CN101181646A - Method for preparing toughened cemented metal netted polyporous material - Google Patents
Method for preparing toughened cemented metal netted polyporous material Download PDFInfo
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- CN101181646A CN101181646A CNA2007101718620A CN200710171862A CN101181646A CN 101181646 A CN101181646 A CN 101181646A CN A2007101718620 A CNA2007101718620 A CN A2007101718620A CN 200710171862 A CN200710171862 A CN 200710171862A CN 101181646 A CN101181646 A CN 101181646A
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Abstract
The invention relates to a method for preparing tenacious sintering metal reticular multi-hole material, pertaining to the technical field of biological project. The method comprises the steps as follows: one or a plurality of layers of stainless steel, titanium or titanium alloy silk screen are adopted as the raw materials, designed, winded, pressed and shaped through lamination; the outermost layer of the lamination pressed silk screen material is welded on the adjacent inner layer silk screen material so as to form an integer; the formed multi-hole stainless steel or multi-hole titanium material is positioned in vacuum or protecting atmosphere to sinter and then the tenacious sintering metal reticular multi-hole stainless steel or multi-hole titanium material is obtained. The invention can get tenacious sintering metal reticular multi-hole stainless steel or multi-hole titanium material with different size specifications, different porosities and different pore diameter distributions. The pore diameter and the porosity have favorable controllability and are beneficial for the growing of the bone cell; the invention has excellent biological confluence, comparatively low elastic modulus, comparatively good obdurability, simple production method, high speed, high yield and low cost.
Description
Technical field
What the present invention relates to is a kind of preparation method of technical field of medical instruments, is specifically related to a kind of preparation method of toughened cemented metal netted polyporous material.
Background technology
It is the main clinical operation of orthopaedics that bone reparation or bone are transplanted, in the employed all kinds of repair materials, metallic biomaterial has experienced the rustless steel of " first generation " and the cobalt chromium or the vitallium of " second filial generation ", but because its elastic modelling quantity is more than the skeleton height, be unfavorable for reproducing and healing of natural skeleton tissue after the implantation, so clinical practice is gradually reducing, just relatively low as the cost of biomaterial in view of rustless steel, just never finally replaced." third generation " titanium and alloy thereof be can bearing load the important biomolecule medical material, yet, at least also there is following problem in these medical titanium materials: (1) a large amount of clinical use experiences confirm, the titanium elasticity modulus of materials is higher than the human body nature bone far away, be easy to generate the stress capture-effect, be unfavorable for the fusion of implant and skeletal tissue, under the situation that is subjected to big load, destroy the human body bone easily, and make the patient feel pain, can cause that for a long time implant is loosening.(2) the surface coated oxide-film of titanium makes that titanium is difficult to combine closely with when injected organism tissue, causes implant to become flexible, influence the performance of its function.
Problem at above-mentioned metallic biomaterial existence, mainly contain the approach of two kinds of solutions, a kind of is the alloying component of seeking low elastic modulus, and bond material forming process control, prepare the titanium or the stainless steel material of low elastic modulus, although this thinking obtains very big progress, the alloy material that is complementary with the natural bone elastic modelling quantity that does not also obtain real using value so far; Another kind is preparation POROUS TITANIUM or a porous stainless steel material, if be designed to loose structure at implant surfaces or with implant itself, can improve the amalgamation of itself and when injected organism tissue effectively.The key of this design is how to control the porosity and the uniformity of loose structure.By control hole gap density, distribution, aperture size, obtain low elastic modulus and mechanical property preferably.
Porous stainless steel or the common preparation method of titanium material have: (1) powder metallurgic method, through process procedures such as metal powder process (metal dust and foaming powder are prepared and mixing in proportion), compression moulding, sintering, advantage is that vesicular tissue is even, porosity is regulated within the specific limits easily, shortcoming is that technical process is very complicated, multiple working procedure, the manufacturing cost height.(2) by injecting gas in liquid metal, the cooling back forms porous metals, and advantage is that technology is simple, and shortcoming is that stomatal frequency and uniformity are not easy accurate control, air-breathing for the titanium material owing to being easy to, can have a strong impact on the foamed materials mechanical property after solidifying.(3) solid-gas phase eutectic freezing method requires metal and a certain gas phase to have eutectic reaction, and gas is separated out as the part in the eutectic phase when solidifying, thereby forms foaming structure.(4) metal electrodeposition method, this method be by the atomic state metal after organic porous matrix inner surface deposition, remove organism and sintering and form, the main feature of the foam metal that method obtained is that the hole is communicated with thus, porosity height (all more than 80%) has three-dimensional net structure.This class A foam A metal material is a kind of functional structure material of excellent performance, but its strength character is subjected to certain restriction.
Find " the The influence ofaddition of TiH that Bing-Yun Li delivered on the 281 phase 169-175 pages or leaves at " Materials Science andEngineering A " in 2000 through literature search to prior art
2In elemental powder sintering porous Ni-Ti alloys " (additive TiH
2Influence to the sintered porous Nitinol of powder), adopt powder metallurgic method to make the porous nickel-titanium alloy material in this article, concrete grammar is: at first with nikel powder, titanium valve and a spot of foaming agent mixing; Secondly the mixture with mixing is pressed into the closely knit block that does not have remaining logical (opening) hole; And then vacuum-sintering.Its technical process is very complicated, multiple working procedure, and manufacturing cost is higher.
In sum, traditional porous metals manufacturing technology ubiquity the deficiency of technology and cost aspect, and still can not solve high strength, high tenacity, this a pair of contradiction of low elastic modulus.
Summary of the invention
The object of the invention is at the deficiencies in the prior art, and a kind of preparation method of toughened cemented metal netted polyporous material is provided, and makes its loose structure improve the biological characteristics of artificial skelecton better, and manufacture method is simple, speed is fast, the yield rate height, and cost is low.
The present invention is achieved by the following technical solutions, specifically may further comprise the steps:
(1) adopting one or more layers rustless steel, titanium or titanium alloy silk screen is raw material, by stack-design, curl compacting, shaping;
Described rustless steel, titanium or titanium alloy silk screen can be plain weave fine groove or twill fine groove web frame; In view of the grow into aperture of required minimum vias of porous implant internal skeleton is 100 μ m, widely accepted preferred pore diameter range is 100～500 μ m, so the design of the order number of silk screen raw material is in 35～140 order scopes (being that the silk screen aperture is 106～500 μ m).
Described multilamellar refers to determine according to concrete required porosity and pore-size distribution that the number of plies can be 1～5 layer.
Described stack-design is meant that following two kinds of situations use or adopt wherein a kind of simultaneously: a, pore size (the being the order number) unanimity of stacked raw material silk screen, obtain the silk screen porous material of porosity and even aperture distribution; B, the pore size (being the order number) of stacked raw material silk screen inconsistent, obtain the silk screen porous material that porosity and aperture distribute by cyclic gradient.
Described curling compacting is meant that employing " wheel roll-type " device curls simultaneously to twine also compression moulding.
(2) will be the outermost layer of the web material that suppresses of lamination be welded on the contiguous nexine web material, make it form an integral body;
(3) porous stainless steel or the porous titanium products that (2) step was formed places sintering under vacuum or the protective atmosphere, obtains the mesh structural porous rustless steel of toughening type sintering or the porous titanium material of different size specification, different porosities and pore-size distribution behind the sintering.
The shape of described porous stainless steel or porous titanium products is decided according to concrete needs, can be hollow or bar-shaped.
Described sintering, the sintering parameter is decided according to required porosity, material material, can be 1200～1300 ℃ of sintering ranges, and sintering time 1～5 hour when material is stainless steel cloth, can select hydrogen as protective atmosphere; When material is titanium/titanium alloy silk screen, can select straight argon as protective atmosphere.
The present invention utilizes sintered metal mesh manufacturing porous material to have quite outstanding advantage: have the uniform characteristic of mesh size, can reasonably mate and design pore-size, permeance property and the mechanical strength of material neatly, porosity can be controlled at bigger scope (～95%), and under the porosity of maximum, still keep the structural behaviour of material.Under identical porosity, the toughness of intensity exceeds more than several times than other preparation methoies.Pore all is the intercommunicating pore that connects mutually; Have good permeability, permeability; Also have higher mechanical strength, corrosion resistance and thermal stability.For example: the silk screen multiporous biological titanium material of the present invention's preparation, porosity 61%, hole is interconnected, yield strength 155.8MPa, bending strength 163.0MPa, elastic modelling quantity 4.06GPa.
Mesh structural porous rustless steel of toughening type sintering that the present invention obtains or silk screen porous titanium material are mainly as skeleton reparation and graft materials, for example artificial femur, artificial knee joint etc.As implanting repair materials, the very similar bone structure of the material of this structure (promptly having good emulation), and aspect physical characteristic and mechanical property than other prosthese metals more near bone, the loose structure of permeability its uniqueness, high, high heavy burden intensity, high tenacity, low elastic modulus, can bear the physiological load, allow under the physiology heavy burden condition stress shielding is minimized; Help very much to induce the formation of bone, and the soft tissue infiltration is also adhered to securely.In brief, mesh structural porous rustless steel of toughening type sintering or titanium material increase the compatibility of interface binding power, improvement and when injected organism tissue, and the success rate of raising bone reparation or transplanting aspect wide application prospect is arranged.
Description of drawings
Fig. 1 is the inventive method flow chart
The specific embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated: present embodiment has provided detailed embodiment and process being to implement under the prerequisite with the technical solution of the present invention, but protection scope of the present invention is not limited to following embodiment.
As shown in Figure 1, with 1～5 layer of specification is 35～140 purpose rustless steels or titanium/titanium alloy silk screen, by stack-design, curl compacting, shaping, the outermost layer of the web material that lamination is suppressed is welded on the contiguous nexine web material, then, should preformed porous stainless steel or the titanium material place vacuum (vacuum be 1 * 10
-3Pa) or protective atmosphere (when material is stainless steel cloth, can select hydrogen as protective atmosphere; When material is titanium/titanium alloy silk screen, can select straight argon as protective atmosphere) sintering down, sintering range: 1200～1300 ℃, sintering time: 1～5 hour.Obtain the mesh structural porous rustless steel of toughening type sintering or the porous titanium material of different size specification, different porosities and pore-size distribution behind the sintering.
Embodiment 1
With 1 layer of specification is 70 purpose stainless steel cloths, by stack-design, curl compacting, shaping, the outermost layer of the web material that lamination is suppressed is welded on the contiguous nexine web material, and then, (vacuum is 1 * 10 should preformed hollow porous stainless steel to place vacuum
-3Pa) sintering under, sintering range: 1200 ℃, sintering time: 1 hour.Obtain porosity behind the sintering and be 54% the mesh structural porous stainless steel material of toughening type sintering, hollow type, sample diameter 10mm.
Embodiment 2
With specification is each stainless steel cloth of 1 layer of 50 and 100 orders, by stack-design, curl compacting, shaping, the outermost layer of the web material that lamination is suppressed is welded on the contiguous nexine web material, then, should place sintering under the hydrogen atmosphere by preformed hollow porous stainless steel, sintering range: 1300 ℃, sintering time: 3 hours.Obtain the mesh structural porous stainless steel material of toughening type sintering that the aperture distributes by cyclic gradient behind the sintering, hollow type, mean porosities is 63%, sample diameter 20mm.
Embodiment 3
With specification is 1 layer of 40,2 layers 60 and 1 layers various stainless steel cloth of 100 orders, by stack-design, curl compacting, shaping, the outermost layer of the web material that lamination is suppressed is welded on the contiguous nexine web material, then, (vacuum is 1 * 10 should preformed porous stainless rod iron to place vacuum
-3Pa) sintering under, sintering range: 1250 ℃, sintering time: 5 hours.Obtain the mesh structural porous stainless steel material of toughening type sintering that the aperture distributes by cyclic gradient behind the sintering, bar-shaped type, mean porosities are 46%, sample diameter 15mm.
Embodiment 4
With 5 layers of specification is 100 purpose TA9 titanium alloy silk screens, by stack-design, curl compacting, shaping, the outermost layer of the web material that lamination is suppressed is welded on the contiguous nexine web material, and then, (vacuum is 1 * 10 should preformed POROUS TITANIUM rod to place vacuum
-3Pa) sintering under, sintering range: 1200 ℃, sintering time: 2 hours.Obtain porosity behind the sintering and be 38% the mesh structural porous titanium material of toughening type sintering, bar-shaped type, sample diameter 30mm.
Embodiment 5
With specification is each pure titanium wire network of TA0 of 1 layer of 35 and 80 orders, by stack-design, curl compacting, shaping, the outermost layer of the web material that lamination is suppressed is welded on the contiguous nexine web material, then, should place sintering under the straight argon atmosphere by preformed hollow porous titanium products, sintering range: 1300 ℃, sintering time: 4 hours.Obtain the mesh structural porous titanium material of toughening type sintering that the aperture distributes by cyclic gradient behind the sintering, hollow type, mean porosities is 71%, sample diameter 15mm.
Embodiment 6
With specification is 2 layer of 50 order, 2 layer of 80 order and 1 layer of 140 pure titanium wire network of purpose TA2, by stack-design, curl compacting, shaping, the outermost layer of the web material that lamination is suppressed is welded on the contiguous nexine web material, then, (vacuum is 1 * 10 should preformed POROUS TITANIUM rod to place vacuum
-3Pa) sintering under, sintering range: 1250 ℃, sintering time: 5 hours.Obtain the mesh structural porous titanium material of toughening type sintering that the aperture distributes by cyclic gradient behind the sintering, bar-shaped type, mean porosities are 58%, sample diameter 25mm.
Claims (10)
1. the preparation method of a toughened cemented metal netted polyporous material is characterized in that, may further comprise the steps:
(1) adopting one or more layers rustless steel, titanium or titanium alloy silk screen is raw material, by stack-design, curl compacting, shaping;
(2) will be the outermost layer of the web material that suppresses of lamination be welded on the contiguous nexine web material, make it form an integral body;
(3) porous stainless steel or the porous titanium products that (2) step was formed places sintering under vacuum or the protective atmosphere, obtains mesh structural porous rustless steel of toughening type sintering or porous titanium material behind the sintering.
2. the preparation method of toughened cemented metal netted polyporous material according to claim 1 is characterized in that, described rustless steel, titanium or titanium alloy silk screen are plain weave fine groove or twill fine groove web frame.
3. the preparation method of toughened cemented metal netted polyporous material according to claim 1 and 2 is characterized in that, described rustless steel, titanium or titanium alloy silk screen, and its order number is in 35～140 order scopes.
4. the preparation method of toughened cemented metal netted polyporous material according to claim 1 is characterized in that, described multilamellar, its number of plies are 1～5 layer.
5. the preparation method of toughened cemented metal netted polyporous material according to claim 1 is characterized in that, described stack-design is meant in following two kinds of situations one or both:
A, the pore size unanimity of stacked raw material silk screen, obtain the silk screen porous material of porosity and even aperture distribution;
B, the pore size of stacked raw material silk screen inconsistent, obtain the silk screen porous material that porosity and aperture distribute by cyclic gradient.
6. the preparation method of toughened cemented metal netted polyporous material according to claim 1 is characterized in that, described curling compacting is meant that employing " wheel roll-type " device curls simultaneously to twine also compression moulding.
7. the preparation method of toughened cemented metal netted polyporous material according to claim 1 is characterized in that, the shape of described porous stainless steel or porous titanium products, be hollow or bar-shaped.
8. the preparation method of toughened cemented metal netted polyporous material according to claim 1 is characterized in that, described sintering, and its temperature is 1200～1300 ℃, the time is 1～5 hour.
9. the preparation method of toughened cemented metal netted polyporous material according to claim 1 is characterized in that, described vacuum, its vacuum are 1 * 10
-3Pa.
10. the preparation method of toughened cemented metal netted polyporous material according to claim 1 is characterized in that, described protective atmosphere is meant: when material is stainless steel cloth, select hydrogen as protective atmosphere; When material is titanium/titanium alloy silk screen, select straight argon as protective atmosphere.
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| CNA2007101718620A CN101181646A (en) | 2007-12-06 | 2007-12-06 | Method for preparing toughened cemented metal netted polyporous material |
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| CNA2007101718620A CN101181646A (en) | 2007-12-06 | 2007-12-06 | Method for preparing toughened cemented metal netted polyporous material |
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| CN103300945A (en) * | 2013-06-06 | 2013-09-18 | 上海交通大学 | Medical porous composite material |
| CN103418989A (en) * | 2012-05-24 | 2013-12-04 | 中国核动力研究设计院 | Reactor filter assembly screen production method |
| CN103589888A (en) * | 2013-11-05 | 2014-02-19 | 上海交通大学 | Preparation method of structure-controllable magnesium-based three-dimensional porous material |
| CN103599560A (en) * | 2013-11-05 | 2014-02-26 | 上海交通大学 | Medical titanium/magnesium composite material and preparation method thereof |
| CN104212990A (en) * | 2014-08-30 | 2014-12-17 | 广东省工业技术研究院(广州有色金属研究院) | Preparation method of gradient porous titanium |
| CN104827246A (en) * | 2015-04-07 | 2015-08-12 | 新乡市利尔过滤技术有限公司 | High-precision sintering net for filtering |
| CN107837133A (en) * | 2017-12-14 | 2018-03-27 | 中奥汇成科技股份有限公司 | A kind of novel bionic titanium artificial joint prosthesis |
| CN109552942A (en) * | 2017-09-27 | 2019-04-02 | 村田机械株式会社 | Bobbin pallet for conveying |
| CN110450506A (en) * | 2019-08-02 | 2019-11-15 | 南京意西欧环境科技有限公司 | A kind of Liqiud-gas mixing device preparation method of gradient woven fabric network pressure electric arc sintering equipment and agglomerated material |
| CN110953909A (en) * | 2019-12-12 | 2020-04-03 | 中船重工（上海）新能源有限公司 | Manufacturing process of annular heat accumulator and annular heat accumulator |
| CN112843329A (en) * | 2020-12-30 | 2021-05-28 | 苏州晶俊新材料科技有限公司 | Degradable metal patch and preparation method thereof |
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2007
- 2007-12-06 CN CNA2007101718620A patent/CN101181646A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103418989B (en) * | 2012-05-24 | 2015-08-26 | 中国核动力研究设计院 | A kind of reactor filter assemblies guard preparation method |
| CN103418989A (en) * | 2012-05-24 | 2013-12-04 | 中国核动力研究设计院 | Reactor filter assembly screen production method |
| CN103300945A (en) * | 2013-06-06 | 2013-09-18 | 上海交通大学 | Medical porous composite material |
| CN103589888A (en) * | 2013-11-05 | 2014-02-19 | 上海交通大学 | Preparation method of structure-controllable magnesium-based three-dimensional porous material |
| CN103599560A (en) * | 2013-11-05 | 2014-02-26 | 上海交通大学 | Medical titanium/magnesium composite material and preparation method thereof |
| CN103599560B (en) * | 2013-11-05 | 2015-04-15 | 上海交通大学 | Medical titanium/magnesium composite material and preparation method thereof |
| CN104212990A (en) * | 2014-08-30 | 2014-12-17 | 广东省工业技术研究院(广州有色金属研究院) | Preparation method of gradient porous titanium |
| CN104827246A (en) * | 2015-04-07 | 2015-08-12 | 新乡市利尔过滤技术有限公司 | High-precision sintering net for filtering |
| CN109552942A (en) * | 2017-09-27 | 2019-04-02 | 村田机械株式会社 | Bobbin pallet for conveying |
| CN109552942B (en) * | 2017-09-27 | 2022-03-22 | 村田机械株式会社 | Tray for conveying bobbin |
| CN107837133A (en) * | 2017-12-14 | 2018-03-27 | 中奥汇成科技股份有限公司 | A kind of novel bionic titanium artificial joint prosthesis |
| CN110450506A (en) * | 2019-08-02 | 2019-11-15 | 南京意西欧环境科技有限公司 | A kind of Liqiud-gas mixing device preparation method of gradient woven fabric network pressure electric arc sintering equipment and agglomerated material |
| CN110953909A (en) * | 2019-12-12 | 2020-04-03 | 中船重工（上海）新能源有限公司 | Manufacturing process of annular heat accumulator and annular heat accumulator |
| CN112843329A (en) * | 2020-12-30 | 2021-05-28 | 苏州晶俊新材料科技有限公司 | Degradable metal patch and preparation method thereof |
| WO2023087445A1 (en) * | 2021-11-22 | 2023-05-25 | 东睦新材料集团股份有限公司 | Method for preparing metal support plate for fuel cell |
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