CN109482995A - A kind of metallic matrix and its construction method with spheroid character array microstructure - Google Patents
A kind of metallic matrix and its construction method with spheroid character array microstructure Download PDFInfo
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- CN109482995A CN109482995A CN201811352335.4A CN201811352335A CN109482995A CN 109482995 A CN109482995 A CN 109482995A CN 201811352335 A CN201811352335 A CN 201811352335A CN 109482995 A CN109482995 A CN 109482995A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/008—Soldering within a furnace
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials For Medical Uses (AREA)
- Prostheses (AREA)
Abstract
The invention discloses a kind of metallic matrix and its construction method with spheroid character array microstructure, 1) using metal material as matrix, first carry out heat treatment in advance to sample: cleaning is then used distilled water flushing, is dried for standby in mixed solution with scale removal；2) one layer of solder is uniformly coated on metal matrix material surface；3) upper metal form is covered in the metal material surface of one layer of solder of coating, there is the hole of certain array to arrange in the template, will be then sequentially placed into metal form gap with the metal microbead of matrix corresponding material；4) it is slowly withdrawn metal form, using soldering tech, under condition of high vacuum degree and suitable welding temperature, metal microbead is soldered to metal matrix material surface, forms the complete uniform micro-structure with spheroid character.The treatment process is simple, low manufacture cost, is easy to large-scale production, obtained structure and matrix adhesive force with higher, value is had important application in terms of biomedical implant.
Description
Technical field
The invention belongs to metal base surface processing technology field, in particular to one kind makes metal surface have spheroid character
The metallic matrix and its construction method of array microstructure.There is spheroid character array microstructure metal surface constructed by the present invention
Application to promotion metallic matrix in fields such as bio-medical, aerospace, ships has important practice significance.
Background technique
Natural bone tissue is made of nearly fine and close compact bone and porous cancellous bone, and surface includes micron, sub-micron and receives
The multilevel structures such as rice[1].Based on bionics principle, the implant surfaces with micro nano structure are than smooth surface closer to day
The surface texture of right bone tissue, is more favorable to differentiation and the Integrated implant of osteocyte[2-3].In addition, some researches show that micro-nano knots
The surface of structure can be improved the hydrophily of material surface, promote adherency, proliferation and mineralising of cell etc., and be implanted into bioactivity
Synergistic effect is produced with micro-nano structure surface after ion, its biocompatibility can be further increased.In view of the above advantage, surface
Implant metal with micro nano structure is the research hotspot of current people, also there is relatively broad application prospect.
Common bio-medical metal has titanium alloy, magnesium alloy, cobalt-base alloys etc., wherein the application of titanium alloy more at
Ripe and extensive, the present invention targetedly carries out the design of surface micro-structure to above-mentioned common bio-medical metal alloy compositions
With construct.In the patent for disclosing report, common surface treatment method of titanium alloy has sandblasting, acid etching, alkali heat, anodic oxidation
Deng.However, the surface micro-structure of these methods building has certain inhomogeneities, surface micro-structure all has a large amount of rib
Corner characteristics easily lead to and locally generate stress concentration phenomenon in implant, so as to cause the bond strength of implant and internal cell
Decline, the consequences such as biocompatible phenomenon is obvious.
Summary of the invention
It is an object of the invention to propose a kind of Metal Substrate that spheroid character array microstructure is prepared in metal base surface
Body and its construction method, to solve the problems, such as that smooth surface is unfavorable for adherency, proliferation, differentiation and the Integrated implant of osteocyte.
A kind of construction method of the metallic matrix with spheroid character array microstructure, comprising the following steps:
1) using metal material as matrix, heat treatment in advance first is carried out to sample: is cleaned in mixed solution to remove oxidation
Skin is then used distilled water flushing, is dried for standby；
2) one layer of solder is uniformly coated on metal matrix material surface；
3) upper metal form is covered in the metal material surface of one layer of solder of coating, there is the hole of certain array in the template
Gap arrangement, will then be sequentially placed into metal form gap with the metal microbead of matrix corresponding material；
4) it is slowly withdrawn metal form, it is under condition of high vacuum degree and suitable welding temperature, metal is micro- using soldering tech
Bead weld is connected to metal matrix material surface, forms the complete uniform micro-structure with spheroid character.
The construction method, in step 1), metal matrix material be titanium alloy, magnesium alloy, cobalt-base alloys, aluminium alloy,
Stainless steel.
The construction method, in step 2), used solder is Ag72Cu silver-base solder, Ti-Zr-Ni-Cu titanium-based
The routine solder such as solder.
The construction method, in step 3), bead diameter is (0.1-1.0mm, preferably 0.5mm, the sky between microballon
Gap is that may be configured as 0.1-0.8mm, metal form materials'use stainless steel, titanium alloy.
The construction method, in step 4), welding temperature is at 800~890 DEG C, 5~30min of soaking time, heating speed
5~10 DEG C/min of rate.
The construction method, in step 4), the soldering tech parameter used for Ag72Cu silver-base solder is as follows: vacuum
Degree is about -0.01MPa, rises to 400 DEG C first with the heating rate of 10 DEG C/min and carries out heat preservation dehumidifying, then with 5 DEG C/min's
Heat preservation 5min homogenizes in-furnace temperature after heating rate rises to 750 DEG C, is warming up to 880 DEG C simultaneously with the rate of 10 DEG C/min later
0~20min is kept the temperature, finally with the cooling rate slow cooling of 10 DEG C/min to room temperature.
The metallic matrix with spheroid character array microstructure obtained according to the construction method.
The present invention proposes a kind of construction method with spheroid character array microstructure, is closed with titanium alloy, magnesium alloy, cobalt-based
For the metals such as gold as basis material, the metal for equably welding one layer of corresponding material on metallic matrix by the method for soldering is micro-
Ball is conducive to mitigate institute in actual application to construct a kind of with novel spheroid character array microstructure surface
Phenomena such as stress of generation concentrates, biocompatible.The treatment process is simple, low manufacture cost, is easy to large-scale production, acquired
Structure and matrix adhesive force with higher, value is had important application in terms of biomedical implant.
It is had the following characteristics that using spheroid character array microstructure prepared by method of the invention
1) spheroid character array microstructure has certain roughness, has place mat to the preparation of micro-nano compound structure later
Effect.
2) spheroid character array microstructure performance is more uniform, and spheroid character higher with basis material bond strength exists
Stress concentration phenomenon can be avoided in application process completely.
3) spheroid character array microstructure is for fields such as biomedical implants.
4) spheroid character array microstructure can also be used in other composite material interface bonding fields.
Detailed description of the invention
Fig. 1 is the schematic diagram of spheroid character array microstructure prepared by the method for embodiment 1 in the present invention；
Fig. 2 is the process flow chart of spheroid character array microstructure prepared by the method for embodiment 1 in the present invention；
Fig. 3 is to use the spheroid character array microstructure formed after metal form in the present invention in the method for embodiment 1；
Fig. 4 is the spheroid character array microstructure formed after the method for embodiment 1 in the present invention is brazed.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
It is proposed by the present invention to have spheroid character array microstructure construction method as follows:
Basis material is processed into 60mm × 25mm using wire cutting using Ti6Al4V titanium alloy as basis material by the first step
× 3mm size is successively polished substrate material surface using 1~No. 6 abrasive paper for metallograph, until visually observe it is lower there is no scratch until,
Then mechanically polished until under metallographic microscope without apparent scratch, then in mixed solution (volume ratio: HF:
HNO3: H2O=1:1:2) cleaning 15s removes surface scale, then quickly uses distilled water flushing, is dried for standby.
Second step marks the square area of 25mm × 25mm at titanium plate center, uniformly applies be covered with a layer thickness wherein
For the Ag72Cu solder of 0.3mm.By aperture diameter 0.5mm, spacing is the gold of 0.15mm (circle center distance 0.65mm) between aperture
Belong to template and is covered on the region for being coated with solder.It is that there is 0.5mm the titanium pearl of corresponding material to be paved with aperture by diameter, then by metal
Template is carefully taken out.Another piece of titanium plate is covered on titanium pearl, and is fixed two pieces of titanium plates with stainless steel dovetail clip.
Third step is brazed in tube type vacuum furnace, and vacuum degree is lower than -0.1MPa, with the heating rate of 10 DEG C/min
It rises to 400 DEG C and carries out heat preservation dehumidifying, 5min is kept the temperature after then rising to 750 DEG C with the heating rate of 5 DEG C/min keeps in-furnace temperature equal
It homogenizes, be warming up to 880 DEG C later with the rate of 5 DEG C/min and keep the temperature 0~20min, it is finally slow with the cooling rate of 10 DEG C/min
It is cooled to room temperature.
It can get the Ti6Al4V titanium alloy surface with spheroid character array microstructure according to upper method.
Embodiment 2
It is proposed by the present invention to have spheroid character array microstructure construction method as follows:
The first step, using Ti6Al7Nb titanium alloy as basis material, using wire cutting by basis material be processed into 60mm ×
25mm × 3mm size is successively polished substrate material surface using 1~No. 6 abrasive paper for metallograph, until visually observing and lower being without scratch
Only, then mechanically polished until under metallographic microscope without apparent scratch, then in mixed solution (volume ratio:
HF:HNO3: H2O=1:1:2) cleaning 15s removes surface scale, then quickly uses distilled water flushing, is dried for standby.Locating in advance
After reason, sample is done to the blasting treatment of 60 mesh.
Second step marks the square area of 25mm × 25mm at titanium plate center, uniformly applies be covered with a layer thickness wherein
For the Ag72Cu solder of 0.4mm.By aperture diameter 0.5mm, the metal form that spacing is 0.15mm between aperture, which is covered on, is coated with pricker
The region of material.It is that there is 0.5mm the titanium pearl of corresponding material to be paved with aperture by diameter, then carefully takes out metal form.It will be another
One piece of titanium plate is covered on titanium pearl, and is fixed two pieces of titanium plates with stainless steel dovetail clip.
Third step is brazed in tube type vacuum furnace, and vacuum degree is lower than -0.1MPa, with the heating rate liter of 8 DEG C/min
Heat preservation dehumidifying is carried out to 400 DEG C, 5min is kept the temperature after then rising to 750 DEG C with the heating rate of 8 DEG C/min keeps in-furnace temperature uniform
Change, is warming up to 880 DEG C later with the rate of 8 DEG C/min and keeps the temperature 15min, finally with the cooling rate slow cooling of 10 DEG C/min to room
Temperature.
It can get 60 mesh sandblastings according to upper method and with the Ti6Al7Nb titanium alloy surface of spheroid character array microstructure.
Embodiment 3
Spheroid character array microstructure of the invention the preparation method is as follows:
Basis material is processed into 60mm × 25mm using wire cutting using Ti6Al4V titanium alloy as basis material by the first step
× 3mm size is successively polished substrate material surface using 1~No. 6 abrasive paper for metallograph, until visually observe it is lower there is no scratch until,
Then mechanically polished until under metallographic microscope without apparent scratch, then in mixed solution (volume ratio: HF:
HNO3: H2O=1:1:2) cleaning 15s removes surface scale, then quickly uses distilled water flushing, is dried for standby.Pretreated
Afterwards, sample is done to the blasting treatment of 60 mesh, micro-nano second level composite structure surface is then obtained by acid two-step etching.Acid
Property two-step etching method is as follows: obtaining sand blasted surface concaveconvex structure first in the sample after sandblasting, then equally first carries out
In 40wt% sulfuric acid solution, 60min is etched under the conditions of 65 DEG C, further obtains dimple structure, then in 1M HCL solution,
Etch 12h, 85 DEG C of solution temperature.
Second step marks the square area of 25mm × 30mm at titanium plate center, uniformly applies be covered with a layer thickness wherein
For the Ag72Cu solder of 0.5mm.By aperture diameter 0.6mm, the metal form that spacing is 0.2mm between aperture, which is covered on, is coated with solder
Region.It is that there is 0.6mm the titanium pearl of corresponding material to be paved with aperture by diameter, then carefully takes out metal form.It will be another
Block titanium plate is covered on titanium pearl, and is fixed two pieces of titanium plates with stainless steel dovetail clip.
Third step is brazed in tube type vacuum furnace, and vacuum degree is lower than -0.1MPa, with the heating rate liter of 8 DEG C/min
Heat preservation dehumidifying is carried out to 400 DEG C, 5min is kept the temperature after then rising to 750 DEG C with the heating rate of 8 DEG C/min keeps in-furnace temperature uniform
Change, is warming up to 880 DEG C later with the rate of 8 DEG C/min and keeps the temperature 15min, finally with the cooling rate slow cooling of 10 DEG C/min to room
Temperature.
It can get 60 mesh sandblastings according to upper method and add acid two steps etching and Ti6Al4V with spheroid character array microstructure
Titanium alloy surface.
Embodiment 4
Spheroid character array microstructure of the invention the preparation method is as follows:
The first step, using Ti6Al7Nb titanium alloy as basis material, using wire cutting by basis material be processed into 60mm ×
25mm × 4mm size is successively polished substrate material surface using 1~No. 6 abrasive paper for metallograph, until visually observing and lower being without scratch
Only, then mechanically polished until under metallographic microscope without apparent scratch, then in mixed solution (volume ratio:
HF:HNO3: H2O=1:1:2) cleaning 15s removes surface scale, then quickly uses distilled water flushing, is dried for standby.
Second step marks the square area of 25mm × 25mm at titanium plate center, uniformly applies be covered with a layer thickness wherein
For the Ag72Cu solder of 0.2mm.By aperture diameter 0.6mm, the metal form that spacing is 0.2mm between aperture, which is covered on, is coated with solder
Region.It is that there is 0.6mm the titanium pearl of corresponding material to be paved with aperture by diameter, then carefully takes out metal form.It will be another
Block titanium plate is covered on titanium pearl, and is fixed two pieces of titanium plates with stainless steel dovetail clip.
Third step is brazed in tube type vacuum furnace, and vacuum degree is lower than -0.1MPa, with the heating rate liter of 8 DEG C/min
Heat preservation dehumidifying is carried out to 400 DEG C, 5min is kept the temperature after then rising to 750 DEG C with the heating rate of 8 DEG C/min keeps in-furnace temperature uniform
Change, is warming up to 880 DEG C later with the rate of 5 DEG C/min and keeps the temperature 10min, finally with the cooling rate slow cooling of 10 DEG C/min to room
Temperature.
It can get the Ti6Al7Nb titanium alloy surface containing titanium pearl array microstructure according to upper method.
Embodiment 5
Spheroid character array microstructure of the invention the preparation method is as follows:
It is big to be processed into 60mm × 25mm × 4mm using wire cutting using magnesium alloy as basis material by the first step for basis material
It is small, successively polished substrate material surface using 1~No. 6 abrasive paper for metallograph, until visually observe it is lower there is no scratch until, then by it
Mechanical polishing is until without apparent scratch under metallographic microscope, the subsequent (volume ratio: HF:HNO in mixed solution3: H2O=
1:1:2) cleaning 15s removes surface scale, then quickly uses distilled water flushing, is dried for standby.After pretreated, by sample
The blasting treatment of 60 mesh is done,
Second step marks the rectangular region of 40mm × 25mm at magnesium plate center, uniformly applies be covered with a layer thickness wherein
For the Ti-Zr-Ni-Cu solder of 0.3mm.By aperture diameter 0.5mm, spacing is that the metal form of 0.15mm is covered on painting between aperture
There is the region of solder.The magnesium globule with corresponding material that diameter is 0.5mm is paved with aperture, then carefully takes metal form
Out.Another piece of magnesium plate is covered on titanium pearl, and is fixed two pieces of magnesium plates with stainless steel dovetail clip.
Third step is brazed in tube type vacuum furnace, and vacuum degree is lower than -0.1MPa, with the heating rate of 10 DEG C/min
It rises to 400 DEG C and carries out heat preservation dehumidifying, 5min is kept the temperature after then rising to 750 DEG C with the heating rate of 5 DEG C/min keeps in-furnace temperature equal
It homogenizes, be warming up to 880 DEG C later with the rate of 5 DEG C/min and keep the temperature 10min, finally extremely with the cooling rate slow cooling of 10 DEG C/min
Room temperature.
According to the available 60 mesh sandblastings of upper method and the Mg alloy surface with spheroid character array microstructure.
It should be understood that for those of ordinary skills, it can be modified or changed according to the above description,
And all these modifications and variations should all belong to the protection domain of appended claims of the present invention.
Claims (7)
1. a kind of construction method of the metallic matrix with spheroid character array microstructure, which comprises the following steps:
1) using metal material as matrix, heat treatment in advance first is carried out to sample: being cleaned in mixed solution with scale removal, with
Distilled water flushing is used afterwards, is dried for standby；
2) one layer of solder is uniformly coated on metal matrix material surface；
3) upper metal form is covered in the metal material surface of one layer of solder of coating, there is the hole of certain array to arrange in the template
Cloth will be then sequentially placed into metal form gap with the metal microbead of matrix corresponding material；
4) it is slowly withdrawn metal form, is welded metal microbead under condition of high vacuum degree and suitable welding temperature using soldering tech
It is connected to metal matrix material surface, forms the complete uniform micro-structure with spheroid character.
2. construction method according to claim 1, which is characterized in that in step 1), metal matrix material is titanium alloy, magnesium
Alloy, cobalt-base alloys, aluminium alloy, stainless steel.
3. construction method according to claim 1, which is characterized in that in step 2), used solder is Ag72Cu silver
The routine solder such as base solder, Ti-Zr-Ni-Cu titanium based solder.
4. construction method according to claim 1, which is characterized in that in step 3), bead diameter be (0.1-1.0mm, it is excellent
It is selected as 0.5mm, the gap between microballon is that may be configured as 0.1-0.8mm, metal form materials'use stainless steel, titanium alloy.
5. construction method according to claim 1, which is characterized in that in step 4), welding temperature is protected at 800~890 DEG C
Warm 5~30min of time, 5~10 DEG C/min of heating rate.
6. construction method described in, in step 4), the soldering tech parameter used for Ag72Cu silver-base solder is as follows: vacuum degree
About -0.01MPa rises to 400 DEG C first with the heating rate of 10 DEG C/min and carries out heat preservation dehumidifying, then with the liter of 5 DEG C/min
Heat preservation 5min homogenizes in-furnace temperature after warm rate rises to 750 DEG C, is warming up to 880 DEG C later with the rate of 10 DEG C/min and protects
0~20min of temperature, finally with the cooling rate slow cooling of 10 DEG C/min to room temperature.
7. the Metal Substrate with spheroid character array microstructure that -6 any construction methods obtain according to claim 1
Body.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111674058A (en) * | 2020-06-01 | 2020-09-18 | 南京航空航天大学 | Preparation device and method of carbon fiber three-dimensional woven honeycomb composite material |
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| CN103108599A (en) * | 2010-09-20 | 2013-05-15 | 新特斯有限责任公司 | Method for joining two or more segments of a surgical implant |
| CN104203293A (en) * | 2012-02-07 | 2014-12-10 | 加利福尼亚大学董事会 | Products of manufacture having tantalum coated nanostructures, and methods of making and using them |
| CN107335879A (en) * | 2017-06-21 | 2017-11-10 | 深圳市汉尔信电子科技有限公司 | A kind of method for packing of face array |
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| US4834756A (en) * | 1982-02-18 | 1989-05-30 | Pfizer Hospital Products Group, Inc. | Bone prosthesis with porous coating |
| CN101889911A (en) * | 2009-05-19 | 2010-11-24 | 爱尔兰国立大学,戈尔韦 | The bone implant that has surface anchoring structure |
| CN201609797U (en) * | 2010-03-18 | 2010-10-20 | 正中科技股份有限公司 | Metal template |
| CN103108599A (en) * | 2010-09-20 | 2013-05-15 | 新特斯有限责任公司 | Method for joining two or more segments of a surgical implant |
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