CN116065118B - Method for oxygen permeation of titanium alloy ions - Google Patents
Method for oxygen permeation of titanium alloy ions Download PDFInfo
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- CN116065118B CN116065118B CN202310161734.7A CN202310161734A CN116065118B CN 116065118 B CN116065118 B CN 116065118B CN 202310161734 A CN202310161734 A CN 202310161734A CN 116065118 B CN116065118 B CN 116065118B
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 119
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 239000001301 oxygen Substances 0.000 title claims abstract description 98
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 98
- 238000000034 method Methods 0.000 title claims abstract description 55
- 150000002500 ions Chemical class 0.000 title description 30
- 238000011282 treatment Methods 0.000 claims abstract description 111
- 238000009792 diffusion process Methods 0.000 claims abstract description 74
- 230000003647 oxidation Effects 0.000 claims abstract description 62
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 62
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 38
- 229910052786 argon Inorganic materials 0.000 claims description 19
- 238000004321 preservation Methods 0.000 claims description 16
- 238000010849 ion bombardment Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims 2
- 238000004381 surface treatment Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 7
- 239000002131 composite material Substances 0.000 abstract description 4
- 239000010410 layer Substances 0.000 description 71
- 230000000052 comparative effect Effects 0.000 description 16
- 239000007789 gas Substances 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 239000006104 solid solution Substances 0.000 description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004372 laser cladding Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
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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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
Abstract
The invention belongs to the technical field of titanium alloy surface treatment, and discloses a titanium alloy ion oxygen permeation method, which specifically comprises the following steps: step S1, performing thermal oxidation treatment; performing thermal oxidation treatment on the titanium alloy to be treated, and forming a first oxide layer on the surface of the titanium alloy; step S2, oxygen diffusion treatment; performing oxygen diffusion treatment on the titanium alloy with the first oxide layer, and completely decomposing the first oxide layer to generate oxygen elements required by diffusion to form an oxygen diffusion layer; step S3, reheat oxidation treatment; and (3) performing thermal oxidation treatment again on the titanium alloy with the obtained oxygen diffusion layer to form a second oxide layer on the surface of the titanium alloy. By adopting the method for the ion oxygen permeation of the titanium alloy, a composite hardening layer with high hardness, low friction coefficient, high thickness and good binding force can be obtained on the surface of the titanium alloy, so that a better hardening effect on the titanium alloy is achieved.
Description
Technical Field
The invention belongs to the technical field of titanium alloy surface treatment, and particularly relates to a titanium alloy ion oxygen permeation method.
Background
Titanium alloys have been used in a number of fields because of their extremely high specific strength, excellent corrosion resistance and excellent biocompatibility. However, titanium alloys are poor in tribological properties, and are mainly characterized by high and unstable friction factors, strong adhesion transfer tendencies, and low seizure resistance, and therefore titanium alloys are generally subjected to surface hardening treatments when used under wearing conditions.
In view of the fact that the corrosion resistance of coatings such as thermal spraying, overlaying, laser cladding and the like is inferior to that of titanium alloys, the surface hardening treatment of the current titanium alloys mostly adopts means such as nitriding, oxygen permeation, micro-arc oxidation, carburization and the like. Compared with other processes, the oxygen permeation process has the advantages of small deformation, thick permeation layer, good binding force and the like, and is the best prospect in various titanium alloy surface hardening treatment technologies.
The conventional titanium alloy oxygen permeation process at present is generally divided into two steps, firstly, oxygen or air is introduced into a box-type furnace for thermal oxidation to obtain an oxide layer (compound layer) with a certain thickness, then the titanium alloy is placed into a vacuum furnace for heating and diffusion, the oxide layer is decomposed in the diffusion process, an oxygen reservoir is provided for diffusion to form a diffusion layer, and therefore a hardened layer structure is formed on the surface of the titanium alloy, the surface hardness of the hardened layer structure is improved, and the friction coefficient is reduced.
However, when the titanium alloy obtained by the above process is applied to some environments having high requirements for surface hardness, it is found that the surface hardness is insufficient, and the friction coefficient of the surface is reduced, but the tribological properties of the titanium alloy are still comparable to those of the titanium alloy matrix, and the higher requirements cannot be satisfied. In addition, in the above-mentioned titanium alloy oxygen permeation process, the process steps are complicated because the oxygen permeation process needs to be carried out in two different devices, and the treatment time is relatively long because the diffusion rate of oxygen atoms in the titanium alloy is relatively slow.
Disclosure of Invention
In view of the above, the present invention discloses a method for ion-doping of titanium alloys to overcome or at least partially solve the above-mentioned problems.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the method for the ion oxygen permeation of the titanium alloy specifically comprises the following steps:
step S1, performing thermal oxidation treatment; performing thermal oxidation treatment on the titanium alloy to be treated, and forming a first oxide layer on the surface of the titanium alloy;
step S2, oxygen diffusion treatment; performing oxygen diffusion treatment on the titanium alloy with the first oxide layer, and completely decomposing the first oxide layer to generate oxygen elements required by diffusion to form an oxygen diffusion layer;
step S3, reheat oxidation treatment; and (3) performing thermal oxidation treatment again on the titanium alloy with the obtained oxygen diffusion layer to form a second oxide layer on the surface of the titanium alloy.
Preferably, in the step S1, a first oxide layer having a thickness of 1 to 5 μm is formed on the surface of the titanium alloy.
Preferably, the temperature of the oxygen diffusion treatment process in the step S2 is the same as the temperature of the thermal oxidation treatment process in the step S1, and the heat preservation time of the oxygen diffusion treatment process in the step S2 is longer than the heat preservation time of the thermal oxidation treatment process in the step S1.
Preferably, in the step S1, the temperature in the thermal oxidation treatment process is controlled to be 700-800 ℃, and the heat preservation time is controlled to be 0.3-0.7 h; in step S2, the same temperature as in step S1 is adopted, and the heat preservation time is controlled to be more than 10h.
Preferably, the temperature of the reheat oxidation process in the step S3 is the same as the temperature of the thermal oxidation process in the step S1, and the heat preservation time of the reheat oxidation process in the step S3 is shorter than the heat preservation time of the thermal oxidation process in the step S1.
Preferably, in the step S1, the temperature in the thermal oxidation treatment process is controlled to be 700-800 ℃, and the heat preservation time is controlled to be 0.3-0.7 h; in the step S3, the same temperature as that in the step S1 is adopted, and the heat preservation time is controlled to be 0.1-0.3 h.
Preferably, the treatment of steps S1-S3 is accomplished using an ion diffusion furnace.
Preferably, in the step S1, argon is introduced into the ion diffusion furnace, ion bombardment heating is carried out on the titanium alloy to be treated, oxygen is introduced after the temperature in the ion diffusion furnace reaches 700-800 ℃, the ratio of the argon to the oxygen is less than 1, and the heat preservation time is controlled to be 0.3-0.7 h; in the step S2, oxygen is stopped from being introduced, ion bombardment is carried out by utilizing argon, the temperature in the ion permeation and expansion furnace is kept at 700-800 ℃, and the temperature is kept for 10-16 hours; in the step S3, oxygen is re-introduced, and oxygen and argon are used for ion bombardment, so that the temperature in the ion diffusion furnace is kept at 700-800 ℃, and the temperature is kept for 0.1-0.3 h.
Preferably, the method for ion-diffusing oxygen of the titanium alloy further comprises a step S4, specifically, after the step S3 is completed, oxygen is stopped being introduced, ion bombardment is carried out by utilizing argon gas, the temperature in the ion-diffusing furnace is slowly cooled to 600 ℃, and then heating is stopped, so that the ion-diffusing furnace is cooled to below 150 ℃.
Preferably, the surface cleaning and drying treatment of the titanium alloy to be treated is further included before the step S1.
The invention has the advantages and beneficial effects that:
in the method for diffusing oxygen by titanium alloy ions, the titanium alloy is subjected to thermal oxidation treatment, oxygen diffusion treatment and reheat oxidation treatment in sequence, a first oxide layer serving as an oxygen reservoir is formed on the surface of the titanium alloy by means of thermal oxidation treatment, then the first oxide layer serving as the oxygen reservoir is completely decomposed by oxygen diffusion treatment to generate oxygen elements required by diffusion so as to form an oxygen diffusion layer with a certain thickness, thereby forming a supersaturated solid solution structure of the titanium alloy which has a certain thickness and high hardness but is easy to generate adhesive wear and has a higher friction coefficient on the surface of the titanium alloy, and finally, the reheat oxidation treatment is carried out to reform an oxide layer on the surface of the titanium alloy, so that a composite hardening layer with high hardness, low friction coefficient, high thickness and good binding force is finally obtained, and a better hardening effect on the titanium alloy is achieved.
Drawings
FIG. 1 is a schematic flow chart of the titanium alloy ion oxygen permeation method of the invention;
FIG. 2 is a 500-time metallographic photograph of a test piece obtained in example 1;
FIG. 3 is a 500-time metallographic photograph of the test piece obtained in comparative example 1;
FIG. 4 is a 500-time metallographic photograph of the test piece obtained in comparative example 2;
FIG. 5 is a 500-time metallographic photograph of a test piece obtained in comparative example 3;
FIG. 6 is a 500-fold metallographic photograph of the test piece obtained in comparative example 4.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to specific embodiments of the present invention and corresponding drawings. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The technical scheme of the invention is described and illustrated in detail below with reference to the accompanying drawings.
Referring to FIG. 1, the process of oxygen permeation treatment of titanium alloy by adopting the titanium alloy ion oxygen permeation method of the invention is as follows:
step S1, performing thermal oxidation treatment; and performing thermal oxidation treatment on the titanium alloy to be treated, and forming a first oxide layer on the surface of the titanium alloy.
Step S2, oxygen diffusion treatment; and performing oxygen diffusion treatment on the titanium alloy with the obtained first oxide layer, and completely decomposing the first oxide layer to generate oxygen elements required for diffusion to form an oxygen diffusion layer.
Step S3, reheat oxidation treatment; and (3) performing thermal oxidation treatment again on the titanium alloy with the obtained oxygen diffusion layer to form a second oxide layer on the surface of the titanium alloy.
According to the invention, the titanium alloy is subjected to thermal oxidation treatment, oxygen diffusion treatment and reheat oxidation treatment in sequence, a first oxide layer serving as an oxygen reservoir is formed on the surface of the titanium alloy by means of the thermal oxidation treatment process, then the first oxide layer serving as the oxygen reservoir is completely decomposed by the oxygen diffusion treatment to generate oxygen elements required by diffusion so as to form an oxygen diffusion layer, thereby forming a supersaturated solid solution structure of the titanium alloy which has a certain thickness and high hardness, is easy to generate adhesive wear and has a higher friction coefficient on the surface of the titanium alloy, and finally, the reheat oxidation treatment is performed, and an oxide layer is formed on the supersaturated solid solution structure surface of the titanium alloy again, so that a composite hardening layer with high hardness, low friction coefficient, high thickness and good binding force is finally obtained, and a better hardening effect on the titanium alloy is achieved.
Preferably, in step S1 of the present invention, the thickness of the first oxide layer formed on the surface of the titanium alloy is controlled to be 1 to 5 μm by controlling the thermal oxidation treatment process, for example, temperature, holding time, etc. At this time, it is ensured that sufficient oxygen is obtained by decomposing the first oxide layer in step S2, so that the amount of oxygen required for forming the diffusion layer of a certain thickness is satisfied, and it is also possible to avoid the situation that the second oxide layer formed in step S3 is peeled off from the titanium alloy substrate due to the inability of complete decomposition in step S2 due to the excessively thick thickness of the first oxide layer, so that it is finally ensured that the diffusion layer formed has a certain thickness and the second oxide layer forms tight bonding with the titanium alloy.
Further, in the invention, by controlling the temperature of the oxygen diffusion treatment process in the step S2 to be the same as the temperature of the thermal oxidation treatment process in the step S1, and controlling the heat preservation time of the oxygen diffusion treatment process in the step S2 to be longer than the heat preservation time of the thermal oxidation treatment process in the step S1, the first oxide layer formed in the oxygen diffusion treatment process can be completely decomposed in the oxygen diffusion treatment process, the second oxide layer is prevented from being influenced by the residue of the first oxide layer to be combined with the titanium alloy substrate, and further the second oxide layer formed by the secondary thermal oxidation treatment in the step S3 is ensured to be tightly combined with the titanium alloy.
Specifically, in step S1, after the titanium alloy to be treated is placed in the treatment equipment, the temperature in the treatment equipment is raised and kept at 700-800 ℃, then oxygen is introduced, and the temperature is kept for 0.3-0.7 h, so that a first oxide layer with the thickness of 1-5 μm is formed on the surface of the titanium alloy, and in step S2, the temperature keeping time is controlled to be more than 10h under the condition that the temperature in the treatment equipment is kept unchanged, so that the first oxide layer can be completely decomposed and a diffusion layer with a certain thickness can be formed.
Preferably, in step S3 of the present invention, the temperature of the reheat oxidation treatment process is controlled to be the same temperature as that in the thermal oxidation treatment process in step S1, and the warm-up time of the reheat oxidation treatment process is controlled to be shorter than that in the thermal oxidation treatment process in step S1. In this way, the second oxide layer with proper thickness can be formed on the surface of the titanium alloy with the supersaturated solid solution tissue of oxygen, so that the problems of cracking and peeling caused by the too thick second oxide layer are avoided, and finally the second oxide layer with proper thickness and tightly combined with the titanium alloy matrix is obtained.
Specifically, in the step S1, the temperature in the thermal oxidation treatment process is controlled to be 700-800 ℃, the heat preservation time is controlled to be 0.3-0.7 h, and in the case that the same temperature as that in the step S1 is adopted in the step S3, the heat preservation time is controlled to be 0.1-0.3 h, so that the effect of obtaining the second oxide layer with proper thickness and tightly combined with the titanium alloy matrix is achieved.
Preferably, in the present invention, an ion diffusion furnace, such as an ion nitriding furnace, may be used as the treatment apparatus to complete the oxygen permeation treatment of the titanium alloy to be treated. Therefore, the thermal oxidation treatment, the oxygen diffusion treatment and the reheat oxidation treatment of the titanium alloy can be sequentially completed in the ion diffusion furnace, the time of oxygen permeation of the titanium alloy is shortened, the complex processes of multiple times of furnace loading and temperature rising are avoided, the efficiency of oxygen permeation treatment of the titanium alloy is improved, and the decomposition of the first oxide layer in the step S2 can be promoted by means of ion bombardment, so that the tight combination of the second oxide layer and the titanium alloy matrix in the step S3 is ensured.
Specifically, when the ion diffusion furnace is adopted, in step S1, argon gas can be introduced into the ion diffusion furnace, ion bombardment heating is performed on the titanium alloy to be treated, oxygen gas is introduced after the temperature in the ion diffusion furnace reaches 700-800 ℃, the introducing ratio of the argon gas to the oxygen gas is controlled to be less than 1, and the heat preservation time is controlled to be 0.3-0.7 h, so that a first oxide layer with the thickness of 1-5 μm is formed. In the step S2, oxygen is stopped from being introduced, argon is adopted for ion bombardment, the temperature in the ion diffusion furnace is kept at 700-800 ℃, and the temperature is kept for 10-16 hours, so that the first oxide layer is completely decomposed, and a diffusion layer with a certain thickness is obtained. In the step S3, oxygen is re-introduced, the oxygen and argon are used for ion bombardment, the temperature in the ion diffusion furnace is kept at 700-800 ℃, the heat preservation time is controlled at 0.1-0.3 h, and therefore a second oxide layer is formed on the surface of the titanium alloy again, a composite hardening layer with high hardness, low friction coefficient, high thickness and good binding force is obtained, and the hardening treatment of the titanium alloy is completed.
In addition, the titanium alloy ion oxygen permeation method of the invention further comprises a step S4, specifically, after the step S3 is completed, oxygen is stopped from being introduced, the temperature in the ion permeation and expansion furnace is slowly cooled to 600 ℃ by utilizing argon ion bombardment, then heating is stopped, the ion permeation and expansion furnace is cooled to below 150 ℃, and the treated titanium alloy is taken out.
In addition, before the thermal oxidation treatment of step S1 is performed on the titanium alloy, surface cleaning and drying treatment may be performed on the titanium alloy in advance to remove impurities adhering to the surface of the titanium alloy, thereby improving the effect of the surface hardening treatment on the titanium alloy.
Next, advantageous technical effects of the technical scheme of the present invention are further described through examples and comparative examples.
Example 1
And (5) carrying out surface treatment on the titanium alloy test piece with the mark TA 2. Firstly, carrying out surface degreasing cleaning treatment and drying treatment on a titanium alloy test piece to be treated by utilizing an ultrasonic cleaner, so as to avoid the influence of greasy dirt impurities on subsequent ion oxygen permeation. Then, placing the titanium alloy test piece in an ion diffusion furnace for ion oxygen permeation treatment, wherein the specific treatment steps are as follows:
and S1, performing thermal oxidation treatment. And vacuumizing the air pressure in the ion diffusion furnace to below 10Pa, placing the titanium alloy test piece subjected to surface treatment and drying treatment in the ion diffusion furnace, adjusting the voltage and the duty ratio, introducing argon into the ion diffusion furnace, keeping the voltage at 800-1000V and the air pressure at 300-500 Pa, starting introducing oxygen after the temperature of the titanium alloy test piece reaches 750 ℃, and preserving the temperature for 0.5h.
And S2, oxygen diffusion treatment. Stopping introducing oxygen, keeping argon as a bombardment air source, keeping the voltage at 800-1000V, the air pressure at 300-500 Pa, and keeping the temperature of the test piece at 750 ℃ for 12h.
And S3, performing reheat oxidation treatment. And (3) introducing oxygen again, performing ion bombardment by using argon and oxygen, maintaining the voltage at 800-1000V and the gas pressure at 300-500 Pa, and preserving the temperature of the test piece at 750 ℃ for 0.3h.
And S4, stopping introducing oxygen, slowly cooling the temperature in the furnace to 600 ℃ by utilizing argon ion bombardment, stopping heating, cooling the ion diffusion furnace to below 150 ℃, and then opening the furnace to obtain a test piece corresponding to the metallographic photograph shown in FIG. 2.
Comparative example 1
The same brand of titanium alloy test pieces were subjected to surface treatment in the same manner as in example 1, except that the titanium alloy work pieces were subjected to the thermal oxidation treatment of step S1, without the oxygen diffusion treatment of step S2 and the reheat oxidation treatment of step S3, to obtain test pieces corresponding to metallographic photographs shown in fig. 3.
Comparative example 2
The same brand of titanium alloy test pieces were subjected to surface treatment in the same manner as in example 1, except that the titanium alloy work pieces were subjected to the heat oxidation treatment of step S1 and the oxygen diffusion treatment of step S2, without the reheat oxidation treatment of step S3, to obtain test pieces corresponding to metallographic photographs shown in fig. 4.
Comparative example 3
The same brand of titanium alloy test pieces were subjected to surface treatment in the same manner as in example 1, except that the heat-retaining time of the oxygen diffusion treatment in step S2 was reduced to 8 hours, and test pieces corresponding to metallographic photographs shown in fig. 5 were obtained.
Comparative example 4
The same brand of titanium alloy test pieces were subjected to surface treatment in the same manner as in example 1, except that the heat-retaining time of the reheat oxidation treatment in step S3 was increased to 0.5h, and test pieces corresponding to metallographic photographs shown in fig. 6 were obtained.
The untreated titanium alloy test pieces and the treated test pieces obtained in example 1, comparative example 2, comparative example 3 and comparative example 4 were subjected to surface hardness, hardened layer thickness and friction coefficient detection, respectively, to obtain the data shown in table 1.
TABLE 1
As can be seen from a combination of Table 1 and FIG. 2, the titanium alloy test piece obtained by the treatment of example 1 had not only an increased surface hardness of 911HV compared with the untreated titanium alloy test piece 0.05 The thickness of the hardness layer reaches 80 mu m, the hardness layer comprises a complete and uniform 4.64 mu m surface hardness layer, the friction coefficient is greatly reduced to 0.18, and the low friction coefficient and high resistance are obtainedThe abrasive outer surface layer and the hard and thick inner surface layer have good binding force, and achieve better hardening effect on the titanium alloy.
As can be seen from a combination of Table 1 and FIG. 3, the titanium alloy specimen obtained by the treatment of comparative example 1 had a higher surface hardness than the untreated titanium alloy specimen, although the surface hardness was also improved to 862HV 0.05 . However, the surface hardness of the titanium alloy test piece obtained in example 1 was lower than that of the test piece, and at the same time, since it was not subjected to oxygen diffusion treatment, it formed only a surface hardness layer of approximately 3.45 μm in thickness, almost no diffusion layer was present, and the entire hardened layer thickness was less than 20 μm.
As can be seen from a combination of Table 1 and FIG. 4, the titanium alloy test piece obtained by the treatment of comparative example 2, as it was subjected to the thermal oxidation treatment and the oxygen diffusion treatment, obtained a hardened layer having a thickness of about 75 μm, had a surface hardness increased to 862HV 0.05 However, the friction coefficient of the surface is still higher without effective improvement due to no reheat oxidation treatment, and the tribological performance is poor.
As can be seen from the combination of table 1 and fig. 5, compared with the titanium alloy test piece obtained in example 1, the titanium alloy test piece obtained by the treatment of comparative example 3, because the oxygen diffusion treatment time in step S2 was shortened from 12h to 8h, the first oxide layer was not completely decomposed, which not only reduced the thickness of the diffusion layer (about only 50 μm), but also the remaining first oxide layer affected the formation of the subsequent second oxide layer, resulting in occurrence of film cracking and peeling of the second oxide layer, greatly reduced the bonding force between the second oxide layer and the titanium alloy test piece, and also resulted in higher surface friction coefficient.
As can be seen from the combination of table 1 and fig. 6, the titanium alloy test piece obtained by the treatment of comparative example 4 had a surface hardness and a hardened layer thickness decreased and a friction coefficient could not be effectively decreased because the reheat oxidation treatment time in step S3 was prolonged from 0.3h to 0.5h, that is, the reheat oxidation treatment time in step S3 was the same as the thermal oxidation treatment time in step S1, resulting in an excessively thick second oxide layer formed on the surface of the titanium alloy test piece, compared with the titanium alloy test piece obtained in example 1.
The foregoing is merely a specific embodiment of the invention and other modifications and variations can be made by those skilled in the art in light of the above teachings. It is to be understood by persons skilled in the art that the foregoing detailed description is provided for the purpose of illustrating the invention more fully, and that the scope of the invention is defined by the appended claims.
Claims (5)
1. The method for the ion oxygen permeation of the titanium alloy is characterized by comprising the following steps of:
step S1, performing thermal oxidation treatment; performing thermal oxidation treatment on the titanium alloy to be treated, and forming a first oxide layer with the thickness of 1-5 mu m on the surface of the titanium alloy;
step S2, oxygen diffusion treatment; performing oxygen diffusion treatment on the titanium alloy with the first oxide layer, and completely decomposing the first oxide layer to generate oxygen elements required by diffusion to form an oxygen diffusion layer;
step S3, reheat oxidation treatment; performing thermal oxidation treatment again on the titanium alloy with the obtained oxygen diffusion layer to form a second oxide layer on the surface of the titanium alloy;
adopting an ion diffusion furnace to finish the treatment of the steps S1-S3; in the step S1, argon is introduced into the ion diffusion furnace, ion bombardment heating is carried out on the titanium alloy to be treated, oxygen is introduced after the temperature in the ion diffusion furnace reaches 700-800 ℃, the ratio of the argon to the oxygen is less than 1, and the heat preservation time is controlled to be 0.3-0.7 h; in the step S2, oxygen is stopped from being introduced, ion bombardment is carried out by utilizing argon, the temperature in the ion permeation and expansion furnace is kept at 700-800 ℃, and the temperature is kept for 10-16 hours; in the step S3, oxygen is re-introduced, and oxygen and argon are used for ion bombardment, so that the temperature in the ion diffusion furnace is kept at 700-800 ℃, and the temperature is kept for 0.1-0.3 h.
2. The method according to claim 1, wherein the temperature of the oxygen diffusion treatment process in the step S2 is the same as the temperature of the thermal oxidation treatment process in the step S1.
3. The method according to claim 1, wherein the temperature of the thermal oxidation treatment process in the step S3 is the same as the temperature of the thermal oxidation treatment process in the step S1, and the thermal insulation time of the thermal oxidation treatment process in the step S3 is shorter than the thermal insulation time of the thermal oxidation treatment process in the step S1.
4. A method of ion-diffusing titanium alloy according to any one of claims 1 to 3, further comprising step S4, specifically, after step S3 is completed, stopping introducing oxygen, performing ion bombardment with argon, gradually cooling the temperature in the ion-diffusing furnace to 600 ℃, and then stopping heating, and cooling the ion-diffusing furnace to below 150 ℃.
5. A method of ion-doping oxygen of a titanium alloy according to any one of claims 1 to 3, further comprising surface cleaning and drying the titanium alloy to be treated prior to step S1.
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| CN114107879A (en) * | 2021-11-30 | 2022-03-01 | 河南科技大学 | Surface treatment method for improving wear resistance of titanium alloy under spent oil lubrication condition |
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