CN104762578A - Preparation method for TLM titanium alloy foil with nanocrystalline structure - Google Patents
Preparation method for TLM titanium alloy foil with nanocrystalline structure Download PDFInfo
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Abstract
The invention provides a preparation method for TLM titanium alloy foil with a nanocrystalline structure. The method includes the following steps of firstly, conducting homogenizing annealing on a TLM titanium alloy plate; secondly, conducting surface processing; thirdly, conducting cold rolling to obtain a foil blank; fourthly, conducting stress relieving; fifthly, sequentially conducting shearing, acid pickling, washing and drying, and then conducting sheath ply rolling till the accumulated deformation amount of rolling reaches 80% to 90%; sixthly, repeatedly executing the fifth step till the average grain size of the foil blank is smaller than 100 nm, and obtaining the TLM titanium alloy foil with the nanocrystalline structure. Production is conducted through an existing conventional device, namely, a two-roller rolling mill or a four-roller rolling mill, the method is particularly suitable for industrially preparing the nanocrystalline foil, production procedures are simple, the limitation on the panel size and materials is small, and grains and the weight of the foil can be easily controlled. Accumulative ply rolling is conducted on the foil of multiple layers, and the nanocrystalline foil with the unique performance can be obtained.
Description
Technical field
The invention belongs to titanium or titanium alloy materials processing technology field, be specifically related to a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure.
Background technology
The titanium or titanium alloy foil with nanometer crystal microstructure is structure or the functional materials that a class has specific physical performance and mechanical property, is highly suitable for national defence, military project and the high-tech area such as civilian.Especially in field development such as high-strength low modulus foil, precise foil, plasticity micro shaping foil, superlastic instrument foil, bio-medical material, damping materials rapidly.Be mainly used at present making the decorations net on jet engine incendiary pencil, the composite thermal protection tile in space shuttle thermal desorption system and titanium compound wall, sound mould material etc.
When the grain-size of titanium or titanium alloy foil is reduced to nanocrystalline (being less than 100nm), under room temperature will there is a series of huge and useful change in the performance of material.Particularly at room temperature nanocrystalline metal can obtain high strength and good ductility, this has great practical value to the retrofit of titanium or titanium alloy and plasticity micro shaping, and significant change will occur the over-all properties with nanocrystalline titanium or titanium alloy material.
In biomedical materials field, nanometer titanium alloy has possessed the special mechanical property less than common titanium material, and simultaneously nanostructure provides favourable condition to the sticking of cells in vivo, Differentiation and proliferation.In addition, Nano-mter Ti-alloy surface has more particle edges, material surface is made to obtain a large amount of unbound electron, nano material is made to possess higher activation energy, facilitate material surface calcium phosphorus precipitation, more can promote Integrated implant in body compared to smooth surface, these results are disclosed Nanosurface titanium alloy structure and have good medical science suitability as a kind of new type bone embedded material, can effectively improve implanting prosthetic interface and osseous tissue in conjunction with effect.And nanocrystalline technology of preparing is the important channel that material obtains the inaccessiable special performance of coarse grain material.Just because of this, Chinese scholars have employed various method and prepares nanocrystalline material.
At present, mostly adopt severe plastic deformation method directly to carry out the refinement of material both at home and abroad, make its grain fineness number reach nano level.Severe plastic deformation method main at present has equal channel angular pressing (ECAP), high-pressure rotary (HPT), high pressure and torsion, repeatedly wrinkle-straightening method, accumulative roll bonding, repeatedly forging method and cycle extrusion method etc.But these methods are due to the restriction of mould, or the restriction of equipment (severe plastic deformation may damage the surface of milling train), all cannot realize the continuous prodution of nanocrystalline foil, or because production cost is high and the throughput of conventional commercial equipment does not reach the requirement of severe plastic deformation.
The seventies, the production method of metal foil had electro deposition method, vacuum vapour deposition, powqder rolling process, turning method and rolling etc., but a large amount of production high-quality foil is mainly by rolling, wherein the most frequently used aluminum foil thickness is 0.005 ~ 0.008mm, is generally to carry out ply rolling from below 0.15mm.Be at present 0.001mm with the aluminium foil minimum thickness that rolling is produced in the world, generally all adopt six rollers, 12 rollers, 20 rollers or 30 six-high mills to produce.Adopt two rollers or four-high mill can only the softer metal of rolling, as Al and Alalloy paper tinsel, lead foil, tinfoil paper etc., but cannot roll out the titanium alloy foil of high precision, best bright finish.Common titanium material coarse-grain foil prepared by current employing rolling is as thin as 0.008mm most, and is only applicable to the rolling of pure titanium, for the preparation of the ultra-thin foil of nanocrystalline TLM titanium alloy, adopts duo mill or four-high mill also cannot realize at present.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure.The method utilizes existing conventional equipment duo mill or four-high mill to produce, and is specially adapted to the nanocrystalline foil of preparation of industrialization, and production process is simple, less to the limitation of board dimension and material, is easy to the crystal grain and the quality that control foil.Accumulation ply rolling is repeatedly carried out to multilayer foil, the nanocrystalline foil with special performance can be obtained.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure, and it is characterized in that, the method comprises the following steps:
Step one, homogenizing annealing process is carried out to TLM titanium alloy sheet;
Step 2, surface treatment is carried out to the TLM titanium alloy sheet after homogenizing annealing process in step one, detailed process is: first carry out ultrasonic cleaning to TLM titanium alloy sheet, adopt again sandblasting method removing plate surface zone of oxidation and by plate surface hacking, then cleanup acid treatment is carried out, afterwards by the clean post-drying of running water;
Step 3, employing duo mill or four-high mill carry out cold rolling to the TLM titanium alloy sheet after surface treatment in step 2, obtain the paper tinsel base that thickness is 0.1mm; Described cold rolling accumulative deflection is 85% ~ 95%;
Step 4, the base of paper tinsel described in step 3 being placed in vacuum annealing furnace, is be incubated 15min ~ 20min under the condition of 623K ~ 673K to carry out stress relief annealing process in temperature;
Step 5, the paper tinsel base after stress relief annealing process in step 4 carried out successively shear, pickling, washing and drying treatment, then the paper tinsel base after multilayer drying treatment is stacked neatly and put into jacket, adopting duo mill or four-high mill to carry out jacket ply rolling, is till 80% ~ 90% until the accumulative deflection of rolling; Carry out process annealing process to paper tinsel base in jacket ply rolling process, detailed process is: when the accumulative deflection of rolling is 30% ~ 50%, paper tinsel base is placed in vacuum annealing furnace, is to be incubated 15min ~ 20min under the condition of 623K ~ 673K in temperature;
Step 6, repeating step five, until make the grain-size of paper tinsel base be less than 100nm, obtain the TLM titanium alloy foil with nanometer crystal microstructure.
Above-mentioned a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure, it is characterized in that, the detailed process of the process of homogenizing annealing described in step one is: TLM titanium alloy sheet is placed in vacuum annealing furnace, is to be incubated 20min ~ 40min under the condition of 923K ~ 1023K in temperature.
Above-mentioned a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure, is characterized in that, the average grain size of the titanium alloy sheet of TLM described in step one is 20 μm ~ 100 μm.
Above-mentioned a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure, is characterized in that, the fineness of sand of sandblasting described in step 2 is 80 orders or 100 orders, and the pressure of described sandblasting is 0.4MPa ~ 0.8MPa.
Above-mentioned a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure, it is characterized in that, pass deformation cold rolling described in step 3 is not more than 30%.
Above-mentioned a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure, it is characterized in that, the pickle solution that described in step 2 and step 5, pickling adopts is hydrofluoric acid-nitric acid complex pickling solution, and hydrofluoric acid, mass percent concentration that described hydrofluoric acid-nitric acid complex pickling solution is more than 40% by mass percent concentration are nitric acid and the deionized water in mass ratio 1 of more than 60%: (4 ~ 5): (3 ~ 4) mix and form.
Above-mentioned a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure, it is characterized in that, the rolling speed of the ply rolling of jacket described in step 5 is 10m/s ~ 20m/s, and the pass deformation of rolling is not more than 30%, the material of jacket is 304 stainless steels.
Above-mentioned a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure, is characterized in that, when in step 5, described in multilayer, paper tinsel base stacks, and equal applying solid lubricant MoS between adjacent two layers paper tinsel base
2carry out lubricating and isolating.
Above-mentioned a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure, it is characterized in that, when paper tinsel base stacks described in multilayer in step 5, all adopt sandwich material to isolate between adjacent two layers paper tinsel base, described sandwich material is the Copper Foil material that thickness is not more than 5 μm.
The present invention compared with prior art has the following advantages:
1, the present invention is adopted to utilize existing conventional equipment duo mill or four-high mill to produce, enhance productivity, utilize each less deflection, by repetitious distortion, realize the gross distortion of foil, also can realizing the nanocrystalline preparation of difficult-to-deformation material, being also applicable to the preparation of the light metal such as nanocrystalline Al, Mg and alloy foil thereof by changing individual process parameters.
2, the present invention is specially adapted to the nanocrystalline foil of preparation of industrialization, and production process is simple, less to the limitation of board dimension and material, is easy to the crystal grain and the quality that control foil.Accumulation ply rolling is repeatedly carried out to multilayer foil, the nanocrystalline foil with special performance can be obtained.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the metallographic microstructure photo of embodiment of the present invention 1TLM titanium alloy sheet.
Fig. 2 is the SEM macrograph that embodiment of the present invention 1TLM titanium alloy sheet is cold-rolled to that accumulative deflection is 50%.
Fig. 3 is the SEM macrograph that embodiment of the present invention 1TLM titanium alloy sheet is cold-rolled to that accumulative deflection is 90%.
Fig. 4 is the TEM microtexture photo with the TLM titanium alloy foil of nanometer crystal microstructure prepared by the embodiment of the present invention 1.
Fig. 5 is the metallographic microstructure photo of embodiment of the present invention 3TLM titanium alloy sheet.
Fig. 6 is the TEM microtexture photo with the TLM titanium alloy foil of nanometer crystal microstructure prepared by the embodiment of the present invention 3.
Embodiment
Embodiment 1
The preparation method that the present embodiment has the TLM titanium alloy foil of nanometer crystal microstructure comprises the following steps:
Step one, carry out homogenizing annealing process to TLM titanium alloy sheet, the detailed process of described homogenizing annealing process is: TLM titanium alloy sheet is placed in vacuum annealing furnace, is to be incubated 30min under the condition of 1023K in temperature; The thickness of described TLM titanium alloy sheet is 1mm, and average grain size is 20 μm (its metallographic microstructure photo as shown in Figure 1);
Step 2, surface treatment is carried out to the TLM titanium alloy sheet after homogenizing annealing process in step one, detailed process is: first carry out ultrasonic cleaning to TLM titanium alloy sheet, adopt again sandblasting method removing plate surface zone of oxidation and by plate surface hacking, then cleanup acid treatment is carried out, afterwards by the clean post-drying of running water; The fineness of sand of described sandblasting is 80 orders, and the pressure of described sandblasting is 0.4MPa; The pickle solution that pickling adopts is hydrofluoric acid-nitric acid complex pickling solution, hydrofluoric acid, mass percent concentration that described hydrofluoric acid-nitric acid complex pickling solution is 45% by mass percent concentration be 65% nitric acid and deionized water mix form at 1: 4: 3 in mass ratio;
Step 3, employing four-high mill carry out cold rolling to the TLM titanium alloy sheet after surface treatment in step 2, and pass deformation is respectively: 30%, and 18%, 13%, 13%, 12%, 12%, 12%, 10%, 10%, 10%, 10%, 10%, 10%, 10%, 10%, 10%, 10%, accumulative deflection is 90%, obtains the paper tinsel base that thickness is 0.1mm;
When cold rolling accumulative deflection is 50% (the 3rd passes complete after), adopt SEM electron microscopic observation crystal grain and tissue (its SEM macrograph as shown in Figure 2), as shown in Figure 2, crystal grain is completely broken;
After cold rolling completing, when accumulative deflection is 90%, adopt SEM electron microscopic observation crystal grain and tissue (its SEM macrograph as shown in Figure 3), as shown in Figure 3, there is fragmentation in great number of grains substantially;
Step 4, the base of paper tinsel described in step 3 being placed in vacuum annealing furnace, is be incubated 20min under the condition of 673K to carry out stress relief annealing process in temperature;
Step 5, the paper tinsel base after stress relief annealing process in step 4 carried out successively shear, pickling, washing and drying treatment, then the paper tinsel base after 10 layers of drying treatment is stacked neat after put into jacket, adopt four-high mill to carry out jacket ply rolling, the rolling speed of jacket ply rolling is 20m/s, and the material of jacket is 304 stainless steels, and pass deformation is respectively: 30%, 25%, 20%, 18%, 15%, 12%, 12%, 10%, accumulative deflection is 80%, obtains the paper tinsel base that thickness is 0.02mm; Carry out process annealing process to paper tinsel base in jacket ply rolling process, detailed process is: when the accumulative deflection of rolling is 47.5%, paper tinsel base is placed in vacuum annealing furnace, is to be incubated 20min under the condition of 673K in temperature; The pickle solution that pickling adopts is hydrofluoric acid-nitric acid complex pickling solution, hydrofluoric acid, mass percent concentration that described hydrofluoric acid-nitric acid complex pickling solution is 45% by mass percent concentration be 65% nitric acid and deionized water mix form at 1: 5: 4 in mass ratio; When multilayer paper tinsel base is stacked, equal applying solid lubricant MoS between adjacent two layers paper tinsel base
2carry out lubricating and isolating;
Detect the grain-size of this paper tinsel base, the average grain size recording paper tinsel base is 900nm, does not meet nanocrystalline requirement;
Step 6, by thickness be 0.02mm paper tinsel base repeating step five in shearing, pickling, washing, drying and jacket ply rolling operation (specific operation process of each operation is identical with step 5), obtain the paper tinsel base that thickness is 0.004mm; Detect the grain-size of this paper tinsel base, the average grain size recording paper tinsel base is 50nm (its TEM microtexture photo as shown in Figure 4), obtains the TLM titanium alloy foil with nanometer crystal microstructure.
The present embodiment utilizes existing conventional equipment four-high mill to produce, and is specially adapted to the nanocrystalline foil of preparation of industrialization, and production process is simple, less to the limitation of board dimension and material, is easy to the crystal grain and the quality that control foil.Accumulation ply rolling is repeatedly carried out to multilayer foil, the nanocrystalline foil with special performance can be obtained.
Embodiment 2
The preparation method that the present embodiment has the TLM titanium alloy foil of nanometer crystal microstructure comprises the following steps:
Step one, carry out homogenizing annealing process to TLM titanium alloy sheet, the detailed process of described homogenizing annealing process is: TLM titanium alloy sheet is placed in vacuum annealing furnace, is to be incubated 30min under the condition of 1023K in temperature; The thickness of described TLM titanium alloy sheet is 2mm, and average grain size is 100 μm;
Step 2, surface treatment is carried out to the TLM titanium alloy sheet after homogenizing annealing process in step one, detailed process is: first carry out ultrasonic cleaning to TLM titanium alloy sheet, adopt again sandblasting method removing plate surface zone of oxidation and by plate surface hacking, then cleanup acid treatment is carried out, afterwards by the clean post-drying of running water; The fineness of sand of described sandblasting is 80 orders, and the pressure of described sandblasting is 0.8MPa; The pickle solution that pickling adopts is hydrofluoric acid-nitric acid complex pickling solution, hydrofluoric acid, mass percent concentration that described hydrofluoric acid-nitric acid complex pickling solution is 47% by mass percent concentration be 63% nitric acid and deionized water mix form at 1: 4: 3 in mass ratio;
Step 3, employing duo mill carry out cold rolling to the TLM titanium alloy sheet after surface treatment in step 2, and pass deformation is respectively: 30%, and 30%, 30%, 28%, 25%, 25%, 20%, 20%, 18%, 15%, 15%, accumulative deflection is 95%, obtains the paper tinsel base that thickness is 0.1mm;
Step 4, the base of paper tinsel described in step 3 being placed in vacuum annealing furnace, is be incubated 20min under the condition of 673K to carry out stress relief annealing process in temperature;
Step 5, the paper tinsel base after stress relief annealing process in step 4 carried out successively shear, pickling, washing and drying treatment, then the paper tinsel base after 15 layers of drying treatment is stacked neat after put into jacket, adopt duo mill to carry out jacket ply rolling, the rolling speed of jacket ply rolling is 20m/s, and the material of jacket is 304 stainless steels, and pass deformation is respectively: 30%, 30%, 25%, 25%, 20%, 20%, 18%, 18%, 15%, accumulative deflection is 90%, obtains the paper tinsel base that thickness is 0.01mm; Carry out process annealing process to paper tinsel base in jacket ply rolling process, detailed process is: when the accumulative deflection of rolling is 30%, paper tinsel base is placed in vacuum annealing furnace, is to be incubated 20min under the condition of 673K in temperature; The pickle solution that pickling adopts is hydrofluoric acid-nitric acid complex pickling solution, hydrofluoric acid, mass percent concentration that described hydrofluoric acid-nitric acid complex pickling solution is 47% by mass percent concentration be 63% nitric acid and deionized water mix form at 1: 5: 4 in mass ratio; When stacking multilayer paper tinsel base, between adjacent two layers paper tinsel base, all adopt sandwich material to isolate, described sandwich material is Copper Foil material, and the thickness of described sandwich material is not more than 5 μm;
Detect the grain-size of paper tinsel base, the average grain size recording paper tinsel base is 5 μm, does not meet nanocrystalline requirement;
Step 6, by thickness be 0.01mm paper tinsel base repeating step five in shearing, pickling, washing, drying and jacket ply rolling operation (specific operation process of each operation is identical with step 5), obtain the paper tinsel base that thickness is 0.001mm; Detect the grain-size of this paper tinsel base, the average grain size recording paper tinsel base is 70nm, obtains the TLM titanium alloy foil with nanometer crystal microstructure.
The present embodiment utilizes existing conventional equipment duo mill to produce, and is specially adapted to the nanocrystalline foil of preparation of industrialization, and production process is simple, less to the limitation of board dimension and material, is easy to the crystal grain and the quality that control foil.Accumulation ply rolling is repeatedly carried out to multilayer foil, the nanocrystalline foil with special performance can be obtained.
Embodiment 3
The preparation method that the present embodiment has the TLM titanium alloy foil of nanometer crystal microstructure comprises the following steps:
Step one, carry out homogenizing annealing process to TLM titanium alloy sheet, the detailed process of described homogenizing annealing process is: TLM titanium alloy sheet is placed in vacuum annealing furnace, is to be incubated 20min under the condition of 923K in temperature; The thickness of described TLM titanium alloy sheet is 0.7mm, and average grain size is 100 μm (its metallographic microstructure as shown in Figure 5);
Step 2, surface treatment is carried out to the TLM titanium alloy sheet after homogenizing annealing process in step one, detailed process is: first carry out ultrasonic cleaning to TLM titanium alloy sheet, adopt again sandblasting method removing plate surface zone of oxidation and by plate surface hacking, then cleanup acid treatment is carried out, afterwards by the clean post-drying of running water; The fineness of sand of described sandblasting is 100 orders, and the pressure of described sandblasting is 0.6MPa; The pickle solution that pickling adopts is hydrofluoric acid-nitric acid complex pickling solution, hydrofluoric acid, mass percent concentration that described hydrofluoric acid-nitric acid complex pickling solution is 40% by mass percent concentration be 60% nitric acid and deionized water mix form at 1: 5: 3 in mass ratio;
Step 3, employing four-high mill carry out cold rolling to the TLM titanium alloy sheet after surface treatment in step 2, and pass deformation is respectively: 25%, and 22%, 20%, 18%, 18%, 16%, 15%, 15%, 12%, 10%, accumulative deflection is 85%, obtains the paper tinsel base that thickness is 0.1mm;
Step 4, the base of paper tinsel described in step 3 being placed in vacuum annealing furnace, is be incubated 15min under the condition of 623K to carry out stress relief annealing process in temperature;
Step 5, the paper tinsel base after stress relief annealing process in step 4 carried out successively shear, pickling, washing and drying treatment, then the paper tinsel base after 16 layers of drying treatment is stacked neat after put into jacket, adopt four-high mill to carry out jacket ply rolling, the rolling speed of jacket ply rolling is 10m/s, and the material of jacket is 304 stainless steels, and the pass deformation of rolling is respectively: 30%, 28%, 25%, 25%, 20%, 20%, 16%, accumulative deflection is 85%, obtains the paper tinsel base that thickness is 0.015mm; Carry out process annealing process to paper tinsel base in jacket ply rolling process, detailed process is: when the accumulative deflection of rolling is 50%, paper tinsel base is placed in vacuum annealing furnace, is to be incubated 20min under the condition of 623K in temperature; The pickle solution that pickling adopts is hydrofluoric acid-nitric acid complex pickling solution, hydrofluoric acid, mass percent concentration that described hydrofluoric acid-nitric acid complex pickling solution is 40% by mass percent concentration be 60% nitric acid and deionized water mix form at 1: 5: 4 in mass ratio; When stacking multilayer paper tinsel base, between adjacent two layers paper tinsel base, all adopt sandwich material to isolate, described sandwich material is Copper Foil material, and the thickness of described sandwich material is not more than 5 μm;
After jacket ply rolling completes, detect the grain-size of paper tinsel base, the average grain size recording paper tinsel base is 3 μm, does not meet nanocrystalline requirement;
Step 6, by thickness be 0.015mm paper tinsel base repeating step five in shearing, pickling, washing, drying and jacket ply rolling operation (specific operation process of each operation is identical with step 5), obtain the paper tinsel base that thickness is 0.002mm; Detect the grain-size of this paper tinsel base, the average grain size recording paper tinsel base is 90nm, obtains the TLM titanium alloy foil with nanometer crystal microstructure.
The present embodiment utilizes existing conventional equipment four-high mill to produce, and is specially adapted to the nanocrystalline foil of preparation of industrialization, and production process is simple, less to the limitation of board dimension and material, is easy to the crystal grain and the quality that control foil.Accumulation ply rolling is repeatedly carried out to multilayer foil, the nanocrystalline foil with special performance can be obtained.
Embodiment 4
The preparation method that the present embodiment has the TLM titanium alloy foil of nanometer crystal microstructure comprises the following steps:
Step one, carry out homogenizing annealing process to TLM titanium alloy sheet, the detailed process of described homogenizing annealing process is: TLM titanium alloy sheet is placed in vacuum annealing furnace, is to be incubated 20min under the condition of 953K in temperature; The thickness of described TLM titanium alloy sheet is 0.8mm, and average grain size is 60 μm;
Step 2, surface treatment is carried out to the TLM titanium alloy sheet after homogenizing annealing process in step one, detailed process is: first carry out ultrasonic cleaning to TLM titanium alloy sheet, adopt again sandblasting method removing plate surface zone of oxidation and by plate surface hacking, then cleanup acid treatment is carried out, afterwards by the clean post-drying of running water; The fineness of sand of described sandblasting is 100 orders, and the pressure of described sandblasting is 0.8MPa; The pickle solution that pickling adopts is hydrofluoric acid-nitric acid complex pickling solution, hydrofluoric acid, mass percent concentration that described hydrofluoric acid-nitric acid complex pickling solution is 42% by mass percent concentration be 66% nitric acid and deionized water mix form at 1: 5: 3 in mass ratio;
Step 3, employing duo mill carry out cold rolling to the TLM titanium alloy sheet after surface treatment in step 2, and pass deformation is respectively: 25%, and 25%, 20%, 18%, 18%, 16%, 15%, 15%, 12%, 12%, 10%, accumulative deflection is 87.5%, obtains the paper tinsel base that thickness is 0.1mm;
Step 4, the base of paper tinsel described in step 3 being placed in vacuum annealing furnace, is be incubated 15min under the condition of 623K to carry out stress relief annealing process in temperature;
Step 5, the paper tinsel base after stress relief annealing process in step 4 carried out successively shear, pickling, washing and drying treatment, then the paper tinsel base after 16 layers of drying treatment is stacked neat after put into jacket, adopt duo mill to carry out jacket ply rolling, the rolling speed of jacket ply rolling is 10m/s, and the material of jacket is 304 stainless steels, and the pass deformation of rolling is respectively: 30%, 28%, 25%, 25%, 20%, 20%, 16%, accumulative deflection is 85%, obtains the paper tinsel base that thickness is 0.015mm; Carry out process annealing process to paper tinsel base in jacket ply rolling process, detailed process is: when the accumulative deflection of rolling is 50%, paper tinsel base is placed in vacuum annealing furnace, is to be incubated 20min under the condition of 623K in temperature; The pickle solution that pickling adopts is hydrofluoric acid-nitric acid complex pickling solution, hydrofluoric acid, mass percent concentration that described hydrofluoric acid-nitric acid complex pickling solution is 42% by mass percent concentration be 66% nitric acid and deionized water mix form at 1: 5: 4 in mass ratio; When multilayer paper tinsel base is stacked, equal applying solid lubricant MoS between adjacent two layers paper tinsel base
2carry out lubricating and isolating;
After jacket ply rolling completes, detect the grain-size of paper tinsel base, the average grain size recording paper tinsel base is 5 μm, does not meet nanocrystalline requirement;
Step 6, by thickness be 0.015mm paper tinsel base repeating step five in shearing, pickling, washing, drying and jacket ply rolling operation (specific operation process of each operation is identical with step 5), obtain the paper tinsel base that thickness is 0.002mm; Detect the grain-size of this paper tinsel base, the average grain size recording paper tinsel base is 70nm, obtains the TLM titanium alloy foil with nanometer crystal microstructure.
The present embodiment utilizes existing conventional equipment duo mill to produce, and is specially adapted to the nanocrystalline foil of preparation of industrialization, and production process is simple, less to the limitation of board dimension and material, is easy to the crystal grain and the quality that control foil.Accumulation ply rolling is repeatedly carried out to multilayer foil, the nanocrystalline foil with special performance can be obtained.
The above is only preferred embodiment of the present invention, not imposes any restrictions the present invention.Every above embodiment is done according to invention technical spirit any simple modification, change and equivalence change, all still belong in the protection domain of technical solution of the present invention.
Claims (9)
1. have a preparation method for the TLM titanium alloy foil of nanometer crystal microstructure, it is characterized in that, the method comprises the following steps:
Step one, homogenizing annealing process is carried out to TLM titanium alloy sheet;
Step 2, surface treatment is carried out to the TLM titanium alloy sheet after homogenizing annealing process in step one, detailed process is: first carry out ultrasonic cleaning to TLM titanium alloy sheet, adopt again sandblasting method removing plate surface zone of oxidation and by plate surface hacking, then cleanup acid treatment is carried out, afterwards by the clean post-drying of running water;
Step 3, employing duo mill or four-high mill carry out cold rolling to the TLM titanium alloy sheet after surface treatment in step 2, obtain the paper tinsel base that thickness is 0.1mm; Described cold rolling accumulative deflection is 85% ~ 95%;
Step 4, the base of paper tinsel described in step 3 being placed in vacuum annealing furnace, is be incubated 15min ~ 20min under the condition of 623K ~ 673K to carry out stress relief annealing process in temperature;
Step 5, the paper tinsel base after stress relief annealing process in step 4 carried out successively shear, pickling, washing and drying treatment, then the paper tinsel base after multilayer drying treatment is stacked neatly and put into jacket, adopting duo mill or four-high mill to carry out jacket ply rolling, is till 80% ~ 90% until the accumulative deflection of rolling; Carry out process annealing process to paper tinsel base in jacket ply rolling process, detailed process is: when the accumulative deflection of rolling is 30% ~ 50%, paper tinsel base is placed in vacuum annealing furnace, is to be incubated 15min ~ 20min under the condition of 623K ~ 673K in temperature;
Step 6, repeating step five, until make the grain-size of paper tinsel base be less than 100nm, obtain the TLM titanium alloy foil with nanometer crystal microstructure.
2. a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure according to claim 1, it is characterized in that, the detailed process of the process of homogenizing annealing described in step one is: TLM titanium alloy sheet is placed in vacuum annealing furnace, is to be incubated 20min ~ 40min under the condition of 923K ~ 1023K in temperature.
3. a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure according to claim 1, is characterized in that, the average grain size of the titanium alloy sheet of TLM described in step one is 20 μm ~ 100 μm.
4. a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure according to claim 1, is characterized in that, the fineness of sand of sandblasting described in step 2 is 80 orders or 100 orders, and the pressure of described sandblasting is 0.4MPa ~ 0.8MPa.
5. a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure according to claim 1, it is characterized in that, pass deformation cold rolling described in step 3 is not more than 30%.
6. a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure according to claim 1, it is characterized in that, the pickle solution that described in step 2 and step 5, pickling adopts is hydrofluoric acid-nitric acid complex pickling solution, and hydrofluoric acid, mass percent concentration that described hydrofluoric acid-nitric acid complex pickling solution is more than 40% by mass percent concentration are nitric acid and the deionized water in mass ratio 1 of more than 60%: (4 ~ 5): (3 ~ 4) mix and form.
7. a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure according to claim 1, it is characterized in that, the rolling speed of the ply rolling of jacket described in step 5 is 10m/s ~ 20m/s, and the pass deformation of rolling is not more than 30%, and the material of jacket is 304 stainless steels.
8. a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure according to claim 1, is characterized in that, when in step 5, described in multilayer, paper tinsel base stacks, and equal applying solid lubricant MoS between adjacent two layers paper tinsel base
2carry out lubricating and isolating.
9. a kind of preparation method with the TLM titanium alloy foil of nanometer crystal microstructure according to claim 1, it is characterized in that, when in step 5, described in multilayer, paper tinsel base stacks, all adopt sandwich material to isolate between adjacent two layers paper tinsel base, described sandwich material is the Copper Foil material that thickness is not more than 5 μm.
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| CN105414219A (en) * | 2015-12-31 | 2016-03-23 | 中国航空工业集团公司北京航空制造工程研究所 | Preparation method of metallic/intermetallic compound laminar composite material |
| CN113477706A (en) * | 2021-07-15 | 2021-10-08 | 太原理工大学 | Nano-lubrication-based micro-flexible rolling method for laminated metal composite thin strip |
| CN115404481A (en) * | 2022-08-10 | 2022-11-29 | 琅泰美康医疗器械有限公司 | Preparation method of hydrophilic surface of medical titanium-zirconium-based alloy microporous structure |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105414219A (en) * | 2015-12-31 | 2016-03-23 | 中国航空工业集团公司北京航空制造工程研究所 | Preparation method of metallic/intermetallic compound laminar composite material |
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| CN113477706A (en) * | 2021-07-15 | 2021-10-08 | 太原理工大学 | Nano-lubrication-based micro-flexible rolling method for laminated metal composite thin strip |
| CN115404481A (en) * | 2022-08-10 | 2022-11-29 | 琅泰美康医疗器械有限公司 | Preparation method of hydrophilic surface of medical titanium-zirconium-based alloy microporous structure |
| CN115404481B (en) * | 2022-08-10 | 2024-04-16 | 琅泰美康医疗器械有限公司 | Preparation method of medical titanium-zirconium-based alloy microporous structure hydrophilic surface |
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