CN102212729A - TiB2-TiC-TiN-NiAl porous composite material with combined hole pattern and preparation method thereof - Google Patents
TiB2-TiC-TiN-NiAl porous composite material with combined hole pattern and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a TiB2-TiC-TiN-NiAl porous composite material with a combined hole pattern and a preparation method thereof. In the preparation method, Ti powder, B4C powder, Ni powder and Al powder are taken as raw materials, and meanwhile nitrogen in air also participates in reaction; and the raw material powder and the nitrogen are subjected to self-propagating high-temperature synthesis reaction so as to synthesize the porous composite material the framework of which consists of granular TiC, TiB2 and TiN as well as NiAl distributed among the particles, wherein open pores and closed pores form a combined hole structure. The porous composite material can be widely applied to filtering and separating components, catalyst carriers and the like in the fields of metallurgy, chemical industry, environmental conservation, energy sources, biology, food, medicines and the like.
Description
Technical field
The present invention relates to a kind of porous material and preparation technology thereof, especially a kind of TiB
2-TiC-TiN-NiAl compound porous material and preparation method thereof belongs to the synthetic and manufacture field of material.
Background technology
TiC, TiB
2, TiN, Ti (C, N) be all the non-oxide ceramic material of excellent property, have the fusing point height, hardness is big, corrosion-resistant and the characteristics of good in oxidation resistance, obtained using widely in many fields such as machinery, chemical industry, automobile making and aerospace, Chang Zuowei hard tool material, abrasive material, alloy addition, wear parts and noble electrode material and high temperature electrical material are used.Chinese patent CN101555137 (application number 200910027763.4) discloses a kind of with TiH
2, Si, graphite and B
4C is a raw material, by (the TiB of gas-protecting sintering preparation
2+ TiC)/Ti
3SiC
2Diphase ceramic material and preparation method thereof.Chinese patent CN101941843A (application number 201010253986.5) discloses a kind of with TiB
2-TiC, WC and Ni are raw material, prepare TiB by ball milling and high temperature sintering
2-TiC-WC superhard material and preparation method thereof.Chinese invention patent CN101161374 (application number 200710056355.2) discloses a kind of with Cr, Ti and B
4C is a raw material, brings out the combustion synthesis reaction of pressed compact by casting hot metal molten steel, and original position forms TiB
2Mix ceramic particle reinforced metal base composites and preparation method thereof with the TiC complex phase.It is raw material with Ti, B and BN that Chinese patent CN101445370 (application number 200810209771) discloses a kind of, prepares TiN/TiB by ball milling, hot pressed sintering
2The matrix material its preparation method.Chinese patent CN101139204 (application number 200710044847.X) discloses a kind of with Ti, BN and Si
3N
4Powder is a raw material, prepares TiN-TiB by reaction in
2-Ti
5Si
3(perhaps TiSi
2) the ceramic base composite diphase material and preparation method thereof.Patent ZL90103830.X invention is a kind of with TiH
2, Ti, BN, B
4C, C are raw material, make Ti (C by the hot pressed sintering reaction
xN
y) and Ti
BThe method of 2 matrix materials.Chinese patent CN101787476A has announced a kind of with Ni, Ti, B
4C and BN are raw material, synthesize with pressure auxiliary phase bonded method by burning and have prepared TiC
xN
y-TiB
2/ Ni metal-ceramic composite material.U.S. Pat No.4492764 has invented employing Ti (C
αN
β) and TiB
2Powder stock by the high-temperature atmosphere sintering, has prepared the Ti (C with higher density, bonding strength and high rigidity
αN
β)-TiB
2Composite ceramic material and technology thereof.But do not see relevant for TiC-TiB
2-TiN matrix material and invention or the report of making the method aspect of porous material about wherein a kind of material or two or more matrix materials.
The Ni-Al series intermetallic compound has that density is low, high temperature specific tenacity and advantages such as specific rigidity height, oxidation-resistance and corrosion resistance and good, have the thermostability of obdurability, electrical and thermal conductivity and the pottery of metal concurrently, of many uses aspect high-temperature structural material and coating.Inter-metallic compound material is prepared into porous material, can further widens its Application Areas, make full use of its performance advantage.It is raw material with Ni, Al, Co, Fe, Cu and NiAl powder that Chinese patent publication number CN1584083 discloses a kind of, adds the method that thermal booster reaction prepares the Ni-Al intermetallic compound porous material by energising.Chinese patent publication number CN101301630B discloses a kind of with Ni, Al, TiH
2And Al
2O
3Powder is a raw material, adds the ethanol wet-mixed, is matrix by the preparation of self propagating high temperature building-up reactions with NiAl, NiTi, TiAl intermetallic compound, TiO
2And Al
2O
3The composite porous method that disperse distributes.But the porosity of porous material is limited, and also not seeing has Ni-Al series intermetallic compound material and TiC, TiB
2, stupalith such as TiN forms the composite study report.
Summary of the invention
The TiC-TiN-TiB that provides a kind of performance good is provided the object of the invention
2-NiAl matrix material is also made the method for the porous material of special construction with it, with further performance TiC, TiB
2, stupalith such as TiN and Ni-Al series intermetallic compound material performance advantage, enlarge of the application of these materials at aspects such as filtration, separation, catalysis.
Porous material of the present invention is with Ti powder, B
4C powder, Ni powder and Al powder are raw material, and airborne nitrogen also participates in reaction simultaneously, raw material powder and nitrogen generation self propagating high temperature building-up reactions:
Ti+B
4C+Ni+Al+N
2→TiC+TiB
2+TiN+NiAl+Q......①
Generate product TiC, TiB
2, TiN, NiAl, promptly in air by the synthetic skeleton of solid state reaction by granular TiC, TiB
2, TiN and be distributed in composite porous that NiAl between the particle forms, inside has vesicular structure, hole is the unitized construction of perforate and closed pore, porosity is 38.2%~48.6%, perforate aperture 80~200 μ m, closed pore aperture 50~80 μ m, closed pore is distributed in the skeleton of perforate, closed pore wall thickness 4~8 μ m; Whole closed pore wall is the structural form that coarse particle is closely piled up, and has high ultimate compression strength, and compressive strength at room temperature reaches 31.2~46.2Mpa.
The present invention controls blank density by changing proportioning, can obtain the porous TiC-TiB of different porosities, intensity
2-TiN-NiAl matrix material, this porous material can be widely used in this porous material can be widely used in filtration, separating component and support of the catalyst etc. in metallurgy, chemical industry, environmental protection, the energy, biology, food, the medicine and other fields.
Porous TiB of the present invention
2-TiC-TiN-NiAl matrix material is prepared by following method:
The first step: powder is prepared
Raw material adopts titanium valve (Ti), the norbide (B of commercial powder shape
4C), nickel powder (Ni) and aluminium powder (Al),, norbide (B wherein
4C), nickel powder (Ni) granularity is 200 orders, titanium valve (Ti), aluminium powder (Al) granularity are 100 orders.
Second step: reaction mass configuration
At first respectively with reaction mass Ti and B
4C becomes (4Ti+B according to 4: 1 proportionings of mol ratio
4C) powder, reaction mass Ni and Al become (Ni+Al) powder according to 1: 1 proportioning of mol ratio; And then with (the 4Ti+B of above-mentioned acquisition
4C) powder and (Ni+Al) powder are according to (4Ti+B
4C): (Ni+Al)=(40~70): the part by weight of (30~60) is made into reaction mass.
The 3rd step: base
Make cylindrical green compact with colding pressing after second step, the reaction mass that configures mixed;
Three-dimensional mixer dry mixed 6-8h is generally adopted in the mixing of above-mentioned reaction mass;
The general Φ 50mm of the diameter of above-mentioned cylindrical green compact, height are generally 100mm, and the pressure during base is generally 50~65Mpa.
The 4th step: composite porous is synthetic
With the preheating of sample pressed compact, obtain porous TiC-TiN-TiB by the self propagating high temperature building-up reactions
2-NiAl matrix material, this composite porous hole are the unitized constructions of perforate and closed pore, and porosity is 38.2%~48.6%, perforate aperture 80~200 aperture μ m, closed pore aperture 50~80 μ m.Closed pore is distributed in the skeleton of perforate, wall thickness 4~8 μ m, and compressive strength at room temperature reaches 31.2~46.2Mpa.
Above-mentioned porosity and compressive strength at room temperature detect respectively according to standard GB/T1966-1996 and GB/T1964-1996.
The said sample pressed compact generally adopts 300 ℃ of preheatings of process furnace 1 hour.
The present invention can prepare the porous TiC-TiN-TiB of different porosities, intensity by the content of adjusting base pressure, (Ni+Al)
2-NiAl matrix material.The sample pressed compact is put into process furnace, 300 ℃ of preheatings of temperature 1 hour.
The national standard that above-mentioned porosity and compressive strength at room temperature detect foundation is respectively GB/T1966-1996, GB/T1964-1996.
Adopt above-mentioned technical scheme, the present invention has the following advantages:
(1) technology is simple, and is with low cost, need not additionally to add pore-forming material, toughener, and reaction process is utilized Ti+B
4C+Ni+Al+N
2→ TiC+TiB
2+ TiN+NiAl+Q system self heat release makes TiC, TiN, TiB
2With NiAl mutually generation and acquisition one step of porous material finish, and in air, under lower temperature, carry out, reduced porous TiC-TiN-TiB
2The manufacturing cost of-NiAl matrix material.
(2) porous TiB
2The hole of-TiC-TiN-NiAl matrix material is the unitized construction of perforate and closed pore, and porosity is 38.2%~48.6%, perforate aperture 80~200 aperture μ m, closed pore aperture 50~80 μ m.Closed pore is distributed in the skeleton of perforate, wall thickness 4~8 μ m.
(3) composite porous skeleton microtexture is by the bonding TiC of NiAl, TiN, TiB
2Granulometric composition, whole closed pore wall is the structural form that coarse particle is closely piled up, and has high ultimate compression strength, compressive strength at room temperature reaches 31.2~46.2Mpa.
(4) by regulating base pressure and content (Ni+Al), can prepare the porous TiB of different porosities and ultimate compression strength
2-TiC-TiN-NiAl matrix material.This porous material can be widely used in filtration, separating component and the support of the catalyst etc. in metallurgy, chemical industry, environmental protection, the energy, biology, food, the medicine and other fields.
Description of drawings
Fig. 1 is porous TiB of the present invention
2The X-ray diffraction material phase analysis collection of illustrative plates of-TiC-TiN-NiAl matrix material, wherein (Ni+Al) content is 30wt%;
Fig. 2 is porous TiB of the present invention
2The X-ray diffraction material phase analysis collection of illustrative plates of-TiC-TiN-NiAl matrix material, wherein (Ni+Al) content is 50wt%;
Fig. 3 is porous TiB of the present invention
2-TiC-TiN-NiAl matrix material hole microscopic appearance figure, wherein hole is the unitized construction of perforate and closed pore;
Fig. 4 is the microscopic appearance figure of porous TiC-TiN-TiB2-NiAl matrix material closed pore of the present invention
Embodiment
Porous TiC-TiB of the present invention is described below with reference to the accompanying drawings
2The thing phase composite of-TiN-NiAl matrix material and microtexture characteristics.
By Fig. 1, Fig. 2 as can be seen, porous TiB of the present invention
2The thing phase composite of-TiC-TiN-NiAl matrix material is TiC, TiN, TiB
2With NiAl four mutually.As seen from Figure 3, the hole of porous material is the unitized construction of perforate and closed pore, perforate aperture 80~200 aperture μ m, and closed pore aperture 50~80 μ m, closed pore is distributed on the skeleton of perforate, wall thickness 4~8 μ m.As seen from Figure 4, closed pore is distributed on the skeleton of perforate, wall thickness 4~8 μ m, and hole wall is distributed with tiny TiC, TiN and TiB
2Particle, NiAl is distributed in TiC, TiN and TiB mutually as bonding
2Between the particle, whole closed pore wall is the structural form that coarse particle is closely piled up, and improves the intensity of porous material.
Embodiment 1
The first step: powder is prepared
Get commercial powder shape titanium valve (Ti), norbide (B
4C), nickel powder (Ni) and aluminium powder (Al), wherein norbide (B
4C), nickel powder (Ni) granularity is 200 orders, titanium valve (Ti), aluminium powder (Al) granularity are 100 orders.
Second step: the Ti+B
4The C configuration
With reaction mass Ti powder and B
4The C powder is labeled as (4Ti+B according to 4: 1 proportionings of mol ratio
4C), prepare standby.
The 3rd step: Ni+Al configuration
With reaction mass Ni powder and 1: 1 in molar ratio proportioning of Al powder, be labeled as (Ni+Al); In reaction system of the present invention, Ni and Al be reagent be again binding agent.
The 4th step: reaction mass configuration
(4Ti+B with above-mentioned acquisition
4C) powder and (Ni+Al) powder are according to (4Ti+B
4C): (Ni+Al)=70: 30 part by weight is made into reaction mass, in this reaction mass, and (4Ti+B
4C) with (Ni+Al) all as reagent.
The 5th step: powder mixes
Behind step 4 weighing reaction mass, adopt three-dimensional mixer dry mixed 6~8h, the powder that is uniformly mixed.
The 6th step: base
The powder that mixes packed into is cold-pressed into cylindrical green compact in the steel die, and diameter of phi 50mm, high 100mm, base pressure are 60Mpa.
The 7th step: preheating
The sample pressed compact put into 300 ℃ process furnace preheating 1 hour.
The 8th step: composite porous synthetic
The tungsten filament of will switching on places the sample top, causes the reaction between powder, and the self propagating high temperature building-up reactions takes place, and reaction finishes after the sample cooling, promptly obtain NiAl as bonding phase, be distributed in TiC, TiB
2, the porous TiB between the TiN particle
2-TiC-TiN-NiAl matrix material.The sample correlated performance is as shown in table 1.
The national standard of porosity of porous material and compressive strength at room temperature detection foundation is respectively GB/T1966-1996, GB/T1964-1996 in the table 1.
Table 1.
Proportioning raw materials (4Ti+B 4C)∶(Ni+Al)(wt.%) | 70∶30 |
Make bad pressure (Mpa) | 60 |
Product thing phase relative content order | TiB 2>NiAl>TiC>TiN |
Porosity (%) | 48.6 |
Ultimate compression strength (Mpa) | 31.2 |
With the difference of embodiment 1 be that (Ni+Al) content is the 40wt.% of reaction system total mass, base pressure is 65Mpa.The sample correlated performance is as shown in table 2.
Table 2
Proportioning raw materials (4Ti+B 4C)∶(Ni+Al)(wt.%) | 60∶40 |
Base pressure (Mpa) | 65 |
Product thing phase relative content order | TiB 2>NiAl>TiN>TiC |
Porosity (%) | 41.6 |
Ultimate compression strength (Mpa) | 37.5 |
Embodiment 3
With the difference of embodiment 2 be that (Ni+Al) content is the 46.3wt.% of system total mass, base pressure is 50Mpa.The sample correlated performance is as shown in table 3.
Table 3
Proportioning raw materials (4Ti+B 4C)∶(Ni+Al)(wt.%) | 53.7∶46.3 |
Base pressure (Mpa) | 50 |
Product thing phase relative content order | NiAl>TiB 2>TiN>TiC |
Porosity (%) | 43.5 |
Ultimate compression strength (Mpa) | 41.3 |
Embodiment 4
With the difference of embodiment 3 be that (Ni+Al) content is the 56.4wt% of system total mass, the sample correlated performance is as shown in table 4.
Table 4
Proportioning raw materials (4Ti+B 4C)∶(Ni+Al)(wt.%) | 43.6∶56.4 |
Base pressure (Mpa) | 50 |
Product thing phase relative content order | NiAl>TiB 2>TiN>TiC |
Porosity (%) | 39.5 |
Ultimate compression strength (Mpa) | 44.7 |
Embodiment 5
With the difference of embodiment 4 be that (Ni+Al) content is the 60wt% of system total mass, base pressure is 65Mpa.The sample correlated performance is as shown in table 5.
Table 5
Proportioning raw materials (4Ti+B 4C)∶(Ni+Al)(wt.%) | 40∶60 |
Base pressure (Mpa) | 65 |
Product thing phase relative content order | NiAl>TiB 2>TiN>TiC |
Porosity (%) | 38.2 |
Ultimate compression strength (Mpa) | 46.2 |
Claims (9)
1. TiB with combined pass
2-TiC-TiN-NiAl is composite porous, it is characterized in that, it is with Ti powder, B
4C powder, Ni powder and Al powder are raw material, and airborne nitrogen also participates in reaction simultaneously, raw material powder and nitrogen generation self propagating high temperature building-up reactions, and synthetic skeleton is by granular TiC, TiB
2, TiN and be distributed in composite porous that NiAl between the particle forms, inside has vesicular structure, hole is the unitized construction of perforate and closed pore, porosity is 38.2%~48.6%, compressive strength at room temperature reaches 31.2~46.2Mpa, perforate aperture 80~200 μ m, closed pore aperture 50~80 μ m, closed pore is distributed in the skeleton of perforate, closed pore wall thickness 4~8 μ m; Reaction formula is:
Ti+B
4C+Ni+Al+N
2→TiC+TiB
2+TiN+NiAl+Q......。
2. composite porous preparation method as claimed in claim 1 is characterized in that step is as follows:
The first step: powder is prepared
Raw material adopts titanium valve, norbide, nickel powder and the aluminium powder of commercial powder shape, and wherein boron carbide powder and nickel powder granularity are 200 orders, and titanium valve and aluminum powder particle size are 100 orders;
Second step: reaction mass configuration
At first respectively with reaction mass Ti and B
4C becomes (4Ti+B according to 4: 1 proportionings of mol ratio
4C) powder, reaction mass Ni and Al become (Ni+Al) powder according to 1: 1 proportioning of mol ratio; And then with (the 4Ti+B of above-mentioned acquisition
4C) powder and (Ni+Al) powder are according to (4Ti+B
4C): (Ni+Al)=(40~70): the part by weight of (30~60) is made into reaction mass.
The 3rd step: base
The reaction mass that second step was configured adopts three-dimensional mixer dry method uniform mixing, colds pressing then and makes cylindrical green compact;
The 4th step: composite porous is synthetic
With the preheating of sample pressed compact, obtain porous TiC-TiN-TiB by the self propagating high temperature building-up reactions
2-NiAl matrix material, this composite porous hole is the unitized construction of perforate and closed pore, porosity is 38.2%~48.6%, perforate aperture 80~200 aperture μ m, closed pore aperture 50~80 μ m, closed pore is distributed in the skeleton of perforate, wall thickness 4~8 μ m, and compressive strength at room temperature reaches 31.2~46.2Mpa.
3. preparation method as claimed in claim 2 is characterized in that,
In the 3rd step, the mixing time of reaction mass is 6-8h; The diameter of the cylindrical green compact made of colding pressing is Φ 50mm, highly is 100mm that the pressure during base is 50~65Mpa;
In the 4th step, adopt 300 ℃ of preheatings of process furnace 1 hour during the sample pressed compact.
4. preparation method as claimed in claim 2 is characterized in that,
In second step, in reaction mass when preparation, is according to (4Ti+B
4C): (Ni+Al)=70: 30 part by weight carries out;
In the 3rd step, the pressure during base is 60Mpa;
In the 4th step, the porosity of the porous material of acquisition is 48.6%, and compressive strength at room temperature is 31.2Mpa.
5. preparation method as claimed in claim 2 is characterized in that,
In second step, in reaction mass when preparation, is according to (4Ti+B
4C): (Ni+Al)=60: 40 part by weight carries out;
In the 3rd step, the pressure during base is 65Mpa;
In the 4th step, the porosity of the porous material of acquisition is 41.6%, and compressive strength at room temperature is 37.5Mpa.
6. preparation method as claimed in claim 2 is characterized in that,
In second step, in reaction mass when preparation, is according to (4Ti+B
4C): (Ni+Al)=53.7: 46.3 part by weight carries out;
In the 3rd step, the pressure during base is 50Mpa;
In the 4th step, the porosity of the porous material of acquisition is 43.5%, and compressive strength at room temperature is 41.3Mpa.
7. preparation method as claimed in claim 2 is characterized in that,
In second step, in reaction mass when preparation, is according to (4Ti+B
4C): (Ni+Al)=43.6: 56.4 part by weight carries out;
In the 3rd step, the pressure during base is 50Mpa;
In the 4th step, the porosity of the porous material of acquisition is 39.5%, and compressive strength at room temperature is 44.7Mpa.
8. preparation method as claimed in claim 2 is characterized in that,
In second step, in reaction mass when preparation, is according to (4Ti+B
4C): (Ni+Al)=40: 60 part by weight carries out;
In the 3rd step, the pressure during base is 65Mpa;
In the 4th step, the porosity of the porous material of acquisition is 38.2%, and compressive strength at room temperature is 46.2Mpa.
9. the application in filtration, separating component and the support of the catalyst of porous material as claimed in claim 1 in metallurgy, chemical industry, environmental protection, the energy, biology, food, field of medicaments.
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CN109136607A (en) * | 2017-06-27 | 2019-01-04 | 中国科学院上海硅酸盐研究所 | A kind of self-propagating synthesis of aluminum-base composite powder and its application |
CN110372346A (en) * | 2019-07-18 | 2019-10-25 | 马桂明 | A kind of high temperature resistant, lightweight, efficient NEW TYPE OF COMPOSITE heat-barrier material |
CN114289713A (en) * | 2021-12-14 | 2022-04-08 | 北京科技大学 | Method for preparing fully-compact TiN/Cu material with golden surface by two-step sintering |
CN115583839A (en) * | 2022-11-09 | 2023-01-10 | 山东科技大学 | Three-dimensional integrated double-layer porous ceramic material and preparation method and application thereof |
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CN114289713B (en) * | 2021-12-14 | 2023-01-10 | 北京科技大学 | Method for preparing fully-compact TiN/Cu material with golden surface by two-step sintering |
CN115583839A (en) * | 2022-11-09 | 2023-01-10 | 山东科技大学 | Three-dimensional integrated double-layer porous ceramic material and preparation method and application thereof |
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