CN107012365A - A kind of control method of titanium alloy material protium content uniformity - Google Patents

A kind of control method of titanium alloy material protium content uniformity Download PDF

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Publication number
CN107012365A
CN107012365A CN201710197696.5A CN201710197696A CN107012365A CN 107012365 A CN107012365 A CN 107012365A CN 201710197696 A CN201710197696 A CN 201710197696A CN 107012365 A CN107012365 A CN 107012365A
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CN
China
Prior art keywords
titanium alloy
alloy material
control method
content uniformity
hydrogen
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Pending
Application number
CN201710197696.5A
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Chinese (zh)
Inventor
王强
杨春晟
王志远
王荣
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AECC Beijing Institute of Aeronautical Materials
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AECC Beijing Institute of Aeronautical Materials
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Priority to CN201710197696.5A priority Critical patent/CN107012365A/en
Publication of CN107012365A publication Critical patent/CN107012365A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C14/00Alloys based on titanium
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D3/00Diffusion processes for extraction of non-metals; Furnaces therefor
    • C21D3/02Extraction of non-metals
    • C21D3/06Extraction of hydrogen
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing 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
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • C22F1/183High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C8/00Solid 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
    • C23C8/06Solid 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
    • C23C8/08Solid 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

A kind of control method of titanium alloy material protium content uniformity disclosed by the invention.For example, the titanium alloy plate chosen is processed with after necessary milling processing, vacuum heat removes the hydrogen content of titanium alloy body.Titanium alloy plate after dehydrogenation is kept into vacuum at a certain temperature, hydrogeneous mixed gas is filled into heating furnace, and is incubated after a few hours, room temperature is cooled to, hydrogen standard substance in titanium alloy of the present invention is obtained.By detection, the hydrogen content in the serial titanium alloy hydrogen standard substance is effectively controlled, hydrogen content uniformity.

Description

A kind of control method of titanium alloy material protium content uniformity
Technical field
The present invention is a kind of control method of titanium alloy material protium content uniformity, belongs to titanium alloy material, especially It is to be flushed with hydrogen preparation technology field in titanium alloy standard substance, for preparing titanium alloy hydrogen standard substance.
Background technology
TC4 is a kind of type alpha+beta diphasic titanium alloy of moderate strength, and with excellent combination property, alloy works long hours Temperature is used widely up to 400 DEG C in Aero-Space, be in the national defence industry such as aircraft, naval vessel purposes at most, consumption most Big titanium alloy material.Protium belongs to harmful element in titanium alloy, after hydrogen content exceeds certain limit, can cause material , there are the failure modes such as hydrogen embrittlement, directly affects product quality in the drastically decline of performance.Therefore, the hydrogen in strict control titanium alloy Content, is to ensure one of important means of titanium alloy product quality.Hydrogen content determines general using thermal conductivity method and red in titanium alloy Outer method, above two method is instrumental method.And the titanium alloy hydrogen standard substance of solid is to carry out hydrogen content in titanium alloy The necessity of measure.How to ensure to be flushed with hydrogen smoothly completing with the uniformity of hydrogen content in titanium alloy for process is titanium alloy hydrogen standard Vital task prepared by material.
The content of the invention
Goal of the invention
It is an object of the invention to provide a kind of control method of titanium alloy material protium content uniformity, solve domestic existing There is titanium alloy hydrogen standard substance content, without effective distributed point in the range of the μ g/g of 30 μ g/g~200, it is impossible to meet hydrogen in titanium alloy The problem of detection.
Technical scheme
A kind of control method of titanium alloy material protium content uniformity is provided, this method comprises the following steps:
Step 1, dehydrogenation
Titanium alloy material is placed in vacuum environment, and by ambient temperature to 300 DEG C~800 DEG C, the heat time is At least 30min, wherein, the pressure of vacuum environment is no more than 1 × 10-3Pa;
Step 2, it is flushed with hydrogen
So that titanium alloy material is maintained in vacuum environment, and causes environment temperature to be cooled to, by quantitative uniform mixing Gas, which is filled into described vacuum environment, forms gaseous mixture environment, and described mixed gas includes hydrogen and inert gas;Afterwards Gaseous mixture environment is heated to 300 DEG C~800 DEG C, and is incubated more than 30min, room temperature is cooled to.
Preferably, described titanium alloy material is titanium alloy plate or titanium alloy rod bar.
Preferably, described vacuum environment is provided by vacuum furnace.
Preferably, the element mass fraction of described titanium alloy material is as follows:Aluminium Al be 5.5~6.8%, vanadium V be 3.5~ 4.5%th, iron Fe is titanium Ti less than 0.15%, surplus less than 0.3%, silicon Si.
Preferably, in step 2, quantitative gaseous mixture is filled into vacuum environment by way of multiple spot air inlet.
Preferably, in step one, before heating titanium alloy material, plate surface is carried out after milling processing.
Preferably, in vacuum environment, described titanium alloy material is placed on frock bracket.
Preferably, in the mixed gas, the volumn concentration of hydrogen is 5~15%
Technique effect
Process route is flushed with hydrogen by solid-state dehydrogenation, the mode of multiple spot air inlet is taken in vacuum drying oven, control heating-up temperature is delayed Slow heating, is incubated a few hours, is cooled to room temperature.TC4 titanium alloy hydrogen standard substances are obtained, are had good uniformity, stability is strong, reaches The international advanced level with class standard.
Embodiment
It is described in further detail with reference to this method technical scheme.
A kind of control method of titanium alloy material protium content uniformity is provided, following steps are specifically included:
Step 1:Dehydrogenation
To the titanium alloy plate (such as TC4 titanium alloys) of selection, the mass fraction of each element is as follows:Ti~90%, Al~ 6%, V~4%, Fe~0.05%, Si~0.05%, carry out milling processing by titanium alloy plate afterwards, are placed in heating in vacuum Carry out dehydrogenation heating in stove, the interior pressure of heating-up temperature to 300 DEG C~500 DEG C, vacuum drying oven for 1 × 10-3Pa, soaking time extremely Few 30min;Wherein, titanium alloy plate can be machined as coupon after the heating;
Step 2:It is flushed with hydrogen
Titanium alloy plate after dehydrogenation is cooled to environment temperature in vacuum furnace, be filled with a vacuum furnace hydrogen with it is lazy Property gas gaseous mixture, and take the mode of multiple spot air inlet to inflate, gas be filled into after heating furnace, control heating-up temperature is slow 400 DEG C~500 DEG C are warming up to, after being incubated 6~8 hours, room temperature is cooled to.

Claims (8)

1. a kind of control method of titanium alloy material protium content uniformity, this method comprises the following steps:
Step 1, dehydrogenation
Titanium alloy material is placed in vacuum environment, and by ambient temperature to 300 DEG C~800 DEG C, the heat time is at least 30min, wherein, the pressure values of vacuum environment are less than or equal to 10-3Pa;
Step 2, it is flushed with hydrogen
So that titanium alloy material is maintained in vacuum environment, and causes environment temperature to be cooled to, quantitative homogeneous mixture is filled Enter into described vacuum environment to be formed gaseous mixture environment, described mixed gas includes hydrogen and inert gas;Afterwards will be mixed Close compression ring border and be heated to 300 DEG C~800 DEG C, and be incubated more than 30min, be cooled to room temperature.
2. a kind of control method of titanium alloy material protium content uniformity according to claim 1, it is characterised in that: Described vacuum environment is provided by vacuum furnace.
3. a kind of control method of titanium alloy material protium content uniformity according to claim 1, it is characterised in that: Each element mass fraction is as follows in described titanium alloy material:Aluminium Al is that 5.5~6.8%, vanadium V is that 3.5~4.5%, iron Fe is low It is titanium Ti to be less than 0.15%, surplus in 0.3%, silicon Si.
4. a kind of control method of titanium alloy material protium content uniformity according to claim 1, it is characterised in that: In step 2, quantitative gaseous mixture is filled into vacuum environment by way of multiple spot air inlet.
5. a kind of control method of titanium alloy material protium content uniformity according to claim 1, it is characterised in that: In step one, before heating titanium alloy material, titanium alloy material surface is carried out after milling processing.
6. a kind of control method of titanium alloy material protium content uniformity according to claim 1, it is characterised in that: In vacuum environment, described titanium alloy material is placed on frock bracket.
7. a kind of control method of titanium alloy material protium content uniformity according to claim 1, it is characterised in that: In the mixed gas, the volumn concentration of hydrogen is 5~15%.
8. a kind of control method of titanium alloy material protium content uniformity according to claim 1, it is characterised in that: Described titanium alloy material is titanium alloy plate or titanium alloy rod bar.
CN201710197696.5A 2017-03-29 2017-03-29 A kind of control method of titanium alloy material protium content uniformity Pending CN107012365A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710197696.5A CN107012365A (en) 2017-03-29 2017-03-29 A kind of control method of titanium alloy material protium content uniformity

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710197696.5A CN107012365A (en) 2017-03-29 2017-03-29 A kind of control method of titanium alloy material protium content uniformity

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CN107012365A true CN107012365A (en) 2017-08-04

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101975750A (en) * 2010-08-17 2011-02-16 中国船舶重工集团公司第十二研究所 Standard substance for TC11 titanium alloy photoelectric spectral analysis and preparation method thereof
CN103255317A (en) * 2013-05-23 2013-08-21 北京科技大学 Method for preparing Ti6Al4V alloy through high-speed press forming
CN104087772A (en) * 2014-07-03 2014-10-08 昆明冶金研究院 Powder metallurgy method for preparing high-density titanium and titanium alloy
CN106637015A (en) * 2016-12-08 2017-05-10 沈阳铸造研究所 Heat treatment technology for refining Ti-5Al-2.5Sn ELI alloy casting structure

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101975750A (en) * 2010-08-17 2011-02-16 中国船舶重工集团公司第十二研究所 Standard substance for TC11 titanium alloy photoelectric spectral analysis and preparation method thereof
CN103255317A (en) * 2013-05-23 2013-08-21 北京科技大学 Method for preparing Ti6Al4V alloy through high-speed press forming
CN104087772A (en) * 2014-07-03 2014-10-08 昆明冶金研究院 Powder metallurgy method for preparing high-density titanium and titanium alloy
CN106637015A (en) * 2016-12-08 2017-05-10 沈阳铸造研究所 Heat treatment technology for refining Ti-5Al-2.5Sn ELI alloy casting structure

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
张克顺等: "钛中氢成分分析标准物质研制", 《冶金分析》 *
张建军等: "《机械工程材料》", 31 March 2015, 西南师范大学出版社 *
杨春晟等: "《理化检测技术进展》", 31 January 2012, 国防工业出版社 *

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