CN100398686C - CrB2-FeNiCr composite material, its preparation method and aluminothermy-quick solidification apparatus - Google Patents

CrB2-FeNiCr composite material, its preparation method and aluminothermy-quick solidification apparatus Download PDF

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CN100398686C
CN100398686C CNB2005101325069A CN200510132506A CN100398686C CN 100398686 C CN100398686 C CN 100398686C CN B2005101325069 A CNB2005101325069 A CN B2005101325069A CN 200510132506 A CN200510132506 A CN 200510132506A CN 100398686 C CN100398686 C CN 100398686C
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aluminothermy
boride
fenicr
metal
crb
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CN1789470A (en
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席文君
张涛
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Beihang University
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Beihang University
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Abstract

The present invention discloses CrB2-FeNiCr composite material and a preparation method and an aluminothermy-quick solidification device for the CrB2-FeNiCr composite material. The composite material has the components of 70% to 97% of metal alloy base material FeNiCr and 3% to 30% of boride reinforcement body material CrB2 by weight, wherein the metal alloy base material has the components of 20% to 70% of iron Fe, 20% to 50% of nickel Ni and 10% to 30% of chromium Cr 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 CrB2 reinforcement metal composite material with uniform organization and small crystal grains is obtained.

Description

CrB 2The preparation method of-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 CrB that metallographic phase and ceramic phase mix 2-FeNiCr matrix material.
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 provides the little and uniform CrB of composition of a kind of grain-size 2-FeNiCr matrix material.
Two of purpose of the present invention provides a kind of CrB that is used to prepare 2Aluminothermy-the coagulation system of-FeNiCr matrix material, this apparatus structure is reasonable in design, has simplified preparation section, has reduced the preparation cost of material.
Three of purpose of the present invention is to propose a kind of preparation CrB 2The method of-FeNiCr 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.
A kind of CrB of the present invention 2-FeNiCr matrix material strengthens body by alloy base material and boride and forms, and the weight percent of described alloy base material FeNiCr is 70~97%, and described boride strengthens body material C rB 2Weight percent be 3~30%; In its alloy base material the weight percent of iron Fe be 20~70%, the weight percent of nickel be 20~50% and the weight percent of chromium Cr be 10~30%.Matrix material is Cr 6B 12Fe 40Ni 25Cr 17Perhaps Cr 6B 12Fe 20Ni 50Cr 12Perhaps Cr 6B 12Fe 22Ni 30Cr 30
Described CrB 2TiB in the-FeNiCr matrix material 2Crystal grain is 1~3 μ m, CrB 2The compound CrB of-FeNiCr 2Fe-Ni-Cr crystal grain in the-FeNiCr matrix material is 0.1~1.0 μ m, CrB 2-FeNiCr composite material strength is 1200~2100MPa.
A kind of CrB that is used to prepare of the present invention 2Aluminothermy-the quick solidification apparatus of-FeNiCr matrix material 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.Described supply unit output voltage is 10V~36V, and output rating is 1800W~2500W; Described lagging material is alumina firebrick or refractory fireclay block; The diameter of described tungsten filament is 0.5~1mm.
A kind of preparation CrB of the present invention 2Aluminothermy-the quick setting method of-FeNiCr matrix material, it includes following steps:
(A) take by weighing an amount of metal oxide and aluminium powder, make the starting material of aluminothermy-rapid solidification after mixing at normal temperatures, and starting material are packed in the carbon tube of aluminothermy-quick solidification apparatus;
50~75wt% metal oxide and 25~50wt% 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 CrB 2, 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 melt and boride 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 CrB fast 2-FeNiCr matrix material.
Described aluminothermy-quick setting method, its metal oxide is: the Fe of 20~50wt% 2O 3, the NiO of 30~45wt%, the CrO of 10~20wt% 3B with 10~20wt% 2O 3, and the content sum of above-mentioned each composition is 100%; The perhaps CrO of the NiO of the FeO of 20~50wt%, 20~50wt%, 25~40wt% 3B with 10~20wt% 2O 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 CrO of 25~35wt% 3B with 10~20wt% 2O 3, and the content sum of above-mentioned each composition is 100%.
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 melt 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. starting material
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 CrB that is used to prepare of the present invention 2Aluminothermy-the quick solidification apparatus of-FeNiCr matrix material comprises water cooled copper mould 1, supply unit and reaction vessel 2, and 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.
A kind of CrB of the present invention 2-FeNiCr matrix material strengthens body by alloy base material and boride and forms, and the weight percent of described alloy base material FeNiCr is 70~97%, and described boride strengthens body material TiB 2Weight percent be 3~30%; In its alloy base material the weight percent of iron Fe be 20~70%, the weight percent of nickel be 20~50% and the weight percent of chromium Cr be 10~30%.
CrB among the present invention 2-FeNiCr matrix material is Cr 6B 12Fe 40Ni 25Cr 17Perhaps Cr 6B 12Fe 20Ni 50Cr 12Perhaps Cr 6B 12Fe 22Ni 30Cr 30
CrB 2TiB in the-FeNiCr matrix material 2Crystal grain is 1~3 μ m, CrB 2Fe-Ni-Cr crystal grain in the-FeNiCr matrix material is 0.1~1.0 μ m, CrB 2-FeNiCr composite material strength is 1200~2100MPa.
A kind of preparation CrB of the present invention 2Aluminothermy-the quick setting method of-FeNiCr matrix material includes following steps:
(A) take by weighing and make the former of aluminothermy-rapid solidification after an amount of metal oxide and aluminium powder mix at normal temperatures
(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;
50~75wt% metal oxide and 25~50wt% 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 CrB 2, 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 melt and boride 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 CrB fast 2-FeNiCr matrix material.
In (C) of aluminothermy-rapid solidification preparation method of the present invention step, behind " startup " switch of pressing on the supply unit, tungsten filament energising back heating, 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 condition 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) be reduced the reduction of agent aluminium Al powder, reaction product is metal melt and aluminium oxide Al 2O 3Melt, chromium Cr and boron chemical combination generate CrB in the metal melt simultaneously 2, 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, take out and contain aluminium oxide Al 2O 3The matrix material of slag blanket is removed slag blanket and has just been obtained CrB of the present invention 2-FeNiCr composite material section bar.
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,, weave construction tiny in order to obtain organizing evenly, the matrix material of 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 30~45wt%, the CrO of 10~20wt% 3B with 10~20wt% 2O 3, and the content sum of above-mentioned each composition is 100%; The component two of metal oxide is: the CrO of the FeO of 20~50wt%, the NiO of 20~50wt%, 25~40wt% 3B with 10~20wt% 2O 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 CrO of 25~35wt% 3B with 10~20wt% 2O 3, and the content sum of above-mentioned each composition is 100%.Be that particle diameter is the simple substance aluminium powder of 0.5~500 μ m with agent between the each component, the particle diameter of boron powder is 0.1~200 μ m.According to the different preparation-obtained CrB of component 2The microstructure of-FeNiCr matrix material, tissue topography, hardness and wear resisting property are different.
Embodiment 1:The Cr of system 500g 6B 12Fe 40Ni 25Cr 17Matrix material
Take by weighing the B of Cr, the 12.9g of 28.8g, the Fe of 318.9g 2O 3, the NiO of 187.0g, the Cr of 84.8g 2O 3, 57.7g CrO 3With the Al of 213.8g, the particle diameter of above-mentioned materials is 50 μ m, in the carbon tube 201 of the aluminothermy-coagulation system 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 Cr 6B 12Fe 40Ni 25Cr 17Matrix material.
The above-mentioned Cr for preparing 6B 12Fe 40Ni 25Cr 17Matrix material is used scanning electron microscopic observation tissue topography, and this microstructure of composite is fine and closely woven, the TiB in the material 2Crystal grain is 1.8 μ m, and the Fe-Ni-Cr crystal grain in the material is less than 1 μ m.Measure this Cr with MTS material comprehensive test machine 6B 12Fe 40Ni 25Cr 17The compressive strength of matrix material is 1870MPa.
Embodiment 2:The Cr of system 500g 6B 12Fe 20Ni 50Cr 12Matrix material
Take by weighing the B of Cr, the 12.9g of 28.8g, the Fe of 318.9g 2O 3, the NiO of 187.0g, the Cr of 84.8g 2O 3, 57.7g CrO 3With the Al of 213.8g, 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 Ti 6B 12Fe 40Ni 25Cr 17Matrix material.
The above-mentioned Cr for preparing 6B 12Fe 40Ni 25Cr 17Matrix material is used scanning electron microscopic observation tissue topography, and this microstructure of composite is fine and closely woven, the CrB in the material 2Crystal grain is 1.8 μ m, and the Fe-Ni-Cr crystal grain in the material is less than 1 μ m.Measuring microhardness with MTS material comprehensive test machine is 1500MPa.
Embodiment 3:The Cr of system 500g 6B 12Fe 12Ni 30Cr 30Matrix material
Take by weighing the B of Cr, the 12.9g of 28.8g, the Fe of 318.9g 2O 3, the NiO of 187.0g, the Cr of 84.8g 2O 3, 57.7g CrO 3With the Al of 213.8g, 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.
Cr 2O 3, 100.0g CrO 3With the Al of 222.5g, 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 Cr 6B 12Fe 40Ni 25Cr 17Matrix material.
The above-mentioned Cr for preparing 6B 12Fe 40Ni 25Cr 17Matrix material is used scanning electron microscopic observation tissue topography, and this microstructure of composite is fine and closely woven, the TiB in the material 2The crystal grain median size is 2.35 μ m, and the Fe-Ni-Cr crystal grain in the material is less than 1 μ m.Measuring microhardness with MTS material comprehensive test machine is 1350MPa.
The CrB that the present invention obtains 2-FeNiCr matrix material: alloy base is ultrafine-grained (UFG) microstructure even is nanostructure to have excellent more mechanical property than general cast alloy, is used for the CrB of wild phase 2Deng boride, not only can refinement matrix structure, can also play the effect of dispersion-strengthened.
Aluminothermy-fast solidification technology among the present invention has the following advantages: 1, the thermite reaction thermal discharge is big, the adiabatic temperature height, all reaction product that comprise dystectic boride all are in molten state, therefore can use castmethod to obtain complex-shaped fine and close workpiece; 2, the boride reaction in generates, with metallographic phase bonding strength height; 3,, can obtain the thinner boride of crystal grain and strengthen metal composite by the quick cooled and solidified of copper mold; 4, cost is low, and technology is simple, and prepared boride strengthens the metal composite excellent performance.In addition, the present invention uses aluminium powder to make reductive agent, at first is because aluminium powder is lower than the price of reductive agents such as magnesium, zirconium and titanium, secondly is because the oxide products that obtains as reductive agent with aluminium is an aluminum oxide, the wettability of it and metal melting product is relatively poor, so aluminum oxide separates with metallic product easily.
CrB of the present invention 2-FeNiCr matrix material has the excellent abrasive energy, and good high-temperature corrosion resistance performance is arranged under the hot environment, not only can be used as structured material, and is a kind of important coated material, is widely used in machinery, chemical industry, oil and national defence field.

Claims (2)

1. CrB 2Aluminothermy-the quick setting method of-FeNiCr matrix material is characterized in that including following steps:
(A) take by weighing and make aluminothermy-rapid solidification starting material (3) 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;
50~75wt% metal oxide and 25~50wt% aluminium powder are arranged in the starting material (3);
Described metal oxide is: the Fe of 20~50wt% 2O 3, the NiO of 30~45wt%, the CrO of 10~20wt% 3B with 10~20wt% 2O 3, and the content sum of above-mentioned each composition is 100%; Perhaps
The CrO of the FeO of 20~50wt%, the NiO of 20~50wt%, 25~40wt% 3B with 10~20wt% 2O 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 CrO of 25~35wt% 3B with 10~20wt% 2O 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 regulates 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 CrB 2, 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 melt and boride 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 CrB fast 2-FeNiCr matrix material.
2. aluminothermy-quick setting method according to claim 1 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 0.1~200 μ m, and the particle diameter of described boride is 0.1~200 μ m.
CNB2005101325069A 2005-12-27 2005-12-27 CrB2-FeNiCr composite material, its preparation method and aluminothermy-quick solidification apparatus Expired - Fee Related CN100398686C (en)

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