CN109536876A - A kind of preprocess method for improving TC11 titanium alloy surface and seeping oxygen ability - Google Patents
A kind of preprocess method for improving TC11 titanium alloy surface and seeping oxygen ability Download PDFInfo
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- CN109536876A CN109536876A CN201811451793.3A CN201811451793A CN109536876A CN 109536876 A CN109536876 A CN 109536876A CN 201811451793 A CN201811451793 A CN 201811451793A CN 109536876 A CN109536876 A CN 109536876A
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- oxygen
- seeping
- titanium alloy
- alloy surface
- cooled
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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
- C23C8/08—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
- C23C8/10—Oxidising
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
-
- 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
- C23C8/02—Pretreatment of the material to be coated
-
- 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
- C23C8/80—After-treatment
Abstract
The present invention provides a kind of preprocess method of raising TC11 titanium alloy surface infiltration oxygen ability, the present invention is under the premise of not changing original mature oxygen permeation process parameter, by using processing dimension control appropriate after the pre-heat treatment appropriate and heat treatment, to improve TC11 osmosizing oxygen to Ti alloy ability, so that TC11 titanium alloy component surface hardness and oxygen diffusion layer depth significantly improve, the requirement of piece surface wearability has been better met.
Description
Technical field
The invention belongs to surface protection technique fields, especially provide it is a kind of raising TC11 titanium alloy surface seep oxygen ability it is pre-
Processing method.
Background technique
It is excellent that TC11 titanium alloy has that fusing point is high, specific strength is high, density is low, fatigue behaviour is high and corrosion resistance is high etc.
Performance, but because surface endurance, hardness, wear-resistant and poor Fretting disadvantage are restricted its application, in order to mention
The surface hardness and its wearability of high material are generally handled using Surface Oxygen Diffusion.But under the oxygen permeation process that early-stage study determines
Oxygen is seeped, the phenomenon of oxygen diffusion layer surface hardness and oxygen diffusion layer depth deficiency often occurs, the requirement of piece surface wearability is not achieved.Mesh
Before, seep oxygen ability to improve TC11 titanium alloy surface, the prior art can only be adjusted oxygen permeation process, improve seep oxygen temperature and
Soaking time, but this method will cause surface quality of workpieces to decline, and oxide skin phenomenon occur, and may produce to matrix mechanical property
Raw certain influence.
The field needs a kind of side that TC11 osmosizing oxygen to Ti alloy ability is improved under the premise of not changing oxygen permeation process parameter
Method.
Summary of the invention
The purpose of the present invention is to provide the preprocess method that a kind of raising TC11 titanium alloy surface seeps oxygen ability, this method
Under the premise of not changing former mature oxygen permeation process parameter, add by using appropriate after conditioning treatment appropriate and heat treatment
Work size Control, Lai Tigao TC11 osmosizing oxygen to Ti alloy ability, to improve TC11 osmosizing oxygen to Ti alloy layer surface hardness and infiltration layer depth
Degree, greatly improves part oxygen diffusion layer quality, has better met the requirement of piece surface wearability.
Technical solution of the present invention is as follows:
It is a kind of improve TC11 titanium alloy surface seep oxygen ability preprocess method, which is characterized in that the method be
TC11 titanium alloy component carries out vacuum pre-treatment, treatment process before seeping oxygen are as follows: 60-70min is kept the temperature at 950 DEG C, after heat preservation
It fills 0.2-0.4MPa argon gas and is cooled to 80 DEG C or less and come out of the stove.
The key point of the method for the invention is to break conventional theory, that is, improves oxygen diffusion layer surface hardness and oxygen diffusion layer is deep
Degree by just may be implemented by changing oxygen permeation process, can also not merely be realized by conditioning treatment appropriate.
In the present invention, by weight percentage, the group of the TC11 titanium alloy becomes 5.8~7.0%Al, 2.8~3.8%
Mo, 0.8~2.0%Zr, 0.2~0.35%Si, remaining be Ti.
Vacuum intraventricular pressure is evacuated to by force 0.067Pa or less before vacuum pre-treatment heating.
After the completion of vacuum pre-treatment, the present invention seeps oxygen using emergy implantation, and oxygen permeation process is preferred are as follows: 800 DEG C/
10h, it is air-cooled.
Part of the present invention carries out double annealing after seeping oxygen, and annealing process is preferably 530 DEG C/6h, air-cooled.
The method of the invention can significantly improve TC11 titanium alloy surface and seep oxygen ability, and can there are certain after pre-processing
Machining allowance, be suitable for all parts of TC11 titanium alloy.The i.e. described part can directly carry out seeping at oxygen after vacuum pre-treatment
Reason, can also it is machined after carry out seeping oxygen processing, machining allowance need to control within 0.5mm.
The study found that carrying out vacuum annealing by an annealing schedule of material before TC11 titanium alloy component infiltration oxygen, vacuum is moved back
The control of piece surface machining allowance is remarkably improved alloy and seeps oxygen ability within 0.5mm after fire.This is because oxygen diffusion layer is oxygen
Saturated solid solution layer in α phase, and part near surface α phase content can be improved in vacuum heat treatment, to effectively improve alloy
Oxygen ability is seeped, and then improves surface hardness and depth of penetration.Therefore vacuum pre-treatment of the present invention becomes key problem in technology.
The present invention also provides a kind of methods that oxygen is seeped in TC11 titanium alloy surface, which is characterized in that specific step is as follows:
(1) it checks: parcel received is carried out process inspection (blank stage can without heat treatment), the part should clean, nothing
The defects of bump injury；
(2) it cleans: part being cleaned out and dried with acetone；
(3) vacuum pre-treatment: vacuum intraventricular pressure is evacuated to 0.067Pa by force hereinafter, being warming up to 950 DEG C before heating, keeps the temperature 60-
70min fills 0.2-0.4MPa argon gas and is cooled to 80 DEG C or less and comes out of the stove after heat preservation；
(4) it seeps oxygen: seeping oxygen, oxygen permeation process are as follows: 800 DEG C/10h, air-cooled using emergy implantation；
(5) double annealing: 530 DEG C/6h, air-cooled.
The method of the present invention that oxygen is seeped in TC11 titanium alloy surface, it is characterised in that: after step 3) vacuum pre-treatment
It can be machined, must make to seep the control of oxygen surface machine-finish allowance within 0.5mm.
The present invention carries out part to seep oxygen and double annealing using mature oxygen permeation process, cuts hardness after coming out of the stove on part
Sample is detected, surface microhardness and depth of penetration detection are carried out, the piece surface hardness through seeping oxygen processing is 561kg/mm2-
695kg/mm2, depth of penetration 0.07-0.12mm, with the part (455kg/mm for not carrying out vacuum pre-treatment2-510kg/mm2,
Depth of penetration is 0.04-0.06mm) it compares, hardenability significantly improves.
The invention has the benefit that
The present invention be under the premise of not changing original mature oxygen permeation process parameter, by using the pre-heat treatment appropriate and
Processing dimension control appropriate after heat treatment, so that TC11 osmosizing oxygen to Ti alloy ability is improved, so that titanium alloy component surface hardness
And oxygen diffusion layer depth significantly improves, and has better met the requirement of piece surface wearability.
The method of the invention is not only suitable for machine and adds finished parts, while being suitable for the part with certain machining allowance.With
TC11 titanium alloy manufactures wearing piece, and using oxygen is seeped after the preprocess method, 23%-53% is can be improved in oxygen diffusion layer surface hardness, seeps
42%-111% can be improved in oxygen layer thickness.
The method of the invention has been applied to TC11 titanium alloy zero of the long-term work under high abrasion environment at present
In the production of part, engineering application is realized.This method simple process, it is easily operated, replace part to exist using vacuum pre-treatment
The primary annealing in woollen stage can reach the effect that TC11 alloy seeps oxygen ability that improves, extend to other manufacturing enterprises and
Other titanium alloy materials seep the pretreatment before oxygen, are with a wide range of applications.
Detailed description of the invention
Fig. 1 is the near surface metallographic structure under different pretreatments state before TC11 alloy infiltration oxygen, wherein A is not pre-process
Near surface tissue, B are vacuum pre-treatment near surface tissue.
Fig. 2 is influence of 1 vacuum pre-treatment of embodiment to oxygen diffusion layer surface hardness.
Fig. 3 is influence of 1 vacuum pre-treatment of embodiment to oxygen diffusion layer depth.
Specific embodiment
Part base solid material used in the embodiment of the present invention is TC11 titanium alloy, chemical component and weight percent are as follows: 5.8
~7.0%Al, 2.8~3.8%Mo, 0.8~2.0%Zr, 0.2~0.35%Si, remaining be Ti.
Embodiment 1
A kind of preprocess method for improving TC11 titanium alloy surface and seeping oxygen ability, follows the steps below:
(1) it checks: process inspection is carried out to parcel received；
(2) it cleans: part being cleaned out and dried with acetone；
(3) vacuum intraventricular pressure vacuum pre-treatment: is evacuated to 0.067Pa by force hereinafter, 950 DEG C/60min, heat preservation knot before heating
0.4MPa argon gas is filled after beam be cooled to 80 DEG C or less come out of the stove；Metallographic specimen is cut in part after coming out of the stove, by pretreated sample
It is compared with unpretreated sample, it is found that the near surface tissue α phase content of part after pretreatment is 50.9%, hence it is evident that high
In the near surface tissue α phase content (40.3%) (see Fig. 1) of not preprocessed part.
(4) it seeps oxygen: seeping oxygen, oxygen permeation process using emergy implantation are as follows: 800 DEG C of heat preservation 10h are heated to, it is air-cooled；
(5) double annealing: 530 DEG C of heat preservation 6h, it is air-cooled；
(6) it examines: being tested using microhardness testers to α hardened layer surface microhardness and hardening depth.Fig. 2,3 are
Carry out vacuum pre-treatment and the influence comparison without vacuum pre-treatment to final oxygen diffusion layer surface hardness and depth of penetration, You Tuke
To find out, using preprocess method of the present invention, oxygen diffusion layer surface hardness and depth of penetration can be significantly improved.
Embodiment 2
A kind of preprocess method for improving TC11 titanium alloy surface and seeping oxygen ability, follows the steps below:
(1) it checks: process inspection is carried out to parcel received；
(2) it cleans: part being cleaned out and dried with acetone；
(3) vacuum intraventricular pressure vacuum pre-treatment: is evacuated to 0.067Pa by force hereinafter, 950 DEG C/65min, fills before heating
0.2MPa argon gas is cooling；
(4) it is machined: seeping the control of oxygen surface machine-finish allowance and be not more than 0.3mm；
(5) it seeps oxygen: seeping oxygen, oxygen permeation process are as follows: 800 DEG C/10h, air-cooled using emergy implantation；
(6) double annealing: 530 DEG C of heat preservation 6h, it is air-cooled；
(7) it examines: being tested using microhardness testers to α hardened layer surface microhardness and hardening depth.Through seeping oxygen
The piece surface hardness of processing is 690kg/mm2, depth of penetration 0.11mm.
Embodiment 3
A kind of preprocess method for improving TC11 titanium alloy surface and seeping oxygen ability, follows the steps below:
(1) it checks: process inspection is carried out to parcel received；
(2) it cleans: part being cleaned out and dried with acetone；
(3) vacuum intraventricular pressure vacuum pre-treatment: is evacuated to 0.067Pa by force hereinafter, 950 DEG C/70min, fills before heating
0.3MPa argon gas is cooling；
(4) it is machined: seeping the control of oxygen surface machine-finish allowance and be not more than 0.5mm；
(5) it seeps oxygen: seeping oxygen, oxygen permeation process are as follows: 800 DEG C/10h, air-cooled using emergy implantation；
(6) double annealing: 530 DEG C of heat preservation 6h, it is air-cooled；
(7) it examines: being tested using microhardness testers to α hardened layer surface microhardness and hardening depth.Through seeping oxygen
The piece surface hardness of processing is 630kg/mm2, depth of penetration 0.08mm.
Unaccomplished matter of the present invention is well-known technique.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (9)
1. a kind of preprocess method for improving TC11 titanium alloy surface and seeping oxygen ability, which is characterized in that the method is in TC11
Titanium alloy component carries out vacuum pre-treatment, treatment process before seeping oxygen are as follows: keeps the temperature 60-70min at 950 DEG C, fills after heat preservation
0.2-0.4MPa argon gas is cooled to 80 DEG C or less and comes out of the stove.
2. seeping the preprocess method of oxygen ability according to raising TC11 titanium alloy surface described in claim 1, it is characterised in that: by weight
Measure percentages, the group of the TC11 titanium alloy become 5.8~7.0%Al, 2.8~3.8%Mo, 0.8~2.0%Zr, 0.2~
0.35%Si, remaining be Ti.
3. seeping the preprocess method of oxygen ability according to raising TC11 titanium alloy surface described in claim 1, it is characterised in that: true
Vacuum intraventricular pressure is evacuated to by force 0.067Pa or less before sky pretreatment heating.
4. seeping the preprocess method of oxygen ability according to raising TC11 titanium alloy surface described in claim 1, it is characterised in that: use
Emergy implantation seeps oxygen, oxygen permeation process are as follows: 800 DEG C/10h, air-cooled.
5. seeping the preprocess method of oxygen ability according to raising TC11 titanium alloy surface described in claim 1, it is characterised in that: part
Double annealing is carried out after seeping oxygen, annealing process is 530 DEG C/6h, air-cooled.
6. seeping the preprocess method of oxygen ability according to raising TC11 titanium alloy surface described in claim 1, it is characterised in that: part
After vacuum pre-treatment directly carry out seep oxygen processing or it is machined after carry out seep oxygen processing, machining allowance control 0.5mm it
It is interior.
7. a kind of method for seeping oxygen in TC11 titanium alloy surface, which is characterized in that specific step is as follows:
(1) it checks: process inspection is carried out to parcel received；
(2) it cleans: part being cleaned out and dried with acetone；
(3) vacuum pre-treatment: vacuum intraventricular pressure is evacuated to 0.067Pa by force hereinafter, being warming up to 950 DEG C before heating, keeps the temperature 60-
70min fills 0.2-0.4MPa argon gas and is cooled to 80 DEG C or less and comes out of the stove after heat preservation；
(4) it seeps oxygen: seeping oxygen, oxygen permeation process are as follows: 800 DEG C/10h, air-cooled using emergy implantation；
(5) double annealing: 530 DEG C/6h, air-cooled.
8. according to the method for seeping oxygen described in claim 7 in TC11 titanium alloy surface, it is characterised in that: locate in advance in step 3) vacuum
It is machined after reason, makes to seep within oxygen surface machine-finish allowance control 0.5mm.
9. according to the method for seeping oxygen described in claim 7 in TC11 titanium alloy surface, it is characterised in that: final gained TC11 titanium closes
Golden oxygen diffusion layer surface hardness is 561kg/mm2-695kg/mm2, depth of penetration 0.07-0.12mm.
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| CN201811451793.3A CN109536876B (en) | 2018-11-30 | 2018-11-30 | Pretreatment method for improving oxygen permeability of TC11 titanium alloy surface |
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| CN201811451793.3A CN109536876B (en) | 2018-11-30 | 2018-11-30 | Pretreatment method for improving oxygen permeability of TC11 titanium alloy surface |
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Citations (6)
| 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 |
| 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 |
| 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 |
-
2018
- 2018-11-30 CN CN201811451793.3A patent/CN109536876B/en active Active
Patent Citations (6)
| 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 |
| 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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