium alloy is easy to generate sticking, occlusion and scratch; in addition, the high-temperature oxidation resistance of the titanium alloy is not ideal, and when the temperature exceeds 550 ℃, Ti can react with oxygen and nitrogen in the air strongly to generate TiO2Or the TiN reaction product layer is loose and porous, and the protection is poor. Practical engineering applications of titanium alloys are therefore greatly restricted.
The preparation of the surface protective coating is a convenient and effective way for improving the wear resistance and the oxidation resistance of the surface of the titanium alloy, and scientific researchers at home and abroad do a lot of work and make good progress. Various protective coating systems, such as TiAl-based coatings (TiAl), are prepared on the surface of the titanium alloy by adopting various processes or composite processes such as magnetron sputtering, laser cladding, ion implantation, plasma spraying and the like3,TiAl2And TiAlCr, etc.), M-CrAlY (M stands for Ni, Co, NiCo, etc.) coating, ceramic coating (Al2O3Coating, enamel coating and ZrO2Thermal barrier coatings, etc.). The coatings improve the frictional wear or high-temperature oxidation resistance of titanium alloyThe titanium alloy has certain effects in the aspects of chemical properties and the like, but the defects of poor impact resistance, weak combination with a matrix, obvious reduction of matrix fatigue performance and the like exist generally, and the research results of the titanium alloy with both wear resistance and high-temperature oxidation resistance are rarely seen. For example, nitriding the surface of titanium alloy can improve the hardness and wear resistance of the surface, but when the temperature exceeds 550 ℃, N reacts with the Ti matrix strongly, so that the brittleness of the matrix is increased; the coating prepared by adopting the plasma spraying or magnetron sputtering method is influenced by the activity of the titanium alloy matrix, so that the bonding strength of the coating and the matrix is not high; the coating prepared by the laser cladding process generally has the defects of large internal stress of the coating, more internal cracks or microcracks and the like. Therefore, the problem of further application of titanium alloy is far from being solved, and a better protective coating system and a preparation technology thereof need to be explored.
In a plurality of coating systems, the silicide coating has the advantages of low density, high hardness, excellent wear resistance and the like, and simultaneously can form SiO with strong fluidity and self-healing capability under the high-temperature aerobic environment2The protective film has excellent high-temperature oxidation resistance, so the protective film belongs to an ideal titanium alloy surface wear-resistant and oxidation-resistant protective coating. However, the single silicide coating has high brittleness, and is easy to crack and even fall off under the action of friction load, so that the protection is lost, and the preparation of the composite coating is an effective means for improving the toughness. Co is an important raw material for producing heat-resistant alloy, hard alloy and the like, the hardness, toughness and wear resistance of the alloy can be obviously improved, and good results can be obtained by adding Co into the silicide coating to improve the toughness and wear resistance of the silicide coating. In addition, the preparation process also has important influence on the service performance of the coating, a silicide coating which has a gradient structure and is tightly combined with the matrix alloy (metallurgical combination) can be prepared on the surface of the titanium alloy by adopting a diffusion infiltration method, but the Si-Co composite infiltration gradient coating is difficult to prepare on the surface of the titanium alloy by adopting the diffusion infiltration method under the influence of the activity of Ti and Co alloys, and the technology and the application of the aspect are blank at present.
Disclosure of Invention
Aiming at the problem that the application of the titanium alloy is limited in the prior art, the invention provides a method for forming a Si-Co composite infiltration gradient coating on the surface of the titanium alloy, which can improve the surface wear resistance and oxidation resistance of the titanium alloy and promote the practical engineering application of the titanium alloy. Meanwhile, the technical problem that the Si-Co composite infiltration is difficult to realize on the surface of the titanium alloy is solved.
The method for forming the Si-Co composite infiltration gradient coating on the surface of the titanium alloy comprises the following steps:
pretreating the surface of the titanium alloy; and then immersing the titanium alloy in a penetrating agent, sealing, heating to 1050-1200 ℃, preserving heat for 2-20 hours, cooling, cleaning and drying. Preferably, the heat preservation temperature is 1050-1200 ℃, and the heat preservation time is 4 hours.
Specifically, the pretreatment comprises the following steps:
polishing the surface of the titanium alloy to be smooth, then ultrasonically cleaning the titanium alloy in an acetone solution for 5-10 min, and drying the titanium alloy; placing the mixture in NaOH solution for alkali washing for 0.5-1 minute; pickling in HF solution for 0.5-1 min; is placed in Cr2O3The surface activation treatment is carried out for 20 minutes to 1 hour in the solution. The pretreatment is performed in order to sufficiently clean and activate the surface structure of the Ti alloy, so that active atoms of the element to be infiltrated in the co-infiltration process can be effectively adsorbed on the surface of the sample. Preferably, the concentration of the NaOH solution is 30-50 g/L, the concentration of the HF solution is 40-60 g/L, and the Cr is2O3The solution is saturated solution. Preferably, the alkali washing time is 0.5min, the acid washing time is 0.5min, and the activation treatment time is 20-60 min.
Further, the invention also provides a formula of the penetrant, which comprises the following components in percentage by weight:
si powder: 5-20% by weight;
co powder: 5-20% by weight;
NH4cl powder: 2-4% by weight;
NaF powder: 1-3% by weight;
SiC powder: and (4) the balance.
For the purposes of the present invention, preference is given to the formulationThe square is 10Si-10Co-3NH4Cl-2NaF-75SiC, namely the components and the contents are as follows: si powder 10%, Co powder 10%, NH43% of Cl powder, 2% of NaF powder and 75% of SiC powder. When the formula is adopted, the co-permeation effect is best, and the wear resistance and the oxidation resistance are best.
The penetrant is obtained by the following method: weighing the components of the penetrant according to the weight percentage, mixing, and then carrying out ball milling for 2-4 h to fully mix and refine the penetrant. The granularity of the powder of each component is preferably less than or equal to 200 meshes.
Specifically, the immersion comprises the following steps: filling a penetrating agent into the high-temperature-resistant and corrosion-resistant container, then embedding the titanium alloy into the penetrating agent, compacting, and covering the penetrating agent on the upper layer, wherein the thickness of the upper layer is more than 10 mm. The high-temperature-resistant and corrosion-resistant container is preferably a ceramic crucible. The thickness of the covering infiltration agent is preferably 12 mm.
Specifically, the sealing medium adopted in the sealing is silica sol, water glass and Al2O3A mixture of (a). Further, the sealing medium comprises the following components in percentage by weight: 60-70 parts of silica sol, 18-22 parts of water glass and 45-55 parts of Al2O3. Preferably, about 20g of water glass, Al, is added per 50ml of silica sol2O3About 50 g.
Specifically, the heating rate is 6-10 ℃/min, if the heating rate is too high, the sealed crucible is easy to explode, and if the heating rate is too low, the catalyst is easy to decompose prematurely, so that the co-permeation effect is poor. For the present invention, 6 ℃/min is preferred.
Specifically, the cleaning and drying are to ultrasonically clean the treated titanium alloy in alcohol for 10 minutes and then dry the titanium alloy.
The method provided by the invention finally forms a composite gradient layer on the surface of the titanium alloy, wherein the composite gradient layer is made of (Ti, Co) Si2Outer layer, TiSi intermediate layer and Ti5Si4+Ti5Si3The inner layer.
Has the advantages that: the invention adopts a specific surface activation process, a penetrating agent formula and a diffusion Co-penetration process, prepares the Si-Co composite gradient coating with uniform and compact structure and compact combination with the matrix on the surface of the titanium alloy, realizes the quantitative control of the structure and the components of the coating, and has very important significance for improving the wear resistance and the high-temperature oxidation resistance of the surface of the titanium alloy and expanding the engineering application of the titanium alloy.
The invention can prepare the composite gradient coating with controllable Si and Co contents, uniform and compact tissue and tight combination with the matrix on the surface of the titanium alloy by utilizing the specific surface activation technology and the formula of the penetrating agent (comprising the catalyst and the filler) in combination with the diffusion Co-penetration process. Meanwhile, the method has the advantages of simple process, low cost, strong repeatability and the like, and is suitable for production and application.
Drawings
FIG. 1 is a surface topography diagram of a Si-Co composite infiltration gradient coating on the surface of a titanium alloy.
FIG. 2 is a sectional view of the Si-Co composite infiltration gradient coating on the surface of the titanium alloy.
FIG. 3 is the element distribution diagram of Si-Co composite infiltration gradient coating on the surface of titanium alloy.
FIG. 4 is a diagram of the shapes of a titanium alloy substrate, a pure Si-infiltrated coating on the surface of the titanium alloy and a Si-Co composite infiltrated gradient coating on the surface of the titanium alloy after friction and abrasion.
FIG. 5 is a diagram of the shapes of a titanium alloy substrate, a pure Si-infiltrated coating on the surface of the titanium alloy and a Si-Co composite infiltrated gradient coating on the surface of the titanium alloy after high-temperature oxidation.
Detailed Description
In order to make the technical solutions better understood by those skilled in the art, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only partial embodiments of the present application, but not all embodiments.
Example 1
① sample preparation, namely sequentially polishing each surface of a Ti alloy sample to be smooth by using No. 180-2000 waterproof abrasive paper, ② surface cleaning and activating, namely placing the polished sample in an acetone solution for ultrasonic cleaning for 10min, drying the sample by cold air, and then sequentially placing the sample in NaOH, HF and Cr2O3Alkali washing in solution for 0.5min →Acid washing for 0.5min → surface activating for 20min, ③ preparing penetrant, which comprises (by weight) Si powder of 200 meshes 5%, Co powder of 200 meshes 5%, and NH of 99%42 percent of Cl, 1 percent of analytically pure (99 percent) NaF and the balance of 200-mesh SiC powder, ④ grinding material, namely placing the prepared penetrating agent into a planetary gear ball mill for ball milling for 4 hours to fully refine and mix the materials, ⑤ charging, namely filling the ball-milled penetrating agent into a crucible, embedding a sample with the surface cleaned and activated into the penetrating agent for compaction, covering the surface of the sample with the penetrating agent with the thickness of about 12mm after the sample is compacted, ⑥ sealing, namely covering and sealing the crucible with the sample, wherein the sealing medium is silica sol and water glass (Na)2SiO3·9H2O) and Al2O3(Al is added to about 20g of water glass per 50ml of silica sol)2O3About 50g), ⑦ high-temperature diffusion, namely, putting the sealed crucible into a high-temperature controllable heat treatment furnace, heating the heat treatment furnace to 1050 ℃ according to the heating rate of 6 ℃/min, preserving the heat for 4 hours, cooling the heat treatment furnace to room temperature, cleaning and drying ⑧, namely, taking the sample out of the diffusion agent, ultrasonically cleaning the sample in alcohol for 10 minutes, and then drying the sample, thus finishing the process.
Example 2
The preparation procedure was the same as in example 1, except for the activation time of the sample surface, the Si powder, Co powder and catalyst (NH) in the impregnation agent4Cl and NaF) content and diffusion and permeation temperature, specifically, preparing an ① sample, namely sequentially polishing each surface of a Ti alloy sample to be smooth by using No. 180-2000 waterproof abrasive paper, cleaning and activating ② surface, namely placing the polished sample in acetone solution for ultrasonic cleaning for 10min, drying by cold air, and then sequentially placing the sample in NaOH, HF and Cr2O3Alkali washing 0.5min → acid washing 0.5min → surface activating treatment 40min, ③ preparing penetrating agent, accurately weighing the penetrating agent components according to weight percentage, including 200 mesh Si powder with 10%, 200 mesh Co powder with 10%, analytically pure (99%) NH43 percent of Cl, 2 percent of analytically pure (99 percent) NaF and the balance of 200-mesh SiC powder, ④ grinding material, namely placing the prepared penetrating agent in a planetary gear ball mill for ball milling for 4 hours to ensure thatFully refining and mixing, ⑤ loading, loading the ball-milled penetrating agent into crucible, burying the sample with surface cleaned and activated into the penetrating agent, compacting to obtain a sample with surface covered by the penetrating agent with a thickness of about 12mm, ⑥ sealing, covering the crucible with silica sol and water glass (Na) as sealing medium, and sealing2SiO3·9H2O) and Al2O3(Al is added to about 20g of water glass per 50ml of silica sol)2O3About 50g), ⑦ high-temperature diffusion, namely, putting the sealed crucible into a high-temperature controllable heat treatment furnace, heating the heat treatment furnace to 1100 ℃ according to the heating rate of 6 ℃/min, preserving the heat for 4 hours, cooling the heat treatment furnace to room temperature, cleaning and drying ⑧, namely, taking out the sample from the penetrating agent, ultrasonically cleaning the sample in alcohol for 10 minutes, and then drying the sample, thus finishing the process.
Example 3
The preparation procedure was the same as in examples 1 and 2, except for the activation time of the sample surface, the Si powder, Co powder and catalyst (NH) in the infiltrant4Cl and NaF) content and diffusion and permeation temperature, specifically, preparing an ① sample, namely sequentially polishing each surface of a Ti alloy sample to be smooth by using No. 180-2000 waterproof abrasive paper, cleaning and activating ② surface, namely placing the polished sample in acetone solution for ultrasonic cleaning for 10min, drying by cold air, and then sequentially placing the sample in NaOH, HF and Cr2O3Alkali washing 0.5min → acid washing 0.5min → surface activating treatment 60min, ③ preparing penetrating agent, accurately weighing the penetrating agent components according to weight percentage, including 200 mesh Si powder with 20%, 200 mesh Co powder with 20%, analytically pure (99%) NH44 percent of Cl, 3 percent of analytically pure (99 percent) NaF and the balance of 200-mesh SiC powder, ④ grinding material, namely placing the prepared penetrating agent into a planetary gear ball mill for ball milling for 4 hours to fully refine and mix the materials, ⑤ charging, namely filling the ball-milled penetrating agent into a crucible, embedding a sample with the surface cleaned and activated into the penetrating agent for compaction, covering the surface of the sample with the penetrating agent with the thickness of about 12mm after the sample is compacted, ⑥ sealing, namely covering and sealing the crucible with the sample, wherein the sealing medium is silica sol and water glass (Na)2SiO3·9H2O) and Al2O3Mixture of (2) (per 50ml of silica sol)Adding 20g of water glass and Al into the glue2O3About 50g), ⑦ high-temperature diffusion, namely, putting the sealed crucible into a high-temperature controllable heat treatment furnace, heating the heat treatment furnace to 1200 ℃ according to the heating rate of 6 ℃/min, preserving the heat for 4 hours, cooling the heat treatment furnace to room temperature, cleaning and drying ⑧, namely, taking out the sample from the penetrating agent, ultrasonically cleaning the sample in alcohol for 10 minutes, and then drying the sample, thus finishing the process.
As shown in fig. 1, the surface topography of the composite gradient coating obtained in examples 1 to 3 under different process conditions was compared. Wherein the preparation conditions of the coating shown in FIG. 1(a) are as follows: surface activation is carried out for 20min, the diffusion infiltration temperature is 1050 ℃, the diffusion infiltration time is 4h, and the infiltration agent component is 5Si-5Co-2NH4Cl-1NaF-87SiC (wt%); the coating shown in FIG. 1(b) was prepared under the following conditions: surface activation is carried out for 40min, the diffusion infiltration temperature is 1100 ℃, the diffusion infiltration time is 4h, and the infiltration agent component is 10Si-10Co-3NH4Cl-2NaF-75SiC (wt%); the coating shown in FIG. 1(c) was prepared under the following conditions: surface activation is carried out for 60min, diffusion infiltration temperature is 1200 ℃, diffusion infiltration time is 4h, and infiltration agent component is 20Si-20Co-4NH4Cl-3NaF-53SiC (wt.%). It can be seen that the composite gradient coating prepared in example 2 has a denser structure.
As shown in fig. 2, the microscopic topography of the coating cross section of the composite gradient coating cross section obtained in examples 1 to 3 under different process conditions was compared. Wherein the preparation conditions of the coating shown in FIG. 2(a) are as follows: surface activating for 20min at 1050 deg.C for 4 hr, and 5Si-5Co-2NH as penetrating agent4Cl-1NaF-87SiC (wt.%); the coating shown in FIG. 2(b) was prepared under the following conditions: surface activation for 40min, diffusion infiltration temperature of 1100 deg.C, diffusion infiltration time of 4h, and infiltration agent component of 10Si-10Co-3NH4Cl-2NaF-75SiC (wt.%); the coating shown in FIG. 2(c) was prepared under the following conditions: surface activation for 60min at 1200 deg.C for 4h, and diffusion permeation agent component of 20Si-20Co-4NH4Cl-3NaF-53SiC (wt.%). It can be seen that the prepared coating has a multilayer composite structure, wherein the composite gradient coating prepared in example 2 has moderate thickness, compact structure and good co-permeation effect.
As shown in FIG. 3, the composite gradient coating obtained in examples 1-3 under different process conditions was cutThe element distribution of the surface was compared. Wherein the preparation conditions of the coating shown in FIG. 3(a) are as follows: surface activating for 20min at 1050 deg.C for 4 hr, and 5Si-5Co-2NH as penetrating agent4Cl-1NaF-87SiC (wt.%); fig. 3(b) shows the distribution of Ti element in the coating of fig. 3(a), fig. 3(c) shows the distribution of Si element in the coating of fig. 3(a), fig. 3(d) shows the distribution of Co element in the coating of fig. 3(a), and fig. 3(e) shows the distribution of Al element in the coating of fig. 3 (a). It can be seen that the composite gradient coating prepared according to the embodiment contains Ti, Si, Co and Al elements, and the Si-Co Co-cementation effect is realized.
As shown in FIG. 4, the shapes of the Ti alloy substrate, the pure Si-doped coating on the Ti alloy surface and the Si-Co composite doped gradient coating after frictional wear and high-temperature oxidation, and FIG. 4(a) shows the shapes of the Ti alloy substrate sample and Al at normal temperature2O3The appearance of grinding marks after ball-on-ball grinding for 60min is shown in FIG. 4(b) in which a sample with a Si-only coating is mixed with Al at room temperature2O3The appearance of grinding marks after ball-on-ball grinding for 60min is shown in FIG. 4(c) in which a Si-Co composite infiltration gradient coating sample is mixed with Al at normal temperature2O3Grinding trace appearance after ball pair grinding for 60 min;
as shown in fig. 5, fig. 5(a) is a macro morphology of a Ti alloy matrix sample after being oxidized at a constant temperature of 1000 ℃ for 100 hours, fig. 5(b) is a macro morphology of a pure Si-infiltrated coating sample after being oxidized at a constant temperature of 1000 ℃ for 100 hours, and fig. 5(c) is a macro morphology of a Si-Co composite infiltrated gradient coating sample after being oxidized at a constant temperature of 1000 ℃ for 100 hours; the preparation process of the pure Si-infiltrated coating is that the surface is activated for 40min, the infiltration agent component is 10Si-2NaF-88SiC (wt.%), the diffusion infiltration temperature is 1100 ℃, the heat preservation time is 4h, and the preparation process of the Si-Co composite infiltration gradient coating is as follows: surface activation is carried out for 40min, the penetrating agent component is 10Si-10Co-3NH4Cl-2NaF-75SiC (wt.%), the diffusion penetration temperature is 1100 ℃, and the heat preservation time is 4 h. As can be seen, compared with the Ti alloy matrix and the pure Si-infiltrated coating, the Si-Co composite Si-infiltrated gradient coating has narrower grinding mark after being worn, less peeling of the worn surface, no obvious peeling of the oxidized film, and serious peeling of the Ti alloy matrix and the pure Si-infiltrated coating.
Product performance testing
The titanium alloy composite gradient coatings obtained by the methods of examples 1 to 3 were subjected to frictional wear and high-temperature oxidation resistance tests.
Comparative examples 1 to 3 were prepared at the same temperature and for the same time as in examples 1 to 3, except that the infiltrant contained no Co and the formed coating was a simple siliconized coating.
Comparative example 0 was a titanium alloy without surface treatment, and was subjected to frictional wear and high-temperature oxidation resistance tests.
The results obtained are shown in the following table:
| wearing at normal temperature for 60min | Wearing at 600 deg.C for 60min | Oxidizing at 1000 deg.C for 100h | |
| Comparative example 0 | Loss on abrasion of 1.9mg | Loss on abrasion of 2.4mg | 17.8mg/cm2 |
| Comparative example 1 | Abrasion weight loss of 0.9mg | Loss on abrasion of 1.2mg | 2.6mg/cm2 |
| Comparative example 2 | Abrasion weight loss of 0.8mg | Loss on abrasion of 1.1mg | 2.4mg/cm2 |
| Comparative example 3 | Abrasion weight loss of 0.9mg | Loss on abrasion of 1.2mg | 2.7mg/cm2 |
| Example 1 | Abrasion weight loss of 0.4mg | Abrasion weight loss of 0.6mg | 1.3mg/cm2 |
| Example 2 | Abrasion weight loss of 0.3mg | Abrasion weight loss of 0.5mg | 1.2mg/cm2 |
| Example 3 | Abrasion weight loss of 0.4mg | Abrasion weight loss of 0.7mg | 1.5mg/cm2 |
As can be seen from the above table, the titanium alloy treated by the method of the present application is significantly superior to the untreated titanium alloy substrate and the pure siliconized coating in terms of both wear resistance and high temperature oxidation resistance. For the present application, example 2 performed best in terms of abrasion resistance and high temperature oxidation resistance.
In conclusion, the results of friction wear and high-temperature oxidation resistance experiments on the prepared composite gradient coating show that the coating provided by the invention has excellent wear resistance and high-temperature oxidation resistance.
The above embodiments are preferred embodiments of the present application and are not intended to limit the present application.
Claims (8)
1. A method for forming a Si-Co composite infiltration gradient coating on the surface of a titanium alloy is characterized by comprising the following steps:
pretreating the surface of the titanium alloy; then immersing the titanium alloy in a penetrating agent, sealing, heating to 1050-1200 ℃, preserving heat for 2-20 hours, cooling, cleaning and drying;
the pretreatment comprises the following steps:
polishing the surface of the titanium alloy to be smooth, then ultrasonically cleaning the titanium alloy in an acetone solution for 5-10 minutes, and drying the titanium alloy; placing the mixture in NaOH solution for alkali washing for 0.5-1 minute; pickling in HF solution for 0.5-1 min; is placed in Cr2O3Surface activation treatment is carried out for 20 minutes to 1 hour in the solution;
the concentration of the NaOH solution is 30-50 g/L, the concentration of the HF solution is 40-60 g/L, and the Cr is2O3The solution is selected from saturated solution, the alkali washing time is 0.5min, the acid washing time is 0.5min, the activation treatment time is 20-60 min,
wherein the penetrating agent comprises the following components in percentage by weight:
si powder: 5-20% by weight;
co powder: 5-20% by weight;
NH4cl powder: 2-4% by weight;
NaF powder: 1-3% by weight;
SiC powder: and (4) the balance.
2. The method for forming the Si-Co composite infiltration gradient coating on the surface of the titanium alloy according to claim 1, wherein the infiltration agent is obtained by the following method: weighing the components of the penetrant according to the weight percentage, mixing, and then carrying out ball milling for 2-4 h to fully mix and refine the penetrant.
3. The method for forming the Si-Co composite infiltration gradient coating on the surface of the titanium alloy according to claim 1, wherein the immersing comprises the following specific steps: filling a penetrating agent into the high-temperature-resistant and corrosion-resistant container, then embedding the titanium alloy into the penetrating agent, compacting, and covering the penetrating agent on the upper layer, wherein the thickness of the penetrating agent on the upper layer is more than 10 mm.
4. The method for forming the Si-Co composite infiltration gradient coating on the surface of the titanium alloy as claimed in claim 1, wherein the sealing is carried out by adopting the sealing media of silica sol, water glass and Al2O3A mixture of (a).
5. The method for forming the Si-Co composite infiltration gradient coating on the surface of the titanium alloy according to claim 1, wherein the sealing medium comprises the following components in percentage by weight: 60-70 parts of silica sol, 18-22 parts of water glass and 45-55 parts of Al2O3。
6. The method for forming the Si-Co composite infiltration gradient coating on the surface of the titanium alloy according to claim 1, wherein the heating rate is 6-10 ℃/min.
7. The method for forming the Si-Co composite infiltration gradient coating on the surface of the titanium alloy as claimed in claim 1, wherein the cleaning and drying are carried out by ultrasonic cleaning in alcohol for 10 minutes and then drying.
8. The method for forming Si-Co composite infiltration gradient coating on titanium alloy surface according to any one of claims 1 to 7, characterized in that the composite gradient coating is formed by (Ti, Co) Si2Outer layer, TiSi intermediate layer and Ti5Si4+Ti5Si3The inner layer.
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| US4084025A (en) * | 1974-08-02 | 1978-04-11 | General Electric Company | Process of applying protective aluminum coatings for non-super-strength nickel-chromium alloys |
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