CN100449015C - Method of preparing WB-FeNiCr composite material alnminothermic-fast solidification technology and its device - Google Patents

Method of preparing WB-FeNiCr composite material alnminothermic-fast solidification technology and its device Download PDF

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CN100449015C
CN100449015C CNB2005101325976A CN200510132597A CN100449015C CN 100449015 C CN100449015 C CN 100449015C CN B2005101325976 A CNB2005101325976 A CN B2005101325976A CN 200510132597 A CN200510132597 A CN 200510132597A CN 100449015 C CN100449015 C CN 100449015C
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aluminothermy
fenicr
boride
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metal oxide
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CN1786235A (en
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席文君
张涛
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Beihang University
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Abstract

The present invention discloses a method and a device thereof which use an aluminothermy-quick solidification technique to prepare WB-FeNiCr composite material. The WB-FeNiCr composite material prepared by the aluminothermy-quick solidification technique has the components of 70% to 97% of metal alloy base material FeNiCr and 3% to 30% of boride reinforcement body material WB by weight. The device of the present invention is composed of a water cooling copper mould, a power supply device and a reaction vessel, wherein the reaction vessel is arranged on the water cooling copper mould; tungsten filaments are connected with the positive pole and the negative pole of the power supply device; heat insulating material is filled between a graphite pipe and a casing; a port at the other end of the graphite pipe is provided with aluminum foil; the cooling water circulation cavity of the water cooling copper mould in an S shape, and the forming cavity is in a hopper shape. The invention combines aluminothermy and quick solidification technique to directly inject fusant products obtained by aluminothermy reaction into the copper mould; the characteristic of the high thermal conduction coefficient of copper metal is used for realizing the quick cooling and the solidification of the fusant products, so the WB reinforcement metal composite material with uniform formation and small crystal grains is obtained.

Description

A kind of method that adopts aluminothermy-fast solidification technology to prepare the WB-FeNiCr matrix material
Technical field
The present invention relates to a kind of preparation method that thermite process is combined with fast solidification technology, the melt product that the thermite reduction reaction is obtained directly is injected in the copper mould, utilize the high characteristic of copper metal heat-conducting coefficient realize the melt product quick cooling, solidify, thereby obtain the WB-FeNiCr matrix material that metallographic phase and ceramic phase mix.
Background technology
At present, boride enhancing metal composite mainly adopts powder metallurgy process and liquid metal-boride hybrid system preparation.
Wherein, the process of powder metallurgy process is, before this with metallic substance with ceramic powder mixes after press forming strengthens metal composite after sintering obtains boride.There are certain hole and grain-size big between the boride enhancing metal composite of powder metallurgic method preparation.The ceramic phase surface is vulnerable to pollute in preparation process, thereby causes the bonding strength of ceramic phase and metallographic phase to reduce.In addition, last sintering process also makes grain growth easily, and the boride that is difficult to obtain thin crystalline substance strengthens metal composite.
Wherein, the technological process of liquid metal-boride hybrid system is that elder generation joins the metallic substance fusing in the liquid metal melt then with boride particle, obtain boride and strengthen metal composite after cooling.Boride distributes evenly inadequately in the matrix material of this method preparation, and particle is bigger, and the boride particle surface is polluted easily, influences the wettability between boride and the metallic matrix.
Summary of the invention
One of purpose of the present invention is the method that proposes a kind of WB-FeNiCr of preparation matrix material, this method combines thermite process with fast solidification technology, flow into the forming cavity of copper mold behind the high-temperature fusant burn through aluminium foil that produces by raw-material redox reaction after cooling, solidify and make boride and strengthen metal composite.
Two of purpose of the present invention provides the little and uniform WB-FeNiCr matrix material of composition of a kind of grain-size.
Three of purpose of the present invention provides a kind of aluminothermy-quick solidification apparatus that is used to prepare the WB-FeNiCr matrix material, and this apparatus structure is reasonable in design, has simplified preparation section, has reduced the preparation cost of material.
The present invention is a kind of method that adopts aluminothermy-fast solidification technology to prepare the WB-FeNiCr matrix material, includes following steps:
(A) take by weighing the starting material that make aluminothermy-rapid solidification after an amount of metal oxide and aluminium powder mix at normal temperatures, and starting material are packed in the carbon tube of aluminothermy-quick solidification apparatus;
50～83wt% metal oxide and 17～50wt% aluminium powder are arranged in the starting material;
(B) flow velocity of regulating in the cooling water circulation chamber is 0.3～0.5m 3/ min;
Regulate supply unit output voltage 10～36V, output rating 1800～2500W;
(C) switch on the opening power device, tungsten filament igniting produces under 1800～2500 ℃ the hot conditions starting material and is lighted in carbon tube;
The metal oxide that takes by weighing in above-mentioned under hot conditions (A) step is reduced by aluminium Al, produces redox reaction, obtains WB, Fe, Ni, Cr and Al 2O 3Blend melt;
In redox reaction, the Al in the above-mentioned blend melt 2O 3Float on the top of metal and boride blend melt, under the effect of gravity, flow into behind described metal and the boride blend melt burn through aluminium foil in the forming cavity of water cooled copper mould, cooled and solidified becomes the WB-FeNiCr matrix material fast.
Described employing aluminothermy-fast solidification technology prepares the method for WB-FeNiCr matrix material, and its metal oxide is: the Fe of 20～50wt% 2O 3, the NiO of 20～50wt%, the Cr of 10～20wt% 2O 3, 5～15wt% B 2O 3WO with 10～20wt% 3, and the content sum of above-mentioned each composition is 100%; The perhaps Cr of the NiO of the FeO of 20～50wt%, 20～50wt%, 20～30wt% 2O 3, 5～10wt% B 2O 3WO with 10～20wt% 3, and the content sum of above-mentioned each composition is 100%; The perhaps Fe of 20～50wt% 3O 4, the NiO of 20～50wt%, the Cr of 20～30wt% 2O 3, 5～15wt% B 2O 3WO with 10～20wt% 3, and the content sum of above-mentioned each composition is 100%.
Described employing aluminothermy-fast solidification technology prepares the method for WB-FeNiCr matrix material, and described aluminium powder is that particle diameter is the simple substance aluminium powder of 0.5～500 μ m, and the particle diameter of described metal oxide is 0.5～200 μ m.
A kind of WB-FeNiCr matrix material that adopts aluminothermy-fast solidification technology to prepare of the present invention, strengthening body by alloy base material and boride forms, the weight percent of described alloy base material WB-FeNiCr is 70～97, and the weight percent that described boride strengthens body material TiC is 3～30; In its alloy base material the weight percent of iron Fe be 20～60, the weight percent of nickel be 30～55 and the weight percent of chromium Cr be 10～25, and the content sum of above-mentioned each composition is 100%.
Described WB-FeNiCr matrix material is W 6B 6Fe 40Ni 25Cr 23Perhaps W 6B 6Fe 23Ni 40Cr 25
A kind of aluminothermy-quick solidification apparatus that is used to prepare the WB-FeNiCr matrix material of the present invention comprises water cooled copper mould, supply unit and reaction vessel, and reaction vessel is installed on the water cooled copper mould, and the tungsten filament in the reaction vessel is connected with supply unit; Described reaction vessel is made of housing, carbon tube, lagging material, tungsten filament and aluminium foil, filled thermal insulation materials is between carbon tube and housing, tungsten filament is installed on the end cap of carbon tube, and the two ends of tungsten filament are stretched out carbon tube and are connected with the positive and negative electrode of supply unit, and the other end port of carbon tube is provided with aluminium foil; The cooling water circulation chamber of described water cooled copper mould is a S shape, and its forming cavity is a doline, and flare opening and carbon tube port size are adaptive.
Preparation technology of the present invention has utilized the high characteristic of boride fusing point, boride at first in the melt that reaction obtains forming core, separate out.In process of setting, boride provides the forming core place for metal melt, and metal melt is at boride surface heterogeneous body forming core.Just the forming core boride of separating out is very tiny, and distribution disperse, evenly is for metal melt provides a large amount of heterogeneous body forming core places.In addition, utilized the characteristic of rapid solidification, utilization copper mold fast cooling technology improves the solution speed of cooling, solidifying cooling rate accelerates, the boride of a large amount of forming cores and the metallic matrix nucleus has little time to grow up or can not get sufficient room owing to growing up simultaneously at a high speed,, thereby obtain the tiny boride of crystal grain and strengthen metal composite, because the dispersion-strengthened action of the tiny and boride of crystal grain, the boride of aluminothermy-fast solidification technology preparation strengthen the intensity of metal composite, toughness, performance such as wear-resisting is improved significantly.
Description of drawings
Fig. 1 is the structural representation of aluminothermy-quick solidification apparatus of the present invention.
Among the figure: 1. water cooled copper mould 101. cooling water circulation chamber 102. forming cavities, 2. reaction vessels, 201. carbon tubes, 202. lagging materials, 203. aluminium foils, 204. housings, 205. tungsten filaments, 3. raw materials
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
See also shown in Figure 1, a kind of aluminothermy-quick solidification apparatus that is used to prepare the WB-FeNiCr matrix material of the present invention, comprise water cooled copper mould 1, supply unit and reaction vessel 2, reaction vessel 2 is installed on the water cooled copper mould 1, and the tungsten filament 205 in the reaction vessel 2 is connected with supply unit; Described reaction vessel 2 is made of housing 204, carbon tube 201, lagging material 202, tungsten filament 205 and aluminium foil 203, lagging material 202 is filled between carbon tube 201 and the housing 204, tungsten filament 205 is installed on the end cap of carbon tube 201, and the two ends of tungsten filament 205 are stretched out carbon tube 201 and are connected with the positive and negative electrode of supply unit, and the other end port of carbon tube 201 is provided with aluminium foil 203; The cooling water circulation chamber 101 of described water cooled copper mould 1 is a S shape, and its forming cavity 102 is dolines, and flare opening and carbon tube 201 port size are adaptive.Described supply unit output voltage is 10V～36V, and output rating is 1800W～2500W; Described lagging material 202 is alumina firebrick or refractory fireclay block; The diameter of described tungsten filament 205 is 0.5～1mm.
The present invention is a kind of method that adopts aluminothermy-fast solidification technology to prepare the WB-FeNiCr matrix material, it is characterized in that including following steps:
(A) take by weighing the starting material 3 that make aluminothermy-rapid solidification after an amount of metal oxide and aluminium powder mix at normal temperatures, and starting material 3 are packed in the carbon tube 201 of aluminothermy-quick solidification apparatus;
50～83wt% metal oxide and 17～50wt% aluminium powder are arranged in the starting material 3;
(B) flow velocity of regulating in the cooling water circulation chamber 101 is 0.3～0.5m 3/ min;
Regulate supply unit output voltage 10～36V, output rating 1800～2500W;
(C) switch on the opening power device, tungsten filament 205 igniting, starting material 3 are lighted under the hot conditions of 1800～2500 ℃ of generations carbon tube 201 in;
The metal oxide that takes by weighing in above-mentioned under hot conditions (A) step is reduced by aluminium Al, produces redox reaction, obtains WB, Fe, Ni, Cr, Mo and Al 2O 3Blend melt;
In redox reaction, the Al in the above-mentioned blend melt 2O 3Float on the top of metal and boride blend melt, under the effect of gravity, described metal and boride blend melt burn through aluminium foil 203 backs flow in the forming cavity 102 of water cooled copper mould 1, and cooled and solidified becomes the WB-FeNiCr matrix material fast.
In (C) of aluminothermy-rapid solidification preparation method of the present invention step, behind " startup " switch of pressing on the supply unit, tungsten filament 205 energising back heatings, the starting material 3 in the carbon tube 201 have been lighted, chemical reaction takes place in starting material 3, release of heat makes temperature in the carbon tube 201 reach high temperature more than 3200 ℃.Metal oxide (is chosen metal oxide according to prepared metal matrix material, three groups in patent application of the present invention, are disclosed, these three groups of metal oxides will be described hereinafter) in redox reaction as reductive agent aluminium Al powder, the aluminium oxide Al that density is little 2O 3Melt floats on the top of metal+boride blend melt; Under hot conditions, the metal of carbon tube 201 bottoms+boride blend melt at first burn through aluminium foil 203 flows in the forming cavity 102 of water cooled copper mould 1, realize quick cooled and solidified by quick mobile water coolant in the cooling water circulation chamber 101, open water cooled copper mould 1 then, taking out surface coverage has aluminium oxide Al 2O 3The matrix material of slag blanket is removed slag blanket and has just been obtained WB-FeNiCr composite material section bar of the present invention.
In the present invention, cooled and solidified technology is relevant with the grain-size of the size of forming cavity 102, cooling water circulation chamber 101 flow velocities, metal+boride blend melt fast, material structure is tiny in order to obtain, weave construction even, no large dendritic crystal, just can realize by the flow velocity of regulating cooling water circulation chamber 101, its quick cooled and solidified technology is simple, easy to operate.
In the present invention, the component one of metal oxide is: the Fe of 20～50wt% 2O 3, the NiO of 20～50wt%, the Cr of 10～20wt% 2O 3, 5～15wt% B 2O 3WO with 10～20wt% 3, and the content sum of above-mentioned each composition is 100%; The component two of metal oxide is: the Cr of the FeO of 20～50wt%, the NiO of 20～50wt%, 20～30wt% 2O 3, 5～10wt% B 2O 3WO with 10～20wt% 3, and the content sum of above-mentioned each composition is 100%; The component three of metal oxide is: the Fe of 20～50wt% 3O 4, the NiO of 20～50wt%, the Cr of 20～30wt% 2O 3, 5～15wt% B 2O 3WO with 10～20wt% 3, and the content sum of above-mentioned each composition is 100%.Use the CrO of equal quantities between the each component 3Cr in the surrogate response thing 2O 3Can improve adiabatic temperature, more help the starting material 3 in the carbon tube 201 are fused into melt.The metal oxide particle diameter that is adopted is 0.5～200 μ m, and the aluminum reduction agent is that particle diameter is the simple substance aluminium powder of 0.5～500 μ m.Microstructure, tissue topography, hardness and wear resisting property according to the different preparation-obtained WB-FeNiCr matrix materials of component are different.
Embodiment 1:The W of system 500g 6B 6Fe 40Ni 25Cr 23Matrix material
Take by weighing the C of Ti, the 7.2g of 28.8g, the Fe of 287g 2O 3, the NiO of 168g, the Cr of 84.8g 2O 3, 41g CrO 3With the Al of 218.5g, the particle diameter of above-mentioned materials is 50 μ m, in the carbon tube 201 of the aluminothermy-quick solidification apparatus as shown in Figure 1 of packing into after mixing.
The forming cavity 102 of the water cooled copper mould of selecting for use during preparation 1 is that diameter is the circle of 3cm, and it regulates water coolant flow velocity 0.03m 3/ min, supply unit output voltage 12V, output rating 2000W.
Behind the switch of pressing on the supply unit, above-mentioned raw materials in the carbon tube 201 is lighted by tungsten filament 205, redox reaction takes place, obtain blend melt, after aluminium foil 203 was by burn through, blend melt flowed in the forming cavity 102 of water cooled copper mould 1, the water that is cooled is frozen into cylindric fast, open water cooled copper mould 1, take out columned matrix material, remove the Al on cylindric top 2O 3Slag blanket promptly obtains W 6B 6Fe 40Ni 25Cr 23Matrix material.
The above-mentioned W for preparing 6B 6Fe 40Ni 25Cr 23Matrix material is used scanning electron microscopic observation tissue topography, sees also shown in Fig. 3 A and Fig. 3 B, and this microstructure of composite is fine and closely woven, and the WB crystal grain in the material is 1.8 μ m, and the Fe-Ni-Cr crystal grain in the material is less than 1 μ m.Measure this W with MTS material comprehensive test machine 6B 6Fe 40Ni 25Cr 23The compressive strength of matrix material is 2750MPa.
Embodiment 2:The W of system 500g 6B 6Fe 23Ni 40Cr 25Matrix material
Take by weighing NiO, the Cr of 84.8g of FeO, 261.4g of C, 125.2g of Ti, the 7.2g of 28.8g 2O 3, 69.6g CrO 3, 100.2g MoO 3With the Al of 199.3g, the particle diameter of above-mentioned materials is 50 μ m, in the carbon tube 201 of the aluminothermy-quick solidification apparatus as shown in Figure 1 of packing into after mixing.
The forming cavity 102 of the water cooled copper mould of selecting for use during preparation 1 is that diameter is the circle of 3cm, and it regulates water coolant flow velocity 0.03m 3/ min, supply unit output voltage 12V, output rating 2000W.
Behind the switch of pressing on the supply unit, above-mentioned raw materials in the carbon tube 201 is lighted by tungsten filament 205, redox reaction takes place, obtain blend melt, after aluminium foil 203 was by burn through, blend melt flowed in the forming cavity 102 of water cooled copper mould 1, the water that is cooled is frozen into cylindric fast, open water cooled copper mould 1, take out columned matrix material, remove the Al on cylindric top 2O 3Slag blanket promptly obtains W 6B 6Fe 23Ni 40Cr 25Matrix material.
The above-mentioned W for preparing 6B 6Fe 23Ni 40Cr 25Matrix material is used scanning electron microscopic observation tissue topography, and this microstructure of composite is fine and closely woven, and the WB crystal grain in the material is 1.8 μ m, and the Fe-Ni-Cr crystal grain in the material is less than 1 μ m.Measure this W with MTS material comprehensive test machine 6B 6Fe 23Ni 40Cr 25The compressive strength of matrix material is 2420MPa.
Embodiment 3:The W of system 500g 6B 6Fe 23Ni 40Cr 25Matrix material
Take by weighing the C of Ti, the 7.2g of 28.8g, the Fe of 45.9g 3O 4, the NiO of 200.0g, the Cr of 84.8g 2O 3, 155.2g CrO 3, 102.3g MoO 3With the Al of 243.0g, the particle diameter of above-mentioned materials is 50 μ m, in the carbon tube 201 of the aluminothermy-quick solidification apparatus as shown in Figure 1 of packing into after mixing.
The forming cavity 102 of the water cooled copper mould of selecting for use during preparation 1 is that diameter is the circle of 3cm, and it regulates water coolant flow velocity 0.03m 3/ min, supply unit output voltage 12V, output rating 2000W.
Behind the switch of pressing on the supply unit, above-mentioned raw materials in the carbon tube 201 is lighted by tungsten filament 205, redox reaction takes place, obtain blend melt, after aluminium foil 203 was by burn through, blend melt flowed in the forming cavity 102 of water cooled copper mould 1, the water that is cooled is frozen into cylindric fast, open water cooled copper mould 1, take out columned matrix material, remove the Al on cylindric top 2O 3Slag blanket promptly obtains W 6B 6Fe 23Ni 40Cr 25Matrix material.
The above-mentioned W for preparing 6B 6Fe 23Ni 40Cr 25Matrix material is used scanning electron microscopic observation tissue topography, and this microstructure of composite is fine and closely woven, and the TiC crystal grain in the material is 1.8 μ m, and the Fe-Ni-Cr crystal grain in the material is less than 1 μ m.Measure this W with MTS material comprehensive test machine 6B 6Fe 23Ni 40Cr 25The compressive strength of matrix material is 2380MPa.
The W that the present invention obtains 6B 6Fe 23Ni 40Cr 25Matrix material: alloy base is ultrafine-grained (UFG) microstructure even is nanostructure, has excellent more mechanical property than general cast alloy, the borides such as TiC that are used for wild phase not only can refinement matrix structure, can also play the effect of dispersion-strengthened.
Aluminothermy-fast solidification technology among the present invention is compared with above-mentioned two kinds of technologies and is had the following advantages: 1, thermit reaction Thermal discharge is big, and the adiabatic temperature height comprises that all product of dystectic boride all are in molten condition, Therefore can use casting method to obtain complex-shaped fine and close workpiece; 2, the boride reaction in-situ generates, with Metal Phase The bond strength height; 3, by the quick cooled and solidified of copper mold, can obtain the thinner boride of crystal grain and strengthen Metals composite Material; 4, cost is low, and technology is simple, and prepared boride strengthens the metallic composite excellent performance. In addition, originally Invention uses aluminium powder to make reducing agent, at first is because aluminium powder is lower than the price of the reducing agents such as magnesium, zirconium and titanium, secondly be because of For the oxide products that obtains as reducing agent with aluminium is aluminium oxide, the wetability of it and metal melting product is relatively poor, therefore Aluminium oxide separates with metallic product easily.
W of the present invention6B 6Fe 23Ni 40Cr 25Composite has excellent anti-wear performance, has good under the hot environment The high-temperature corrosion resistance performance, not only can be used as structural material, and be a kind of important coating material, machinery, Chemical industry, oil and national defence field are widely used.

Claims (2)

1, a kind of method that adopts aluminothermy-fast solidification technology to prepare the WB-FeNiCr matrix material is characterized in that including following steps:
(A) take by weighing an amount of metal oxide and aluminium powder and mix at normal temperatures and make starting material (3), and starting material (3) are packed in the carbon tube (201) of aluminothermy-quick solidification apparatus;
50～83wt% metal oxide and 17～50wt% aluminium powder are arranged in the starting material (3);
Described metal oxide is the Fe of 20～50wt% 2O 3, the NiO of 20～50wt%, the Cr of 10～20wt% 2O 3, 5～15wt% B 2O 3WO with 10～20wt% 3, and the content sum of above-mentioned each composition is 100%; Perhaps
The Cr of the FeO of 20～50wt%, the NiO of 20～50wt%, 20～30wt% 2O 3, 5～10wt% B 2O 3WO with 10～20wt% 3, and the content sum of above-mentioned each composition is 100%; Perhaps
The Fe of 20～50wt% 3O 4, the NiO of 20～50wt%, the Cr of 20～30wt% 2O 3, 5～15wt% B 2O 3WO with 10～20wt% 3, and the content sum of above-mentioned each composition is 100%;
(B) flow velocity of regulating in the cooling water circulation chamber (101) is 0.3～0.5m 3/ min,
Regulate supply unit output voltage 10～36V, output rating 1800～2500W;
(C) switch on the opening power device, tungsten filament (205) igniting, starting material (3) are lighted under the hot conditions of 1800～2500 ℃ of generations carbon tube (201) in;
The metal oxide that takes by weighing in above-mentioned under hot conditions (A) step is reduced by aluminium Al, produces redox reaction, obtains WB, Fe, Ni, Cr and Al 2O 3Blend melt;
In redox reaction, the Al in the above-mentioned blend melt 2O 3Float on the top of metal and boride blend melt, under the effect of gravity, described metal and boride blend melt burn through aluminium foil (203) back flow in the forming cavity (102) of water cooled copper mould (1), and cooled and solidified becomes the WB-FeNiCr matrix material fast.
2, employing aluminothermy-fast solidification technology according to claim 1 prepares the method for WB-FeNiCr matrix material, it is characterized in that: described aluminium powder is that particle diameter is the simple substance aluminium powder of 0.5～500 μ m, and the particle diameter of described metal oxide is 0.5～200 μ m.
CNB2005101325976A 2005-12-27 2005-12-27 Method of preparing WB-FeNiCr composite material alnminothermic-fast solidification technology and its device Expired - Fee Related CN100449015C (en)

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CN1786231A (en) * 2005-12-27 2006-06-14 北京航空航天大学 Method of preparing TaC-FeNiCr composite material using aluminium tbermo-fast solidificntion technology and device thereof
CN1789470A (en) * 2005-12-27 2006-06-21 北京航空航天大学 CrB2-FeNiCr composite material, its preparation method and aluminothermy-quick solidification apparatus
CN1789447A (en) * 2005-12-27 2006-06-21 北京航空航天大学 Method and apparatus for preparing VC-FeNiCr composite material by employing aluminothermy-quick solidification process
CN1793392A (en) * 2005-12-27 2006-06-28 北京航空航天大学 Process for preparing Cr7C3-FeNiCr composite by heating aluminium fast solidification tech, and apparatus thereof

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