CN107699830B - Method that is a kind of while improving industrially pure titanium intensity and plasticity - Google Patents

Method that is a kind of while improving industrially pure titanium intensity and plasticity Download PDF

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CN107699830B
CN107699830B CN201710696551.XA CN201710696551A CN107699830B CN 107699830 B CN107699830 B CN 107699830B CN 201710696551 A CN201710696551 A CN 201710696551A CN 107699830 B CN107699830 B CN 107699830B
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plasticity
intensity
ball
titanium
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CN107699830A (en
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陈宏良
朱心昆
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Kunming University of Science and Technology
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    • 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

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  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
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Abstract

The present invention relates to a kind of methods for improving industrially pure titanium intensity and plasticity simultaneously, belong to materials processing technology field.Titanium board material is surface-treated through milling machine processing first, after removing surface defect and impurity, keeps the temperature 2 hours in 700 DEG C;By Titanium board material under vacuum or inert gas shielding, rotation speed is 860 ~ 890r/min, and frequency is 50 ~ 60Hz, 1 ~ 3h of ball-milling treatment;Titanium board material is immersed in liquid nitrogen and is rolled after cooling 5 ~ 10min;The dependent variable of rolling front and back plate reaches 92% ~ 98%, and cooling 5 ~ 10min in liquid nitrogen will be immersed before rolling per pass, and plate final thickness is 1mm;By plate at 450 ~ 520 DEG C 5 ~ 10min of vacuum annealing, be prepared while improving the industrially pure titanium plate of intensity and plasticity.The method that this method is combined by ball-milling treatment, liquid nitrogen rolling, low-temperature annealing, it is a kind of better than large plastometric set plasticity to obtain, the material of excellent combination property higher than conventional annealing intensity.

Description

Method that is a kind of while improving industrially pure titanium intensity and plasticity
Technical field
The present invention relates to a kind of methods for improving industrially pure titanium intensity and plasticity simultaneously, belong to materials processing technology field.
Background technique
The means of usual strengthening material have solution strengthening, refined crystalline strengthening, second-phase strength etc., and essence is all in the material All kinds of defects are introduced, keep dislocation motion difficult, to achieve the purpose that strengthening material.And refined crystalline strengthening is that unique one kind is improving The method that the strength of materials can improve plasticity again simultaneously.
In the past few decades, Development of Nanometer Material is rapid, is studied extensively due to its excellent mechanical property, with tradition Coarse grain material is compared, and nano material strong hardness is high, and wearability, corrosion resistance, fatigue resistance are good.At the same time, also occur being permitted More Nanostructured bulk technologies of preparing.These preparation methods can be divided into two major classes: a kind of method " from bottom to top ", with single former Son or nano particle are prepared for basic unit;Another kind of method " from top to bottom ", by specific processing technology in material Inside introduces the defects of a large amount of dislocation twin, refines former coarse-grain crystal grain.Severe Plastic Deformation Methods be the 1990s by Russian scientist R.Z.Valiev is developed on the basis of carrying out pure shear large deformation test, and so-called big plasticity becomes Shape just refers to method of the material by forming the bulk nanostructured material with nanocrystal after violent plastic deformation, now Common large plastometric set technique has: high pressure torsion (HPT), Equal Channel Angular Pressing (ECAP), Hopkinson technology (SHPB) etc..
The nano material as made from large plastometric set technique, although intensity is increased substantially, plasticity is often Very poor, fracture elongation is usually less than 5%, and which limits applications to nanostructures fields.Its reason can be concluded are as follows: nanometer material Expect that crystallite dimension is tiny, dislocation is caused to be absorbed and can not be accumulated in subsequent plastic deformation by crystal boundary, it is hard to lose processing Change ability, to show low elongation percentage.
By ball-milling technology, material surface crystal grain can be refined to 100nm hereinafter, still center portion still maintains former coarse-grain Crystal grain, to form a kind of gradient-structure constantly refined from table and inner crystal grain, this gradient within the scope of the certain depth of surface The combination of structure and coarse structure makes the strength of materials remain good plasticity again while raising.But by ball milling Reason, the strength of materials improve very limited.How to improve industrially pure titanium intensity and plasticity is a problem.
Summary of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provide it is a kind of and meanwhile improve industrially pure titanium intensity with The method of plasticity.The method that this method is combined by ball-milling treatment, liquid nitrogen rolling, low-temperature annealing, obtains a kind of than big plasticity It is good to deform plasticity, the material of excellent combination property higher than conventional annealing intensity, and by this technique, material surface obtains Strengthen, wearability, corrosion resistance, fatigue behaviour are largely increased.The invention is realized by the following technical scheme.
The present invention makes material generate large plastometric set using surface ball-milling technology, and then forms grain size gradient point The gradient-structure of cloth;Then liquid nitrogen rolling is carried out again, further increases its intensity while gradient-structure is kept;Finally pass through It anneals between low-temperature short-time, there is material and change in gradient from table and inner crystallite dimension, and there is partial region little crystal grain packet The surface and little crystal grain of enclosing large grain character surround the center portion of big crystal grain, to form a kind of material of strong plasticity no-float Material.
Method that is a kind of while improving industrially pure titanium intensity and plasticity, specific steps include:
Titanium board material is surface-treated by step 1 through milling machine processing first, after removing surface defect and impurity, in 700 DEG C heat preservation 2 hours;
Step 2, by the Titanium board material handled through step 1 under vacuum or inert gas shielding, rotation speed be 860 ~ 890r/min, frequency are 50 ~ 60Hz, 1 ~ 3h of ball-milling treatment;
Titanium board material after step 2 ball-milling treatment is immersed in liquid nitrogen and is rolled after cooling 5 ~ 10min by step 3;Before rolling The dependent variable of plate reaches 92% ~ 98% afterwards, and it is final that cooling 5 ~ 10min, plate in liquid nitrogen will be immersed before rolling per pass With a thickness of 1mm;
Step 4, by the plate handled through step 3 at 450 ~ 520 DEG C 5 ~ 10min of vacuum annealing, be prepared while mentioning The high industrially pure titanium plate of intensity and plasticity.
Titanium board material is in the step 1 with a thickness of 2mm.
The steel ball that 5 ~ 10 4 ~ 8mm of Φ are put into step 2 ball-milling treatment carries out ball milling.
The beneficial effects of the present invention are:
(1) modeling that the intensity of the industrially pure titanium of the method for the invention preparation is largely increased, while keeping its good again Property, and surface property is improved;Specifically: carrying out ball-milling treatment, material can obtain one from surface to center portion crystal grain ruler The gradient-structure that very little gradient increases.And since titanium belongs to close-packed hexagonal, keeps dislocation motion difficult in high strain rate deformation, hold Easily go out to generate twin.
(2) present invention carries out zerolling after surface mechanical attrition treatment, crystallite dimension up to 100 nanometers with Under, according to Hall-Petch formula, the strength of materials is significantly increased, but crystallite dimension reach nanoscale after plasticity it is very poor.Using 450 ~ 520 DEG C of short time annealing.Under this temperature, time, material has to be changed in gradient from table and inner crystallite dimension, and is had The surface of partial region little crystal grain encirclement large grain character;The center portion of little crystal grain encirclement big crystal grain.This special microstructure So that material has good plasticity while keeping intensity again.
Detailed description of the invention
Fig. 1 is the present invention through embodiment 1,2,3 while improving the industrially pure titanium and annealed state (700 of intensity and plasticity DEG C annealing 2 hours) industrially pure titanium plate room temperature tensile curve compare figure.
Specific embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
The method for improving industrially pure titanium intensity and plasticity simultaneously, specific steps include:
Titanium board material (2mm) is surface-treated by step 1 through milling machine processing first, after removing surface defect and impurity, 2 hours are kept the temperature in 700 DEG C;
Step 2, by the Titanium board material handled through step 1 under vacuum or inert gas shielding, be fixed on ball grinder center, And the steel ball for being put into 5 Φ 8mm carries out ball milling, the rotation speed of ball grinder is 860r/min, frequency 50Hz, handles the time 1h;
Titanium board material after step 2 ball-milling treatment is immersed in liquid nitrogen and is rolled after cooling 5min by step 3;Rolling front and back The dependent variable of plate reaches 92% ~ 98%, and will immerse cooling 5min, plate final thickness in liquid nitrogen before rolling per pass and be 1.045mm;
Step 4, by the plate handled through step 3 at 450 DEG C vacuum annealing 10min, be prepared while improving strong The industrially pure titanium plate of degree and plasticity.
It is bent that the stretching of the industrially pure titanium plate of intensity and plasticity at room temperature is improved while the present embodiment is prepared Line is as shown in figure 1 shown in curve 2, and as seen from the figure: preparation-obtained pure titanium yield strength is 255.6MPa, and tensile strength is 365.5MPa, uniform elongation 16.6%;The industrially pure titanium annealed 2 hours with 700 DEG C is compared, what the present embodiment was prepared Pure titanium yield strength promotes 34%, and uniform elongation improves 44%, has an excellent mechanical property, wearability, corrosion resistance, resist it is tired Labor gets a promotion simultaneously.
Embodiment 2
The method for improving industrially pure titanium intensity and plasticity simultaneously, specific steps include:
Titanium board material (2mm) is surface-treated by step 1 through milling machine processing first, after removing surface defect and impurity, In 700 DEG C of heat preservation 2h;
Step 2, by the Titanium board material handled through step 1 under vacuum or inert gas shielding, be fixed on ball grinder center, And the steel ball for being put into 10 Φ 4mm carries out ball milling, the rotation speed of ball grinder is 890r/min, frequency 60Hz, handles the time 3h;
Titanium board material after step 2 ball-milling treatment is immersed in liquid nitrogen and is rolled after cooling 10min by step 3;Rolling front and back The dependent variable of plate reaches 92% ~ 98%, and cooling 10min, plate final thickness in liquid nitrogen will be immersed before rolling per pass For 1.062mm;
Step 4, by the plate handled through step 3 at 520 DEG C vacuum annealing 5min, be prepared while improving intensity With the industrially pure titanium plate of plasticity.
It is bent that the stretching of the industrially pure titanium plate of intensity and plasticity at room temperature is improved while the present embodiment is prepared Line is as shown in figure 1 shown in curve 3, and as seen from the figure: preparation-obtained pure titanium yield strength is 252.4MPa, and tensile strength is 359.3MPa, uniform elongation 15.5%;The industrially pure titanium annealed 2 hours with 700 DEG C is compared, what the present embodiment was prepared Pure titanium yield strength promotes 32.7%, and uniform elongation improves 34.8%, has an excellent mechanical property, wearability, corrosion resistance, Fatigue resistance gets a promotion simultaneously.
Embodiment 3
The method for improving industrially pure titanium intensity and plasticity simultaneously, specific steps include:
Titanium board material (2mm) is surface-treated by step 1 through milling machine processing first, after removing surface defect and impurity, 2 hours are kept the temperature in 700 DEG C;
Step 2, by the Titanium board material handled through step 1 under vacuum or inert gas shielding, be fixed on ball grinder center, And the steel ball for being put into 8 Φ 6mm carries out ball milling, the rotation speed of ball grinder is 880r/min, frequency 55Hz, handles the time 2h;
Titanium board material after step 2 ball-milling treatment is immersed in liquid nitrogen and is rolled after cooling 8min by step 3;Rolling front and back The dependent variable of plate reaches 92% ~ 98%, and will immerse cooling 8min, plate final thickness in liquid nitrogen before rolling per pass and be 1.085mm;
Step 4, by the plate handled through step 3 at 470 DEG C vacuum annealing 8min, be prepared while improving intensity With the industrially pure titanium plate of plasticity.
It is bent that the stretching of the industrially pure titanium plate of intensity and plasticity at room temperature is improved while the present embodiment is prepared Line is as shown in figure 1 shown in curve 4, and as seen from the figure: preparation-obtained pure titanium yield strength is 282.2MPa, and tensile strength is 371.9MPa, uniform elongation 11.2%;The industrially pure titanium annealed 2 hours with 700 DEG C is compared, what the present embodiment was prepared Pure titanium yield strength promotes 48.4%, and uniform elongation is held essentially constant, and has an excellent mechanical property, wearability, corrosion-resistant Property, fatigue resistance get a promotion simultaneously.
In conjunction with attached drawing, the embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned Embodiment within the knowledge of a person skilled in the art can also be before not departing from present inventive concept Put that various changes can be made.

Claims (2)

1. a kind of method for improving industrially pure titanium intensity and plasticity simultaneously, it is characterised in that specific steps include:
Titanium board material is surface-treated by step 1 through milling machine processing first, after removing surface defect and impurity, is protected in 700 DEG C Temperature 2 hours;
Step 2, by the Titanium board material handled through step 1 under vacuum or inert gas shielding, rotation speed be 860 ~ 890r/ Min, frequency are 50 ~ 60Hz, 1 ~ 3h of ball-milling treatment;
Step 3 will roll after cooling 5 ~ 10min in the Titanium board material immersion liquid nitrogen after step 2 ball-milling treatment;Roll front and rear panel The dependent variable of material reaches 92% ~ 98%, and cooling 5 ~ 10min, plate final thickness in liquid nitrogen will be immersed before rolling per pass For 1mm;
Step 4, by the plate handled through step 3 at 450 ~ 520 DEG C 5 ~ 10min of vacuum annealing, be prepared while improving The industrially pure titanium plate of intensity and plasticity;
The steel ball that 5 ~ 10 4 ~ 8mm of Φ are put into step 2 ball-milling treatment carries out ball milling.
2. method that is according to claim 1 while improving industrially pure titanium intensity and plasticity, it is characterised in that: the step Titanium board material is in 1 with a thickness of 2mm.
CN201710696551.XA 2017-08-15 2017-08-15 Method that is a kind of while improving industrially pure titanium intensity and plasticity Active CN107699830B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111041395B (en) * 2018-10-12 2021-07-06 南京理工大学 Ultra-high density twin crystal titanium and preparation method thereof
CN110295334B (en) * 2019-07-16 2020-11-24 常州大学 Preparation method of high-strength high-plasticity industrial pure titanium with multi-level structure
CN110976855A (en) * 2019-11-01 2020-04-10 昆明理工大学 Method for simultaneously improving strength and plasticity of titanium material
CN111004987B (en) * 2019-12-27 2021-04-27 湖南大学 Method for regulating and controlling mechanical property of metastable beta titanium alloy
CN113414548A (en) * 2021-06-11 2021-09-21 兰州理工大学 Preparation method of large-size high-strength high-conductivity CuCr alloy with ultrafine crystal structure

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101580924A (en) * 2009-06-25 2009-11-18 上海交通大学 Pure titanium two-step plastic deformation processing method
CN105483588A (en) * 2015-12-09 2016-04-13 东北大学 Preparation method for high-strength pure titanium panels
CN106367634A (en) * 2010-01-22 2017-02-01 冶联科技地产有限责任公司 Method for increasing strength and toughness of titanium alloy

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101580924A (en) * 2009-06-25 2009-11-18 上海交通大学 Pure titanium two-step plastic deformation processing method
CN106367634A (en) * 2010-01-22 2017-02-01 冶联科技地产有限责任公司 Method for increasing strength and toughness of titanium alloy
CN105483588A (en) * 2015-12-09 2016-04-13 东北大学 Preparation method for high-strength pure titanium panels

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