CN110640156B - A kind of gas atomization preparation process of iron powder for additive manufacturing and repair - Google Patents
A kind of gas atomization preparation process of iron powder for additive manufacturing and repair Download PDFInfo
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Abstract
一种增材制造与修复用铁粉的气雾化制备工艺，将镍硼合金、钒铁合金、铁、镍、石墨碳颗粒和铬制备母合金电极棒；将母合金电极棒转输进至感应加热室，母合金电极切割感应线圈内的磁感线产生热，熔化母合金电极棒为金属熔液，金属熔液流从感应加热室流入雾化室，通过高压氩气喷口通入氩气进行雾化操作，使得金属熔液流在超音速氩气气流的撞击下破碎成液滴，冷却即可。本发明提出制粉过程中气体介质的温度对粉末流动性及收得率有较为显著的影响，通过多工艺耦合优化设计，得到球形度好、流动性好、含氧量低，可作为航空航天、国防军工、医疗器械、汽车制造、注塑模具等领域高硬度复杂精密结构件增材制造与修复用的粉末材料。
A gas atomization preparation process of iron powder for additive manufacturing and repairing, preparing master alloy electrode rods from nickel-boron alloy, vanadium-iron alloy, iron, nickel, graphite carbon particles and chromium; In the heating chamber, the magnetic induction line in the induction coil is cut by the mother alloy electrode to generate heat, and the electrode rod of the mother alloy is melted into a molten metal. The atomization operation makes the molten metal flow break into droplets under the impact of the supersonic argon gas flow, and then it can be cooled. The invention proposes that the temperature of the gas medium in the pulverizing process has a relatively significant effect on the powder fluidity and yield. Through the multi-process coupling optimization design, good sphericity, good fluidity and low oxygen content are obtained, which can be used as aerospace materials. , national defense and military industry, medical equipment, automobile manufacturing, injection molds and other fields of high hardness and complex precision structural parts additive manufacturing and repair powder materials.
Description
Technical Field
The invention belongs to the field of preparation of raw materials of metal additive manufacturing and repairing technologies, and particularly relates to a gas atomization preparation process of iron powder for additive manufacturing and repairing.
Background
Compared with the traditional machining 'material reduction manufacturing', the material increase manufacturing and repairing are the bottom-up addition manufacturing processes based on the raw material dispersion-accumulation principle. The metal additive manufacturing and repairing technology is manufactured and repaired layer by using special metal powder materials in a melting mode, a spraying mode and the like, can be used for manufacturing and repairing single-piece small-batch complex components such as turbine engine working blades, airplane landing gears, airplane engines, industrial gas turbines and the like, and has important application value in the additive manufacturing and repairing of complex curved surface components in the fields of aerospace, national defense and military industry, medical instruments, automobile manufacturing, injection molds and the like.
The quality of the raw material powder for additive manufacturing and repairing directly relates to the formability in the additive manufacturing process and the quality of a final formed part, is different from the traditional powder metallurgy raw material, and the additive manufacturing and repairing process has higher requirements on the yield, the fluidity, the purity and the like of metal powder.
The powder preparation method widely used at present mainly comprises the following steps: vacuum induction gas atomization, plasma rotating electrode atomization powder making and electrode induction gas atomization. In the vacuum induction gas atomization powder preparation method, liquid metal is contacted with the inner wall of a crucible and a ceramic discharge spout in the smelting and atomization processes, so that metal melt is easily polluted, and the preparation of powder with high impurity content requirement is difficult to meet. The average particle size of the powder prepared by the plasma rotary electrode atomization method is relatively large, and the production cost is high. The EIGA (electrochemical induced atomization) powder making technology is an advanced powder making technology at present, molten metal does not contact with a crucible and a liquid guide tube in the powder making process, instantaneous smelting atomization is performed, impurity elements are effectively prevented from being mixed, powder impurities are controllable, and the purity is high. However, the preparation method is a complex multi-factor coupling process, and is influenced by interaction of multiple process parameters such as atomization pressure and smelting temperature and multiple factors such as physical and chemical properties of the material, and the influence mechanism of each factor on the powder performance needs to be proved by multi-factor coupling optimization design of the iron powder preparation process, so that high-quality and high-hardness iron powder suitable for additive manufacturing and repair can be prepared.
Disclosure of Invention
The invention aims to provide a gas atomization preparation process of iron powder for additive manufacturing and repairing, the process can prepare high-hardness iron powder with high sphericity and good fluidity (14.1s/50g), wherein the percentage of powder with the particle size distribution in the range of 53-180 mu m is up to 68.24%, the oxygen content is lower than 0.008%, and the process cost is low, so that the requirements of high-quality additive manufacturing and repairing are met.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
an air atomization preparation process of iron powder for additive manufacturing and repairing comprises the following steps:
1) according to the mass percentage, 0.12-0.2% of C, 1.5-2.8% of Ni, 0.5-1% of Si, 16-17% of Cr, 0.4-1% of B, 0.1-0.3% of V, less than or equal to 0.03% of P, less than or equal to 0.03% of S, and the balance of Fe; preparing a master alloy electrode rod from a nickel-boron alloy, a ferrovanadium alloy, iron, nickel, graphite carbon particles and chromium;
2) transferring the master alloy electrode bar into an induction heating chamber, adjusting smelting power, cutting a magnetic induction line in an induction coil by the master alloy electrode to generate heat, and melting the master alloy electrode bar into molten metal;
3) under the action of pressure difference between the induction heating chamber and the atomizing chamber, enabling the molten metal flow to flow into the atomizing chamber from the induction heating chamber, and introducing argon through a high-pressure argon nozzle to carry out atomizing operation, so that the molten metal flow is crushed into liquid drops under the impact of supersonic argon gas flow;
4) and cooling the liquid drops in an atomizing chamber, solidifying the liquid drops into spherical powder, and screening the spherical powder to obtain the iron powder for additive manufacturing and repairing.
The further improvement of the invention is that in the step 1), the nickel-boron alloy, the ferrovanadium alloy, the iron, the nickel, the graphite carbon particles and the chromium are prepared into the master alloy electrode bar by adopting the vacuum induction smelting and vacuum consumable remelting technology.
The further improvement of the invention is that in the step 2), the smelting power is 15-25 kW.
The further improvement of the invention is that before the step 3), the atomizing chamber is vacuumized, then argon is filled, and the induction heating chamber and the atomizing chamber are respectively adjusted to be positive pressure and negative pressure.
The further improvement of the invention is that in the step 3), when the liquid flow freely falls to a high-pressure argon nozzle of the atomizing chamber, argon is introduced through the high-pressure argon nozzle to carry out atomizing operation.
The invention is further improved in that in the step 4), the pressure difference between the induction heating chamber and the atomizing chamber is 33.5-36.5 kPa.
The invention is further improved in that in the step 4), the temperature of argon is within the range of 20-80 ℃, and the atomization pressure is within the range of 1.0-2.0 MPa.
The further improvement of the invention is that in the step 4), the particle size of the iron powder for additive manufacturing and repairing is 53-180 μm.
Compared with the prior EIGA powder preparation technology, the invention has the beneficial effects that the yield of the high-hardness iron powder prepared by the process is obviously improved within the granularity range (53-180 mu m) required by the additive manufacturing and repairing technology, and the cost of powder consumables is obviously reduced. In addition, the invention provides that the temperature of the gas medium has more remarkable influence on the fluidity and yield of the powder in the powder preparation process, and the powder material which has good sphericity, good fluidity and low oxygen content and can be used for material increase manufacturing and repairing of high-hardness complex precise structural parts in the fields of aerospace, national defense and military industry, medical instruments, automobile manufacturing, injection molds and the like is obtained through multi-process coupling optimization design.
Furthermore, the smelting power range of the induction coil is 15-25 kW, and the standard deviation of powder distribution can be controlled to fluctuate within the range of 1.65-1.70 through regulation and control of the smelting power, wherein the standard deviation is the smallest when the smelting power is 20kW, and the powder distribution is the most concentrated; through the adjustment of the smelting power, the fluctuation of the powder yield within the range of 56.04-60.59 percent can be controlled, along with the increase of the smelting power, the alloy liquid drops are not easy to form balls, irregular waste slag is easy to form, the powder yield is reduced,
further, the temperature range of argon is 20-80 ℃, the standard deviation of powder distribution can be controlled to fluctuate within the range of 1.66-1.70 through the regulation and control of the temperature of atomizing gas, wherein the powder distribution is most dispersed when the temperature of atomizing gas is 40 ℃; the powder yield can be controlled to fluctuate within the range of 54.88-61.23% by adjusting the temperature of the atomizing gas, wherein the yield reaches 61.23% when the temperature of the atomizing gas is 40 ℃; through the adjustment of the temperature of the atomizing gas, the powder flowability can be controlled to fluctuate within the range of 12.83-13.48 s/50g, wherein the powder flowability reaches 13.48s/50g when the temperature of the atomizing gas is 40 ℃.
Furthermore, the atomization pressure range is 1.0-2.0 MPa, the fluctuation of the median particle size of the powder in the range of 87.6-100.03 mu m can be controlled through the regulation and control of the atomization pressure, and the larger the atomization pressure is, the smaller the median particle size is; through the adjustment of the atomization pressure, the standard deviation of the powder distribution can be controlled to fluctuate within the range of 1.65-1.73, wherein the powder distribution is most dispersed when the atomization pressure is 1.5 MPa; the powder yield can be controlled to fluctuate within the range of 51.88-64.53% by adjusting the atomization pressure, wherein the powder yield can reach 64.53% when the atomization pressure is 1.5 MPa; through the adjustment of the atomization pressure, the powder fluidity can be controlled to fluctuate within the range of 12.84-13.59 s/50g, and the powder fluidity is improved along with the increase of the atomization pressure. The invention adopts the coupling optimization process of the temperature of the atomizing gas, the smelting power and the atomizing pressure, and has more remarkable improvement effects on the yield and the particle size distribution of the powder and the inhibition of the satellite powder.
Drawings
FIG. 1 shows the effect of smelting power on powder properties.
FIG. 2 is a graph showing the effect of atomizing gas temperature on powder properties.
Fig. 3 is a graph of the effect of atomization pressure on powder properties.
Fig. 4 shows the surface morphology of the high-hardness martensite powder prepared in examples 2, 4 and 8. Wherein (a) is example 4, (b) is example 8, (c) is example 2, and (d) is example 8.
FIG. 5 is a graph showing the particle size distribution under each parameter of the orthogonal test in examples 1 to 9. Wherein (a) is example 1, (b) is example 2, (c) is example 3, (d) is example 4, (e) is example 5, (f) is example 6, (g) is example 7, (h) is example 8, and (i) is example 9.
Detailed Description
The present invention will be described in further detail with reference to specific examples according to the spirit of the present invention.
The invention provides a preparation process of high-hardness powder for additive manufacturing and repair based on an EIGA (enhanced inert gas oxygen gas) powder preparation technology, which is a method for realizing regulation and control of the yield and the fluidity of high-hardness iron powder by researching and finding an influence mechanism of gas medium temperature on the fluidity and the yield of the powder and by means of the optimization of coupling processes of regulating the gas medium temperature, smelting power and atomizing pressure based on the traditional EIGA powder preparation technology. The method specifically comprises the following steps:
s1, preparing raw materials: selecting nickel-boron alloy, ferrovanadium alloy, metallic iron, high-purity nickel, graphite carbon particles and metallic chromium as raw materials for smelting and preparing the master alloy according to the component proportion requirement;
s2, preparing a master alloy: the method comprises the following steps of preparing 300 kg of mother alloy electrode rods by combining a Vacuum Induction Melting (VIM) technology with a vacuum consumable remelting (VAR) technology, wherein the mother alloy comprises, by mass, 0.12-0.2% of C, 1.5-2.8% of Ni, 0.5-1% of Si, 16-17% of Cr, 0.4-1% of B, 0.1-0.3% of V, less than or equal to 0.03% of P, less than or equal to 0.03% of S, and the balance of Fe;
s3, the EIGA powder making process comprises the following steps:
1) 300 kg of the homogenized mother alloy bar stock with the size of phi 45 multiplied by 600mm is arranged in a feeding chamber;
2) vacuumizing the atomizing chamber, filling more than 99.999 percent of high-purity argon when the pressure is reduced to be below 0.1Pa, and regulating the induction heating chamber and the atomizing chamber to be micro-positive pressure and micro-negative pressure respectively through the air guide tube; facilitating the flow of liquid from the heating chamber to the atomizing chamber.
3) Conveying the mother alloy bar to an induction heating chamber by rotating an automatic feeding system, adjusting the smelting power to be within the range of 15-25 kW, then cutting a bar into magnetic induction lines in an induction coil to generate heat, and melting the mother alloy bar to be molten metal;
4) under the action of micro pressure difference (33.5-36.5 kPa), molten metal flows into a guide pipe from an induction heating chamber and flows into an atomizing chamber from the guide pipe, when the molten metal flows freely fall to a high-pressure argon nozzle, high-purity argon (99.999%) is started to carry out atomizing operation, the argon temperature and the atomizing pressure are adjusted, the argon temperature is in the range of 20-80 ℃ (preferably 30-80 ℃), and the atomizing pressure is in the range of 1.0-2.0 MPa, so that the alloy liquid flows are crushed into liquid drops under the impact of supersonic argon gas flow;
5) the liquid drops are naturally cooled in the atomizing chamber, and finally solidified into spherical powder which falls into a powder collecting bin;
s4, powder screening and collecting: and under the protection of inert gas, carrying out mechanical vibration and airflow classification screening on the metal powder in the powder collection bin, and carrying out vacuum-pumping sealing packaging on the screened high-hardness powder with the particle size range of 53-180 mu m for additive manufacturing and repairing.
In the step S3, the size of the master alloy bar is phi 45 × 600mm, and in S3, the induction heating chamber and the atomization chamber regulated by the gas guide tube 2) are respectively in micro positive pressure and micro negative pressure, and the pressure difference between the induction heating chamber and the atomization chamber is 33.5-36.5 kPa.
In the step S3, the smelting power range of the induction coil is 15 to 25kW, and the standard deviation of the powder distribution can be controlled to fluctuate within a range of 1.65 to 1.70 by regulating and controlling the smelting power, wherein the standard deviation is the smallest when the smelting power is 20kW, and the powder distribution is the most concentrated; through the adjustment of the smelting power, the fluctuation of the powder yield within the range of 56.04-60.59% can be controlled, along with the increase of the smelting power, alloy liquid drops are not easy to form balls, irregular waste residues are easy to form, and the powder yield is reduced, as shown in figure 1.
In the step S3, the temperature range of the argon gas is 20 to 80 ℃, and the standard deviation of the powder distribution can be controlled to fluctuate within a range of 1.66 to 1.70 by regulating and controlling the temperature of the atomizing gas, wherein the powder distribution is most dispersed when the temperature of the atomizing gas is 40 ℃; the powder yield can be controlled to fluctuate within the range of 54.88-61.23% by adjusting the temperature of the atomizing gas, wherein the yield reaches 61.23% when the temperature of the atomizing gas is 40 ℃; through the adjustment of the temperature of the atomizing gas, the powder flowability can be controlled to fluctuate within the range of 12.83-13.48 s/50g, wherein when the temperature of the atomizing gas is 40 ℃, the powder flowability reaches 13.48s/50g, as shown in figure 2.
In the step S3, the atomization pressure range (i.e., the pressure range of supersonic argon gas) is 1.0 to 2.0MPa, and the median particle size of the powder can be controlled to fluctuate within an interval of 87.6 to 100.03 μm by adjusting and controlling the atomization pressure, wherein the larger the atomization pressure is, the smaller the median particle size is; through the adjustment of the atomization pressure, the standard deviation of the powder distribution can be controlled to fluctuate within the range of 1.65-1.73, wherein the powder distribution is most dispersed when the atomization pressure is 1.5 MPa; the powder yield can be controlled to fluctuate within the range of 51.88-64.53% by adjusting the atomization pressure, wherein the powder yield can reach 64.53% when the atomization pressure is 1.5 MPa; through the adjustment of the atomization pressure, the powder fluidity can be controlled to fluctuate within the range of 12.84-13.59 s/50g, and the powder fluidity is improved along with the increase of the atomization pressure, as shown in figure 3.
The coupling optimization process of the temperature of the atomizing gas, the smelting power and the atomizing pressure provided by the invention has a remarkable improvement effect on the yield and the particle size distribution of the powder and the inhibition of the satellite powder, and is shown in fig. 2-4.
The alloy components adopted in the invention enable the finally prepared high-hardness iron powder to be high-hardness iron powder.
The following are specific examples.
Example 1
S1, preparing raw materials: selecting nickel-boron alloy, ferrovanadium alloy, metallic iron, high-purity nickel, graphite carbon particles and metallic chromium as raw materials for smelting and preparing the master alloy according to the component proportion requirement;
s2, preparing a master alloy: 300 kg of mother alloy electrode rods are prepared by combining Vacuum Induction Melting (VIM) with a vacuum consumable remelting (VAR) technology, and the mother alloy comprises, by mass, 0.16% of C, 2.0% of Ni, 1% of Si, 16% of Cr, 0.62% of B, 0.20% of V, 0.02% of P, 0.02% of S, and Fe: 79.9 percent;
s3, the EIGA powder making process comprises the following steps:
1) 300 kg of the homogenized mother alloy bar stock with the size of phi 45 multiplied by 600mm is arranged in a feeding chamber;
2) vacuumizing the atomizing chamber, filling more than 99.999 percent of high-purity argon when the pressure is reduced to be below 0.1Pa, and regulating the induction heating chamber and the atomizing chamber to be micro-positive pressure and micro-negative pressure respectively through the air guide tube; facilitating the flow of liquid from the heating chamber to the atomizing chamber.
3) Conveying the mother alloy bar to an induction heating chamber by an automatic feeding system in a rotating manner, adjusting the smelting power within the range of 15kW, then cutting the bar into magnetic induction lines in an induction coil to generate heat, and melting the mother alloy bar to obtain molten metal;
4) under the action of micro pressure difference, molten metal flows into a guide pipe from an induction heating chamber and flows into an atomizing chamber from the guide pipe, when the molten metal flows freely fall to a high-pressure argon nozzle, high-purity argon (99.999%) is started to carry out atomizing operation, the temperature and the atomizing pressure of the argon are adjusted, the temperature of the argon is within 20 ℃, and the atomizing pressure is within 1MPa, so that the alloy liquid flows are crushed into liquid drops under the impact of supersonic argon gas flow;
5) the liquid drops are naturally cooled in the atomizing chamber, and finally solidified into spherical powder which falls into a powder collecting bin;
s4, powder screening and collecting: and under the protection of inert gas, carrying out mechanical vibration and airflow classification screening on the metal powder in the powder collection bin, and carrying out vacuum-pumping sealing packaging on the screened high-hardness powder with the particle size range of 53-180 mu m for additive manufacturing and repairing.
Example 2
Example 2 is different from example 1 in that the master alloy is prepared with the master alloy composition shown in table 2, and the preparation process shown in table 1, and the rest is the same as example.
Example 3
Example 3 is different from example 1 in that the master alloy is prepared with the master alloy composition shown in table 2, and the preparation process shown in table 1, and the rest is the same as example.
Example 4
S1, preparing raw materials: selecting nickel-boron alloy, ferrovanadium alloy, metallic iron, high-purity nickel, graphite carbon particles and metallic chromium as raw materials for smelting and preparing the master alloy according to the component proportion requirement;
s2, preparing a master alloy: 300 kg of mother alloy electrode rods are prepared by combining Vacuum Induction Melting (VIM) with a vacuum consumable remelting (VAR) technology, and the mother alloy comprises, by mass, 0.19% of C, 2.05% of Ni, 1% of Si, 16% of Cr, 0.611% of B, 0.209% of V, 0.02% of P, 0.02% of S, and Fe: 79.9 percent;
s3, the EIGA powder making process comprises the following steps:
1) 300 kg of the homogenized mother alloy bar stock with the size of phi 45 multiplied by 600mm is arranged in a feeding chamber;
2) vacuumizing the atomizing chamber, filling more than 99.999 percent of high-purity argon when the pressure is reduced to be below 0.1Pa, and regulating the induction heating chamber and the atomizing chamber to be micro-positive pressure and micro-negative pressure respectively through the air guide tube; facilitating the flow of liquid from the heating chamber to the atomizing chamber.
3) Conveying the mother alloy bar to an induction heating chamber by an automatic feeding system in a rotating manner, adjusting the smelting power within the range of 15kW, then cutting the bar into magnetic induction lines in an induction coil to generate heat, and melting the mother alloy bar to obtain molten metal;
4) under the action of micro pressure difference, molten metal flows into a guide pipe from an induction heating chamber and flows into an atomizing chamber from the guide pipe, when the molten metal flows freely fall to a high-pressure argon nozzle, high-purity argon (99.999%) is started to carry out atomizing operation, the temperature and the atomizing pressure of the argon are adjusted, the temperature of the argon is within 40 ℃, and the atomizing pressure is within 1.5MPa, so that the alloy liquid flows are crushed into liquid drops under the impact of supersonic argon gas flow;
5) the liquid drops are naturally cooled in the atomizing chamber, and finally solidified into spherical powder which falls into a powder collecting bin;
s4, powder screening and collecting: and under the protection of inert gas, carrying out mechanical vibration and airflow classification screening on the metal powder in the powder collection bin, and carrying out vacuum-pumping sealing packaging on the screened high-hardness powder with the particle size range of 53-180 mu m for additive manufacturing and repairing. The composition of the powder is shown in Table 2.
The preparation process of this example 4 includes that the temperature of the atomizing gas is 40 ℃, the melting power is 15kW, the atomizing pressure is 1.5MPa, and the pressure difference between the induction heating chamber and the atomizing chamber is 35kPa, so that the surface morphology of the prepared powder is good, the powder fluidity is 13.40s/50g, and the mass ratio of the powder with the particle size distribution of 53-180 μm is up to 68.24% (shown in table 1). The powder obtained in inventive example 4 had an oxygen content of 46ppm and a nitrogen content of 45 ppm.
Example 5
Example 5 differs from example 1 in that the preparation process is as shown in table 1, and the rest is the same as example 1.
Example 6
Example 6 differs from example 1 in that the preparation process is as shown in table 1, and the rest is the same as example 1.
Example 7
Example 7 differs from example 1 in that the preparation process is as shown in table 1, and the rest is the same as example 1.
Example 8
Example 8 differs from example 1 in that the preparation process is as shown in table 1, and the rest is the same as example 1.
Example 9
Example 9 differs from example 1 in that the preparation process is as shown in table 1, otherwise it is the same as example 1.
Example 10
S1, preparing raw materials: selecting nickel-boron alloy, ferrovanadium alloy, metallic iron, high-purity nickel, graphite carbon particles and metallic chromium as raw materials for smelting and preparing the master alloy according to the component proportion requirement;
s2, preparing a master alloy: the method comprises the following steps of preparing 300 kg of mother alloy electrode rods by combining Vacuum Induction Melting (VIM) with a vacuum consumable remelting (VAR) technology, wherein the mother alloy comprises, by mass, 0.12% of C, 2.8% of Ni, 1% of Si, 16% of Cr, 1% of B, 0.30% of V, 0.03% of P, 0.02% of S and the balance of Fe;
s3, the EIGA powder making process comprises the following steps:
1) 300 kg of the homogenized mother alloy bar stock with the size of phi 45 multiplied by 600mm is arranged in a feeding chamber;
2) vacuumizing the atomizing chamber, filling more than 99.999 percent of high-purity argon when the pressure is reduced to be below 0.1Pa, and regulating the induction heating chamber and the atomizing chamber to be micro-positive pressure and micro-negative pressure respectively through the air guide tube; facilitating the flow of liquid from the heating chamber to the atomizing chamber.
3) Conveying the mother alloy bar to an induction heating chamber by an automatic feeding system in a rotating manner, adjusting the smelting power within the range of 15kW, then cutting the bar into magnetic induction lines in an induction coil to generate heat, and melting the mother alloy bar to obtain molten metal;
4) under the action of micro pressure difference, molten metal flows into a guide pipe from an induction heating chamber and flows into an atomizing chamber from the guide pipe, when the molten metal flows freely fall to a high-pressure argon nozzle, high-purity argon (99.999%) is started to carry out atomizing operation, the temperature and the atomizing pressure of the argon are adjusted, the temperature of the argon is within 20 ℃, and the atomizing pressure is within 1MPa, so that the alloy liquid flows are crushed into liquid drops under the impact of supersonic argon gas flow;
5) the liquid drops are naturally cooled in the atomizing chamber, and finally solidified into spherical powder which falls into a powder collecting bin;
s4, powder screening and collecting: and under the protection of inert gas, carrying out mechanical vibration and airflow classification screening on the metal powder in the powder collection bin, and carrying out vacuum-pumping sealing packaging on the screened high-hardness powder with the particle size range of 53-180 mu m for additive manufacturing and repairing.
Example 11
S1, preparing raw materials: selecting nickel-boron alloy, ferrovanadium alloy, metallic iron, high-purity nickel, graphite carbon particles and metallic chromium as raw materials for smelting and preparing the master alloy according to the component proportion requirement;
s2, preparing a master alloy: the method comprises the following steps of preparing 300 kg of mother alloy electrode rods by combining Vacuum Induction Melting (VIM) with a vacuum consumable remelting (VAR) technology, wherein the mother alloy comprises, by mass, 0.2% of C, 1.5% of Ni, 0.7% of Si, 16.5% of Cr, 0.7% of B, 0.20% of V, 0.02% of P, 0.03% of S and the balance of Fe;
s3, the EIGA powder making process comprises the following steps:
1) 300 kg of the homogenized mother alloy bar stock with the size of phi 45 multiplied by 600mm is arranged in a feeding chamber;
2) vacuumizing the atomizing chamber, filling more than 99.999 percent of high-purity argon when the pressure is reduced to be below 0.1Pa, and regulating the induction heating chamber and the atomizing chamber to be micro-positive pressure and micro-negative pressure respectively through the air guide tube; facilitating the flow of liquid from the heating chamber to the atomizing chamber.
3) Conveying the mother alloy bar to an induction heating chamber by an automatic feeding system in a rotating manner, adjusting the smelting power within the range of 25kW, then cutting the bar into magnetic induction lines in an induction coil to generate heat, and melting the mother alloy bar into molten metal;
4) under the action of micro pressure difference, molten metal flows into a guide pipe from an induction heating chamber and flows into an atomizing chamber from the guide pipe, when the molten metal flows freely fall to a high-pressure argon nozzle, high-purity argon (99.999%) is started to carry out atomizing operation, the temperature and the atomizing pressure of the argon are adjusted, the temperature of the argon is within 60 ℃, and the atomizing pressure is within 2MPa, so that the alloy liquid flows are crushed into liquid drops under the impact of supersonic argon gas flow;
5) the liquid drops are naturally cooled in the atomizing chamber, and finally solidified into spherical powder which falls into a powder collecting bin;
s4, powder screening and collecting: and under the protection of inert gas, carrying out mechanical vibration and airflow classification screening on the metal powder in the powder collection bin, and carrying out vacuum-pumping sealing packaging on the screened high-hardness powder with the particle size range of 53-180 mu m for additive manufacturing and repairing.
Example 12
S1, preparing raw materials: selecting nickel-boron alloy, ferrovanadium alloy, metallic iron, high-purity nickel, graphite carbon particles and metallic chromium as raw materials for smelting and preparing the master alloy according to the component proportion requirement;
s2, preparing a master alloy: the method comprises the following steps of preparing 300 kg of mother alloy electrode rods by combining Vacuum Induction Melting (VIM) with a vacuum consumable remelting (VAR) technology, wherein the mother alloy comprises, by mass, 0.15% of C, 2.3% of Ni, 0.5% of Si, 17% of Cr, 0.4% of B, 0.10% of V, 0.01% of P, 0.01% of S and the balance of Fe;
s3, the EIGA powder making process comprises the following steps:
1) 300 kg of the homogenized mother alloy bar stock with the size of phi 45 multiplied by 600mm is arranged in a feeding chamber;
2) vacuumizing the atomizing chamber, filling more than 99.999 percent of high-purity argon when the pressure is reduced to be below 0.1Pa, and regulating the induction heating chamber and the atomizing chamber to be micro-positive pressure and micro-negative pressure respectively through the air guide tube; facilitating the flow of liquid from the heating chamber to the atomizing chamber.
3) Conveying the mother alloy bar to an induction heating chamber by an automatic feeding system in a rotating manner, adjusting the smelting power within the range of 20kW, then cutting the bar into magnetic induction lines in an induction coil to generate heat, and melting the mother alloy bar to obtain molten metal;
4) under the action of micro pressure difference, molten metal flows into a flow guide pipe from an induction heating chamber and flows into an atomizing chamber from the flow guide pipe, when the molten metal flows freely fall to a high-pressure argon nozzle, high-purity argon (99.999%) is started to carry out atomizing operation, the temperature and the atomizing pressure of the argon are adjusted, the temperature of the argon is within 80 ℃, and the atomizing pressure is within 1.8MPa, so that the alloy liquid flows are crushed into liquid drops under the impact of supersonic argon gas flow;
5) the liquid drops are naturally cooled in the atomizing chamber, and finally solidified into spherical powder which falls into a powder collecting bin;
s4, powder screening and collecting: and under the protection of inert gas, carrying out mechanical vibration and airflow classification screening on the metal powder in the powder collection bin, and carrying out vacuum-pumping sealing packaging on the screened high-hardness powder with the particle size range of 53-180 mu m for additive manufacturing and repairing.
TABLE 1 test results obtained in the powder preparation process of examples 1-9
Table 2 examples 1-4 alloy compositions
FIG. 4 shows the surface morphology of the high hardness martensitic powder prepared by the orthogonal test, and the powders with different sizes can be seen in the view field under different preparation process parameters. In the powder shown in fig. 4(a), the particle size distribution of the powder is relatively uniform, the number of "satellites" is small, no unformed powder is observed in the field of view, and the morphology of the powder is prepared when the gas atomization pressure, the melting power and the heating temperature of the atomizing gas are appropriate (example 4 process). The proportion of the fine powder in fig. 4(b) becomes large and agglomeration of the fine powder occurs in the central region, which adversely affects the flowability of the powder, and such powder morphology is easily obtained when the gas atomization pressure is too high or the temperature at which the atomizing gas is heated is too low (process of example 8). There are many unformed irregularities in the field of view shown in fig. 4(c) that adhere to the powder, which is easily obtained when the atomization pressure is too low or the melting power is too high (example 2 process). FIG. 4(d) shows the non-spheroidized molten metal left after the primary crushing of the powder, which is easily obtained when the temperature of the atomizing gas is too low (example 8 process). FIGS. 4(b) - (d) all show the defect of powder morphology, which all affect the powder flowability.
The influence of gas atomization pressure, smelting power and atomization gas temperature on powder median diameter, standard deviation of particle size distribution, powder flow rate and powder yield in the electrode induction atomization powder preparation process in different processes is researched, the test results are shown in table 1, and the powder particle size distribution interval and D prepared by 9 groups of parameters50In contrast, function curve (f)D) And cumulative particle size distribution function curve (l)D) Satisfying the formula (1), the particle diameters of the prepared powder are all in lognormal distribution, and each parameter is in the median particle diameter D50The peak value appears, the width of the particle size distribution is changed, and a function curve (f) of the powder prepared by 9 groups of processesD) And cumulative particle size distribution function curve (l)D) The relationship is shown in fig. 5.
As can be seen from FIG. 5, the median particle diameter D of the powders obtained by the processes of example 2, example 4 and example 850The peak was observed, wherein the powder produced by the process of example 4 had a broad particle size distribution in the range of 40-180 um.
According to the invention, the good regulation and control effects on the particle size distribution and the fluidity of the high-hardness iron powder can be realized through the optimization design of the main process parameters of the gas temperature, the smelting power and the atomizing pressure in the EIGA powder preparation process, and the preparation process of the high-hardness iron powder which has high powder yield, cost saving and good fluidity and meets the requirements of additive manufacturing and repairing is finally obtained.
The present invention is described in detail with reference to the accompanying drawings, which are incorporated herein by reference, and the like, and the appended claims are intended to cover all such modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.
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