CN101173332A - Method for producing polyporous material based on solid/gas eutectic directional solidification - Google Patents
Method for producing polyporous material based on solid/gas eutectic directional solidification Download PDFInfo
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- 239000011148 porous material Substances 0.000 claims abstract description 73
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- 238000002844 melting Methods 0.000 claims abstract description 11
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- 239000011344 liquid material Substances 0.000 claims description 7
- 230000006698 induction Effects 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
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- 238000011160 research Methods 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
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Abstract
The invention relates to a method for preparing porosint by solid/gas directional eutectic freezing. The equipment and craft adopted the invention can increase the speed of melting by two to ten times as rapid as the speed of the prior art and monitor the total processes of metal melting and casting by increasing the working pressure, accelerating and control the cooling speed and reducing the nonmetal impurity content. The made porosint has an advantages of even pore space (both radial direction and axial direction of the casting piece). The pore space inside the material can be equal or unequal in size, and also can be subuliform pore space with changeable section. The invention can be used in fluid permeation, filter control, efficient combustion, intensification of mass transfer heat transfer, inflaming and explosion prevention, artificial skeleton, absorption of radiation and noisedamping control in industrial processes such as metallurgical machinery, petrochemical industry, energy source and environmental protection, national defense and war industry, nuclear technology and biopharmaceutical industry, and is the critical technology for breaking through various technology.
Description
Technical field
The present invention relates to the preparing technical field of porous material, refer in particular to solid/solid/gas eutectic directional solidification legal system and be equipped with field of porous materials.
Background technology
From American Crouse (C.Claus) made strainer acquisition United States Patent (USP) in nineteen twenty-three with powder art metallurgy method after, metal polyporous material began to obtain to admit and use.Begin the thirties to produce strainer, be used for filtrated air, fuel, lubricated wet goods with porous materials such as bronze, nickel, iron.After the World War II, be applied to gradually that fluidic pressure, flow control, prevention wing freeze, mercury infiltration switch, gaseous diffusional separation etc.Since the sixties, continuous expansion along with Application Areas, manufacture method and forming technique thereof have also obtained continuous development, and except that the powder sintered porous material, metal fiber polyporous material, foamed metal, metal porous membrane, composite porous material etc. have obtained significant progress.On the porous material preparation method, there are types such as foam melt method, powder foam method, fusion casting, metal-powder or fiber sintering method to come out.
United States Patent (USP) (US.Pat in 1993,5181549) a kind of novel method for preparing porous metal material has been proposed: metal/gas eutectic directional solidification method, prepared metal/gas eutectic is solidified porous material, structure is that cylindrical pore rules orientation is arranged in the metallic matrix, be also referred to as solid/gas matrix material, this process quilt thinks to produce the important advance of porous metal material.The comprehensive mechanical performance of the resulting metal polyporous material of this technology is lower than the density of material of identical material, specific modulus and specific tenacity height.The porous material made from traditional method has the performance characteristics of a lot of excellences, by comparison such as little stress concentration, high mechanical property, the good capacity of heat transmission etc.
Owing to these reasons, solid/gas eutectic directional solidification process and resulting regular porous material have caused the very big concern of countries in the world in recent ten years.The enthusiasm of research comes from the theory significance of solid/gas eutectic solidification on the one hand, comes from the wide potential application foreground of this special porous material on the other hand.At present, carry out the Sandia National Labs that mainly contains the state-run metallurgical university of Ukraine, the U.S. of solid/gas eutectic directional freeze research and naval investigation of materials laboratory, Osaka, Japan university etc. in the world.The research work of domestic relevant this respect seldom, some checking sex works have just been done by indivedual units.
Prior art has the following disadvantages:
The relative upset with crucible of body of heater is 180 ° during casting, or casts from crucible bottom.When this causes casting, between the ceramic refractory in the stove in melt and the stove intense impact and stirring take place, cause material in mold during crystallization heat transfer homogeneity inhomogeneous, that be easy to produce bubble, material internal structure destroyed;
The heating of use resistance furnace, smelting time length, melt and refractory materials are easy to react;
Maximum heating temperature can only reach 1650～1700 ℃, and melt internal temperature inequality;
Can't pass through the whole process of production of visual monitoring porous material from melting to casting;
Can't obtain same axial variable cross-section aperture (as tapered bore or back taper vestibule), also can't obtain the porous material in equally distributed micropore in whole cross section and ultra-fine hole;
Gas only just can use when moderate solubility;
Can only utilize this way to prepare the porous material of minority pure metal and alloy part.
Summary of the invention
Problem to be solved by this invention is exactly to overcome the deficiency of this technology at present, invents equipment and technology that a kind of directional freeze prepares porous material.
Utilize equipment of the present invention to prepare: high quality, to have the foundry goods of even pore texture; By improving operating pressure, reducing nonmetallic impurity content, can obtain the porous material in ultra-fine aperture; Speed of melting improves 2～10 times than prior art; Can directly monitor the whole process of melting of metal and casting; Can utilize this equipment to prepare various porous material products quickly and easily.
Utilize technology of the present invention can prepare the various materials porous material of (comprising pure metal, alloy and pottery), the material internal pore dimension can be identical, also can be different, can also form the tapered bore of variable cross-section; No matter the porous material of preparation all can guarantee porous nickel on the foundry goods radial distribution or on axial distribution; Owing to improved speed of cooling, shortened the whole technological process time.
The present invention is achieved through the following technical solutions:
Crystallizer is a standalone module that can change; Furnace crucible and crystallizer axis are 90 ° of layouts; Material heating and melting utilize induction heating; Visual windows can be observed melting and the whole process of casting; The heat pipe that different directions is arranged on the crystallizer.
The given material of fusion in given gaseous tension, then liquid material is poured in the mold and cooled off, material begins crystallographic orientation with a certain temperature more than the T (fusing point) in mold, gaseous tension then raises with certain speed from set-point simultaneously, until temperature of solidification.After crystallization finished, and is cooled to the following a certain temperature of T (fusing point), gaseous tension dropped to fixation pressure, and blank temperature is finally reduced to room temperature.
The given material of fusion in given gaseous tension is poured liquid melt in the mold into then and is cooled off, and material begins crystallographic orientation with a certain temperature more than the T (fusing point) in mold, simultaneously with given speed of cooling cooling, until temperature of solidification.After crystallization finished, and is cooled to the following a certain temperature of T (fusing point), gaseous tension dropped to fixation pressure, and blank temperature is finally reduced to room temperature.
The patent of the U.S. (US005181549A) is the most approaching with the technology of the present invention essence, and the method for the invention and this patented method technical indicator are more as shown in table 1:
Table 1
| The technical indicator project | The present invention | United States Patent (USP) (US005181549A) |
| Suitable material | Any pure metal, alloy and pottery | Pure metal, alloy part and part pottery |
| Type of heating | The electric induction furnace heating | The resistance furnace heating |
| Crystallizer and furnace crucible position | Vertical mutually | Coaxial |
| Foundry goods physical dimension and pore size | Easily change by changing crystallizer | Be difficult to, must do whole the change body of heater |
| The type of cooling | By specified speed of cooling, be cooled to specified temperature | Speed is random |
| Aero operating pressure when saturated | 0.005～3MPa | 0.02～1MPa |
By more as can be seen, the heating of the inventive method furnace charge is heated fast 2～10 times than resistance furnace rapidly; The steady layering of liquid melts can be poured into the mold in the crystallizer; Can easily change product category and shape by changing the crystallizer assembly; The whole preparation process time shortens 1～5 times.
The inventive method has been widened the selection range of making porous material; Both can obtain diameter and length homogeneous phase multi-pore structure together, also can obtain the pore with non-uniform cross section structure of certain-length.
Description of drawings
Present device synoptic diagram each several part is described as follows:
1. smelting pot; 2. crystallizer; 3. electric induction heater; 4. observation window; 5. mold; 6. the flame retardant coating of smelting furnace; 7. melt; 8. porous material
Embodiment:
The material that adds certain mass in smelting pot (1) heats it and final fusing in electric induction heater (3) induction field, by fusion process and the temperature variation in the detection of the observation form (4) on the body of heater shell stove.After being blown into saturated gas to melt (7), 90 ° of tilting furnaces pour into the melt even laminating in the mold (5) of crystallizer (2), and the flame retardant coating of smelting furnace (6) is shorter duration of contact with melt.Utilize the directed heat pipe on the mold to make porous material (8) crystallization.The crystallizer assembly can be for convenience detach and be changed, and can change shape, pore size, the direction of porous material foundry goods fast.
The method that the supercharging cooling prepares porous material is: the material of fusion desire preparation under 0.005～10MPa gaseous tension, then liquid material is poured in the mold and cooled off, material temperature with T (fusing point)+50～250 ℃ in mold begins crystallographic orientation, gaseous tension is then from the speed liter of set-point 0.005～10MPa with 0.001～3MPa/s simultaneously, and height is until temperature of solidification.After the crystallization end, being cooled to T (fusing point)-200 ℃, gaseous tension also drops to 0.1MPa.Blank temperature is finally reduced to 18～20 ℃ of room temperatures.
Constant voltage is cooled off the method for preparing porous material fast: the material of fusion desire preparation under 0.005～10MPa gaseous tension, then liquid material is poured in the mold and cooled off, material temperature with T (fusing point)+50～250 ℃ in mold begins crystallographic orientation, cool off with the speed of cooling of 0.05～500 ℃/s simultaneously, until temperature of solidification.After the crystallization end, being cooled to T (fusing point)-200 ℃, gaseous tension also drops to 0.1MPa.Blank temperature is finally reduced to 18～20 ℃ of room temperatures.
Using method gives an example 1:
In smelting pot, add the Cu of 5Kg, it is carried out charging into H after the vacuum-treat
2, make air pressure reach 0.2MPa.At the saturated H that blows
2Molten metal under the condition, molten metal is poured molten metal into junker mold after 1250 ℃ of insulation for some time, begin progressively to cool off from the cylinder end face in mold.In crystallisation process, with special regulator control system the gaseous tension in the input autoclave is kept regulating, air pressure is raise according to the speed of 0.02MPa/s, like this, all form even vesicular structure in the inner any cross section of strand, pore length can reach 150mm.If pore diameter is 30～35 μ m, then porosity reaches 30～32%.
Using method gives an example 2:
The Ni that adds 3Kg in smelting pot carries out charging into after the vacuum-treat to it and contains H
2Gas makes air pressure reach 1MPa (wherein: H
2: 0.1MPa; Ar:0.9MPa).At the saturated H that blows
2Molten metal under the condition 1550 ℃ of insulation for some time, is poured molten metal into junker mold after the fusion, begins progressively to cool off from the cylinder end face in mold.In crystallisation process, with special regulator control system the gaseous tension in the input autoclave is kept regulating, air pressure is raise according to the speed of 0.04MPa/s, and then avoid hole to solidify, all form even vesicular structure in the inner arbitrary cross section of strand, pore length can reach 100mm.If pore diameter is 70～80 μ m, then porosity reaches 45～48%.
Using method gives an example 3:
In crucible, add the Cu of 5Kg, it is carried out charging into H after the vacuum-treat
2, make air pressure reach 0.2MPa.At the saturated H that blows
2Molten metal under the condition 1250 ℃ of insulation for some time, is poured molten metal into junker mold after the fusion, begins progressively to cool off from the cylinder end face in mold.In the middle of crystallisation process, use the crystallizer of water-cooled copper, speed of cooling is 300 ℃/s, like this, all forms even vesicular structure in the inner arbitrary cross section of strand, pore length can reach 150mm.If pore diameter is 120～125 μ m, then porosity reaches 35～38%.
Using method gives an example 4:
The QAL (xantal) that adds 3Kg in crucible carries out injecting after the vacuum-treat to crucible and contains H
2Gas, make air pressure reach 0.4MPa (H
2: 0.1MPa, Ar:0.3MPa).Molten metal under the saturated gas condition 1150 ℃ of insulation for some time, is poured molten metal into water-cooled column mold after the fusion, and metal begins progressively to cool off from cylinder side wall in mold.In the middle of crystallisation process, use the crystallizer of water-cooled copper, radially radiation hole speed of cooling is 400 ℃/s, like this, all forms even vesicular structure in the inner arbitrary cross section of strand, pore length can reach 80mm.If pore diameter is 80～90 μ m, then porosity reaches 30～33%.
Using method gives an example 5:
The metal Ni that adds 3Kg in crucible carries out injecting after the vacuum-treat to crucible and contains H
2Gas, make air pressure reach 3MPa (H
2: 0.1MPa, Ar:2.9MPa).Molten metal under the saturated gas condition 1550 ℃ of insulation for some time, is poured molten metal into junker mold after the fusion, and metal begins progressively to cool off from the cylinder end face in mold.In the middle of crystallisation process, use the water-cooled copper crystallizer, speed of cooling is 200 ℃/s, like this, all forms even vesicular structure in the inner arbitrary cross section of strand, pore length can reach 120mm.If pore diameter is 100～110 μ m, then porosity reaches 45～48%.
Claims (23)
1. one kind prepares the equipment of porous material, is used to prepare various metals, alloy and ceramic porous material based on solid/solid/gas eutectic directional solidification.Comprise: smelting pot, crystallizer, well heater, viewing window, mold and directed heat pipe.
2. prepare the equipment of porous material according to a kind of of claim 1 based on solid/solid/gas eutectic directional solidification, it is characterized in that described smelting pot axis is vertical mutually with the crystallizer axis, smelting pot can overturn 90 °.
3. prepare the equipment of porous material according to a kind of of claim 1 based on solid/solid/gas eutectic directional solidification, it is characterized in that described crystallizer is not changing under the furnace binding situation and can change arbitrarily by the porous material requirement of preparation different aperture shape, different aperture direction, different aperture size, crystallizer is an independently module.
4. prepare the equipment of porous material, it is characterized in that described melting type of heating is an electrical induction heating based on solid/solid/gas eutectic directional solidification according to a kind of of claim 1.
5. prepare the equipment of porous material, it is characterized in that described viewing window is the viewing window that is arranged on the body of heater, can observe melting and casting cycle by this viewing window based on solid/solid/gas eutectic directional solidification according to a kind of of claim 1.
6. prepare the equipment of porous material according to a kind of of claim 1 based on solid/solid/gas eutectic directional solidification, it is characterized in that described mold places in the crystallizer, directed heat pipe is arranged on the mold, the melt even laminating pours in the mold of crystallizer.
7. prepare the equipment of porous material according to a kind of of claim 1 based on solid/solid/gas eutectic directional solidification, it is characterized in that described directed heat pipe is distributed on the mold with different directions, the direction of directed heat pipe is adjustable.
8. prepare the equipment of porous material, it is characterized in that the material that is suitable for is various pure metal, alloy and pottery based on solid/solid/gas eutectic directional solidification according to a kind of of claim 1.
9. prepare the equipment of porous material, it is characterized in that the gas that is suitable for is H based on solid/solid/gas eutectic directional solidification according to a kind of of claim 1
2, Ar, N
2, O
2, He etc.
10. one kind prepare the method for porous material based on solid/solid/gas eutectic directional solidification supercharging cooling, is used to prepare various metals, alloy and ceramic porous material, and the material internal void size can be identical, also can difference, can also contain the tapered bore of variable cross-section.It is characterized in that:
The given material of fusion in given gaseous tension, then liquid material is poured in the mold and cooled off, material begins crystallographic orientation with a certain temperature more than the T (fusing point) in mold, gaseous tension then raises with certain speed from set-point simultaneously, until temperature of solidification.When the crystallization end, and after being cooled to the following a certain temperature of T (fusing point), gaseous tension drops to fixation pressure, and blank temperature is finally reduced to room temperature.
11. a kind of supercharging cooling according to claim 10 prepares the method for porous material, it is characterized in that: gaseous tension scope given in the melting material is between 0.005～10MPa.
12. a kind of supercharging cooling according to claim 10 prepares the method for porous material, it is characterized in that: liquid material is poured in the mold and is cooled off, and begins crystallographic orientation with T (fusing point)+50～250 ℃ in mold, until temperature of solidification.
13. a kind of supercharging cooling according to claim 10 prepare the method for porous material, it is characterized in that: gaseous tension is with the speed rising with 0.001～3MPa/s of the set-point of 0.005～10MPa.
14. a kind of supercharging cooling according to claim 10 prepare the method for porous material, it is characterized in that: after the crystallization end, being cooled to T fusing point-200 ℃, gaseous tension drops to 0.1MPa.The porous blank temperature is finally reduced to 18～20 ℃ of room temperatures.
15. a kind of supercharging cooling according to claim 10 prepares the method for porous material, it is characterized in that: the material that is suitable for is various pure metal, alloy and pottery.
16. a kind of supercharging cooling according to claim 10 prepares the method for porous material, it is characterized in that: the gas that is suitable for is H
2, Ar, N
2, O
2, He etc.
17. one kind prepare the method for porous material based on solid/solid/gas eutectic directional solidification constant voltage cooling, is used to prepare various metals, alloy and ceramic porous material, the porous material porous nickel of generation (no matter foundry goods directly upwards still axial on).In the process of cooling, shorten whole technological process by improving speed of cooling.It is characterized in that:
The given material of fusion is poured liquid material in the mold into then in given gaseous tension, and material begins crystallographic orientation with a certain temperature more than the T (fusing point) in mold, simultaneously with given speed of cooling cooling, until temperature of solidification.After crystallization finished, and is cooled to the following a certain temperature of T (fusing point), gaseous tension dropped to fixation pressure, and blank temperature is finally reduced to room temperature.
18. a kind of constant voltage cooling according to claim 17 prepares the method for porous material, it is characterized in that: gaseous tension scope given in the melting material is between 0.005～10MPa.
19. a kind of constant voltage cooling according to claim 17 prepares the method for porous material, it is characterized in that: after liquid material is poured mold into, in mold, begin crystallographic orientation, until temperature of solidification with T (fusing point)+50～250 ℃.
20. a kind of constant voltage cooling according to claim 17 prepares the method for porous material, it is characterized in that: the speed of cooling behind the beginning crystallographic orientation is 0.05～500 ℃/s, until temperature of solidification.
21. a kind of constant voltage cooling according to claim 17 prepares the method for porous material, it is characterized in that: after crystallization finished, is cooled to T (fusing point)-200 ℃, gaseous tension dropped to 0.1MPa.Blank temperature is finally reduced to 18～20 ℃ of room temperatures.
22. a kind of constant voltage cooling according to claim 17 prepares the method for porous material, it is characterized in that: the material that is suitable for is various pure metal, alloy and pottery.
23. a kind of constant voltage cooling according to claim 17 prepares the method for porous material, it is characterized in that: the gas that is suitable for is H
2, Ar, He, O
2, N
2Deng.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710158405A CN100584974C (en) | 2007-11-21 | 2007-11-21 | Prepare the method for porous material based on solid/solid/gas eutectic directional solidification |
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|---|---|---|---|
| CN200710158405A CN100584974C (en) | 2007-11-21 | 2007-11-21 | Prepare the method for porous material based on solid/solid/gas eutectic directional solidification |
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|---|---|
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| CN100584974C CN100584974C (en) | 2010-01-27 |
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| CN102242287A (en) * | 2011-05-06 | 2011-11-16 | 昆明理工大学 | Production method of foam magnesium alloy section bar |
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| CN103642459A (en) * | 2013-12-02 | 2014-03-19 | 浙江大学 | Preparation method of porous array graphene ferrite composite material |
| CN104593630A (en) * | 2015-01-22 | 2015-05-06 | 江西理工大学 | Directional solidifying preparation method of lotus-shaped porous aluminum |
| CN108546122A (en) * | 2018-07-10 | 2018-09-18 | 哈尔滨工业大学 | A kind of method that alumina conbustion synthesis aerosol method prepares alumina-based nano eutectic composite ceramics micro mist |
| CN111036913A (en) * | 2019-12-20 | 2020-04-21 | 永州市产商品质量监督检验所 | Pre-alloyed 3D formed high-entropy alloy porous material and preparation method thereof |
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2007
- 2007-11-21 CN CN200710158405A patent/CN100584974C/en not_active Expired - Fee Related
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|---|---|---|---|---|
| CN102242287A (en) * | 2011-05-06 | 2011-11-16 | 昆明理工大学 | Production method of foam magnesium alloy section bar |
| CN103075816A (en) * | 2013-01-11 | 2013-05-01 | 林峰 | High-temperature heat absorber based on disc type solar power system |
| CN103642459A (en) * | 2013-12-02 | 2014-03-19 | 浙江大学 | Preparation method of porous array graphene ferrite composite material |
| CN103642459B (en) * | 2013-12-02 | 2015-05-20 | 浙江大学 | Preparation method of porous array graphene ferrite composite material |
| CN104593630A (en) * | 2015-01-22 | 2015-05-06 | 江西理工大学 | Directional solidifying preparation method of lotus-shaped porous aluminum |
| CN104593630B (en) * | 2015-01-22 | 2017-01-11 | 江西理工大学 | Directional solidifying preparation method of lotus-shaped porous aluminum |
| CN108546122A (en) * | 2018-07-10 | 2018-09-18 | 哈尔滨工业大学 | A kind of method that alumina conbustion synthesis aerosol method prepares alumina-based nano eutectic composite ceramics micro mist |
| CN108546122B (en) * | 2018-07-10 | 2021-10-15 | 哈尔滨工业大学 | Method for preparing alumina-based nano eutectic composite ceramic micro powder by using alumina combustion synthesis aerosol method |
| CN111036913A (en) * | 2019-12-20 | 2020-04-21 | 永州市产商品质量监督检验所 | Pre-alloyed 3D formed high-entropy alloy porous material and preparation method thereof |
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