CN114433854A - Gas atomization powder preparation equipment, atomization powder preparation method and amorphous powder - Google Patents
Gas atomization powder preparation equipment, atomization powder preparation method and amorphous powder Download PDFInfo
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- CN114433854A CN114433854A CN202210129606.XA CN202210129606A CN114433854A CN 114433854 A CN114433854 A CN 114433854A CN 202210129606 A CN202210129606 A CN 202210129606A CN 114433854 A CN114433854 A CN 114433854A
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- 238000000889 atomisation Methods 0.000 title claims abstract description 40
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- 238000002360 preparation method Methods 0.000 title abstract description 28
- 239000000956 alloy Substances 0.000 claims abstract description 127
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 127
- 239000007788 liquid Substances 0.000 claims abstract description 106
- 239000007921 spray Substances 0.000 claims abstract description 67
- 238000005507 spraying Methods 0.000 claims abstract description 40
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/002—Making metallic powder or suspensions thereof amorphous or microcrystalline
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
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Abstract
The application relates to the technical field of amorphous powder preparation, in particular to gas atomization powder preparation equipment, an atomization powder preparation method and amorphous powder. The apparatus comprises: spraying a powder bag; the atomization bin is positioned below the powder spraying bag; a spray disk is arranged between the powder spray bag and the atomization bin, and a nozzle of the spray disk comprises a flow limiting hole with the diameter of 0.1-2.5 mm; the powder spraying bag is used for receiving alloy liquid, and the alloy liquid passes through the flow limiting hole and is sprayed to the atomization bin to form powder jet; wherein the flow of the alloy liquid passing through the flow limiting hole is less than 5 kg/min; the atomization bin is used for receiving and cooling the powder jet flow to obtain amorphous powder. The equipment can limit the flow of the alloy liquid to be below 5kg/min, prevent the alloy liquid from being solidified, further avoid hole blocking, improve the smoothness of the powder preparation process, and prepare amorphous powder with higher amorphous degree and good high-temperature stability.
Description
Technical Field
The embodiment of the application relates to the technical field of amorphous powder preparation, in particular to gas atomization powder preparation equipment, an atomization powder preparation method and amorphous powder.
Background
Atomization pulverization refers to a powder preparation method in which a metal or alloy liquid is broken into fine droplets by the impact of a rapidly moving fluid (atomizing medium), and then condensed into solid powder. The gas atomization method is a simple and economic powder preparation process, and the sphericity of powder particles is better. The cooling rate of the conventional gas atomization process was 103-104C/s, difficulty in producing a cooling rate of 105Fe-based spherical amorphous powder of not less than DEG C/s. The cooling rate in the atomization process can be increased by improving the mass ratio (gas-liquid ratio) of the atomized gas and the alloy liquid, on one hand, the crushing rate of the alloy liquid column is favorably accelerated, so that the alloy liquid in the center of the alloy liquid column is in quick contact with the atomized gas, and the cooling rate is improved. On the other hand, the air film with larger thermal resistance on the surface of the molten drop is quickly damaged, and the heat transfer of an air/solid interface is accelerated, so that the cooling rate is improved.
Increasing the gas-liquid ratio can be achieved by increasing the atomizing gas flow or decreasing the alloy liquid flow, but increasing the atomizing gas flow significantly increases production costs. Therefore, a technical route for reducing the flow rate of the alloy liquid is generally adopted. The diameter of the flow limiting hole of the nozzle plate leakage nozzle is a main factor influencing the flow of the alloy liquid. At conventional atomizing gas flow rate, to achieve 105The cooling rate is higher than the temperature per second, and the steel flow is generally less than 5 kg/min. In this case, the orifice diameter of the discharge spout is generally less than 3 mm. However, too small a restricted orifice can worsen the smooth flow of the casting because: 1) impurities in the alloy liquid are easy to block holes; 2) the alloy liquid near the restricted orifice is updated slowly, the temperature of the area around the restricted orifice is reduced too fast, and the alloy liquid is solidified to cause hole blockage.
Disclosure of Invention
The gas atomization powder manufacturing equipment provided by the embodiment of the application can limit the flow of the alloy liquid to be below 5kg/min, meanwhile, the temperature around the flow limiting hole is improved, the alloy liquid is prevented from being solidified, then, the hole blockage is avoided, and the smoothness of the powder manufacturing process is improved.
In a first aspect, a gas atomization powder making device is provided, which comprises: spraying a powder bag; the atomization bin is positioned below the powder spraying bag; a spray disk is arranged between the powder spray bag and the atomization bin, and a nozzle of the spray disk comprises a flow limiting hole with the diameter of 0.1-2.5 mm; the powder spraying bag is used for receiving alloy liquid, and the alloy liquid passes through the flow limiting hole and is sprayed to the atomization bin to form powder jet; wherein the flow of the alloy liquid passing through the flow limiting hole is less than 5 kg/min; the atomization bin is used for receiving and cooling the powder jet flow to obtain amorphous powder.
In one embodiment, the nozzle of the spray disk further comprises a plurality of spray slits positioned around the flow restriction orifice; each spray slit in the plurality of spray slits is rectangular, one end of each spray slit in the length direction faces the flow limiting hole, and the other end of each spray slit is far away from the flow limiting hole; the alloy liquid passes through the flow limiting hole and the plurality of spray slits and is sprayed to the atomization bin to form the powder jet; the flow rate of the alloy liquid passing through the flow limiting holes and the plurality of spray slits is less than 5 kg/min.
In one embodiment, the slot is open to an end of the flow restriction orifice and is connected to the flow restriction orifice such that the slot and the flow restriction orifice are in communication.
In one embodiment, the length of the spray slot is 0.05mm-4mm, and the width is 0.05-0.1 mm; the flow restriction orifice is circular.
In one embodiment, the flow rate of the alloy liquid passing through the flow limiting hole and the plurality of spray slits is 0.8-5.4 kg/min.
In one embodiment, the powder spraying bag is fixed at the top end of the atomization bin through a detachable fastening mechanism.
In one embodiment, the equipment further comprises a tundish, a flow guide pipe and a plug rod which are positioned above the powder spraying bag; the upper end of the draft tube is connected to a water gap at the bottom of the tundish, and the lower end of the draft tube extends into the powder spraying bag; the lower end of the plug rod is matched with the water gap, so that the plug rod can block the water gap, and when the tundish injects alloy liquid into the powder spraying package, the plug rod moves upwards to expose the water gap, so that the alloy liquid is injected into the powder spraying package through the water gap and the flow guide pipe.
In one embodiment, the equipment further comprises a smelting furnace, wherein the smelting furnace is used for smelting alloy raw materials into alloy liquid and pouring the alloy liquid into the tundish when the temperature of the alloy liquid reaches a preset temperature; wherein the stopper rod blocks the nozzle when the melting furnace pours the alloy liquid into the tundish.
In one embodiment, the smelting furnace comprises a smelting furnace launder, the tundish comprising a tundish launder; when the smelting furnace pours alloy liquid into the tundish, the tundish diversion trench is positioned below the smelting furnace diversion trench to receive the alloy liquid poured by the smelting furnace through the smelting furnace diversion trench.
In a second aspect, there is provided an atomization method based on the apparatus of the first aspect, comprising: the powder spraying bag receives alloy liquid, and the alloy liquid is sprayed to the atomizing bin through the flow limiting hole to form powder jet; wherein the flow of the alloy liquid passing through the flow limiting hole is less than 5 kg/min; and the atomization bin receives and cools the powder jet to obtain amorphous powder.
In one embodiment, the nozzle of the spray disk further comprises a plurality of spray slits positioned around the flow restriction orifice; each spray slit in the plurality of spray slits is rectangular, one end of each spray slit in the length direction faces the flow limiting hole, and the other end of each spray slit is far away from the flow limiting hole; the alloy liquid passes through restricted orifice spouts to the atomizing storehouse includes: the alloy liquid is sprayed to an atomization bin through the flow limiting hole and the plurality of spray seams; wherein the flow rate of the alloy liquid passing through the flow limiting hole and the plurality of spray gaps is less than 5 kg/min.
In one embodiment, the equipment further comprises a tundish, a flow guide pipe and a plug rod which are positioned above the powder spraying bag; the upper end of the draft tube is connected to a water gap at the bottom of the tundish, and the lower end of the draft tube extends into the powder spraying bag; the lower end of the stopper rod is matched with the water gap, so that the stopper rod can block the water gap; the method further comprises the following steps: and lifting the plug rod to expose the nozzle, so that the alloy liquid is injected into the powder spraying bag through the nozzle and the flow guide pipe.
In one embodiment, the apparatus further comprises a smelting furnace; the method further comprises the following steps: smelting alloy raw materials into alloy liquid by using the smelting furnace; when the temperature of the alloy liquid in the smelting furnace reaches a preset temperature, rotating the smelting furnace to pour the alloy liquid to the tundish; wherein the stopper rod blocks the nozzle when the melting furnace pours the alloy liquid into the tundish.
In one embodiment, the flow rate of the alloy liquid passing through the flow limiting hole is 0.8-5.4 kg/min; the atomized air flow in the atomization bin is not lower than 600Nm3/h。
In a third aspect, there is provided an amorphous powder prepared by the method of the second aspect.
In one embodiment, the amorphous powder contains, per 100 parts by weight of the amorphous powder: 6.5-7.5 weight portions of Si, 2.5-3.0 weight portions of B, 0.5-1.0 weight portion of C, 2.0-3.0 weight portions of Cr and the balance of Fe.
In one embodiment, the amorphous powder has an enthalpy of crystallization of 68-151J/g.
In one embodiment, the glass transition activation energy of the amorphous powder is 256-448 KJ/mol.
In a fourth aspect, there is provided an amorphous powder containing, per 100 parts by weight of the amorphous powder: 6.5-7.5 weight portions of Si, 2.5-3.0 weight portions of B, 0.5-1.0 weight portion of C, 2.0-3.0 weight portions of Cr and the balance of Fe.
In one embodiment, the amorphous powder has an enthalpy of crystallization of 68-151J/g.
In one embodiment, the glass transition activation energy of the amorphous powder is 256-448 KJ/mol.
The equipment and the method provided by the application can limit the flow of the alloy liquid to be below 5kg/min, and simultaneously prevent the alloy liquid from solidifying, thereby avoiding hole blockage and improving the smoothness of the powder making process. The amorphous powder prepared by the equipment and the method has high amorphous degree, high glass transition temperature and good high-temperature stability. The amorphous powder provided by the application has higher amorphous degree, higher glass transition temperature and good high-temperature stability.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments disclosed in the present application, the drawings required to be used in the description of the embodiments will be briefly introduced below, and it is apparent that the drawings in the following description are only embodiments disclosed in the present application, and it is obvious for those skilled in the art that other drawings can be obtained based on the drawings without inventive efforts.
Fig. 1 is a schematic structural diagram of a gas atomization powder making apparatus provided in an embodiment of the present application;
FIG. 2 is a schematic structural diagram of a nozzle plate of the embodiment of the present application;
FIG. 3 is a morphology of amorphous powder prepared in accordance with an embodiment of the present application;
FIG. 4 is a fitted straight line for calculating the glass transition activation energy provided in the examples of the present application.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be described below with reference to the drawings in the embodiments of the present application.
The embodiment of the application provides a gas atomization powder process equipment, and the restricted aperture that its adopted includes restricted aperture and spouts the seam, can improve the temperature around the restricted aperture when restricting alloy liquid flow below 5kg/min, prevents that alloy liquid from solidifying, and then has avoided the stifled hole, has improved the degree of paradigms of powder process.
In addition, the gas atomization powder making equipment provided by the embodiment of the application belongs to non-vacuum clean alloy liquid smelting and casting equipment. Compared with the conventional gas atomization equipment adopting vacuum smelting and atmosphere protection casting, the gas atomization powder making equipment provided by the embodiment of the application does not need a vacuum environment, and is low in production cost
Next, the gas atomization powder making device and the method for atomizing powder making by the device provided by the embodiments of the present application will be described in detail with reference to the accompanying drawings.
Fig. 1 shows a gas atomization powder manufacturing device, which comprises a smelting furnace 1, a smelting furnace diversion trench 2, a tundish diversion trench 3, a tundish 4, a stopper rod 5, a water gap 6, a powder spraying bag 7, a diversion pipe 8, a gas atomization spray plate 9, a spray plate discharge spout 10, an atomization bin 11 and a powder jet 12.
Referring now to fig. 2, the spout 10 includes a flow restriction orifice 101. Illustratively, the spray disk tip 10 also includes a plurality of spray slots 102. A plurality of spray slots 102 are positioned around the flow restriction orifice. Illustratively, as shown in FIG. 2, a plurality of slots 102 are evenly distributed about the flow restriction orifice 101.
The slot 102 is rectangular, and one end of the slot in the length direction faces the orifice 101, and the other end of the slot is far away from the orifice 101. Illustratively, the restrictor orifice 101 is circular. One end of the injection slit 102 in the length direction faces specifically to the center of the flow restriction hole 101, and the other end is far away from the center of the flow restriction hole 101.
The flow of the alloy liquid can be limited to be below 5kg/min by the nozzle 10 of the spray plate, namely the flow of the alloy liquid sprayed to the atomization bin 11 by the tundish 4 through the nozzle 10 of the spray plate is less than 5 kg/min.
In some embodiments, the slot 102 opens toward one end of the flow restriction orifice 101 and is connected to the flow restriction orifice 101 such that the slot 102 and the flow restriction orifice 101 are in communication.
In some embodiments, the length of the nozzle 102 is 3-4mm and the width is 0.05-0.1 mm. The restrictor hole 101 is circular and the diameter of the restrictor hole 101 is 0.5-2.5 mm.
In some embodiments, the number of slots 102 around the flow restriction orifice 101 is four. The four spray slits 102 may be two long powder sprays which intersect perpendicularly, wherein the intersection point is a circular hole, and the circular hole forms the flow restriction hole 101.
The above examples describe the components included in the gas atomization milling apparatus. Next, the relationship and functions between these components will be described.
The melting furnace 1 may receive alloy raw materials and heat-melt the alloy raw materials. Illustratively, the alloying raw materials may be added to the smelting furnace 1 in a certain burden order. And finishing the heating and melting of the alloy raw material under the action of electromagnetic induction. In the smelting furnace 1, the alloy liquid can be purified by selective oxidation as a main technology, an auxiliary adsorption technology or an electromagnetic stirring technology or an automatic argon blowing technology.
In some embodiments, the alloy composition (in mass fraction) may be: si, 6.5-7.5; b, 2.5-3.0; c, 0.5-1.0; 2.0 to 3.0 percent of Cr and the balance of Fe.
The smelting furnace 1 can be an open type smelting furnace, and when the alloy liquid reaches a set temperature, the rotating mechanism can be operated to rotate the smelting furnace 1 to pour at a fixed point. The alloy liquid in the smelting furnace 1 flows into the tundish guide groove 3 from the smelting furnace guide groove 1 and further flows into the tundish 4 through the tundish guide groove 3. Wherein, in the process of pouring or pouring the alloy liquid into the tundish 4, the tundish diversion trench 3 is always positioned under the smelting furnace diversion trench 2.
The alloy liquid is killed in the tundish 4, so that the aims of uniform components, temperature and purification are fulfilled.
The stopper rod 5 is located inside the tundish 4. The upper end of the plug rod 5 is connected with a plug rod lifting mechanism. The stopper rod 5 can vertically move up and down under the driving of the stopper rod lifting structure. For example, the stopper rod lifting device may be a cylinder. The lower end of the stopper rod 5 is matched with the upper end of the water gap 6, so that the water gap 6 can be blocked. During pouring the alloy liquid into the tundish 4 and during heat preservation and calming of the alloy liquid in the tundish 4 by the smelting furnace 1, the lower end of the plug rod 5 is in pressure sealing butt joint with the top end of the water gap 6, so that the alloy liquid is prevented from seeping out of the water gap 6.
The lower end of the water gap 6 is bonded and sealed with the upper end of the draft tube 8 through a refractory material. Wherein the refractory material can be fire clay. The lower end of the draft tube 8 extends into the powder spraying bag 7 to form a channel for alloy liquid to flow into the powder spraying bag 7.
The powder spraying bag 7 is fixed to the top end of the atomizing bin 11 through a detachable fastening mechanism, and the quick replacement of the powder spraying bag 7 can be achieved. An air atomization spray disk 9 is arranged between the bottom of the powder spray bag 7 and the atomization bin 11 through bolts. The nozzle 10 of the spray plate is fixed at the central hole of the gas atomization spray plate 9. The upper part of the spray plate discharge spout 10 is bonded and sealed with the bottom of the powder spraying bag 7 through refractory materials. Wherein the refractory material can be fire clay.
The center of the nozzle plate nozzle 9 is provided with a flow limiting hole 101 and a plurality of spray slits 102 as shown in FIG. 2 for limiting the flow of the alloy liquid.
During powder spraying, the plug rod lifting mechanism drives the plug rod 5 to move upwards, namely the plug rod 5 is lifted, so that the alloy liquid in the tundish 4 flows into the powder spraying ladle 7 through the water gap 6 and the flow guide pipe 8. And then atomized into a powder jet 12 through a restrictive orifice 101 and a plurality of spray slits 102.
The atomization chamber 11 can receive a powder jet 12. The powder jet 12 cools in the atomization chamber 11 and falls into the lower cone. And separating to obtain spherical amorphous powder. Then, the spherical amorphous powder with the target granularity can be obtained by sieving through sieves with different meshes.
Fig. 3 shows a spherical amorphous powder prepared by the apparatus shown in fig. 1.
The above examples describe the function of the various components of the gas atomization powder-making apparatus and the general process of preparing amorphous powder.
Next, the determination of the two alloy performance indexes of enthalpy of crystallization and glass transition activation energy will be described.
Differential Scanning Calorimetry (DSC) curve, the heat flow rate or heating power (difference) to the sample and reference measured by a differential scanning calorimeter, as a function of temperature or time. The ordinate of the curve is the heat flow rate or heat flux in mW (mJ · s)-1) (ii) a The abscissa is temperature or time. The enthalpy of crystallization can be calculated by integrating the area of the crystallization peak on the DSC curve. The crystallization enthalpy of an amorphous material can quantitatively characterize the degree of amorphization. The crystallinity or the non-crystallinity precision angle calculated by the X-ray diffraction characteristic curve is that when the non-crystallinity of the material is higher, the X-ray diffraction characteristic curve is a diffuse scattering peak, and the calculated non-crystallinity or the calculated crystallinity is similar, so that the difference of the non-crystallinity of the material cannot be accurately distinguished. That is, when the degree of amorphousness of the material is larger than a certain value, XRD is uniformThe magnitude of the amorphousness cannot be further characterized for the diffuse scattering peak. That is, there is a limitation in characterizing the size of crystallinity using XRD. The crystallization enthalpy can represent the crystallization enthalpy in a wide range, and when the amorphous degree of the material is large, the specific size of the amorphous degree can be still accurately represented.
The crystallization enthalpy of the amorphous powder prepared by the gas atomization powder preparation device provided by the embodiment of the application is measured, and the fact that the gas atomization powder preparation device provided by the embodiment of the application can prepare the amorphous powder with the crystallization enthalpy of 68-151J/g is found. Further, the gas atomization powder preparation device provided by the embodiment of the application can be used for preparing amorphous powder with crystallization enthalpy of 100-140J/g. The amorphous powder that the gas atomization powder process equipment that this application embodiment provided prepared promptly, the amorphous degree is higher.
The glass transition temperature Tg is the temperature at which an amorphous material changes from a glassy state to a highly elastic state and represents the lowest temperature at which a chain of atoms can move. Below the glass transition temperature, the atoms cannot move but vibrate at their equilibrium positions, and at around the glass transition temperature, the atoms can move slightly, and exhibit high elastic properties. With the increase of the DSC temperature rising rate, the glass transition temperature Tg of the Fe-based amorphous powder gradually shifts to a high-temperature region, which shows that the glass transition process of the alloy has obvious dynamic characteristics.
Wherein, the glass transition activation energy Eg can represent the difficulty and easiness of the glass transition of the Fe-based amorphous powder. Glass transition activation energy Eg, one of the important characteristics of amorphous materials. The characteristic is the energy required for the amorphous material to carry out glass conversion, and the larger the activation energy is, the more difficult the glass conversion is and the higher the stability at high temperature is.
From the glass transition temperature Tg and Ozawa equation (1)), the glass transition activation energy Eg can be calculated, i.e., using equation (1), i.e.:
lnθ＝-1.0516Eg/(RTg)+C (1)
wherein Tg is the glass transition temperature and has the unit of K; theta is the heating rate, and the unit is K/min; eg is glass transition activation energy, and the unit is J/mol; r is a molar gas constant of 8.314J mol-1*K-1(ii) a C is a constant. The glass transition activation energy Eg can be fitted by a graph of the relationship between-ln theta-1000/T at different characteristic temperatures.
The glass transition activation energy of the amorphous powder prepared by the gas atomization powder preparation device provided by the embodiment of the application is measured, and the fact that the gas atomization powder preparation device provided by the embodiment of the application can prepare the amorphous powder with the glass transition activation energy of 256-448KJ/mol is found. Further, the gas atomization powder preparation device provided by the embodiment of the application can be used for preparing amorphous powder with the glass transition activation energy of 320-400 KJ/mol. The amorphous powder prepared by the gas atomization powder preparation equipment provided by the embodiment of the application has higher glass transition temperature and good high-temperature stability.
Next, in specific examples, a description will be given of a scheme for producing an alloy powder using the apparatus shown in FIG. 1, and properties of the produced alloy powder.
Example 1
The amorphous powder prepared in this example had an amorphous composition (in mass percent) of: si: 6.9, B: 2.7, C: 0.7, Cr: 2.5, Fe: 87.2.
the preparation method comprises the following steps:
(1) the smelting furnace 1 heats the alloy raw material to more than 1500 ℃ to melt in the atmosphere to obtain alloy liquid.
(2) Pouring the alloy liquid into a tundish 4, keeping the temperature and calming at 1500 ℃, and removing the slag floating on the surface of the alloy liquid.
(3) The stopper rod 5 in the tundish 4 is lifted, and the alloy liquid flows into a powder spraying ladle 7 from a water gap 6 at the bottom of the tundish 4 and a guide pipe 8 by means of self weight. The alloy liquid level height in the powder spraying bag 7 is controlled by the lifting height of the plug rod 5.
(4) The alloy liquid flows into the gas atomization spray disk 9 through the flow guide pipe at the bottom of the powder spray bag 7 by means of gravity to form a powder jet 12. The flow limiting hole structure comprises two rectangular jet seams which are vertically intersected at the middle point, and the intersection point is a circular flow limiting hole 101. Four jet slots 102 are formed by two rectangular jet slots that intersect perpendicularly at a midpoint. The dimensions of the flow restriction orifice 101 and the slot 102 are shown in table 2. The width and length of the nozzle 102 are 0, which means that there is no nozzle.
(5) The powder jet 12 is broken up into fine droplets in the atomizing chamber 11. The flow rate of the atomized gas is 600Nm3/h。
(6) The fine molten drops fall downwards in the atomization bin 11, are rapidly cooled at the same time, finally fall into a lower cone,
spherical amorphous powder is obtained.
In this embodiment, when the flow-limiting hole has a structure of a nozzle 102 with a length of 3mm, a nozzle width of 0.05mm, and a central hole with a diameter of 2mm, the flow rate of the alloy liquid is 2.4kg/min, and the obtained powder has a crystallization enthalpy of: 127J/g. The glass transition temperatures were measured at different ramp rates and the results are shown in Table 1. Using the measurement results shown in Table 1, the expression of the fitted straight line between-ln θ -1000/T for different characteristic temperatures is obtained from the above equation (1): -ln θ ═ -67.55+49.66 × 1000/T. The calculated glass transition activation energy was obtained as: 392 KJ/mol. Wherein the fitted straight line is shown in fig. 4.
TABLE 1
| θ(K/min) | Tg(K) | - |
1000/ |
| 3 | 475 | -1.0986 | 1.3369 |
| 5 | 480 | 1.6094 | 1.32802 |
| 10 | 487 | 2.3026 | 1.31579 |
| 20 | 496 | 2.9957 | 1.30039 |
| 30 | 501 | 3.4012 | 1.29199 |
| 40 | 505 | 3.6889 | 1.28535 |
| 50 | 507 | -3.912 | 1.28205 |
| 60 | 510 | 4.0943 | 1.27714 |
The enthalpy of crystallization and glass transition activation energy of the amorphous powder prepared using the alloy composition and preparation method of example 1 under different sizes of the restriction orifice 101 and the spray slit 102 are shown in table 2.
TABLE 2
Example 2
The amorphous powder prepared in this example had an amorphous composition (in mass percent) of: si: 7.3, B: 3.0, C: 0.9, Cr: 2.1, Fe: 86.7.
the preparation method comprises the following steps:
(1) the smelting furnace 1 heats the alloy raw material to more than 1500 ℃ to melt in the atmosphere to obtain alloy liquid.
(2) Pouring the molten steel into a tundish 4, keeping the temperature and calming at 1500 ℃, and removing the slag floating on the surface of the molten steel.
(3) The plug rod 5 in the tundish 4 is lifted, and the alloy liquid flows into a powder spraying ladle 7 from a water gap 6 and a flow guide pipe 8 at the bottom of the tundish 4 by self weight. The alloy liquid level height in the powder spraying bag 7 is controlled by the lifting height of the plug rod 5.
(4) The alloy liquid flows into the gas atomization spray disk 9 through the flow guide pipe at the bottom of the powder spray bag 7 by means of gravity to form a powder jet 12. The flow limiting hole structure comprises two rectangular jet seams which are vertically intersected at the middle point, and the intersection point is a circular flow limiting hole 101. Four jet slots 102 are formed by two rectangular jet slots that intersect perpendicularly at a midpoint. The dimensions of the flow restriction orifice 101 and the slot 102 are shown in table 3.
(5) The powder jet 12 is broken up into fine droplets in the atomizing chamber 11. The flow rate of the atomized gas is 600Nm3/h。
(6) The fine molten drops fall downwards in the atomization bin 11, are rapidly cooled at the same time, and finally fall into a lower cone to obtain spherical amorphous powder.
The enthalpy of crystallization and glass transition activation energy of the amorphous powder prepared using the alloy composition and preparation method of example 2 under different sizes of the restriction orifice 101 and the spray slit 102 are shown in table 3. The enthalpy of crystallization and glass transition activation energy calculation methods are described above in example 1.
TABLE 3
Example 3
The amorphous powder prepared in this example had an amorphous composition (in mass percent) of: si: 6.9, B: 2.7, C: 0.7, Cr: 2.5, Fe: 87.2.
the preparation method comprises the following steps:
(1) the smelting furnace 1 heats the alloy raw material to more than 1500 ℃ to melt in the atmosphere to obtain alloy liquid.
(2) Pouring the molten steel into a tundish 4, keeping the temperature and calming at 1500 ℃, and removing the slag floating on the surface of the molten steel.
(3) The stopper rod 5 in the tundish 4 is lifted, and the alloy liquid flows into a powder spraying ladle 7 from a water gap 6 at the bottom of the tundish 4 and a guide pipe 8 by means of self weight. The alloy liquid level height in the powder spraying bag 7 is controlled by the lifting height of the plug rod 5.
(4) The alloy liquid flows into the gas atomization spray disk 9 through the flow guide pipe at the bottom of the powder spray bag 7 by means of gravity to form a powder jet 12. The flow limiting hole structure comprises two rectangular jet seams which are vertically intersected at the middle point, and the intersection point is a circular flow limiting hole 101. Four jet slots 102 are formed by two rectangular jet slots that intersect perpendicularly at a midpoint. The dimensions of the flow restriction orifice 101 and the slot 102 are shown in table 4.
(5) The powder jet 12 is broken up into fine droplets in the atomizing chamber 11. The flow rate of the atomized gas is 600Nm3/h。
(6) The fine molten drops fall downwards in the atomization bin 11, are rapidly cooled at the same time, and finally fall into a lower cone to obtain spherical amorphous powder.
The enthalpy of crystallization and glass transition activation energy of the amorphous powder prepared using the alloy composition and preparation method of example 3 under different sizes of the restriction orifice 101 and the spray slit 102 are shown in table 4. The enthalpy of crystallization and glass transition activation energy calculation methods are described above in example 1.
TABLE 4
Comparative example 1
The amorphous powder prepared in this example had an amorphous composition (in mass percent) of: si: 6.9, B: 2.7, C: 0.7, Cr: 2.5, Fe: 87.2.
the preparation method comprises the following steps:
(1) the smelting furnace 1 heats the alloy raw material to more than 1500 ℃ to melt in the atmosphere to obtain alloy liquid.
(2) Pouring the molten steel into a tundish 4, keeping the temperature and calming at 1500 ℃, and removing the slag floating on the surface of the molten steel.
(3) The stopper rod 5 in the tundish 4 is lifted, and the alloy liquid flows into a powder spraying ladle 7 from a water gap 6 at the bottom of the tundish 4 and a guide pipe 8 by means of self weight. The alloy liquid level height in the powder spraying bag 7 is controlled by the lifting height of the plug rod 5.
(4) The alloy liquid flows into the gas atomization spray disk through the flow guide pipe at the bottom of the powder spray bag 7 by means of gravity to form powder jet flow. The atomizing spray plate used here was a conventional atomizing spray plate, i.e., the atomizing spray plate of comparative example 1 had no nozzle slit. In addition, the diameters of the restricting orifices in the atomizing disk of comparative example 1 are shown in Table 5.
(5) The powder jet is broken up into fine droplets in the atomization bin 11. The flow rate of the atomized gas is 600Nm3/h。
(6) The fine molten drops fall downwards in the atomization bin 11, are rapidly cooled at the same time, and finally fall into a lower cone to obtain spherical amorphous powder.
With the alloy composition and the preparation method of comparative example 1, the crystallization enthalpies and glass transition activation energies of the prepared amorphous powders are shown in table 5 at different sizes of the conventional flow restriction orifice 1. The enthalpy of crystallization and glass transition activation energy calculation methods are described above in example 1.
TABLE 5
The above-mentioned embodiments, objects, technical solutions and advantages of the present application are further described in detail, it should be understood that the above-mentioned embodiments are only examples of the present application, and are not intended to limit the scope of the present application, and any modifications, equivalent substitutions, improvements and the like made on the basis of the technical solutions of the present application should be included in the scope of the present application.
Claims (21)
1. A gas atomization powder manufacturing device is characterized by comprising:
spraying a powder bag;
the atomization bin is positioned below the powder spraying bag;
a spray disk is arranged between the powder spray bag and the atomization bin, and a nozzle of the spray disk comprises a flow limiting hole with the diameter of 0.1-2.5 mm;
the powder spraying bag is used for receiving alloy liquid, and the alloy liquid passes through the flow limiting hole and is sprayed to the atomization bin to form powder jet; wherein the flow of the alloy liquid passing through the flow limiting hole is less than 5 kg/min;
the atomization bin is used for receiving and cooling the powder jet flow to obtain amorphous powder.
2. The apparatus of claim 1 wherein the spray nozzles of the spray disk further comprise a plurality of spray slots positioned about the flow restriction orifice; each spray slit in the plurality of spray slits is rectangular, one end of each spray slit in the length direction faces the flow limiting hole, and the other end of each spray slit is far away from the flow limiting hole;
the alloy liquid passes through the flow limiting hole and the plurality of spray slits and is sprayed to the atomization bin to form the powder jet; the flow rate of the alloy liquid passing through the flow limiting hole and the plurality of spray gaps is less than 5 kg/min.
3. The apparatus of claim 2 wherein said slot opens toward an end of said flow restriction orifice and is connected to said flow restriction orifice such that said slot and said flow restriction orifice are in communication.
4. The apparatus of claim 2 or 3, wherein the length of the slot is 0.05mm to 4mm and the width is 0.05mm to 0.1 mm; the flow restriction orifice is circular.
5. The apparatus of claim 2 or 3, wherein the flow rate of the alloy liquid through the flow-restricting orifice and the plurality of spray slots is 0.8-5.4 kg/min.
6. The apparatus of any one of claims 1-3, wherein the powder spray package is secured to the top end of the aerosolization chamber by a removable fastening mechanism.
7. The apparatus according to any one of claims 1 to 3, further comprising a tundish, a draft tube, a stopper rod, positioned above the powder spray package;
the upper end of the draft tube is connected to a water gap at the bottom of the tundish, and the lower end of the draft tube extends into the powder spraying bag; the lower end of the plug rod is matched with the water gap, so that the plug rod can block the water gap, and when the tundish injects alloy liquid into the powder spraying package, the plug rod moves upwards to expose the water gap, so that the alloy liquid is injected into the powder spraying package through the water gap and the flow guide pipe.
8. The apparatus according to claim 7, further comprising a smelting furnace for smelting alloy raw materials into molten alloy and pouring the molten alloy into the tundish when the temperature of the molten alloy reaches a preset temperature; wherein the stopper rod blocks the nozzle when the melting furnace pours the alloy liquid into the tundish.
9. The apparatus of claim 8, characterized in that the smelting furnace comprises a smelting furnace launder, the tundish comprises a tundish launder; when the smelting furnace pours alloy liquid into the tundish, the tundish diversion trench is positioned below the smelting furnace diversion trench to receive the alloy liquid poured by the smelting furnace through the smelting furnace diversion trench.
10. An atomization method based on the device of claim 1, comprising:
the powder spraying bag receives alloy liquid, and the alloy liquid is sprayed to the atomizing bin through the flow limiting hole to form powder jet; wherein the flow of the alloy liquid passing through the flow limiting hole is less than 5 kg/min;
and the atomization bin receives and cools the powder jet to obtain amorphous powder.
11. The method of claim 10, wherein the spray nozzles of the spray disk further comprise a plurality of spray slots located around the flow-restricting orifice; each of the plurality of spray slits is rectangular, one end of each spray slit in the length direction faces the flow limiting hole, and the other end of each spray slit is far away from the flow limiting hole;
the alloy liquid passes through restricted orifice spouts to the atomizing storehouse includes: the alloy liquid is sprayed to an atomization bin through the flow limiting hole and the plurality of spray seams; wherein the flow rate of the alloy liquid passing through the flow limiting hole and the plurality of spray gaps is less than 5 kg/min.
12. The method according to claim 10 or 11, wherein the apparatus further comprises a tundish, a draft tube, a stopper rod above the powder spray package; the upper end of the draft tube is connected to a water gap at the bottom of the tundish, and the lower end of the draft tube extends into the powder spraying bag; the lower end of the stopper rod is matched with the water gap, so that the stopper rod can block the water gap;
the method further comprises the following steps:
and lifting the plug rod to expose the nozzle, so that the alloy liquid is injected into the powder spraying bag through the nozzle and the flow guide pipe.
13. The method according to claim 12, characterized in that the apparatus further comprises a smelting furnace; the method further comprises the following steps:
smelting alloy raw materials into alloy liquid by using the smelting furnace;
when the temperature of the alloy liquid in the smelting furnace reaches a preset temperature, rotating the smelting furnace to pour the alloy liquid to the tundish; wherein the stopper rod blocks the nozzle when the melting furnace pours the alloy liquid into the tundish.
14. The method according to claim 10 or 11, wherein the flow rate of the alloy liquid through the flow restriction orifice is 0.8-5.4 kg/min; the atomized air flow in the atomization bin is not lower than 600Nm3/h。
15. Amorphous powder prepared by the method of any one of claims 10 to 14.
16. The amorphous powder according to claim 15, comprising, per 100 parts by weight of the amorphous powder: 6.5-7.5 weight portions of Si, 2.5-3.0 weight portions of B, 0.5-1.0 weight portion of C, 2.0-3.0 weight portions of Cr and the balance of Fe.
17. Amorphous powder according to claim 16, characterized in that the crystallization enthalpy of the amorphous powder is 68-151J/g.
18. The amorphous powder according to claim 16 or 17, wherein the glass transition activation energy of the amorphous powder is 256-448 KJ/mol.
19. An amorphous powder, characterized by comprising, per 100 parts by weight of the amorphous powder: 6.5-7.5 weight portions of Si, 2.5-3.0 weight portions of B, 0.5-1.0 weight portion of C, 2.0-3.0 weight portions of Cr and the balance of Fe.
20. The amorphous powder according to claim 19, having a crystallization enthalpy of 68-151J/g.
21. The amorphous powder according to claim 19 or 20, wherein the glass transition activation energy of the amorphous powder is 256-448 KJ/mol.
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