CN107675021B - A kind of intermetallic compound titanium-silicon molybdenum porous material and preparation method thereof - Google Patents
A kind of intermetallic compound titanium-silicon molybdenum porous material and preparation method thereof Download PDFInfo
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Abstract
A kind of intermetallic compound titanium-silicon molybdenum porous material and preparation method thereof, belongs to porous metal material technical field.Titanium valve, silicon powder and molybdenum powder are mixed according to certain mass ratio, carry out ball milling；Then the mixed-powder after pore creating material and ball milling is sufficiently mixed uniformly, is pressed into green body；Green body is heated, pore creating material is made to decompose and remove；Finally green body is put into vacuum sintering furnace, carries out vacuum-sintering, intermetallic compound titanium-silicon molybdenum porous material is made.The preparation method simple process, it is low in cost, there is grading-hole configuration characteristic with intermetallic compound titanium-silicon molybdenum porous material prepared by the method, controlled porosity, high lightweight, intensity, fusing point height and good resistance to high temperature oxidation and corrosion resistance are had both, can be applied to the fields such as sound absorption, the filtering under the unfavorable conditions such as high temperature and corrosion.
Description
Technical field
The invention belongs to porous metal material technical fields, more particularly to a kind of porous material of intermetallic compound titanium-silicon molybdenum
Material and preparation method thereof.
Background technique
Porous material is a kind of material comprising a large amount of holes, has lightweight, high-specific surface area, high permeability and high thermal conductivity
The capillary structure of the excellent characteristics such as rate, small aperture can be used as fluid channel, have been widely used for sound absorption, heat transfer, filtering
With catalysis etc. fields.But limit of the application of porous material greatly by the characteristic of basis material and severe working environment
System.For example, porous ceramic film material brittleness is larger, processing performance is poor；The anti-oxidant and corrosion resistance of porous metal material compared with
Difference；The high temperature resistance and ageing-resistant performance of porous polymer materials are poor.Intermetallic compound have it is excellent anti-oxidant and
Corrosion resistance can use under high temperature environment, while also have preferable ageing-resistant performance and processing performance.
Metal SiClx object has both the double grading of metal and ceramics as a kind of typical intermetallic compound, has molten
The advantages that point is high, intensity is high, elasticity modulus is big, thermal conductivity is good, high temperature oxidation resistance is good, corrosion resistance is good, in aerospace, vapour
Have in the high temperature such as vehicle ternary catalyzing unit, medical treatment, sea water desalination, environmental protection, metallurgy and chemical industry, corrosive environment good
Application prospect, have become the hot issue of scientific research.The density of Ti-Si system silicide is in all refractory metal silicides
In it is very low, fusing point is high, and creep resistance is good, it is considered to be the high-temperature structural material of great potential.The high temperature of Mo-Si system silicide
Antioxygenic property is very excellent in all refractory metal silicides.The advantage of two kinds of metal silicides is integrated in one, simultaneously
The alloying of Mo and Ti can also improve the intensity and temperature-room type plasticity of material, by high temperature resistant possessed by material itself, resistance to
The performances such as burn into is anti-oxidant, and the porous structure with fluid dispersion and transmitting effect is sketched the contours of in material internal, it develops novel
Porous Ti-Si-Mo inter-metallic compound material.
The technology of preparing of porous intermetallic compound can be divided into liquid metal foaming, solid metallic sintering process, deposition
Method etc..PM technique overcomes the difficulty in refractory metal fusion-casting process, have technical maturity, pore-size distribution controllability high and
The advantages that percent opening is high, particularly useful for making porous intermetallic compound.By high-energy ball milling, powder can be refined sufficiently,
In compacting, certain gap can be remained between powder, by selecting pressing pressure appropriate, can produce hole lyriform pore.Pass through
Pore creating material is added, larger-size hole can be obtained.Kinkendal Effect refers to that the different metal of two kinds of diffusion rates is being spread
It will form defect in the process.There are Kinkendal Effect, titanium valve and molybdenum powders in Ti-Mo displaced type diffusion couple fills by ball milling particle
Divide refinement, can use Kinkendal Effect and obtain the lesser hole of size.
Summary of the invention
It is an object of the invention to porous for existing liquid metal foaming, solid metallic sintering process, sedimentation etc.
The preparation method of intermetallic compound is unable to satisfy the problem of refractory metal porous compounds preparation, invents a kind of intermetallic
Object titanium silicon molybdenum porous material, while a kind of collection high-energy ball milling-compression molding-is provided except foaming agent-vacuum non-pressure sintering combines
Preparation method.This method is easy to operate, low in cost, intermetallic compound titanium-silicon molybdenum porous material obtained have lightweight,
The features such as intensity is high, fusing point is high, resistance to high temperature oxidation and corrosion resistance are good.
Technical solution of the present invention first is that:
A kind of intermetallic compound titanium-silicon molybdenum porous material, it is characterised in that: intermetallic compound titanium-silicon molybdenum porous material
Middle Ti content is 74~80wt.%, and silicone content 8wt.%, molybdenum content is 12~18wt.%.
Technical solution of the present invention second is that:
A kind of preparation method of intermetallic compound titanium-silicon molybdenum porous material, which is characterized in that be made by the steps:
(1) high-energy ball milling mixes powder: by titanium valve, silicon powder and molybdenum powder according to 74~80wt.%Ti, 8wt.%Si and 12~18wt.%
The mass ratio of Mo mixes, and carries out ball milling in a planetary ball mill, is put into ball grinder, is placed in ball mill with certain ball milling ginseng
Gained mixed-powder after ball milling is placed in vacuum oven and dries so that tri- kinds of powder of Ti, Si and Mo sufficiently refine by number ball milling
Dry doubling crosses 200 meshes；
(2) conventional compression molding: mixed-powder prepared by step (1) is uniformly mixed with pore creating material unifor,
It is pressed into green body；
(3) it removes foaming agent: the green compact of step (2) compression moulding is put into vacuum oven, heating green compact to 110
DEG C, so that pore creating material unifor is decomposed and is removed；
(4) vacuum non-pressure sintering: the green compact of step (3) is subjected to vacuum non-pressure sintering, so that Ti, Si, Mo alloying, are obtained
Obtain intermetallic compound titanium-silicon molybdenum porous material.
The purity of the titanium valve is 99.0%, and granularity is 200~300 mesh；The purity of the silicon powder is 99.9%, and granularity is
200 mesh；The purity of the molybdenum powder is 99.0%, and granularity is 200 mesh.
The ball-milling technology of the high-energy ball milling are as follows: ratio of grinding media to material 20:1, revolving speed are 300 ~ 500r/min, ball milling total time
At least 48h, every ball milling 50min shut down 10 min.
Mixed-powder after the ball milling is placed in vacuum oven, keeps the temperature at least after being warming up to 60 ~ 80 DEG C with drying box
8 h cross 200 meshes.
The technique of the compression moulding are as follows: for the operating pressure used when compacting for 100 ~ 150 MPa, green compact is round billet.
The green compact is placed in vacuum oven before sintering, is warming up to after 110 DEG C with drying box and keeps the temperature 2 h.Pore creating material
The purity of unifor is 98.0%, and decomposition temperature is 100~110 DEG C, and pore creating material dosage is the 2wt.% of mixed-powder.
The technique of the vacuum non-pressure sintering are as follows: be evacuated to 1 × 10-1Pa, heating rate are 4 ~ 5 DEG C/min, are burnt
Knot technique is 900 DEG C × 2 h+1250 DEG C × 4 h, finally cools to room temperature with the furnace.
The beneficial effects of the present invention are:
(1) present invention innovatively proposes a kind of " high-energy ball milling-compression molding-removes foaming agent-vacuum non-pressure sintering " system
The powder metallurgical technique of standby intermetallic compound titanium-silicon molybdenum porous material.
(2) preparation method of intermetallic compound titanium-silicon molybdenum porous material provided by the invention is easy to operate, easy realization, warp
Ji property is excellent, and the intermetallic compound titanium-silicon molybdenum porous material of preparation has high lightweight, fusing point, resistance to high temperature oxidation and corrosion resistance
Can be good the features such as.
(3) present invention utilizes pore creating material and Kinkendal Effect, by adjusting at be grouped as, pressing pressure and sintering temperature
Regulation is optimized to pore structure.
(4) intermetallic compound titanium-silicon molybdenum porous material prepared by the present invention can be applied to the unfavorable item such as high temperature, corrosion
The fields such as sound absorption, filtering under part push the development of China's porous material industry.
Detailed description of the invention
Fig. 1 is the photomacrograph of intermetallic compound titanium-silicon molybdenum porous material prepared by the present invention；
Fig. 2 is the scanning electron microscope diagram of intermetallic compound titanium-silicon molybdenum porous material prepared by the present invention；
Fig. 3 is the object phase composition XRD diffraction pattern of intermetallic compound titanium-silicon molybdenum porous material prepared by the present invention；
Fig. 4 is the graph of pore diameter distribution of intermetallic compound titanium-silicon molybdenum porous material prepared by the present invention.
Specific embodiment
Below with reference to embodiment, specific embodiments of the present invention will be described in detail, but the present invention is not limited only to implement
Example.
Embodiment 1.
A kind of intermetallic compound titanium-silicon molybdenum porous material the preparation method comprises the following steps:
Firstly, by titanium valve, silicon powder and molybdenum powder according to 80wt.%Ti(8 g), 8wt.%Si(0.8 g) and 12wt.%Mo(1.2
G) mass ratio mixing, mixed-powder is placed in a beaker and is stirred evenly；
It is placed in 500 ml ceramics ball grinders, then will be weighed simultaneously secondly, first weighing 200 g agate balls according to ratio of grinding media to material 20:1
Uniformly mixed mixed-powder is placed in ceramic ball grinder, is sealed；
Then, ball grinder is mounted on planetary ball mill, starts ball milling, ball milling parameter is set as 300 r/min, ball milling
After 50min shutdown 10 min, 48 h of ball milling, the powder in ball grinder is taken out；
Further, the mixed-powder of taking-up is placed in a vacuum drying oven 60 DEG C of 10 h of vacuum drying, then crosses 200
Mesh obtains the powder of uniform granularity；
Later, 2wt.% pore creating material (0.2 gram) unifor is added into mixed-powder to be uniformly mixed, using mold
Gained powder is pressed in the powder compact forming method unidirectionally to pressurize, and mold internal diameter isΦ30 mm, operating pressure are
150 MPa, are madeΦThe round billet of 30mm, 3 ~ 5 mm of thickness；
Then, green compact is placed in vacuum oven, is warming up to after 110 DEG C with drying box and keeps the temperature 2 h, makes pore creating material to first
Benzene sulfonyl hydrazide is decomposed completely and is removed；
Vacuum non-pressure sintering is carried out finally, gained briquetting is placed in vacuum sintering furnace, it will first be evacuated to 1 in furnace ×
10-1Pa, heating rate are 5 DEG C/min, and sintering process is 900 DEG C × 2 h+1250 DEG C × 4 h, finally cool to room with the furnace
Temperature.
Use the porosity of intermetallic compound Ti-8Si-12Mo made from above-mentioned steps for 44.18%, oxygen at 1200 DEG C
Weight gain after changing 100 hours is 0.136 gm-2。
Embodiment 2.
A kind of intermetallic compound titanium-silicon molybdenum porous material the preparation method comprises the following steps::
Firstly, by titanium valve, silicon powder and molybdenum powder according to 78wt.%Ti(7.8 g), 8wt.%Si(0.8 g) and 14wt.%Mo
The mass ratio of (1.4 g) mixes, and mixed-powder is placed in a beaker and is stirred evenly；
It is placed in 500 ml ceramics ball grinders, then will be weighed simultaneously secondly, first weighing 200 g agate balls according to ratio of grinding media to material 20:1
Uniformly mixed mixed-powder is placed in ceramic ball grinder, is sealed；
Then, ball grinder is mounted on planetary ball mill, starts ball milling, ball milling parameter is set as 500 r/min, ball milling
After 50min shutdown 10 min, 48 h of ball milling, the powder in ball grinder is taken out；
Further, the mixed-powder of taking-up is placed in a vacuum drying oven 80 DEG C of 8 h of vacuum drying, then crosses 200 mesh
Sieve, obtains the powder of uniform granularity；
Later, (0.2 gram) of 2wt.% pore creating material unifor is added into mixed-powder to be uniformly mixed, using mold
Gained powder is pressed in the powder compact forming method unidirectionally to pressurize, and mold internal diameter isΦ30 mm, operating pressure are
100 MPa, are madeΦThe round billet of 30mm, 3 ~ 5 mm of thickness；
Then, green compact is placed in vacuum oven, is warming up to after 110 DEG C with drying box and keeps the temperature 2 h, makes pore creating material to first
Benzene sulfonyl hydrazide is decomposed completely and is removed；
Vacuum non-pressure sintering is carried out finally, gained briquetting is placed in vacuum sintering furnace, it will first be evacuated to 1 in furnace ×
10-1Pa, heating rate are 4 DEG C/min, and sintering process is 900 DEG C × 2 h+1250 DEG C × 4 h, finally cool to room with the furnace
Temperature.
Use the porosity of Ti-8Si-14Mo made from above-mentioned steps for 41.94%, at 1200 DEG C after oxidation 100 hours
Weight gain is 0.111 gm-2。
Embodiment 3.
A kind of intermetallic compound titanium-silicon molybdenum porous material the preparation method comprises the following steps::
Firstly, by titanium valve, silicon powder and molybdenum powder according to 76wt.%Ti(7.6 g), 8wt.%Si(0.8 g) and 16wt.%Mo
The mass ratio of (1.6 g) mixes, and mixed-powder is placed in a beaker and is stirred evenly；
It is placed in 500 ml ceramics ball grinders, then will be weighed simultaneously secondly, first weighing 200 g agate balls according to ratio of grinding media to material 20:1
Uniformly mixed mixed-powder is placed in ceramic ball grinder, is sealed；
Then, ball grinder is mounted on planetary ball mill, starts ball milling, ball milling parameter is set as 500 r/min, ball milling
After 50min shutdown 10 min, 60 h of ball milling, the powder in ball grinder is taken out；
Further, the mixed-powder of taking-up is placed in a vacuum drying oven 80 DEG C of 8 h of vacuum drying, then crosses 200 mesh
Sieve, obtains the powder of uniform granularity；
Later, (0.2 gram) of 2wt.% pore creating material unifor is added into mixed-powder to be uniformly mixed, using mold
Gained powder is pressed in the powder compact forming method unidirectionally to pressurize, and mold internal diameter isΦ30 mm, operating pressure are
100 MPa, are madeΦThe round billet of 30mm, 3 ~ 5 mm of thickness；
Then, green compact is placed in vacuum oven, is warming up to after 110 DEG C with drying box and keeps the temperature 2 h, makes pore creating material to first
Benzene sulfonyl hydrazide is decomposed completely and is removed；
Vacuum non-pressure sintering is carried out finally, gained briquetting is placed in vacuum sintering furnace, it will first be evacuated to 1 in furnace ×
10-1Pa, heating rate are 4 DEG C/min, and sintering process is 900 DEG C × 2 h+1250 DEG C × 4 h, finally cool to room with the furnace
Temperature.
Use the porosity of Ti-8Si-16Mo made from above-mentioned steps for 40.58%, at 1200 DEG C after oxidation 100 hours
Weight gain is 0.106 gm-2。
Embodiment 4.
A kind of intermetallic compound titanium-silicon molybdenum porous material the preparation method comprises the following steps::
Firstly, by titanium valve, silicon powder and molybdenum powder according to 74wt.%Ti(7.4 g), 8wt.%Si(0.8 g) and 18wt.%Mo
The mass ratio of (1.8 g) mixes, and mixed-powder is placed in a beaker and is stirred evenly；
It is placed in 500 ml ceramics ball grinders, then will be weighed simultaneously secondly, first weighing 200 g agate balls according to ratio of grinding media to material 20:1
Uniformly mixed mixed-powder is placed in ceramic ball grinder, is sealed；
Then, ball grinder is mounted on planetary ball mill, starts ball milling, ball milling parameter is set as 500 r/min, ball milling
After 50min shutdown 10 min, 60 h of ball milling, the powder in ball grinder is taken out；
Further, the mixed-powder of taking-up is placed in a vacuum drying oven 80 DEG C of 8 h of vacuum drying, then crosses 200 mesh
Sieve, obtains the powder of uniform granularity；
Later, (0.2 gram) of 2wt.% pore creating material unifor is added into mixed-powder to be uniformly mixed, using mold
Gained powder is pressed in the powder compact forming method unidirectionally to pressurize, and mold internal diameter isΦ30 mm, operating pressure are
100 MPa, are madeΦThe round billet of 30mm, 3 ~ 5 mm of thickness；
Then, green compact is placed in vacuum oven, is warming up to after 110 DEG C with drying box and keeps the temperature 2 h, makes pore creating material to first
Benzene sulfonyl hydrazide is decomposed completely and is removed；
Vacuum non-pressure sintering is carried out finally, gained briquetting is placed in vacuum sintering furnace, it will first be evacuated to 1 in furnace ×
10-1Pa, heating rate are 4 DEG C/min, and sintering process is 900 DEG C × 2 h+1250 DEG C × 4 h, finally cool to room with the furnace
Temperature.
Use the porosity of Ti-8Si-18Mo made from above-mentioned steps for 42.54%, at 1200 DEG C after oxidation 100 hours
Weight gain is 0.092 gm-2。
Part that the present invention does not relate to is the same as those in the prior art or can be realized by using the prior art.
Claims (7)
1. a kind of intermetallic compound titanium-silicon molybdenum porous material, in intermetallic compound titanium-silicon molybdenum porous material Ti content be 74~
80wt.%, silicone content 8wt.%, molybdenum content are 12~18wt.%, and porosity is 40%~45%；It is characterized in that the metal
Between compound titanium silicon molybdenum porous material be made by the steps:
(1) high-energy ball milling mixes powder: by titanium valve, silicon powder and molybdenum powder according to 74~80wt.%Ti, 8wt.%Si and 12~18wt.%Mo
Mass ratio mixing, carries out ball milling in a planetary ball mill, is put into ball grinder, is placed in ball mill with certain ball milling parameter ball
Gained mixed-powder after ball milling is placed in vacuum oven and dries simultaneously so that tri- kinds of powder of Ti, Si and Mo sufficiently refine by mill
Cross 200 meshes；
(2) conventional compression molding: mixed-powder prepared by step (1) is uniformly mixed with pore creating material unifor, is molded
It is pressed into green body；
(3) it removes foaming agent: the green compact of step (2) compression moulding is put into vacuum oven, heat green compact to 110 DEG C, make
Pore creating material unifor is decomposed and is removed；
(4) vacuum non-pressure sintering: carrying out vacuum non-pressure sintering for the green compact of step (3), so that Ti, Si, Mo alloying, obtain gold
Compound titanium silicon molybdenum porous material between category.
2. the intermetallic compound titanium-silicon molybdenum porous material as described in claim 1, it is characterised in that: the purity of the titanium valve
It is 99.0%, granularity is 200~300 mesh；The purity of the silicon powder is 99.9%, and granularity is 200 mesh；The purity of the molybdenum powder is
99.0%, granularity is 200 mesh.
3. intermetallic compound titanium-silicon molybdenum porous material as described in claim 1, it is characterised in that: the high-energy ball milling
Ball-milling technology are as follows: ratio of grinding media to material 20:1, revolving speed are 300 ~ 500r/min, are at least 48h ball milling total time, every ball milling 50min stops
10 min of machine.
4. intermetallic compound titanium-silicon molybdenum porous material as described in claim 1, it is characterised in that: mixed after the ball milling
It closes powder and is placed in vacuum oven, be warming up to after 60 ~ 80 DEG C with drying box and keep the temperature at least 8 h, cross 200 meshes.
5. intermetallic compound titanium-silicon molybdenum porous material as described in claim 1, it is characterised in that: the compression moulding
Technique are as follows: for the operating pressure used when compacting for 100 ~ 150 MPa, green compact is round billet.
6. intermetallic compound titanium-silicon molybdenum porous material as described in claim 1, it is characterised in that: the green compact is being sintered
It is preposition in vacuum oven, be warming up to after 110 DEG C with drying box and keep the temperature 2 h；The purity of pore creating material unifor is
98.0%, decomposition temperature is 100~110 DEG C, and pore creating material dosage is the 2wt.% of mixed-powder.
7. intermetallic compound titanium-silicon molybdenum porous material as described in claim 1, it is characterised in that: the vacuum is burnt without pressure
The technique of knot are as follows: be evacuated to 1 × 10-1Pa, heating rate are 4 ~ 5 DEG C/min, and sintering process is 900 DEG C × 2 h+1250
DEG C × 4 h, finally cool to room temperature with the furnace.
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| JPH05131024A (en) * | 1991-02-19 | 1993-05-28 | Sumitomo Light Metal Ind Ltd | Organism compatible material made of titanium aluminite |
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| CN107012352A (en) * | 2017-03-31 | 2017-08-04 | 宝鸡文理学院 | A kind of preparation method of porous titanium or titanium alloy |
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| SU1764813A1 (en) * | 1990-04-23 | 1992-09-30 | Алтайский политехнический институт | Charge for production of porous permeable material |
| JPH05131024A (en) * | 1991-02-19 | 1993-05-28 | Sumitomo Light Metal Ind Ltd | Organism compatible material made of titanium aluminite |
| CN106244852A (en) * | 2016-08-18 | 2016-12-21 | 江苏大学 | A kind of Ti 8Si alloy of Zr alloying and preparation method thereof |
| CN107012352A (en) * | 2017-03-31 | 2017-08-04 | 宝鸡文理学院 | A kind of preparation method of porous titanium or titanium alloy |
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