CN101418391A - Method for preparing gradient porous material - Google Patents
Method for preparing gradient porous material Download PDFInfo
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- CN101418391A CN101418391A CNA2008102097006A CN200810209700A CN101418391A CN 101418391 A CN101418391 A CN 101418391A CN A2008102097006 A CNA2008102097006 A CN A2008102097006A CN 200810209700 A CN200810209700 A CN 200810209700A CN 101418391 A CN101418391 A CN 101418391A
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Abstract
The invention discloses a method for preparing a gradient porous material, relates to a method for preparing a porous material, and solves the problem that the prior method for preparing the porous material has complex technique, high cost, hard control of foaming process, and hard control of aperture size and porosity factor. The method comprises the following steps: firstly, mixing matrix powder and pore-foaming agent, and then adding absolute ethyl alcohol into the mixture to prepare suspension; secondly, pouring the suspension into a mould, and then centrifugating and depositing the suspension; thirdly, after centrifugating and depositing the suspension, drying deposit, taking out rough blank after stripping, and putting the rough blank into a graphite mould to sinter to obtain blank; and fourthly, removing the pore-foaming agent in the blank to obtain the gradient porous material. The method has the advantages of simple preparation technique, low cost, gradually increased porosity factor along the radial direction from outside to inside, and easy control of the aperture size and the porosity factor.
Description
Technical field
The present invention relates to prepare the method for porous material.
Background technology
Porous material is that a kind of inside configuration contains a large amount of holes, function and type material structure-integrated, that have function and structure double attribute, have in light weight, excellent mechanical properties such as height ratio strong, high specific stiffness, height is tough, high-energy absorption, and special property such as damping, heat insulation, sound absorption, electromagnetic shielding, perviousness, particular optical performance, be a kind of multifunctional engineering material of excellent performance, be widely used in industry such as metallurgical machinery, petrochemical complex, energy environment protection, defence and military, nuclear technique, aviation, electronics, medical material and bio-pharmaceuticals.Porous material can be divided into two kinds of closed pore and through holes on the structure, and the former contains a large amount of self-existent pores, and the latter then is the three-dimensional porous structure that connects continuously.
At present, the preparation method of porous material mainly is divided into foaming, sintering process, casting and sedimentation.But ubiquity complex process, apparatus expensive causes production cost height, the difficult control of foaming process, aperture size and the uppity shortcoming of porosity.
Summary of the invention
The present invention seeks to for the preparation method who solves existing porous material exists complex process, cost height, the difficult control of foaming process, aperture size and the uppity problem of porosity, and the method for preparing gradient porous material is provided.
The method for preparing gradient porous material realizes according to the following steps: one, by 1: 1～10 volume ratio matrix powder is mixed with pore-creating agent, add dehydrated alcohol then in mixture, make the mixture total mass concentration and be 2%～50% suspension; Two, suspension is poured in the mould, carried out centrifugal deposition then, centrifuge speed is 500～5000r/min, adds pore-creating agent behind the centrifugal deposition 3min to filling up mould in mould, stops centrifugal deposition; Three, the mould behind the centrifugal deposition places under 50 ℃ the condition and dries 5h, takes out crude green body after the demoulding, puts into graphite jig again, is 10 in vacuum tightness
-2～10
-3Pa, sintering temperature are that 400～1500 ℃, sintering pressure are sintering 10min～3h under the condition of 2～100MPa, blank; Four, the pore-creating agent in the removal blank promptly gets gradient porous material; Wherein matrix powder is powder of stainless steel, cobalt-base alloy powder, magnesium alloy powder, Al alloy powder, titanium alloy powder, tantalum powder, niobium powder, chromium powder, titanium valve, Ni-Ti intermetallic compound powder, Ni-Al intermetallic compound powder, Fe-Al intermetallic compound powder, alumina powder, Zirconium oxide powder, calcium orthophosphate base bioceramic powder, metaphosphoric acid three calcium powders, bioactivity glass powder, titania powder, hydroxyapatite powder or carbon dust in the step 1; Step 1 is identical with pore-creating agent in the step 2, and pore-creating agent is sodium salt, sylvite, aluminium powder, iron powder, copper powder, carbon dust or coal dust; Matrix powder and pore-creating agent are composition inequality in the step 1.
Gradient porous material extexine density maximum among the present invention, radially the ecto-entad porosity increases gradually, the Gradient distribution of hole also can realize cascade filtration, the Young's modulus distribution gradient of gradient porous material, the porous material with the identical mechanical property of natural bone can be obtained, and metal and ceramic gradient porous material can be prepared; The preparation technology of gradient porous material is simple among the present invention, all adopts conventional equipment, and production cost is low, aperture size and porosity are easy to control, porosity radially ecto-entad gradually changes, and porosity increases to 80% from 10% from outside to inside, and pore dimension is 30 μ m～480 μ m; Gradient porous material among the present invention can carry out sintering, makes the performance of material reach requirement, is applied to different fields.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the method that present embodiment prepares gradient porous material realizes according to the following steps: one, by 1: 1～10 volume ratio matrix powder is mixed with pore-creating agent, in mixture, add dehydrated alcohol then, make the mixture total mass concentration and be 2%～50% suspension; Two, suspension is poured in the mould, carried out centrifugal deposition then, centrifuge speed is 500～5000r/min, adds pore-creating agent behind the centrifugal deposition 3min to filling up mould in mould, stops centrifugal deposition; Three, the mould behind the centrifugal deposition places under 50 ℃ the condition and dries 5h, takes out crude green body after the demoulding, puts into graphite jig again, is 10-2～10 in vacuum tightness
-3Pa, sintering temperature are that 400～1500 ℃, sintering pressure are sintering 10min～3h under the condition of 2～100MPa, blank; Four, the pore-creating agent in the removal blank promptly gets gradient porous material; Wherein matrix powder is powder of stainless steel, cobalt-base alloy powder, magnesium alloy powder, Al alloy powder, titanium alloy powder, tantalum powder, niobium powder, chromium powder, titanium valve, Ni-Ti intermetallic compound powder, Ni-Al intermetallic compound powder, Fe-Al intermetallic compound powder, alumina powder, Zirconium oxide powder, calcium orthophosphate base bioceramic powder, metaphosphoric acid three calcium powders, bioactivity glass powder, titania powder, hydroxyapatite powder or carbon dust in the step 1; Step 1 is identical with pore-creating agent in the step 2, and pore-creating agent is sodium salt, sylvite, aluminium powder, iron powder, copper powder, carbon dust or coal dust; Matrix powder and pore-creating agent are composition inequality in the step 1.
Sintering adopts vacuum heating-press sintering, HIP sintering or discharge plasma sintering in the present embodiment step 3.
Gained gradient porous material in the present embodiment can carry out sintering, makes the performance of material reach requirement, is applied to different fields; Sintering adopts pressureless sintering, vacuum heating-press sintering, HIP sintering or discharge plasma sintering, and sintering temperature is 400～2100 ℃, and sintering time is 2～8h.
Embodiment two: present embodiment and embodiment one are different is 1: 2 by volume～8 matrix powder to be mixed with pore-creating agent in the step 1.Other step and parameter are identical with embodiment one.
Embodiment three: present embodiment and embodiment one are different is 1: 4 by volume～6 matrix powder to be mixed with pore-creating agent in the step 1.Other step and parameter are identical with embodiment one.
Embodiment four: present embodiment and embodiment one are different is matrix powder to be mixed with pore-creating agent in 1: 5 by volume in the step 1.Other step and parameter are identical with embodiment one.
Embodiment five: present embodiment and embodiment one are different is matrix powder to be mixed with pore-creating agent in 1: 1 by volume in the step 1.Other step and parameter are identical with embodiment one.
Embodiment six: present embodiment and embodiment one are different is matrix powder to be mixed with pore-creating agent in 1: 10 by volume in the step 1.Other step and parameter are identical with embodiment one.
Embodiment seven: present embodiment and embodiment one are different is that the particle diameter of matrix powder in the step 1 is 3～300 μ m.Other step and parameter are identical with embodiment one.
Embodiment eight: present embodiment and embodiment one are different is that the particle diameter of matrix powder in the step 1 is 10～200 μ m.Other step and parameter are identical with embodiment one.
Embodiment nine: present embodiment and embodiment one are different is that the particle diameter of matrix powder in the step 1 is 100 μ m.Other step and parameter are identical with embodiment one.
Embodiment ten: present embodiment and embodiment one are different is that the particle diameter of pore-creating agent in the step 1 is 3～500 μ m.Other step and parameter are identical with embodiment one.
Embodiment 11: present embodiment and embodiment one are different is that the particle diameter of pore-creating agent in the step 1 is 10～400 μ m.Other step and parameter are identical with embodiment one.
Embodiment 12: present embodiment and embodiment one are different is that the particle diameter of pore-creating agent in the step 1 is 200 μ m.Other step and parameter are identical with embodiment one.
Embodiment 13: present embodiment and embodiment one are different is that preparation mixture total mass concentration is 4%～40% suspension in the step 1.Other step and parameter are identical with embodiment one.
Embodiment 14: present embodiment and embodiment one are different is that preparation mixture total mass concentration is 6%～30% suspension in the step 1.Other step and parameter are identical with embodiment one.
Embodiment 15: present embodiment and embodiment one are different is that preparation mixture total mass concentration is 8%～20% suspension in the step 1.Other step and parameter are identical with embodiment one.
Embodiment 16: present embodiment and embodiment one are different is that preparation mixture total mass concentration is 18% suspension in the step 1.Other step and parameter are identical with embodiment one.
Embodiment 17: what present embodiment and embodiment one were different is that centrifuge speed is 1000～4000r/min in the step 2.Other step and parameter are identical with embodiment one.
Embodiment 18: what present embodiment and embodiment one were different is that centrifuge speed is 3000r/min in the step 2.Other step and parameter are identical with embodiment one.
Embodiment 19: present embodiment and embodiment one are different is to be 10 in vacuum tightness in the step 3
-2Pa, sintering temperature are that 750 ℃, sintering pressure are sintering 2h under the condition of 50MPa.Other step and parameter are identical with embodiment one.
Embodiment 20: present embodiment and embodiment one are different is to be 10 in vacuum tightness in the step 3
-3Pa, sintering temperature are that 760 ℃, sintering pressure are sintering 0.5h under the condition of 25MPa.Other step and parameter are identical with embodiment one.
Embodiment 21: what present embodiment and embodiment one were different is that pore-creating agent is sodium salt or sylvite, and step 4 is leached blank 1h～48h with deionized water.Other step and parameter are identical with embodiment one.
Embodiment 22: what present embodiment and embodiment one were different is that pore-creating agent is sodium salt or sylvite, and step 4 is leached blank 10h with deionized water.Other step and parameter are identical with embodiment one.
Embodiment 23: what present embodiment and embodiment one were different is that pore-creating agent is an aluminium powder, and the step 4 mass concentration is that 50%～90% sodium hydroxide solution leaches blank 2～3h.Other step and parameter are identical with embodiment one.
Embodiment 24: what present embodiment and embodiment one were different is that pore-creating agent is an aluminium powder, and the step 4 mass concentration is that 65% sodium hydroxide solution leaches blank 2h.Other step and parameter are identical with embodiment one.
Embodiment 25: what present embodiment and embodiment one were different is that pore-creating agent is an iron powder, and the step 4 mass concentration is that 30%～70% hydrochloric acid soln leaches blank 2～3h.Other step and parameter are identical with embodiment one.
Embodiment 26: what present embodiment and embodiment one were different is that pore-creating agent is an iron powder, and the step 4 mass concentration is that 50% hydrochloric acid soln leaches blank 2h.Other step and parameter are identical with embodiment one.
Embodiment 27: what present embodiment and embodiment one were different is that pore-creating agent is a copper powder, and the step 4 mass concentration is that 3% hydrochloric acid and mass concentration are that the mixing solutions of 1% nitric acid leaches blank 2～3h.Other step and parameter are identical with embodiment one.
Embodiment 28: what present embodiment and embodiment one were different is that pore-creating agent is a copper powder, and the step 4 mass concentration is that 3% hydrochloric acid and mass concentration are that the mixing solutions of 1% nitric acid leaches blank 2h.Other step and parameter are identical with embodiment one.
Embodiment 29: what present embodiment and embodiment one were different is that pore-creating agent is carbon dust or coal dust, and step 4 is removed pore-creating agent in the blank with combustion method.Other step and parameter are identical with embodiment one.
Embodiment 30: the method that present embodiment prepares gradient porous material realizes according to the following steps: one, by 1: 1 volume ratio titanium valve is mixed with sodium-chlor, in mixture, add dehydrated alcohol then, make the mixture total mass concentration and be 5% suspension; Two, suspension is poured in the mould, carried out centrifugal deposition then, centrifuge speed is 2000r/min, adds sodium-chlor behind the centrifugal deposition 3min to filling up mould in mould, stops centrifugal deposition; Three, the mould behind the centrifugal deposition places under 50 ℃ the condition and dries 5h, takes out crude green body after the demoulding, puts into graphite jig again, is 10 in vacuum tightness
-2Pa, sintering temperature are that 750 ℃, sintering pressure are sintering 2h under the condition of 15MPa, blank; Four, leach blank 5h with deionized water, promptly get gradient porous material.
In the present embodiment gained gradient porous material porosity radially ecto-entad gradually change, porosity increases to 80% from 15% from outside to inside, after tested, pore dimension is 30～480 μ m; Gained gradient porous material in the present embodiment is that behind the pressureless sintering 2h, Young's modulus is 26.5GPa after tested under 1100 ℃ the condition in temperature, and ultimate compression strength is 280MPa, and deflection is less than 2%.
The embodiment hentriaconta-: the method that present embodiment prepares gradient porous material realizes according to the following steps: one, by 1: 3 volume ratio aluminum oxide powder is mixed with iron powder, in mixture, add dehydrated alcohol then, make the mixture total mass concentration and be 10% suspension; Two, suspension is poured in the mould, carried out centrifugal deposition then, centrifuge speed is 3000r/min, adds iron powder behind the centrifugal deposition 3min to filling up mould in mould, stops centrifugal deposition; Three, the mould behind the centrifugal deposition places under 50 ℃ the condition and dries 5h, takes out crude green body after the demoulding, puts into graphite jig again, is 10 in vacuum tightness
-3Pa, sintering temperature are that 1200 ℃, sintering pressure are sintering 10min under the condition of 2MPa, blank; Four, be that 40% hydrochloric acid soln leaches blank 2h with mass concentration, promptly get gradient porous material.
Adopt discharge plasma sintering in the present embodiment step 3.
In the present embodiment gained gradient porous material porosity radially ecto-entad gradually change, porosity increases to 50% from 10% from outside to inside, after tested, pore dimension is 40～450 μ m; Gained gradient porous material in the present embodiment, after tested, Young's modulus is 30GPa, and ultimate compression strength is 56MPa, and deflection is less than 1%.
Embodiment 32: the method that present embodiment prepares gradient porous material realizes according to the following steps: one, by 1: 5 volume ratio hydroxyapatite powder is mixed with sodium-chlor, in mixture, add dehydrated alcohol then, make the mixture total mass concentration and be 15% suspension; Two, suspension is poured in the mould, carried out centrifugal deposition then, centrifuge speed is 3500r/min, adds sodium-chlor behind the centrifugal deposition 3min to filling up mould in mould, stops centrifugal deposition; Three, the mould behind the centrifugal deposition places under 50 ℃ the condition and dries 5h, takes out crude green body after the demoulding, puts into graphite jig again, is 10 in vacuum tightness
-3Pa, sintering temperature are that 780 ℃, sintering pressure are sintering 15min under the condition of 20MPa, blank; Four, leach blank 2h with deionized water, promptly get gradient porous material.
Adopt discharge plasma sintering in the present embodiment step 3.
In the present embodiment gained gradient porous material porosity radially ecto-entad gradually change, porosity increases to 60% from 20% from outside to inside, after tested, pore dimension is 30～470 μ m; Gained gradient porous material in the present embodiment, Young's modulus is 9.2GPa after tested, and ultimate compression strength is 19MPa, and deflection is less than 2%.
Claims (10)
1, the method for preparing gradient porous material, it is characterized in that the method for preparing gradient porous material realizes according to the following steps: one, matrix powder is mixed with pore-creating agent by 1: 1～10 volume ratio, in mixture, add dehydrated alcohol then, make the mixture total mass concentration and be 2%～50% suspension; Two, suspension is poured in the mould, carried out centrifugal deposition then, centrifuge speed is 500～5000r/min, adds pore-creating agent behind the centrifugal deposition 3min to filling up mould in mould, stops centrifugal deposition; Three, the mould behind the centrifugal deposition places under 50 ℃ the condition and dries 5h, takes out crude green body after the demoulding, puts into graphite jig again, is 10 in vacuum tightness
-2～10
-3Pa, sintering temperature are that 400～1500 ℃, sintering pressure are sintering 5min～3h under the condition of 2～100MPa, blank; Four, the pore-creating agent in the removal blank promptly gets gradient porous material; Wherein matrix powder is powder of stainless steel, cobalt-base alloy powder, magnesium alloy powder, Al alloy powder, titanium alloy powder, tantalum powder, niobium powder, chromium powder, titanium valve, Ni-Ti intermetallic compound powder, Ni-Al intermetallic compound powder, Fe-Al intermetallic compound powder, alumina powder, Zirconium oxide powder, calcium orthophosphate base bioceramic powder, metaphosphoric acid three calcium powders, bioactivity glass powder, titania powder, hydroxyapatite powder or carbon dust in the step 1; Step 1 is identical with pore-creating agent in the step 2, and pore-creating agent is sodium salt, sylvite, aluminium powder, iron powder, copper powder, carbon dust or coal dust; Matrix powder and pore-creating agent are composition inequality in the step 1.
2, the method for preparing gradient porous material according to claim 1 is characterized in that in the step 1 that 1: 2 by volume～8 mix matrix powder with pore-creating agent.
3, the method for preparing gradient porous material according to claim 2, the particle diameter that it is characterized in that matrix powder in the step 1 are 3～300 μ m.
4, the method for preparing gradient porous material according to claim 3, the particle diameter that it is characterized in that pore-creating agent in the step 1 are 3～500 μ m.
5, the method for preparing gradient porous material according to claim 4 is characterized in that making in the step 1 mixture total mass concentration and is 6%～30% suspension.
6, the method for preparing gradient porous material according to claim 5 is characterized in that pore-creating agent is sodium salt or sylvite, and step 4 is leached blank 1h～48h with deionized water.
7, the method for preparing gradient porous material according to claim 5 is characterized in that pore-creating agent is an aluminium powder, and the step 4 mass concentration is that 50%～90% sodium hydroxide solution leaches blank 2～3h.
8, the method for preparing gradient porous material according to claim 5 is characterized in that pore-creating agent is an iron powder, and the step 4 mass concentration is that 30%～70% hydrochloric acid soln leaches blank 2～3h.
9, the method for preparing gradient porous material according to claim 5 is characterized in that pore-creating agent is a copper powder, and the step 4 mass concentration is that 3% hydrochloric acid and mass concentration are that the mixing solutions of 1% nitric acid leaches blank 2～3h.
10, the method for preparing gradient porous material according to claim 5 is characterized in that pore-creating agent is carbon dust or coal dust, and step 4 is removed pore-creating agent in the blank with combustion method.
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