CN107523711A - The preparation method of POROUS TITANIUM silver alloy - Google Patents

The preparation method of POROUS TITANIUM silver alloy Download PDF

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Publication number
CN107523711A
CN107523711A CN201610452537.0A CN201610452537A CN107523711A CN 107523711 A CN107523711 A CN 107523711A CN 201610452537 A CN201610452537 A CN 201610452537A CN 107523711 A CN107523711 A CN 107523711A
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China
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preparation
sintering
powder
ball
porous titanium
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CN201610452537.0A
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Chinese (zh)
Inventor
范佳晨
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Zhangjiagang Si Jie Hardware Tools Co Ltd
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Zhangjiagang Si Jie Hardware Tools Co Ltd
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Priority to CN201610452537.0A priority Critical patent/CN107523711A/en
Publication of CN107523711A publication Critical patent/CN107523711A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/11Making porous workpieces or articles
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C14/00Alloys based on titanium

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Materials For Medical Uses (AREA)

Abstract

This application discloses a kind of preparation method of POROUS TITANIUM silver alloy, including step:(1) titanium powder and silver powder are mixed, ball milling is carried out to compound, 4~6mm of ball radius, ratio of grinding media to material is (7~10):1,500~600 turns/min of rotational speed of ball-mill, Ball-milling Time 5~7 hours;(2), the mass ratio of mixed-powder and pore creating material is 1:(1~1.5), it is sintered under vacuum environment:200~250 DEG C are warming up to 0.5~0.7 DEG C/min, heat preservation sintering 50~60 minutes, removes pore creating material;(3), high-sintering process:By vacuum-sintering stove evacuation, 3 × 10 are filled with3~4 × 103Pa argon gas, 1250~1350 DEG C of sintering temperature, sintering time 100~120 minutes;(4), modification, the material of acquisition is added in sodium hydroxide solution, 18~24 hours is incubated under the conditions of 50~60 DEG C, then with deionized water rinsing, finally dries.Silver can improve the intensity, hardness and wearability of titanium alloy by solution strengthening, and silver can promote titanium surface quickly to form stable passivating film, improve the corrosion resistance of titanium alloy.

Description

The preparation method of POROUS TITANIUM silver alloy
Technical field
The application is related to a kind of Medical orthopedic material, more particularly to a kind of preparation method of POROUS TITANIUM silver alloy.
Background technology
Titanium or titanium alloy is as orthopedic implanting material, compared with other traditional medical metal materials, in human body environment With more excellent biocompatibility, more superior corrosion resistance, and high intensity, low elastic modulus, high-fatigue strength, high-ductility Property and high-wearing feature mechanical property, thus as hard tissue substituting and repair preferred metal material.
As a kind of synthetic material, titanium or titanium alloy is under the complicated biotic environment of human body, particularly by long-term After use, clinical problem unavoidably occurs, this is due to that elasticity modulus of materials is too high, bioactivity is undesirable, corrosion-resistant Property and wearability deficiency cause.
POROUS TITANIUM/titanium alloy combines many structure and performance characteristics of porous material and titanium/titanium alloy, has excellent Mechanics and chemical property, such as specific strength height, decay resistance is strong, while also has preferable biocompatibility, is most to send out The medical metal material of exhibition prospect.Titanium or titanium alloy porous can effectively realize the regulation and control of its modulus of elasticity, solve stress screen Problem is covered, realizes the mechanical matching between implant and bone tissue.Meanwhile titanium or titanium alloy porous is advantageous to the attached of cell , breed and break up, the transmission of body fluid and the growth of bone tissue can be promoted.
The content of the invention
It is an object of the invention to provide a kind of preparation method of POROUS TITANIUM silver alloy, with overcome it is of the prior art not Foot.
To achieve the above object, the present invention provides following technical scheme:
The embodiment of the present application discloses a kind of preparation method of POROUS TITANIUM silver alloy, including step:
(1) titanium powder and silver powder are mixed, in compound, the mass ratio of silver powder is 4~5%, and compound is carried out Ball milling, 4~6mm of ball radius, ratio of grinding media to material are (7~10):1,500~600 turns/min of rotational speed of ball-mill, Ball-milling Time 5~7 are small When;
(2), the mass ratio of mixed-powder and pore creating material is 1:(1~1.5), it is sintered under vacuum environment:With 0.5~ 0.7 DEG C/min is warming up to 200~250 DEG C, heat preservation sintering 50~60 minutes, removes pore creating material;
(3), high-sintering process:By vacuum-sintering stove evacuation, 3 × 10 are filled with3~4 × 103Pa argon gas, sintering temperature 1250~1350 DEG C of degree, sintering time 100~120 minutes;
(4), modification, will acquisition material add sodium hydroxide solution in, under the conditions of 50~60 DEG C be incubated 18~ 24 hours, then with deionized water rinsing, finally dry.
Preferably, in the preparation method of above-mentioned POROUS TITANIUM silver alloy, in step (1), ball-milling medium:Absolute ethyl alcohol, Milling atmosphere:Vacuumize and to be filled with argon gas anti-oxidant.
Preferably, in the preparation method of above-mentioned POROUS TITANIUM silver alloy, in step (2), using urea granules as pore creating material.
Preferably, in the preparation method of above-mentioned POROUS TITANIUM silver alloy, urea granules particle diameter is average 450 μm.
Preferably, in the preparation method of above-mentioned POROUS TITANIUM silver alloy, in step (1), 35 μm of titanium powder average grain diameter.
Preferably, in the preparation method of above-mentioned POROUS TITANIUM silver alloy, in step (1), 2 μm of silver powder average grain diameter.
Preferably, in the preparation method of above-mentioned POROUS TITANIUM silver alloy, in step (4), concentration of sodium hydroxide solution is 5mol/L。
Compared with prior art, the advantage of the invention is that:Silver can improve the intensity, hard of titanium alloy by solution strengthening Degree and wearability, silver can promote titanium surface quickly to form stable passivating film, improve the corrosion resistance of titanium alloy, and silver Addition can also reduce POROUS TITANIUM metal alkyl materials implantation infection rate.
Brief description of the drawings
, below will be to embodiment or existing in order to illustrate more clearly of the embodiment of the present application or technical scheme of the prior art There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this Some embodiments described in application, for those of ordinary skill in the art, on the premise of not paying creative work, Other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 show the SEM photograph of POROUS TITANIUM silver alloy in the specific embodiment of the invention.
Embodiment
The present invention is described further by the following example:According to following embodiments, the present invention may be better understood. However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described by embodiment are only used In the explanation present invention, without should be also without limitation on the present invention described in detail in claims.
The preparation method of POROUS TITANIUM silver alloy
Raw material:Titanium powder, 35 μm of average grain diameter;Silver powder, 2 μm of average grain diameter.Urea, grain diameter are average 450 μm.
(1) titanium powder and silver powder are mixed, in compound, the mass ratio of silver powder is 4%, and ball is carried out to compound Mill, ball radius 6mm, ratio of grinding media to material 10:1,600 turns/min of rotational speed of ball-mill, ball-milling medium:Absolute ethyl alcohol, milling atmosphere:Take out true Empty and anti-oxidant, the Ball-milling Time 5 hours that is filled with argon gas;
Powder diameter is obtained at 2.1 μm, body surface area about 3.4m2/mm3
(2), using urea granules as pore creating material, the mass ratio of mixed-powder and urea is 1:1, burnt under vacuum environment Knot:250 DEG C are warming up to 0.5 DEG C/min, heat preservation sintering 60 minutes, removes pore creating material;
(3), high-sintering process:Vacuum sintering furnace is evacuated to 6.68 × 10-3Pa, it is filled with 3 × 103~4 × 103Pa Argon gas, 1350 DEG C of sintering temperature, sintering time 120 minutes.
(4), modification, the material of acquisition is added in 5mol/L sodium hydroxide solution, be incubated under the conditions of 60 DEG C 24 hours, then with deionized water rinsing, finally dry.
Fig. 1 show the SEM photograph of POROUS TITANIUM silver alloy in the specific embodiment of the invention.As can be seen from Figure, hole For size at 350 μm or so, porosity is about 59%.
The material compressive strength of POROUS TITANIUM silver alloy is 32MPa, modulus of elasticity 1.4MPa.
Silver can improve the intensity, hardness and wearability of titanium alloy by solution strengthening, and silver can promote titanium surface quick Stable passivating film is formed, improves the corrosion resistance of titanium alloy, and the addition of silver can also reduce the plant of POROUS TITANIUM metal alkyl materials Enter infection rate.
Here, it should also be noted that, in order to avoid having obscured the present invention because of unnecessary details, in the accompanying drawings only Show and according to the solution of the present invention closely related structure and/or processing step, and eliminate little with relation of the present invention Other details.
Finally, it is to be noted that, term " comprising ", "comprising" or its any other variant be intended to it is non-exclusive Property includes, so that process, method, article or equipment including a series of elements not only include those key elements, and Also include the other element that is not expressly set out, or also include for this process, method, article or equipment inherently Key element.

Claims (7)

1. a kind of preparation method of POROUS TITANIUM silver alloy, it is characterised in that including step:
(1) titanium powder and silver powder being mixed, in compound, the mass ratio of silver powder is 4~5%, and ball milling is carried out to compound, 4~6mm of ball radius, ratio of grinding media to material are (7~10):1,500~600 turns/min of rotational speed of ball-mill, Ball-milling Time 5~7 hours;
(2), the mass ratio of mixed-powder and pore creating material is 1:(1~1.5), it is sintered under vacuum environment:With 0.5~0.7 DEG C/ Min is warming up to 200~250 DEG C, heat preservation sintering 50~60 minutes, removes pore creating material;
(3), high-sintering process:By vacuum-sintering stove evacuation, 3 × 10 are filled with3~4 × 103Pa argon gas, sintering temperature 1250~1350 DEG C, sintering time 100~120 minutes;
(4), modification, the material of acquisition is added in sodium hydroxide solution, it is small that 18~24 is incubated under the conditions of 50~60 DEG C When, then with deionized water rinsing, finally dry.
2. the preparation method of POROUS TITANIUM silver alloy according to claim 1, it is characterised in that:In step (1), ball milling is situated between Matter:Absolute ethyl alcohol, milling atmosphere:Vacuumize and to be filled with argon gas anti-oxidant.
3. the preparation method of POROUS TITANIUM silver alloy according to claim 1, it is characterised in that:In step (2), with urea Grain is pore creating material.
4. the preparation method of POROUS TITANIUM silver alloy according to claim 3, it is characterised in that:Urea granules particle diameter is averaged 450μm。
5. the preparation method of POROUS TITANIUM silver alloy according to claim 1, it is characterised in that:In step (1), titanium powder is put down Equal 35 μm of particle diameter.
6. the preparation method of POROUS TITANIUM silver alloy according to claim 1, it is characterised in that:In step (1), silver powder is put down Equal 2 μm of particle diameter.
7. the preparation method of POROUS TITANIUM silver alloy according to claim 1, it is characterised in that:In step (4), sodium hydroxide Solution concentration is 5mol/L.
CN201610452537.0A 2016-06-21 2016-06-21 The preparation method of POROUS TITANIUM silver alloy Pending CN107523711A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108014369A (en) * 2018-01-24 2018-05-11 山东建筑大学 A kind of preparation method of the compound bone material of renewable titanium-based
CN108543114A (en) * 2018-04-11 2018-09-18 昆明理工大学 A kind of preparation method of NiTi/ porous surfaces Ti-Ag biological gradient composite materials
CN110343894A (en) * 2019-08-09 2019-10-18 南昌大学 A kind of POROUS TITANIUM, preparation method and applications based on vacuum in situ hot melt reaction
CN111957970A (en) * 2020-08-21 2020-11-20 南昌大学 Porous titanium, preparation method and application thereof
CN114433851A (en) * 2022-03-01 2022-05-06 华中科技大学 Preparation method of silver-palladium alloy powder

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KR100699449B1 (en) * 2004-03-10 2007-03-26 롬 앤드 하스 캄파니 Modified Catalysts and Process
CN101353738A (en) * 2008-09-26 2009-01-28 重庆大学 Preparation of porosity controllable porous titanium
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108014369A (en) * 2018-01-24 2018-05-11 山东建筑大学 A kind of preparation method of the compound bone material of renewable titanium-based
CN108543114A (en) * 2018-04-11 2018-09-18 昆明理工大学 A kind of preparation method of NiTi/ porous surfaces Ti-Ag biological gradient composite materials
CN110343894A (en) * 2019-08-09 2019-10-18 南昌大学 A kind of POROUS TITANIUM, preparation method and applications based on vacuum in situ hot melt reaction
CN111957970A (en) * 2020-08-21 2020-11-20 南昌大学 Porous titanium, preparation method and application thereof
CN111957970B (en) * 2020-08-21 2022-03-11 南昌大学 Porous titanium, preparation method and application thereof
CN114433851A (en) * 2022-03-01 2022-05-06 华中科技大学 Preparation method of silver-palladium alloy powder
CN114433851B (en) * 2022-03-01 2024-03-22 华中科技大学 Preparation method of silver-palladium alloy powder

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