CN108588530B - Low-density heat-resistant iron-based alloy and preparation method thereof - Google Patents
Low-density heat-resistant iron-based alloy and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a low-density heat-resistant iron-based alloy and a preparation method thereof, which adopts Ni powder and Al powder to react in the mechanical alloying process to generate NiAl powder particles with a nano B2 ordered structure, diamond is pretreated by a proper process to form a uniform tungsten coating layer on the surface of the diamond, then NiAl powder and pretreated diamond powder are filled into a ball milling tank and are continuously and uniformly mixed with Fe powder to obtain fine and uniform NiAl/diamond enhanced Fe-based alloy composite powder, and a block composite material is obtained by hot-press sintering to obtain a low-density heat-resistant NiAl/diamond enhanced Fe-based material, namely the low-density heat-resistant iron-based alloy. The invention combines the mechanical alloying technology and the hot-pressing sintering technology, and the developed low-density heat-resistant NiAl/diamond reinforced Fe-based alloy product has low cost, high purity, low density and high thermal conductivity, and has the application potential of being applied to the cylinder head material of the high-power-density diesel engine.
Description
Technical Field
The invention relates to an alloy material, in particular to a low-density heat-resistant iron-based alloy and a preparation method thereof.
Background
Along with the improvement of the power density of the diesel engine, the gas detonation pressure of a combustion chamber, the maximum working temperature of a cylinder cover and the movement speed of a piston of the future high-power-density diesel engine are greatly improved, and the work efficiency of the combustion chamber is improvedEven more severe, the combustor materials will be subjected to greater thermal and mechanical loads. The cylinder cover is generally cast by gray cast iron or alloy cast iron, the aluminum alloy has good heat conductivity, is beneficial to improving the compression ratio, but has lower strength, and is not suitable for the use working condition of the cylinder cover material of the diesel engine with high power density; cast iron cylinder head material (density about 7.3 g/cm)3) The performance of the cylinder cover material is stable below 400 ℃, but the performance of the cylinder cover material is greatly reduced along with the temperature rise to 400-600 ℃, so that the use requirement of the cylinder cover material of a future high-power-density engine cannot be met, and therefore, the development of a novel low-density high-strength heat-resistant cylinder cover material is very critical.
For the iron-based alloy, korean researchers in 2015 discovered a method of producing a new type of low density steel. The relevant researchers explain that the technical secret lies in the formation of a new structure during the heat treatment and the use of the right mixed composition, nickel being added in addition to the conventional iron, carbon, aluminum and manganese. Nickel can interact with aluminum during annealing to produce shear resistant nano-scale B2 crystals, resulting in exceptionally strong steels containing such crystals. Therefore, the appropriate component combination and structure optimization are effective ways for developing the low-density heat-resistant iron-based alloy. Further, NiAl (density 5.9 g/cm)3And the room temperature thermal conductivity is about 76W/(m.K)), so that the addition of the NiAl phase with the B2 structure in the iron-based material can improve the thermal conductivity and the strength while reducing the density.
Diamond is used as one of high thermal conductivity materials (room temperature thermal conductivity 1300-2400W/(m.K)), and the density is about 3.47-3.50 g/cm3The hardness is high, the artificial diamond has low cost, and after a proper pretreatment process, the artificial diamond and a substrate can ensure good interface combination, so that the addition of the artificial diamond can improve the hardness and the thermal conductivity of the artificial diamond while reducing the density of the whole material.
Mechanical alloying as a solid-state non-equilibrium processing technology can activate powder particles, uniformly mix the powder to form ultrafine powder particles, and can also achieve interatomic bonding among all components to form uniform solid solutions or compounds. The hot-pressing sintering technology is to fill dry powder into a mold, and then to heat while pressurizing from a uniaxial direction, so that the molding and sintering are completed simultaneously. Therefore, the method can be used for preparing the low-density heat-resistant NiAl/diamond reinforced iron-based alloy, and lays a theoretical foundation for the research and development of high-power-density diesel engine cylinder cover materials in the future.
Disclosure of Invention
The invention aims to provide a low-density heat-resistant iron-based alloy and a preparation method thereof, and the low-density heat-resistant NiAl/diamond reinforced iron-based alloy is prepared, and the obtained product has low cost, high purity, low density and high heat conductivity.
The technical scheme adopted by the invention is as follows:
the preparation method of the low-density heat-resistant iron-based alloy is characterized by comprising the following steps of:
the method is realized by the following steps:
ni powder and Al powder are adopted to react in the process of mechanical alloying to generate NiAl powder particles with a nano B2 ordered structure, diamond is pretreated by a proper process to form a uniform tungsten coating layer on the surface of the diamond, then NiAl powder and pretreated diamond powder are filled into a ball milling tank and are continuously and uniformly mixed with Fe powder to obtain fine and uniform NiAl/diamond enhanced Fe-based alloy composite powder, and the fine and uniform NiAl/diamond enhanced Fe-based alloy composite powder is sintered by hot pressing to obtain a block composite material so as to obtain a low-density heat-resistant NiAl/diamond enhanced Fe-based material, namely a low-density heat-resistant Fe-based alloy.
The preparation method of the low-density heat-resistant iron-based alloy is characterized by comprising the following steps of:
the preparation method specifically comprises the following steps:
the method comprises the following steps: according to the material: grinding ball = 1: 10, proportioning Ni powder and Al powder according to an atomic ratio of 1:1, and then putting the mixture into a ball milling tank which is vacuumized and filled with argon for ball milling, so that the Ni powder and the Al powder are uniformly mixed and completely dissolved to obtain fine and uniform nano NiAl powder with a B2 structure;
step two: diamond pretreatment:
diamond powder, copper powder and tungsten powder are mixed according to the mass ratio of 75%: 20%: 5 percent of the mixture is washed, dried and subjected to vacuum heat treatment; sieving powder by using sieves of 200 meshes, 300 meshes and 400 meshes in sequence, removing copper powder and redundant tungsten powder, and finally obtaining tungsten-coated diamond powder;
step three: weighing 35-50% of Fe powder, 35-50% of NiAl powder with a nanoscale B2 structure and not more than 30% of tungsten-coated diamond powder according to mass fraction;
step four: mixing Fe powder and NiAl powder with a B2 structure according to the mass percent of 1:1, adding tungsten-coated diamond powder with the mass percent of not more than 30%, mixing and ball-milling according to the ball-to-material ratio of 3:1 to obtain final alloy powder;
step five: and filling the final alloy powder obtained in the fourth step into a graphite die, and carrying out hot-pressing sintering to form the required block composite material.
In the first step, ball milling is carried out at the rotating speed of 250r/min, and the running/stopping interval time is 30min, which is 70h in total.
In the second step, the concrete steps of washing, drying and vacuum heat treatment are as follows:
acid washing, namely washing with hydrochloric acid with the mass percentage concentration of 10 percent at the temperature of 60 ℃ for 30min → absolute ethyl alcohol ultrasonic washing for 20min → acetone ultrasonic washing for 20min → absolute ethyl alcohol ultrasonic washing for 20min → 85 ℃ drying → dried mixed powder is subjected to vacuum heat treatment at 1000 ℃ for 60 min.
In the fourth step, the rotation speed of the ball mill is 100r/min, and the time is 5 h.
In the fifth step, the vacuum degree of the hot-pressing sintering is 6.67 multiplied by 10-3And Pa, heating the hot-pressed sintering to the target temperature 1050 ℃ at the heating rate of 10 ℃/min, preserving the heat for 60min, and then cooling to the room temperature along with the furnace.
The low-density heat-resistant iron-based alloy prepared by the preparation method of the low-density heat-resistant iron-based alloy.
The invention has the following advantages:
1. the nanometer NiAl powder with the B2 structure is obtained by mechanically alloying Ni powder and Al powder with the atomic ratio of 1:1, and the powder has small particle size and higher purity; after the artificial diamond is pretreated by a proper process, the artificial diamond is finally tungsten-coated diamond powder so as to be beneficial to improving the interface bonding strength of the artificial diamond and a substrate; the iron powder is added after the nanometer NiAl powder with the B2 structure and the tungsten-coated diamond powder are obtained, the reaction of the nanometer NiAl powder with the B2 structure is more complete, and the diamond is more uniformly distributed in a NiAl/Fe matrix.
2. In the mechanical alloying process, the mass fraction of diamond in the NiAl/diamond reinforced Fe-based alloy is adjusted according to the addition of diamond powder, in the obtained product, the mass fraction of Fe is 35-50%, the mass fraction of NiAl with a B2 structure is 35-50%, and the mass fraction of diamond is 0-30%, so that the density of the material is reduced, and the mechanical property and the thermophysical property of the material are improved.
3. The mechanical alloying technology is combined with the hot-pressing sintering technology, and the developed low-density heat-resistant NiAl/diamond reinforced Fe-based alloy has the application potential of being applied to high-power-density diesel engine cylinder head materials.
Drawings
FIG. 1 shows the results of the morphology and point analysis of the synthetic diamond after pretreatment in example 1.
FIG. 2 is a scanning electron micrograph of the bulk composite after hot press sintering of example 3.
FIG. 3 shows the results of line scan testing of the composite block made in example 4.
Detailed Description
The present invention will be described in detail with reference to specific embodiments.
The invention relates to a low-density heat-resistant iron-based alloy and a preparation method thereof, in particular to a preparation method of a low-density heat-resistant NiAl/diamond reinforced Fe-based alloy, which adopts Ni powder and Al powder to react in the mechanical alloying process to generate NiAl powder particles with a nano B2 ordered structure, diamond is pretreated by a proper process to form a uniform tungsten coating on the surface of the diamond, then NiAl powder and pretreated diamond powder are filled into a ball milling tank and are continuously and uniformly mixed with Fe powder to obtain fine and uniform NiAl/diamond reinforced Fe-based alloy composite powder, and then hot-press sintering is carried out to obtain a block composite material so as to obtain the low-density heat-resistant NiAl/diamond reinforced Fe-based alloy. The method comprises the following steps:
the method comprises the following steps: according to the material: grinding ball = 1: 10, proportioning Ni powder and Al powder according to the atomic ratio of 1:1, putting the mixture into a ball-milling tank which is vacuumized and filled with argon, and carrying out ball milling at the rotating speed of 250r/min, wherein the running/stopping interval time is 30min, and the total time is 70h, so that the Ni powder and the Al powder are uniformly mixed and completely dissolved to obtain fine and uniform nano NiAl powder with a B2 structure.
Step two: diamond pretreatment: diamond powder, copper powder and tungsten powder are mixed according to the mass ratio of 75%: 20%: 5 percent of the raw materials are pretreated after being matched, and the method comprises the following specific steps: acid washing (hydrochloric acid concentration 10% (mass percent), temperature 60 ℃ cleaning 30 min) → absolute ethanol ultrasonic cleaning 20min → acetone ultrasonic cleaning 20min → absolute ethanol ultrasonic cleaning 20min → 85 ℃ drying. Then, the dried mixed powder is subjected to vacuum heat treatment at 1000 ℃ for 60 min. And sequentially sieving powder by using sieves of 200 meshes, 300 meshes and 400 meshes to remove copper powder and redundant tungsten powder, and finally obtaining tungsten-coated diamond powder.
Step three: weighing 35-50% of Fe powder, 35-50% of NiAl powder with a nanoscale B2 structure and 0-30% of pretreated diamond powder according to mass percentage.
Step four: and after the Fe powder and the NiAl powder with the B2 structure are proportioned according to the mass percent of 1:1, adding diamond powder with the mass percent of 0-30% and continuously mixing for 5 hours in a ball mill with the ball-material ratio of 3:1 and the rotating speed of 100r/min to obtain the final alloy powder.
Step five: filling the composite powder obtained in the fourth step into a graphite die, and forming the required block composite material by hot-pressing sintering; wherein the sintering temperature is 1050 ℃, and the sintering pressure is 20 MPa.
In the first step, the third step and the fourth step, the nano NiAl powder and the composite powder with the B2 structure are respectively prepared by adopting a step-by-step ball milling method.
In the second step, a uniform tungsten-containing transition layer is formed on the surface of the diamond after pretreatment, and the interface bonding strength between the diamond and a substrate NiAl/Fe can be improved after hot-pressing sintering in the fifth step.
In the fifth step, the hot-pressing sintering process comprises the following steps: the degree of vacuum was 6.67X 10-3Pa, hot pressingAnd (3) heating to the target temperature 1050 ℃ at the heating rate of 10 ℃/min, preserving the temperature for 60min, and then cooling to the room temperature along with the furnace.
Example 1:
putting Ni powder (20.55g) and Al powder (9.45g) into a zirconium dioxide ball-milling tank according to the atomic ratio of the raw materials of 1:1, adding 300g of zirconium dioxide milling balls with the diameter of 10mm, vacuumizing the ball-milling tank and filling argon after sealing by an O-shaped sealing ring before ball-milling, carrying out ball-milling at the rotating speed of 250r/min, carrying out operation/stop interval time of 30min, and carrying out mixed ball-milling for 70h in total to obtain the fine and uniform nano NiAl powder with the B2 structure.
According to the mass ratio of 75%: 20%: 5 percent of artificial diamond powder (75.00 g), copper powder (20.00 g) and tungsten powder (5.00g) are proportioned and pretreated according to the following process: acid washing (hydrochloric acid concentration 10% (mass percent), temperature 60 ℃ cleaning 30 min) → absolute ethanol ultrasonic cleaning 20min → acetone ultrasonic cleaning 20min → absolute ethanol ultrasonic cleaning 20min → 85 ℃ drying. Then, the dried mixed powder is subjected to vacuum heat treatment at 1000 ℃ for 60 min. And sequentially sieving powder by using sieves of 200 meshes, 300 meshes and 400 meshes to remove copper powder and redundant tungsten powder, and finally obtaining tungsten-coated diamond powder. And testing and observing the micro morphology and line scanning of the powder by using a Hitachi5-2500 scanning electron microscope after the powder is sprayed with gold. FIG. 1 shows the results of the morphology and point analysis of the synthetic diamond after pretreatment in example 1. As can be seen from FIG. 1, the diamond surface after pretreatment is rough and a tungsten-plated layer is formed.
Example 2:
according to the mass fraction of the raw materials: 50.00% Fe powder (50.00g) and 50.00% NiAl (50.00g) powder obtained in example 1 were put into a stainless steel ball mill pot, and mixed for 5 hours in a ball mill at a ball-to-material ratio of 3:1 and a rotation speed of 100r/min to obtain the final alloy powder.
30g of the mixture powder prepared in example 2 was weighed, charged into a high-strength graphite mold, and sintered in a hot-pressing sintering furnace (ZT-40-20Y) manufactured by Shanghai Chenghua electric furnace Co., Ltd. The main sintering process parameters are as follows: the degree of vacuum was 6.67X 10-3Pa, heating up to 1050 ℃ at the heating rate of 10 ℃/min in hot-pressing sintering and preserving heat for 60miAnd n, cooling to room temperature along with the furnace to finally obtain the nanometer NiAl phase reinforced iron-based alloy sintered body with the B2 structure with the mass fraction of 50%.
The sintered body is machined into a certain size through mechanical cutting, and according to the specific operation of experimental polishing, firstly, after being polished on sand paper, the sintered body is polished on a polishing machine, the density, the hardness and the thermal conductivity of the sintered body are tested, and the result is as follows: the density was measured to be 6.67g/cm3The hardness is 68.8HRC, and the room-temperature thermal conductivity is 17.41W/(m.K). The density of the material is higher than that of the prior common cast iron cylinder cover material (the density is about 7.3 g/cm)3) The reduction is 8.63%.
Example 3:
according to the mass fraction of the raw materials: 47.50% of Fe powder (47.50g), 47.50% of NiAl powder (47.50g) obtained in example 1 and 5.00% of diamond powder (5.00g) after pretreatment are placed in a stainless steel ball milling tank, grinding balls are stainless steel grinding balls, and the stainless steel grinding balls are mixed for 5 hours in a ball mill with the ball-material ratio of 3:1 and the rotating speed of 100r/min, so that fine and uniform 5.0% of diamond/NiAl reinforced Fe-based composite powder is obtained.
30g of the mixture powder prepared in example 3 was weighed, charged into a high-strength graphite mold, and sintered in a hot-pressing sintering furnace (ZT-40-20Y) manufactured by Shanghai Chenghua electric furnace Co., Ltd. The specific sintering process was the same as in example 2. The specimens were cut and tested as in example 2,
cutting a sample, grinding and polishing according to the method in the embodiment 2, and observing the microstructure morphology of the processed sample by using a Hitachi5-2500 scanning electron microscope. FIG. 2 is a scanning electron micrograph of the bulk composite after hot press sintering of example 4. As can be seen from fig. 2, the fine-grained diamond phase (black particles) is uniformly distributed in the matrix. The density was measured to be 6.07g/cm3The hardness is 55.5HRC, and the room-temperature thermal conductivity is 25.13W/(m.K). The density of the material is higher than that of the prior common cast iron cylinder cover material (the density is about 7.3 g/cm)3) The reduction was 16.85% and the thermal conductivity increased by about 44.34% over the material in example 2.
Example 4:
according to the mass fraction of the raw materials: 42.50 percent of Fe powder (42.50g), 42.50 percent of NiAl powder (42.50g) obtained in example 1 and 15.00 percent of diamond powder (15.00g) after pretreatment are put into a stainless steel ball milling tank, the grinding balls are stainless steel grinding balls, and the stainless steel grinding balls are mixed for 5 hours in a ball mill with the ball-material ratio of 3:1 and the rotating speed of 100r/min, so as to obtain fine and uniform 15.0 percent of diamond/NiAl reinforced Fe-based composite powder.
30g of the mixture powder prepared in example 4 was weighed, charged into a high-strength graphite mold, and sintered in a hot-pressing sintering furnace (ZT-40-20Y) manufactured by Shanghai Chenghua electric furnace Co., Ltd. The specific sintering process was the same as in example 2.
Cutting a sample, grinding and polishing according to the method in the embodiment 2, and observing the microstructure morphology of the processed sample by using a Hitachi5-2500 scanning electron microscope. FIG. 3 shows the results of line scan testing of the composite block made in example 4. As can be seen from FIG. 3, a white uniform tungsten-containing transition layer appears on the joint surface of the diamond and the matrix in the sintered block material, and the joint strength between the diamond and the matrix is effectively improved. The density was measured to be 5.53g/cm3The hardness is 69.15HRC, and the room-temperature thermal conductivity is 49.2W/(m.K). The density of the material is higher than that of the prior common cast iron cylinder cover material (the density is about 7.3 g/cm)3) The reduction is 24.25% and the thermal conductivity is improved by about 182.60% compared to the material in example 2.
Example 5:
according to the mass fraction of the raw materials: 35.00% of Fe powder (35.00g), 35.00% of NiAl powder (35.00g) obtained in example 1 and 30.00% of diamond powder (30.00g) after pretreatment are put into a stainless steel ball milling tank, and the stainless steel ball milling tank is used for milling stainless steel balls, and the stainless steel ball milling tank are mixed for 5 hours in a ball mill with a ball-material ratio of 3:1 and a rotating speed of 100r/min, so that fine and uniform 30.0% diamond/NiAl reinforced Fe-based composite powder is obtained.
30g of the mixture powder prepared in example 6 was weighed, charged into a high-strength graphite mold, and sintered in a hot-pressing sintering furnace (ZT-40-20Y) manufactured by Shanghai Chenghua electric furnace Co., Ltd. The specific sintering process was the same as in example 2. The specimens were cut and tested as in example 2 with the following results: the density was measured to be 5.03g/cm3The hardness is 61.12HRC, and the room-temperature thermal conductivity is 55.1W/(m.K). The density of the material is higher than that of the prior common cast iron cylinder cover material (the density is about 7.3 g/cm)3) The reduction of 31.10 percent and the higher heat conductivityThe material in example 2 was improved by about 216.48%.
The invention is not limited to the examples, and any equivalent changes to the technical solution of the invention by a person skilled in the art after reading the description of the invention are covered by the claims of the invention.
Claims (6)
1. The preparation method of the low-density heat-resistant iron-based alloy is characterized by comprising the following steps of:
the method is realized by the following steps:
ni powder and Al powder are adopted to react in the process of mechanical alloying to generate NiAl powder particles with a nano B2 ordered structure, diamond is pretreated by a proper process to form a uniform tungsten coating layer on the surface of the diamond, then NiAl powder and pretreated diamond powder are filled into a ball milling tank and are continuously and uniformly mixed with Fe powder to obtain fine and uniform NiAl/diamond enhanced Fe-based alloy composite powder, and then hot-pressing sintering is carried out to obtain a block composite material to obtain a low-density heat-resistant NiAl/diamond enhanced Fe-based material, namely a low-density heat-resistant Fe-based alloy;
the preparation method specifically comprises the following steps:
the method comprises the following steps: according to the material: grinding ball = 1: 10, proportioning Ni powder and Al powder according to an atomic ratio of 1:1, and then putting the mixture into a ball milling tank which is vacuumized and filled with argon for ball milling, so that the Ni powder and the Al powder are uniformly mixed and completely dissolved to obtain fine and uniform nano NiAl powder with a B2 structure;
step two: diamond pretreatment:
diamond powder, copper powder and tungsten powder are mixed according to the mass ratio of 75%: 20%: 5 percent of the mixture is washed, dried and subjected to vacuum heat treatment; sieving powder by using sieves of 200 meshes, 300 meshes and 400 meshes in sequence, removing copper powder and redundant tungsten powder, and finally obtaining tungsten-coated diamond powder;
step three: weighing 35-50% of Fe powder, 35-50% of NiAl powder with a nanoscale B2 structure and not more than 30% of tungsten-coated diamond powder according to mass fraction;
step four: mixing Fe powder and NiAl powder with a B2 structure according to the mass percent of 1:1, adding tungsten-coated diamond powder with the mass percent of not more than 30%, mixing and ball-milling according to the ball-to-material ratio of 3:1 to obtain final alloy powder;
step five: and filling the final alloy powder obtained in the fourth step into a graphite die, and carrying out hot-pressing sintering to form the required block composite material.
2. The method of preparing a low-density heat-resistant iron-based alloy according to claim 1, wherein:
in the first step, ball milling is carried out at the rotating speed of 250r/min, and the running/stopping interval time is 30min, which is 70h in total.
3. The method of preparing a low-density heat-resistant iron-based alloy according to claim 1, wherein:
in the second step, the concrete steps of washing, drying and vacuum heat treatment are as follows:
acid washing, namely washing with hydrochloric acid with the mass percentage concentration of 10 percent at the temperature of 60 ℃ for 30min → absolute ethyl alcohol ultrasonic washing for 20min → acetone ultrasonic washing for 20min → absolute ethyl alcohol ultrasonic washing for 20min → 85 ℃ drying → dried mixed powder is subjected to vacuum heat treatment at 1000 ℃ for 60 min.
4. The method of preparing a low-density heat-resistant iron-based alloy according to claim 1, wherein:
in the fourth step, the rotation speed of the ball mill is 100r/min, and the time is 5 h.
5. The method of preparing a low-density heat-resistant iron-based alloy according to claim 1, wherein:
in the fifth step, the vacuum degree of the hot-pressing sintering is 6.67 multiplied by 10-3And Pa, heating the hot-pressed sintering to the target temperature 1050 ℃ at the heating rate of 10 ℃/min, preserving the heat for 60min, and then cooling to the room temperature along with the furnace.
6. The low-density heat-resistant iron-based alloy according to claim 1.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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