CN101967578B - Preparation method of gradient pore porous high-niobium titanium-aluminum alloy - Google Patents

Preparation method of gradient pore porous high-niobium titanium-aluminum alloy Download PDF

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CN101967578B
CN101967578B CN2010105338482A CN201010533848A CN101967578B CN 101967578 B CN101967578 B CN 101967578B CN 2010105338482 A CN2010105338482 A CN 2010105338482A CN 201010533848 A CN201010533848 A CN 201010533848A CN 101967578 B CN101967578 B CN 101967578B
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niobium
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polyoxyethylene glycol
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CN101967578A (en
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王辉
吕昭平
杨帆
林均品
贺跃辉
陈国良
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University of Science and Technology Beijing USTB
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Abstract

The invention belongs to the field of porous metal materials and particularly relates to a preparation method of a gradient pore porous high-niobium titanium-aluminum alloy. The method comprises the following steps of: mixing pure titanium powder, pure aluminum powder and pure niobium powder and sintering the mixture by a Kerkendill effect reaction pore-forming method and a pore-forming agent physical pore-forming method; adding a plurality of ingredients; compacting the ingredients which contain different pore-forming agents and have different content into single blanks respectively; rolling a plurality of single blanks with different pore-forming agent content into the total blank; and performing a vacuum drying degreasing pore-foaming and high-temperature sintering reaction pore-forming process so as to finally obtain a porous high-niobium titanium-aluminum alloy material with a gradient hole structural characteristic and adjustable porosity. The material has gradient porosity change, optionally-adjustable pore structural characteristic, adjustable stress cross section, light weight, high specific stiffness and high heat insulation performance; simultaneously, the material has high material design flexibility and can be widely applied to the industrial fields of high temperature heat insulation, filtering separation, catalysis and the like.

Description

The preparation method of a kind of gradient hole porous high niobium containing titanium aluminium alloy
Technical field
The present invention relates to the porous intermetallic compound material, disclose the preparation method of a kind of gradient hole porous high niobium containing titanium aluminium alloy.
Background technology
Intermatallic Ti-Al compound is owing to the acting in conjunction of metallic bond between atom and covalent linkage; Thereby have performances such as lightweight, HS, corrosion-resistant and high temperature oxidation resisting; In the titanium aluminium element, add resistance to elevated temperatures and the strength that the formed high-Nb Ti-Al intermetallic compound of a certain amount of niobium element can obviously improve the titanium aluminum, have a wide range of applications at industrial circles such as high temperature insulating, filtration catalytic.Because Kerkendill effect; Adopt the element powders metallurgical method can obtain the porous high niobium containing titanium aluminium alloy; Formed micron order aperture hole has not only further improved the modulus and the lightweight characteristic of high niobium containing titanium aluminium alloy, and thermal conductivity further descends simultaneously, thereby has improved the heat-proof quality of material.In the method for existing bibliographical information; Adopt powder metallurgic method to prepare the porous high niobium containing titanium aluminium alloy; Adjust the pore structure of porous high niobium containing titanium aluminium alloy through control element powder ratio, powder diameter and processing parameters such as becoming base pressure, sintering temperature, temperature rise rate and soaking time; Obtain having the porous high niobium containing titanium aluminium alloy of even porosity; This material porosity is made up of reaction pore-creating porosity and mesopore porosity two portions, porosity 20%～61%, and wherein the formed porosity of mesopore is 2～12%.
The graded pore structure of porous high niobium containing titanium aluminium alloy has the engineering Practical significance; Graded pore structure porous high niobium containing titanium aluminium alloy weight is lighter; Can adapt to load change better and be designed to etc./varying stress cross section structure material; Improve the designability of porous high-Nb Ti-Al, helped further improving the heat-proof quality of material; Simultaneously have higher specific rigidity and permeability as structured material; When being applied to catalysis or filtration condition, the hole flushing of being more convenient for of the filter sieve of graded pore structure, catalytic efficiency (is higher.Present reported literature adopts magnetron sputtering or spraying method to apply one deck titanium aluminium powder in porous high-Nb Ti-Al billet surface, obtains graded pore structure through vacuum sintering then; The perhaps infiltration aluminium lamination etc. on porous high-Nb Ti-Al surface, the cooling back forms the porous high-Nb Ti-Al material with gradient characteristics.The prepared POROUS TITANIUM aluminum of these methods can only form graded pore structure on local or surface; Can't form the graded pore structure that distributes than big scale in the whole cross section of porous high-Nb Ti-Al material, graded is greatly different simultaneously, and the small-bore layer thickness is thin; The pore structure adjustment is also very difficult; Preparation cost is high, and the high porosity that is obtained is not more than 61%, and the preparation method is difficult to obtain big size porous high niobium containing titanium aluminium alloy.
Summary of the invention
To the problem of existing preparation gradient hole porous high niobium containing titanium aluminium alloy, it is simple to the present invention proposes a kind of preparation technology, and cost is low, yield rate is high, and can realize the graded pore structure porous high niobium containing titanium aluminium alloy preparation method of large sizeization.
Technical scheme of the present invention is: the preparation method of a kind of gradient hole porous high niobium containing titanium aluminium alloy, and concrete steps are following:
The first step: with pure titanium valve according to massfraction be 50%-55%, pure aluminium powder according to massfraction be 30% 1 and pure niobium powder be the 10%-15% uniform mixing according to massfraction; Obtain powder 1; Wherein, The particle diameter of said titanium valve is 10-150um, and the particle diameter of said aluminium powder is 5-150um, and the particle diameter of said niobium powder is 2-25um;
Second step: respectively with NH 4HCO 3Pulverize with the polyoxyethylene glycol powder, subsequent use; Said particle diameter NH 4HCO 3With the polyoxyethylene glycol powder be 20-180um;
The 3rd step: will obtain the some parts of 1 one-tenths in powder, every part is mixed respectively that to account for massfraction be 1～51% NH 4HCO 3Powder and mixing;
The 4th step: the polyoxyethylene glycol powder is added in the mixed powder of break into portions in the above-mentioned steps, mixes; Wherein, the addition of said polyoxyethylene glycol and corresponding titanium aluminium niobium powder and NH 4HCO 3NH in the powder powder mix 4HCO 3The ratio of powder is 25: 1;
The 5th step: adopt the compression molding mode with the titanium aluminium niobium powder and the NH that add polyoxyethylene glycol 4HCO 3Powder is pressed into the laminar blank of some corresponding compositions respectively, and wherein each laminar blank is along with the minimizing of titanium aluminium niobium powder content, the corresponding increase of content of NH4HCO3 powder and polyoxyethylene glycol powder, and rolling pressure is 50～80MPa;
The 6th step: the scale according to titanium aluminium niobium powder amount laminates the secondary roll compacting of regular back successively with a plurality of laminar blank, and pressing pressure is 120～200MPa, obtains total base;
The 7th step: total base is put into vacuum drying oven be heated to 100～120 ℃, be incubated 1～2 hour and make NH 4HCO 3Take out with polyoxyethylene glycol volatilization back;
The 8th step: total base is put into the vacuum high-temperature sintering stove; Keep vacuum tightness to be not less than 10-3Pa; Be heated to 1400 ℃, wherein be incubated 1 hour, 2 hours and 3 hours at 120 ℃, 620 ℃ and 1400 ℃ respectively, take out behind the furnace cooling and promptly obtain gradient hole porous alloy material of high niobium-titanium-aluminum.
The invention has the beneficial effects as follows:
1. the present invention can obtain high porosity (>=72%) porous high niobium containing titanium aluminium alloy;
2. the graded pore structure porous high niobium containing titanium aluminium alloy mesoporosity rate graded and the porosity of gained of the present invention can freely be adjusted;
3. the aperture of graded pore structure porous high niobium containing titanium aluminium alloy can be through changing the NH that adds among the present invention 4HCO 3Powder is adjusted with gathering second diester powder diameter;
4. the present invention is in process of vacuum drying, NH 4HCO 3Powder with gather second diester powder and volatilize at a lower temperature, residual through no physics behind the high temperature sintering, thereby to the not influence of graded pore structure porous high niobium containing titanium aluminium alloy composition;
5. in the graded pore structure porous high niobium containing titanium aluminium alloy of gained of the present invention during graded, big small-bore is more or less the same, and only limits to porosity generation graded;
6. preparation technology of the present invention is simple, and cost is low, yield rate is high, and can realize large sizeization.
Description of drawings:
Fig. 1 is a low porosity porous high-Nb Ti-Al cross section microstructure synoptic diagram.
Fig. 2 is a high porosity porous high-Nb Ti-Al cross section microstructure synoptic diagram.
Embodiment
Below through examples of implementation technical scheme of the present invention is further specified.
Embodiment 1:
The first step: respectively according to 50% (massfraction, down together), 40% and 10% ratio is carried out uniform mixing with titanium, aluminium and niobium element powder, and the particle diameter of titanium valve is 50um, and the particle diameter of aluminium powder is 50um, and the particle diameter of niobium powder is 12um;
Second step: adopt the compression molding mode with 5 parts of titanium aluminium niobium powder and NH of mixing 4HCO 3Process 5 laminar blank respectively with polyoxyethylene glycol, pressing pressure 50MPa, thickness are 1.5mm, wherein NH 4HCO 3Content be respectively 46%, 40%, 31%, 25% and 11%, polyoxyethylene glycol and NH 4HCO 3Ratio be 25: 1;
The 3rd step: the scale according to titanium aluminium niobium powder amount laminates the secondary roll compacting of regular back successively with 5 laminar blank, and pressing pressure is 120MPa, obtains total base;
The 4th step: total base is put into vacuum drying oven be heated to 100 ℃, be incubated 1.5 hours and make NH 4HCO 3Take out with polyoxyethylene glycol volatilization back;
The 5th step: total base is put into the vacuum high-temperature sintering stove; Keep vacuum tightness to be not less than 10Pa; Be heated to 1400 ℃, wherein be incubated 1 hour, 2 hours and 3 hours at 120 ℃, 620 ℃ and 1400 ℃ respectively, take out behind the furnace cooling and promptly obtain gradient hole porous high niobium containing titanium aluminium alloy.
Embodiment 2:
The first step: titanium, aluminium and niobium element powder are carried out uniform mixing according to 55%, 35% and 10% ratio respectively, and the particle diameter of titanium valve is 100um, and the particle diameter of aluminium powder is 100um, and the particle diameter of niobium powder is 12um;
Second step: adopt the compression molding mode with 5 parts of titanium aluminium niobium powder and NH of mixing 4HCO 3Process 5 laminar blank respectively with polyoxyethylene glycol, pressing pressure 50MPa, thickness are 2mm, wherein NH 4HCO 3Content be respectively 51%, 41%, 31%, 21%, 11% and 1%, polyoxyethylene glycol and NH 4HCO 3Ratio be 25: 1;
The 3rd step: the scale according to titanium aluminium niobium powder amount laminates the secondary roll compacting of regular back successively with 6 laminar blank, and pressing pressure is 180MPa, obtains total base;
The 4th step: total base is put into vacuum drying oven be heated to 110 ℃, be incubated 2 hours and make NH 4HCO 3Take out with polyoxyethylene glycol volatilization back;
The 5th step: total base is put into the vacuum high-temperature sintering stove; Keep vacuum tightness to be not less than 6Pa; Be heated to 1400 ℃, wherein be incubated 1 hour, 2 hours and 3 hours at 120 ℃, 620 ℃ and 1400 ℃ respectively, take out behind the furnace cooling and promptly obtain gradient hole porous high niobium containing titanium aluminium alloy.
Embodiment 3:
The first step: respectively according to 55% (massfraction, down together), 35% and 10% ratio is carried out uniform mixing with titanium, aluminium and niobium element powder, and the particle diameter of titanium valve is 10um, and the particle diameter of aluminium powder is 5um, and the particle diameter of niobium powder is 2um;
Second step: adopt the compression molding mode with 3 parts of titanium aluminium niobium powder and NH of mixing 4HCO 3Process 3 laminar blank respectively with polyoxyethylene glycol, pressing pressure 50MPa, thickness are 2.5mm, wherein NH 4HCO 3Content be respectively 51%, 31% and 11%, polyoxyethylene glycol and NH 4HCO 3Ratio be 25: 1;
The 3rd step: the scale according to titanium aluminium niobium powder amount laminates the secondary roll compacting of regular back successively with 3 laminar blank, and pressing pressure is 200MPa, obtains total base;
The 4th step: total base is put into vacuum drying oven be heated to 120 ℃, be incubated 2 hours and make NH 4HCO 3Take out with polyoxyethylene glycol volatilization back;
The 5th step: total base is put into the vacuum high-temperature sintering stove; Keep vacuum tightness to be not less than 3Pa; Be heated to 1400 ℃, wherein be incubated 1 hour, 2 hours and 3 hours at 120 ℃, 620 ℃ and 1400 ℃ respectively, take out behind the furnace cooling and promptly obtain gradient hole porous high niobium containing titanium aluminium alloy.
Embodiment 4:
The first step: with particle diameter is that the niobium powder that the titanium valve of 150um, aluminium powder that particle diameter is 150um and particle diameter are 25um compares uniform mixing according to 52%, 38% and 10% quality respectively;
Second step: adopt the compression molding mode with 7 parts of titanium aluminium niobium powder and NH of mixing the metal-powder that mixes 4HCO 3Process 7 laminar blank respectively with polyoxyethylene glycol, pressing pressure 60MPa, thickness are 1mm, wherein NH 4HCO 3Content be respectively 51%, 45%, 36%, 31%, 24%, 19% and 11%, polyoxyethylene glycol and NH 4HCO 3Ratio be 25: 1;
The 3rd step: the scale according to titanium aluminium niobium powder amount laminates the secondary roll compacting of regular back successively with 7 laminar blank, and pressing pressure is 180MPa, obtains total base;
The 4th step: total base is put into vacuum drying oven be heated to 120 ℃, be incubated 2 hours and make NH 4HCO 3Take out with polyoxyethylene glycol volatilization back;
The 5th step: total base is put into the vacuum high-temperature sintering stove; Keep vacuum tightness to be not less than 10-3Pa; Be heated to 1400 ℃, wherein be incubated 1 hour, 2 hours and 3 hours at 120 ℃, 620 ℃ and 1400 ℃ respectively, take out behind the furnace cooling and promptly obtain gradient hole porous high niobium containing titanium aluminium alloy.

Claims (1)

1. the preparation method of a gradient hole porous high niobium containing titanium aluminium alloy is characterized in that concrete steps are following:
The first step: is that 50%-55%, pure aluminium powder are that 30%-40% and pure niobium powder are the 10%-15% uniform mixing according to massfraction according to massfraction with pure titanium valve according to massfraction; Obtain powder 1; Wherein, The particle diameter of said titanium valve is 10-150 μ m, and the particle diameter of said aluminium powder is 5-150 μ m, and the particle diameter of said niobium powder is 2-25 μ m;
Second step: respectively with NH 4HCO 3Pulverize with the polyoxyethylene glycol powder, subsequent use; Said NH 4HCO 3With the polyoxyethylene glycol powder directly be 20-180 μ m;
The 3rd step: will obtain powder 1 break into portions, every part is mixed respectively that to account for massfraction be 1～51% NH 4HCO 3Powder and mixing;
The 4th step: the polyoxyethylene glycol powder is added in the mixed powder of break into portions in the above-mentioned steps, mixes; Wherein, the addition of said polyoxyethylene glycol and corresponding titanium aluminium niobium powder and NH 4HCO 3NH in the powder powder mix 4HCO 3The ratio of powder is 25: 1;
The 5th step: adopt the compression molding mode with the titanium aluminium niobium powder and the NH that add polyoxyethylene glycol 4HCO 3Powder is rolled into the laminar blank of some corresponding compositions respectively, and wherein each laminar blank is along with the minimizing of titanium aluminium niobium powder content, NH 4HCO 3The corresponding increase of the content of powder and polyoxyethylene glycol powder, rolling pressure are 50～80MPa;
The 6th step: the scale according to titanium aluminium niobium powder amount laminates the secondary roll compacting of regular back successively with a plurality of laminar blank, and rolling pressure is 120～200MPa, obtains total base;
The 7th step: total base is put into vacuum drying oven be heated to 100～120 ℃, be incubated 1～2 hour and make NH 4HCO 3Take out with polyoxyethylene glycol volatilization back;
The 8th step: total base is put into the vacuum high-temperature sintering stove; Maintenance vacuum tightness is 10-3Pa; Be heated to 1400 ℃, wherein be incubated 1 hour, 2 hours and 3 hours at 120 ℃, 620 ℃ and 1400 ℃ respectively, take out behind the furnace cooling and promptly obtain gradient hole porous alloy material of high niobium-titanium-aluminum.
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