CN104212990A - Preparation method of gradient porous titanium - Google Patents
Preparation method of gradient porous titanium Download PDFInfo
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- CN104212990A CN104212990A CN201410434922.3A CN201410434922A CN104212990A CN 104212990 A CN104212990 A CN 104212990A CN 201410434922 A CN201410434922 A CN 201410434922A CN 104212990 A CN104212990 A CN 104212990A
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Abstract
The invention discloses a preparation method of gradient porous titanium. The preparation method is characterized in that spherical titanium powder with different particle sizes is put in graphite molds in sequence from thin to thick; the pressure applied on the titanium powder is 5-20 MPa; the vacuum degree is not higher than 3 Pa; the temperature rises to 500-650 DEG C with the heating speed of 50-200 DEG C/min; the sintering is performed for 0-20 minutes; and the porous titanium material with the aperture size gradually changed is obtained. The preparation method has no need to add a pore forming agent or other assistants, so that the environmental pollution is reduced, and the purity of titanium is retained; two steps of pressing and sintering in a traditional powder metallurgy method are synthesized and finished; the porosity and the pore size can be adjusted through controlling the sintering temperature, the heating speed and the temperature keeping time in a certain range; and the development of filtration products is facilitated.
Description
Technical field
The present invention relates to the technology of preparing of POROUS TITANIUM, specifically refer to a kind of preparation method of gradient porous titanium.
Background technology
Titanium is owing to having hot stiff stability excellence, good corrosion resistance, advantage that specific tenacity is high, at present extensive with the form of porous for the manufacture of filtering material, be applied in the industry such as petrochemical complex, energy environment protection, defence and military, nuclear technique, food engineering and bio-pharmaceuticals.
At present, be how to make high filtering accuracy and high filtration efficiency coexist to the study hotspot of filtering material, investigator finds that gradient-structure porous material can address this problem very well simultaneously.Gradient-structure porous material for filtering generally refers to that bore diameter gradient changes.The manufacturing process of gradient porous material is a lot, comprises foaming, centrifugal casting, pressure filtration molding method and electrochemical deposition method etc.But all there is the problem of adding surface contamination that pore-forming material or other auxiliary agents bring and technical process more complicated in these methods.Discharge plasma sintering (Spark Plasma Sintering, SPS) technology is a kind of powder metallurgy activated sintering technology of novelty, complete together with the compacting of prior powder metallurgy method can being merged with sintering process, be a kind of material preparation technology of short route, there is the features such as heating rate is fast, heat-up time is short.And do not need to add auxiliary agent in compacting and sintering process, prepare material surface pollution-free.If adopt SPS technology to prepare gradient porous titanium, investigation and application will be had and be worth.
Research shows, compares with the irregular titanium valve of proterties, and to have pore surface smooth for the filtering material of sized spherical titanium powder sintering preparation, uniform pore diameter and the feature of three-dimensional communication, thus pressure-losses when can reducing filtration, raising filtration efficiency.Be entitled as paper (5 Benders of " relation of the performance of spherical powder POROUS TITANIUM and powder size and sintering schedule ", Guo Fuhe, " Rare Metals Materials and engineering ", 1990,2,34-36) disclose the filtering accuracy of the POROUS TITANIUM of varigrained spherical titanium powder preparation, result shows the porous material that spherical titanium powder makes, its permeability than irregularly shaped ti powder make high 3 ~ 7 times.Therefore, if can discharge plasma sintering method be utilized, adopt the spherical titanium powder of different-grain diameter, the spherical morphology of powder is not changed in preparation process, preparing the POROUS TITANIUM that pore size is graded structure, for filtering material, is a job highly significant, up to now, there is not yet the relevant report adopting the method to prepare gradient porous titanium.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art part, by the collocation of different-grain diameter spherical titanium powder and the optimization of powder metallurgical technique thereof, one preparation method is fast and effectively provided, realizes uniform pore diameter, and the gradient porous titanium material that can adjust flexibly on demand.
Object of the present invention is achieved through the following technical solutions: be positioned over successively in graphite jig by the sized spherical titanium powder of different-grain diameter according to order from fine to coarse; The pressure be applied on titanium valve is 5 ~ 20MPa, vacuum tightness≤3Pa, is warming up to 500 ~ 650 DEG C with the temperature rise rate of 50 ~ 200 DEG C/min, sinters 0 ~ 20 minute, namely obtains and has the porous titanium material that pore size is graded.
The principle of preparation method of the present invention is: adopt pulsed current to be rapidly heated, the sized spherical titanium powder of sintering different-grain diameter.Under the pressure of the temperature of 500 ~ 650 DEG C and 5 ~ 20MPa, occur between powder particle can keep original spherical pattern while bonding is gained in strength.Sintering temperature is too low, is not also formed with effective adhesive between powder, and sintered products is without intensity; Sintering temperature is too high, sintered products quick densifying, and porosity also forms closed pore while reducing, and does not have filteration.Be applied to titanium valve upward pressure too small, be unfavorable for that powder has effective adhesive in sintering process; Be applied to titanium valve upward pressure excessive, the spherical morphology of titanium valve in sintering process, can be changed.Adopt the porosity of the different state modulator resulting materials such as sintering temperature, temperature rise rate, soaking time.
Due to the technique scheme taked, the present invention is had the following advantages:
(1) adopt preparation method of the present invention not need to add pore-forming material or other auxiliary agents, the surface contamination thus do not brought thus, the purity of titanium can be kept while reducing environmental pollution.
(2) compacting of prior powder metallurgy method can complete by the present invention together with sintering two-step process and merging into, and is a kind of material preparation technology of short route, can avoids the shortcoming of current preparing technique process complexity.
(3) the present invention realizes porous by adopting the spherical powder of different-grain diameter distribution successively to superpose
Titanium pore-size gradient distributes.This gradient porous titanium adjusts porosity and pore size within the specific limits by control sintering temperature, temperature rise rate, soaking time, is extremely conducive to the exploitation of filtering product.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the gradient porous titanium of embodiment 1.
Fig. 2 is the room temperature stress under compression strain curve of the gradient porous titanium of embodiment 1.
Embodiment
By following embodiment and accompanying drawing thereof, the invention will be further described, but embodiments of the present invention are not limited only to this.
Embodiment 1
Be that to pour diameter into be in the graphite jig of Φ 20mm to-100+150 object sized spherical titanium powder by particle diameter, then equal in quality particle diameter is poured in mould for-40+50 object sized spherical titanium powder; Graphite jig is put into discharging plasma sintering equipment, and by the first precompressed powder of positive and negative Graphite Electrodes to 10MPa, vacuum tightness≤3Pa, temperature rise rate is 104 DEG C/min, within 5 minutes, is warmed up to 550 DEG C, sinters 10 minutes, obtains the POROUS TITANIUM that diameter is Φ 20mm.The overall porosity of this POROUS TITANIUM is 22.3%, and room temperature breaking tenacity is 459MPa.
Embodiment 2
Be that to pour diameter into be in the graphite jig of Φ 20mm to-100+150 object sized spherical titanium powder by particle diameter, then equal in quality particle diameter is poured in mould for-60+80 object sized spherical titanium powder; Graphite jig is put into discharging plasma sintering equipment, and by the first precompressed powder of positive and negative Graphite Electrodes to 20MPa, vacuum tightness≤3Pa, temperature rise rate is 72 DEG C/min, within 8 minutes, is warmed up to 610 DEG C, obtains the POROUS TITANIUM that diameter is Φ 20mm.The overall porosity of this POROUS TITANIUM is 18.4%, and room temperature breaking tenacity is 615MPa.
Embodiment 3
Be that to pour diameter into be in the graphite jig of Φ 20mm to-100+150 object sized spherical titanium powder by particle diameter, then equal in quality particle diameter is poured in mould for-60+80 object sized spherical titanium powder, finally pour equal in quality particle diameter into mould for-40+50 object sized spherical titanium powder; Graphite jig is put into discharging plasma sintering equipment, and by the first precompressed powder of positive and negative Graphite Electrodes to 15MPa, vacuum tightness≤3Pa, temperature rise rate is 60 DEG C/min, within 10 minutes, is warmed up to 630 DEG C, obtains the POROUS TITANIUM that diameter is Φ 20mm.The overall porosity of this POROUS TITANIUM is 14.1%, and room temperature breaking tenacity is 731MPa.
Claims (1)
1. a preparation method for gradient porous titanium, is characterized in that being positioned over successively in graphite jig by the sized spherical titanium powder of different-grain diameter according to order from fine to coarse; The pressure be applied on titanium valve is 5 ~ 20MPa, vacuum tightness≤3Pa, is warming up to 500 ~ 650 DEG C with the temperature rise rate of 50 ~ 200 DEG C/min, sinters 0 ~ 20 minute, namely obtains and has the porous titanium material that pore size is graded.
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Cited By (6)
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| CN106978550A (en) * | 2017-03-22 | 2017-07-25 | 西安建筑科技大学 | A kind of Ti porous materials and preparation method |
| CN107190190A (en) * | 2017-05-19 | 2017-09-22 | 东莞颠覆产品设计有限公司 | The gradient porous magnesium alloy materials of bone defect healing |
| CN110438525A (en) * | 2019-08-08 | 2019-11-12 | 广东省新材料研究所 | A kind of porous electrode and its application producing gas for electrochemistry |
| CN110814331A (en) * | 2018-08-13 | 2020-02-21 | 株式会社韩亚科技 | Titanium filter for injection and infusion solution for infusion bottle and manufacturing method thereof |
| CN112886021A (en) * | 2021-04-30 | 2021-06-01 | 中南大学 | Three-dimensional porous current collector with gradient pore structure and preparation method and application thereof |
| CN113275569A (en) * | 2021-04-22 | 2021-08-20 | 大连理工大学 | Composite micro-cavity gradient porous surface for liquid film boiling and preparation method thereof |
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| CN110814331A (en) * | 2018-08-13 | 2020-02-21 | 株式会社韩亚科技 | Titanium filter for injection and infusion solution for infusion bottle and manufacturing method thereof |
| CN110814331B (en) * | 2018-08-13 | 2021-07-27 | 株式会社韩亚科技 | Titanium filter for injection and infusion solution for infusion bottle and manufacturing method thereof |
| CN110438525A (en) * | 2019-08-08 | 2019-11-12 | 广东省新材料研究所 | A kind of porous electrode and its application producing gas for electrochemistry |
| CN113275569A (en) * | 2021-04-22 | 2021-08-20 | 大连理工大学 | Composite micro-cavity gradient porous surface for liquid film boiling and preparation method thereof |
| CN112886021A (en) * | 2021-04-30 | 2021-06-01 | 中南大学 | Three-dimensional porous current collector with gradient pore structure and preparation method and application thereof |
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Application publication date: 20141217 |