CN1745922A - Constant diameter right-angle extruding production of micro/nanometer crustal industrial pure titanium block - Google Patents
Constant diameter right-angle extruding production of micro/nanometer crustal industrial pure titanium block Download PDFInfo
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- CN1745922A CN1745922A CN 200510029663 CN200510029663A CN1745922A CN 1745922 A CN1745922 A CN 1745922A CN 200510029663 CN200510029663 CN 200510029663 CN 200510029663 A CN200510029663 A CN 200510029663A CN 1745922 A CN1745922 A CN 1745922A
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Abstract
An isometric angle squeezing technology for preparing micron/nano-crystal industrial-purity Ti block includes such steps as providing an industrial-purity Ti block, annealing, holding its temp, cutting it to become blanks, polishing the surface of blank, coating glass lubricant, coating graphite lubricant on the inner surface of an isometric angle squeezing die with a squeezing channel angle of 90-120 deg, heating said blank and die, and isometric angle squeezing. Its product has high strength, plasticity, biocompatibility and anticorrosion nature, the elastic modulus similar to that of bone, and low cost.
Description
Technical field
The present invention relates to a kind of preparation method of metal material technical field, specifically is the isometrical bent angle extruding production of the brilliant industrially pure titanium bulk of a kind of micro-/ nano.
Background technology
In all bio-medical materials, metal material is used the earliest, is mainly used to repair bone, joint, tooth and blood vessel etc.Being used for bio-medical material at present mainly is stainless steel, titanium or titanium alloy.Titanium reserves in the earth's crust are very abundant, and it is present in compound form in the middle of the ore, and main ore has ilmenite FeTiO
3Titanium has certain intensity and higher plasticity, the σ b=300MPa of high purity titanium, δ=40%, and under hot conditions, also can keep higher intensity, have the advantage of steel (intensity height) and aluminium (quality is light) concurrently, fusing point is (1663 ± 10) ℃, has good corrosion resistance and hear resistance.Simultaneously, titanium is nonmagnetic metal, in very big magnetic field, can not be magnetized yet, titanium and alloy thereof also have to its similar elastic modelling quantity of bone exhaustion, excellent biological compatibility and under biotic environment good corrosion resistance, therefore obtained application more and more widely clinically.But compare with titanium alloy, pure titanium lacks sufficient intensity and hardness, has limited it and has carried the application at position in vivo.Though simultaneously titanium and alloy thereof have that (10～40GPa) the most approaching elastic modelling quantity, but still be higher than the elastic modelling quantity of bone, this just causes not matching of mechanical performance on the interface easily with bone.
Facts have proved: the crystal grain of axle such as tiny can improve the plastic deformation of metal ability, improves the intensity of material and comprehensive mechanical property.And when material grains was refined to nanocrystalline yardstick, not only its comprehensive mechanical performance improved, and its physicochemical characteristics also great change will take place.Crystal grain thinning technology commonly used is divided into four kinds: adds various grain refiners or makes dendrite fragmentation when liquid by external energy, thus refinement cast sturcture; The semi-solid-state shaping crystal grain thinning; Casting powder metallurgy is shaped; Intense plastic strain is such as high pressure distortion (being called for short HPT) method, isometrical bent angle extrusion (hereinafter to be referred as ECAE) etc.First three methods is casting, and grain refining effect is not obvious.High pressure distortion method can only be prepared extremely thin flaky material, and isometrical bent angle extruding rule can be prepared bigger block grained material.
Find through literature search prior art, S.L.Semiatin, D.P.Delo etc. had once delivered one piece of paper about " the ECAE process of less-deformable alloy " (Equal channelangular extrusion of difficult-to-work alloys in " material and design ", Materials and Design21 (2000) 311-322), this article is to pure Ti, the metal of difficulties such as Ti-6Al-4V and 4340 steel distortion has carried out the ECAE process, it is 90 ° mould that the author of the document adopts channel corner, select 25 ℃～325 ℃ temperature range and the strain rate of 0.002/S～2/S that pure titanium has been carried out the ECAE process, the result is because pure titanium is very responsive to the localization of the shearing in the ECAE process, in room temperature (25 ℃), select for use any one strain rate between 0.002/S～2/S all to make pure titanium after the ECAE process, become fragment; And the author of the document is when other temperature (125 ℃～325 ℃) trial is carried out the ECAE process to pure titanium, because the influence of factors such as extrusion temperature, strain rate, lubricating condition are inappropriate, fracture in various degree also can appear in the pure titanium after isometrical bent angle extruding, thereby can not obtain big block grained material.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, provide the brilliant industrially pure titanium bulk of a kind of micro-/ nano isometrical bent angle extruding production, make it can improve the pure titanium of metal intensity at room temperature and comprehensive mechanical property thereof, cut down finished cost, improve its lumber recovery.
The present invention is achieved by the following technical solutions, and the present invention selects for use industrially pure titanium (TA2) bulk as raw material, after the annealing insulation, subsequently the industrially pure titanium bulk cut into blank, and carry out surface smoothness and handle, and the coating glass lubricant.Mould employing squeezing passage angle is 90 °～120 ° an isometrical bent angle extrusion die, mold cavity surface applied graphitic lubricant.With blank and the common heat tracing of mould, and from heating furnace, take out simultaneously and carry out isometrical bent angle extruding, finally obtain the brilliant industrially pure titanium bulk of well behaved micro-/ nano such as intensity, plasticity.
Below the present invention is further illustrated, concrete steps are as follows:
(1) adopts industrially pure titanium (TA2) bulk as raw material, the industrially pure titanium bulk 700 ℃～750 ℃ annealing, is incubated 1～2 hour;
(2) the industrially pure titanium TA2 bulk that will anneal after being incubated cuts into blank (10 * 10 * 120mm
3), blank is carried out surface treatment, reach the surface accuracy more than 4 grades, blank surface processing roughness is not less than Ra=1.25 μ m;
(3) with acetone surface clean is carried out on the blank surface, preheating is 20～60 minutes under 60 ℃～100 ℃ temperature, and the method that adopts dip-coating then is at blank surface applied glass lubricant, and coating is wanted evenly, and coating layer thickness is 0.2～0.4mm.Coating back blank was dried 20～60 minutes under 60 ℃～100 ℃ temperature, if occur falling to being coated with, cut, defective such as peel off, should carry out coating or flush away recoat.
(4) adopt isometrical bent angle extrusion die, the squeezing passage angle of mould is 90 °～120 °.With acetone mould is carried out surface and die cavity and clean, preheating is 60～90 minutes under 100 ℃～150 ℃ temperature, coated graphite lubricant then, and coating layer thickness is wanted evenly mould to be dried 60～90 minutes under 100 ℃～150 ℃ temperature again.
(5) blank that will coat glass lubricant is put in the squeezing passage of the mould that coats graphitic lubricant, heating jointly in 400 ℃～500 ℃ heating furnace then, temperature retention time 40～60 minutes.
(6) blank and the mould that heats taken out simultaneously, on the 300KN universal hydraulic testing machine, blank is pushed rapidly then.Repeat the blank that squeezes out is carried out surface treatment and coating glass lubricant, mold cavity coated graphite lubricant, pushes 2～8 times, can obtain the brilliant industrially pure titanium bulk of micro-/ nano, its microcosmic average grain size is 0.2～0.6 μ m.
The present invention adopts isometrical bent angle extrusion process, is characterized in making sample size constancy before and after distortion, handle simply, and the lumber recovery height, and can realize big workpiece processing.Before the extruding mold cavity and blank to be extruded are carried out different lubricated respectively, the rapid temperature drop that both can effectively stop the high temperature blank, can reduce simultaneously the sliding-frictional resistance between blank and mold work surface significantly, thereby improve the flow uniformity of pure titanium metal material effectively, guarantee carrying out smoothly of extrusion process; The lubricated process is simple, and cost is low, and through after the practical operation, blank and mould come off voluntarily, do not bond together good manufacturability mutually.Determining of blank end radian and blank surface fineness helps blank and reduces friction in extrusion process, improves the mobile uniformity of plasticity of blank.The determining and the blank that heats and mould taken out from heating furnace simultaneously of blank, mold heated time and temperature retention time carries out isometrical bent angle extruding, can prevent grain growth, help forming tiny pure titanium micro-/ nano crystalline substance, finally obtain well behaved industrially pure titanium bulks such as intensity, plasticity.The present invention can improve the pure titanium of metal intensity at room temperature and comprehensive mechanical property thereof, cuts down finished cost, and improves lumber recovery.
The specific embodiment
Below by specific embodiment technical scheme of the present invention is further described.
Embodiment 1:
Adopt industrially pure titanium (TA2) as raw material, with the industrially pure titanium bulk 700 ℃ of annealing, be incubated 2 hours, adopting electro-spark cutting machine that the metal block material of pure titanium is cut into sectional dimension is 10mm * 10mm, length is the blank of 120mm, and blank is carried out surface treatment, reach the surface accuracy more than 4 grades, blank surface processing roughness should be not less than Ra=1.25 μ m.With acetone surface clean is carried out on the blank surface, blank is placed on the clean stainless steel pallet, preheating is 60 minutes under 60 ℃ temperature, the method that adopts dip-coating then is at blank surface applied glass lubricant, coating is wanted evenly, and coating layer thickness is about 0.2mm, and coating back blank was dried 60 minutes under 60 ℃ temperature, if occur falling to being coated with, cut, defective such as peel off, should carry out coating or flush away recoat.Is that 90 ° of moulds carry out surface and die cavity and clean with acetone to the extruding angle, and preheating is 90 minutes under 100 ℃ temperature, coated graphite lubricant then, and it is even that coating is wanted, and the mould that coats graphitic lubricant is placed in 100 ℃ the heating furnace to carry out drying in 90 minutes.
The blank that coats glass lubricant is put into inside the squeezing passage of the mould that coats graphitic lubricant heating jointly in 500 ℃ heating furnace, temperature retention time 40 minutes.Then blank and the mould that heats taken out simultaneously, on the hydraulic universal experimental machine, pushes rapidly, the blank that extruding is come out carries out surface treatment again carry out the extruding of the 2nd passage after, can obtain the brilliant industrially pure titanium bulk of micron.When the grain refinement of industrially pure titanium TA2 bulk during to micron order, σ
0.2600MPa by initial annealed state brings up to 750MPa, σ
bBring up to 810MPa by 670MPa.
Embodiment 2:
Adopt industrially pure titanium (TA2) as raw material, with the industrially pure titanium bulk 750 ℃ of annealing, be incubated 1 hour, adopting electro-spark cutting machine that the metal block material of pure titanium is cut into sectional dimension is 10mm * 10mm, length is the blank of 120mm, and blank is carried out surface treatment, reach the surface accuracy more than 4 grades, blank surface processing roughness should be not less than Ra=1.25 μ m.With acetone surface clean is carried out on the blank surface, blank is placed on the clean stainless steel pallet, preheating is 40 minutes under 80 ℃ temperature, the method that adopts dip-coating then is at blank surface applied glass lubricant, coating is wanted evenly, and coating layer thickness is about 0.3mm, and coating back blank was dried 40 minutes under 80 ℃ temperature, if occur falling to being coated with, cut, defective such as peel off, should carry out coating or flush away recoat.Is that 120 ° of moulds carry out surface and die cavity and clean with acetone to the extruding angle, and preheating is 80 minutes under 120 ℃ temperature, coated graphite lubricant then, and it is even that coating is wanted, and the mould that coats graphitic lubricant is placed in 120 ℃ the heating furnace to carry out drying in 80 minutes.
The blank that coats glass lubricant is put in the squeezing passage of the mould that coats graphitic lubricant heating jointly in 450 ℃ heating furnace, temperature retention time 50 minutes.Then blank and the mould that heats taken out simultaneously, on the hydraulic universal experimental machine, pushes rapidly, the blank that extruding is come out carries out surface treatment again carry out the extruding of 4 passages after, can obtain sub-micron crystal industrially pure titanium bulk.When the grain refinement of industrially pure titanium TA2 bulk during to submicron order, σ
0.2600MPa by initial annealed state brings up to 820MPa, σ
bBring up to 890MPa by 670MPa.
Embodiment 3:
Adopt industrially pure titanium (TA2) bulk as raw material, the industrially pure titanium bulk 750 ℃ of annealing, is incubated 1.5 hours.Adopting electro-spark cutting machine that pure titanium bulk is cut into sectional dimension is 10mm * 10mm, and length is the blank of 120mm, and blank is carried out surface treatment, reaches the surface accuracy more than 4 grades, and blank surface processing roughness should be not less than Ra=1.25 μ m.With acetone surface clean is carried out on the blank surface, blank is placed on the clean stainless steel pallet, preheating is 20 minutes under 100 ℃ temperature, the method that adopts dip-coating then is at blank surface applied glass lubricant, coating is wanted evenly, and coating layer thickness is about 0.4mm, and coating back blank was dried 20 minutes under 100 ℃ temperature, if occur falling to being coated with, cut, defective such as peel off, should carry out coating or flush away recoat.Is that 90 ° of moulds carry out surface and die cavity and clean with acetone to the extruding angle, and preheating is 60 minutes under 150 ℃ temperature, coated graphite lubricant then, and coating is even, the mould that coats graphitic lubricant is placed in 150 ℃ the heating furnace to dry 60 minutes.
The blank that coats glass lubricant is put in the squeezing passage of the mould that coats graphitic lubricant heating jointly in 400 ℃ heating furnace, temperature retention time 60 minutes.Then blank and the mould that heats taken out simultaneously, on the hydraulic universal experimental machine, pushes rapidly, the blank that extruding is come out carries out surface treatment again carry out the extruding of 8 passages after, can obtain the brilliant industrially pure titanium bulk of micrometer/nanometer.When the grain refinement of industrially pure titanium TA2 bulk during to the micrometer/nanometer level, σ
0.2600MPa by initial annealed state brings up to 910MPa, σ
bBring up to 970MPa by 670MPa.
Claims (10)
1, the isometrical bent angle extruding production of the brilliant industrially pure titanium bulk of a kind of micro-/ nano is characterized in that, selects for use industrially pure titanium TA2 bulk as raw material, after the annealing insulation, industrially pure titanium TA2 bulk is cut into blank, carry out surface smoothness and handle, and the coating glass lubricant; Mould adopts isometrical bent angle extrusion die, and mold cavity surface applied graphitic lubricant with blank and the common heat tracing of mould, and takes out from heating furnace simultaneously and carries out isometrical bent angle extruding, finally obtains the brilliant industrially pure titanium bulk of micro-/ nano.
2, the isometrical bent angle extruding production of the brilliant industrially pure titanium bulk of micro-/ nano according to claim 1 is characterized in that, comprises the steps:
(1) select for use the industrially pure titanium bulk as raw material, industrially pure titanium bulk annealing insulation;
(2) the industrially pure titanium bulk that will anneal after being incubated cuts into blank, and blank is carried out surface treatment, reaches the surface accuracy more than 4 grades, blank surface processing roughness Ra≤1.25 μ m;
(3) with acetone surface clean is carried out on the blank surface, after the preheating, the method that adopts dip-coating is at blank surface applied glass lubricant, and coating back blank is dried;
(4) adopt isometrical bent angle extrusion die, with acetone mould is carried out surface and die cavity cleaning, after the preheating, the coated graphite lubricant is dried mould again;
(5) blank that will coat glass lubricant is put in the squeezing passage of the mould that coats graphitic lubricant, heating jointly in heating furnace then, insulation;
(6) blank and the mould that heats taken out simultaneously, rapidly blank is pushed then, repeat the blank that squeezes out is carried out surface treatment and coating glass lubricant, mold cavity coated graphite lubricant, pushes 2～8 times, promptly obtain the brilliant industrially pure titanium bulk of micro-/ nano.
3, the isometrical bent angle extruding production of the brilliant industrially pure titanium bulk of micro-/ nano according to claim 1 is characterized in that in the step (1), the industrially pure titanium bulk is incubated 1～2 hour 700 ℃～750 ℃ annealing.
4, the isometrical bent angle extruding production of the brilliant industrially pure titanium bulk of micro-/ nano according to claim 1 is characterized in that in the step (2), the industrially pure titanium bulk cuts into blank 10 * 10 * 120mm
3
5, the isometrical bent angle extruding production of the brilliant industrially pure titanium bulk of micro-/ nano according to claim 1, it is characterized in that, in the step (3), with acetone surface clean is carried out on the blank surface, preheating is 20～60 minutes under 60 ℃～100 ℃ temperature, evenly apply glass lubricant, coating layer thickness is 0.2～0.4mm.
6, according to claim 1 or the isometrical bent angle extruding production of the brilliant industrially pure titanium bulk of 5 described micro-/ nanos, it is characterized in that in the step (3), coating back blank was dried 20～60 minutes under 60 ℃～100 ℃ temperature, if defective occurs, should carry out coating or flush away recoat.
7, the isometrical bent angle extruding production of the brilliant industrially pure titanium bulk of micro-/ nano according to claim 1 is characterized in that in the step (4), the squeezing passage angle of mould is 90 °～120 °.
8, according to claim 1 or the isometrical bent angle extruding production of the brilliant industrially pure titanium bulk of 7 described micro-/ nanos, it is characterized in that, in the step (4), with acetone mould is carried out surface and die cavity cleaning, preheating is 60～90 minutes under 100 ℃～150 ℃ temperature, evenly behind the coated graphite lubricant, again mould was dried 60～90 minutes under 100 ℃～150 ℃ temperature.
9, the isometrical bent angle extruding production of the brilliant industrially pure titanium bulk of micro-/ nano according to claim 1 is characterized in that, in the step (5), blank and mould be heating jointly in 400 ℃～500 ℃ heating furnace, temperature retention time 40～60 minutes.
10, the isometrical bent angle extruding production of the brilliant industrially pure titanium bulk of micro-/ nano according to claim 1, it is characterized in that, in the step (6), on the 300KN universal hydraulic testing machine, blank is pushed, the brilliant industrially pure titanium bulk of the micro-/ nano that obtains, its microcosmic average grain size is 0.2～0.6 μ m.
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| CN 200510029663 CN1745922A (en) | 2005-09-15 | 2005-09-15 | Constant diameter right-angle extruding production of micro/nanometer crustal industrial pure titanium block |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104646444A (en) * | 2013-11-22 | 2015-05-27 | 北京有色金属研究总院 | Titanium alloy profile extrusion anti-oxidation and lubrication method |
| WO2019100809A1 (en) * | 2017-11-22 | 2019-05-31 | 四川大学 | High strength and toughness filamentous grain pure titanium and preparation method therefor |
| CN112853069A (en) * | 2021-01-08 | 2021-05-28 | 西安交通大学 | Method for regulating and controlling strength and toughness of metal rod wire through non-deformation processing |
| CN114713653A (en) * | 2022-03-24 | 2022-07-08 | 上海工程技术大学 | Machining method and forming die assembly for long rod part with threaded teeth for vehicle |
-
2005
- 2005-09-15 CN CN 200510029663 patent/CN1745922A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104646444A (en) * | 2013-11-22 | 2015-05-27 | 北京有色金属研究总院 | Titanium alloy profile extrusion anti-oxidation and lubrication method |
| WO2019100809A1 (en) * | 2017-11-22 | 2019-05-31 | 四川大学 | High strength and toughness filamentous grain pure titanium and preparation method therefor |
| CN112853069A (en) * | 2021-01-08 | 2021-05-28 | 西安交通大学 | Method for regulating and controlling strength and toughness of metal rod wire through non-deformation processing |
| CN114713653A (en) * | 2022-03-24 | 2022-07-08 | 上海工程技术大学 | Machining method and forming die assembly for long rod part with threaded teeth for vehicle |
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