CN109536876B - Pretreatment method for improving oxygen permeability of TC11 titanium alloy surface - Google Patents
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- 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
- C23C8/08—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 only one element being applied
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- 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
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Abstract
The invention provides a pretreatment method for improving the oxygen permeability of the surface of TC11 titanium alloy, which improves the oxygen permeability of the TC11 titanium alloy by adopting proper preheating treatment and proper processing size control after heat treatment on the premise of not changing the original mature oxygen permeability technological parameters, obviously improves the surface hardness and the depth of an oxygen permeability layer of a TC11 titanium alloy part, and better meets the requirement of the surface wear resistance of the part.
Description
Technical Field
The invention belongs to the technical field of surface protection, and particularly provides a pretreatment method for improving the oxygen permeability of the surface of a TC11 titanium alloy.
Background
The TC11 titanium alloy has excellent properties such as high melting point, high specific strength, low density, high fatigue performance, high corrosion resistance, etc., but its application is limited due to the disadvantage of poor surface fatigue resistance, hardness, wear resistance and fretting wear resistance, and surface oxygen permeation treatment is generally adopted to improve the surface hardness and wear resistance of the material. However, in the case of oxygen permeation in the oxygen permeation process determined by previous research, the phenomena of insufficient surface hardness and depth of the oxygen permeation layer often occur, and the requirement of surface wear resistance of parts cannot be met. At present, in order to improve the oxygen permeability of the surface of the TC11 titanium alloy, the prior art can only adjust the oxygen permeability process, improve the oxygen permeability temperature and the heat preservation time, but the method can cause the surface quality of parts to be reduced, the phenomenon of oxide skin occurs, and certain influence can be caused on the mechanical property of a matrix.
The field needs a method for improving the oxygen permeability of TC11 titanium alloy on the premise of not changing the oxygen permeability process parameters.
Disclosure of Invention
The invention aims to provide a pretreatment method for improving the oxygen permeability of the surface of TC11 titanium alloy, which improves the oxygen permeability of the TC11 titanium alloy by adopting proper preliminary heat treatment and proper processing size control after the heat treatment on the premise of not changing the original mature oxygen permeability process parameters, thereby improving the surface hardness and the depth of an oxygen permeability layer of the TC11 titanium alloy, greatly improving the quality of the oxygen permeability layer of a part and better meeting the requirement of the surface wear resistance of the part.
The technical scheme of the invention is as follows:
a pretreatment method for improving the oxygen permeability of the surface of TC11 titanium alloy is characterized in that the method is to carry out vacuum pretreatment before oxygen permeability of a TC11 titanium alloy part, and the treatment process comprises the following steps: keeping the temperature at 950 ℃ for 60-70min, filling 0.2-0.4MPa of argon after the heat preservation is finished, cooling to below 80 ℃, and discharging.
The key point of the method is that the conventional idea is broken, namely the improvement of the surface hardness and the depth of the oxygen permeation layer can be realized not only by changing the oxygen permeation process, but also by proper preliminary heat treatment.
According to the invention, the TC11 titanium alloy comprises, by weight, 5.8-7.0% of Al, 2.8-3.8% of Mo, 0.8-2.0% of Zr, 0.2-0.35% of Si, and the balance Ti.
Before the vacuum pretreatment heating, the pressure in the vacuum chamber is pumped to be below 0.067 Pa.
After the vacuum pretreatment is finished, the corundum sand embedding method is adopted for oxygen permeation, and the oxygen permeation process is preferably as follows: cooling at 800 deg.c/10 hr in air.
The part is subjected to secondary annealing after oxygen permeation, and the annealing process is preferably 530 ℃/6h and air-cooled.
The method can obviously improve the oxygen permeability of the surface of the TC11 titanium alloy, can leave a certain machining allowance after pretreatment, and is suitable for all parts of the TC11 titanium alloy. Namely, the part can be directly subjected to oxygen permeation treatment after vacuum pretreatment, or can be subjected to oxygen permeation treatment after machining, and the machining allowance is controlled within 0.5 mm.
Researches show that vacuum annealing is carried out according to a one-time annealing system of materials before oxygen permeation of TC11 titanium alloy parts, and the surface machining allowance of the parts is controlled within 0.5mm after the vacuum annealing, so that the oxygen permeation capability of the alloy can be obviously improved. The oxygen permeating layer is a saturated solid solution layer of oxygen in alpha phase, and the vacuum heat treatment can raise the alpha phase content near the surface of the part, so as to raise the oxygen permeating capacity of the alloy and raise the surface hardness and depth of the permeated layer. Therefore, the vacuum pretreatment of the invention becomes a technical key.
The invention also provides a method for permeating oxygen on the surface of the TC11 titanium alloy, which is characterized by comprising the following steps:
(1) and (4) checking: the method comprises the following steps of (1) carrying out process inspection on an incoming part (the blank stage can not carry out heat treatment), wherein the part is required to be clean and has no defects such as collision damage and the like;
(2) cleaning: cleaning the parts with acetone and drying;
(3) vacuum pretreatment: before heating, the pressure in the vacuum chamber is pumped to be below 0.067Pa, the temperature is raised to 950 ℃, the temperature is kept for 60-70min, and after the temperature is kept, argon gas with the pressure of 0.2-0.4MPa is filled for cooling to be below 80 ℃ and then the mixture is discharged;
(4) oxygen permeation: the corundum sand embedding method is used for oxygen permeation, and the oxygen permeation process comprises the following steps: air cooling at the temperature of 800 ℃/10 h;
(5) secondary annealing: cooling at 530 deg.c/6 hr in air.
The invention discloses a method for permeating oxygen on the surface of TC11 titanium alloy, which is characterized in that: after the vacuum pretreatment in the step 3), mechanical processing can be carried out, and the mechanical processing allowance of the oxygen-permeated surface is controlled within 0.5 mm.
The invention adopts a mature oxygen permeation process to perform oxygen permeation and secondary annealing on the part, a hardness detection sample is cut on the part after the part is taken out of a furnace, surface microhardness and depth detection of a permeation layer are performed, and the surface hardness of the part subjected to the oxygen permeation treatment is 561kg/mm2-695kg/mm2Penetration depth of 0.07-0.12mm, and parts without vacuum pretreatment (455 kg/mm)2-510kg/mm2And the depth of the penetrated layer is 0.04-0.06mm), the hardening degree is obviously improved.
The invention has the beneficial effects that:
on the premise of not changing the original mature oxygen permeation technological parameters, the invention improves the oxygen permeation capability of the TC11 titanium alloy by adopting proper preheating treatment and proper processing size control after heat treatment, obviously improves the surface hardness and the oxygen permeation layer depth of the titanium alloy part, and better meets the requirement of the surface wear resistance of the part.
The method is not only suitable for machining finished parts, but also suitable for parts with certain machining allowance. The TC11 titanium alloy is used for manufacturing the wear-resistant part, and after the pretreatment method is adopted, the surface hardness of an oxygen permeation layer can be improved by 23-53 percent, and the thickness of the oxygen permeation layer can be improved by 42-111 percent.
At present, the method disclosed by the invention is applied to the production of TC11 titanium alloy parts which need to work in a high-wear environment for a long time, and the engineering application is realized. The method has simple process and easy operation, can achieve the effect of improving the oxygen permeation capability of the TC11 alloy by adopting vacuum pretreatment to replace one-time annealing of parts at the blank stage, can be popularized to other manufacturing enterprises and pretreatment before oxygen permeation of other titanium alloy materials, and has wide application value.
Drawings
FIG. 1 shows the near-surface metallographic structure of TC11 alloy in different pre-treated states before oxygen permeation, wherein A is the non-pre-treated near-surface structure, and B is the vacuum pre-treated near-surface structure.
FIG. 2 is a graph showing the effect of the vacuum pretreatment on the surface hardness of the oxygen permeated layer in example 1.
FIG. 3 is a graph showing the effect of vacuum pretreatment on the depth of an oxygen permeation layer in example 1.
Detailed Description
The base material of the part used in the embodiment of the invention is TC11 titanium alloy, and the base material comprises the following chemical components in percentage by weight: 5.8 to 7.0% of Al, 2.8 to 3.8% of Mo, 0.8 to 2.0% of Zr, 0.2 to 0.35% of Si, and the balance of Ti.
Example 1
A pretreatment method for improving the oxygen permeability of the surface of TC11 titanium alloy comprises the following steps:
(1) and (4) checking: process inspection is carried out on the incoming piece;
(2) cleaning: cleaning the parts with acetone and drying;
(3) vacuum pretreatment: before heating, the pressure in the vacuum chamber is pumped to be below 0.067Pa, 950 ℃/60min, after heat preservation is finished, argon gas with 0.4MPa is filled, and the mixture is cooled to be below 80 ℃ and discharged; after the part is taken out of the furnace, a metallographic sample is cut from the part, and the pretreated sample is compared with the non-pretreated sample, so that the content of the alpha phase of the near-surface structure of the pretreated part is 50.9 percent and is obviously higher than the content of the alpha phase (40.3 percent) of the near-surface structure of the non-pretreated part (see figure 1).
(4) Oxygen permeation: the corundum sand embedding method is used for oxygen permeation, and the oxygen permeation process comprises the following steps: heating to 800 ℃, preserving heat for 10h, and cooling in air;
(5) secondary annealing: keeping the temperature at 530 ℃ for 6h, and cooling in air;
(6) and (4) checking: the surface microhardness and the hardening depth of the alpha hardened layer are checked by using a microhardness tester. Fig. 2 and 3 are graphs showing the comparison of the influence of vacuum pretreatment and non-vacuum pretreatment on the surface hardness and the depth of the final oxygen permeation layer.
Example 2
A pretreatment method for improving the oxygen permeability of the surface of TC11 titanium alloy comprises the following steps:
(1) and (4) checking: process inspection is carried out on the incoming piece;
(2) cleaning: cleaning the parts with acetone and drying;
(3) vacuum pretreatment: before heating, the pressure in the vacuum chamber is pumped to be below 0.067Pa, 950 ℃/65min, and argon gas of 0.2MPa is filled for cooling;
(4) and (3) machining: controlling the machining allowance of the oxygen-permeated surface to be not more than 0.3 mm;
(5) oxygen permeation: the corundum sand embedding method is used for oxygen permeation, and the oxygen permeation process comprises the following steps: air cooling at the temperature of 800 ℃/10 h;
(6) secondary annealing: keeping the temperature at 530 ℃ for 6h, and cooling in air;
(7) and (4) checking: the surface microhardness and the hardening depth of the alpha hardened layer are checked by using a microhardness tester. The surface hardness of the oxygen-permeated part was 690kg/mm2Seepage, oozeThe depth of layer was 0.11 mm.
Example 3
A pretreatment method for improving the oxygen permeability of the surface of TC11 titanium alloy comprises the following steps:
(1) and (4) checking: process inspection is carried out on the incoming piece;
(2) cleaning: cleaning the parts with acetone and drying;
(3) vacuum pretreatment: before heating, the pressure in the vacuum chamber is pumped to be below 0.067Pa, 950 ℃/70min, and argon gas of 0.3MPa is filled for cooling;
(4) and (3) machining: controlling the machining allowance of the oxygen-permeated surface to be not more than 0.5 mm;
(5) oxygen permeation: the corundum sand embedding method is used for oxygen permeation, and the oxygen permeation process comprises the following steps: air cooling at the temperature of 800 ℃/10 h;
(6) secondary annealing: keeping the temperature at 530 ℃ for 6h, and cooling in air;
(7) and (4) checking: the surface microhardness and the hardening depth of the alpha hardened layer are checked by using a microhardness tester. The surface hardness of the part subjected to the oxygen permeation treatment is 630kg/mm2The depth of the infiltrated layer is 0.08 mm.
The invention is not the best known technology.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (8)
1. A pretreatment method for improving the oxygen permeability of the surface of TC11 titanium alloy is characterized in that the method is to carry out vacuum pretreatment before oxygen permeability of a TC11 titanium alloy part, and the treatment process comprises the following steps: pumping the pressure in the vacuum chamber to below 0.067Pa, heating to 950 ℃, preserving heat for 60-70min, filling 0.2-0.4MPa argon after heat preservation, cooling to below 80 ℃, and discharging.
2. The pretreatment method for improving the oxygen permeability of the surface of the TC11 titanium alloy according to claim 1, wherein the pretreatment method comprises the following steps: the TC11 titanium alloy comprises, by weight, 5.8-7.0% of Al, 2.8-3.8% of Mo, 0.8-2.0% of Zr, 0.2-0.35% of Si, and the balance Ti.
3. The pretreatment method for improving the oxygen permeability of the surface of the TC11 titanium alloy according to claim 1, wherein the pretreatment method comprises the following steps: the corundum sand embedding method is used for oxygen permeation, and the oxygen permeation process comprises the following steps: cooling at 800 deg.c/10 hr in air.
4. The pretreatment method for improving the oxygen permeability of the surface of the TC11 titanium alloy according to claim 1, wherein the pretreatment method comprises the following steps: and (4) carrying out secondary annealing after oxygen permeation of the part, wherein the annealing process is 530 ℃/6h, and air cooling.
5. The pretreatment method for improving the oxygen permeability of the surface of the TC11 titanium alloy according to claim 1, wherein the pretreatment method comprises the following steps: the part is directly treated by oxygen permeation after vacuum pretreatment, or is treated by oxygen permeation after machining, and the machining allowance is controlled within 0.5 mm.
6. A method for permeating oxygen on the surface of TC11 titanium alloy is characterized by comprising the following steps:
(1) and (4) checking: process inspection is carried out on the incoming piece;
(2) cleaning: cleaning the parts with acetone and drying;
(3) vacuum pretreatment: before heating, the pressure in the vacuum chamber is pumped to be below 0.067Pa, the temperature is raised to 950 ℃, the temperature is kept for 60-70min, and after the temperature is kept, argon gas with the pressure of 0.2-0.4MPa is filled for cooling to be below 80 ℃ and then the mixture is discharged;
(4) oxygen permeation: the corundum sand embedding method is used for oxygen permeation, and the oxygen permeation process comprises the following steps: air cooling at the temperature of 800 ℃/10 h;
(5) secondary annealing: cooling at 530 deg.c/6 hr in air.
7. The method for surface oxygen permeation of TC11 titanium alloy as set forth in claim 6, wherein: and (4) carrying out mechanical processing after the vacuum pretreatment in the step (3), and controlling the mechanical processing allowance of the oxygen-permeated surface within 0.5 mm.
8. The method for surface oxygen permeation of TC11 titanium alloy as set forth in claim 6, wherein: the surface hardness of the finally obtained TC11 titanium alloy oxygen permeation layer is 561kg/mm2-695kg/mm2The depth of the penetrated layer is 0.07-0.12 mm.
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| CN1363713A (en) * | 2001-12-06 | 2002-08-14 | 沈阳黎明航空发动机集团公司 | Process for osmosizing oxygen to Ti alloy |
| CN101713060A (en) * | 2009-12-29 | 2010-05-26 | 江苏工业学院 | Method for improving surface comprehensive performance of pure titanium |
| CN103469147A (en) * | 2013-09-24 | 2013-12-25 | 贵州师范大学 | Low-pressure pulse vacuum nitriding method and low-pressure pulse vacuum nitriding device for titanium alloy |
| CN103540796A (en) * | 2012-07-11 | 2014-01-29 | 东港市东方高新金属材料有限公司 | Titanium alloy (TC11) rolled tube and preparation method thereof |
| CN103789717A (en) * | 2014-01-22 | 2014-05-14 | 沈阳理工大学 | Titanium/titanium alloy surface oxygen permeation method |
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| WO2018128160A1 (en) * | 2017-01-03 | 2018-07-12 | カシオ計算機株式会社 | Alloy member and method for hardening surface thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1363713A (en) * | 2001-12-06 | 2002-08-14 | 沈阳黎明航空发动机集团公司 | Process for osmosizing oxygen to Ti alloy |
| CN101713060A (en) * | 2009-12-29 | 2010-05-26 | 江苏工业学院 | Method for improving surface comprehensive performance of pure titanium |
| CN103540796A (en) * | 2012-07-11 | 2014-01-29 | 东港市东方高新金属材料有限公司 | Titanium alloy (TC11) rolled tube and preparation method thereof |
| CN103469147A (en) * | 2013-09-24 | 2013-12-25 | 贵州师范大学 | Low-pressure pulse vacuum nitriding method and low-pressure pulse vacuum nitriding device for titanium alloy |
| CN103789717A (en) * | 2014-01-22 | 2014-05-14 | 沈阳理工大学 | Titanium/titanium alloy surface oxygen permeation method |
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