A method and apparatus for alloying to resolve segregation
By combining a multi-component melting unit, a microreactor unit, and an alloy collecting furnace, the problems of component segregation, high energy consumption, and flexible production in alloy preparation were solved, achieving a highly efficient and uniform alloying process and improving production efficiency and material properties.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- KUNMING UNIV OF SCI & TECH
- Filing Date
- 2026-04-03
- Publication Date
- 2026-07-14
AI Technical Summary
Existing alloy preparation technologies suffer from severe compositional segregation, difficulty in phase control, high energy consumption, and limited flexible production. In particular, they encounter problems such as clogging, material corrosion, and failure of temperature and pressure control in microfluidic technology applications, making it difficult to achieve millisecond-level forced mixing of molten metal and coordinated control of high temperature and high pressure at the microscale.
The device employs a combination of multi-component melting units, microreactor units, and alloy collecting furnaces. By melting the melts independently in groups according to their melting points, mixing them in a microfluidic reactor, and processing them in an alloy collecting furnace, it achieves rapid mixing and homogenization of the melts. Combined with precise temperature and pressure control, it prevents melt blockage and component segregation.
Millisecond-level alloying was achieved, with composition segregation reduced to 0.5 at%, energy consumption reduced by 55-65%, production flexibility improved, material properties significantly optimized, alloying time reduced from several hours to several days to ≤100ms, production efficiency increased by 1000 times, and material properties improved by 15-20%.
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Figure CN122382384A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of metal material preparation technology, and in particular to an alloying method and apparatus for solving segregation. Background Technology
[0002] Current mainstream alloy preparation methods rely on electric arc melting, induction melting, and mechanical alloying, which have the following fundamental limitations: Severe compositional segregation: Low diffusion rate within the macroscopic molten pool (10 -9 -10 -11 m² / s), resulting in uneven element distribution (segregation often > 5 at%), requiring long-term homogenization annealing (several hours to several days). Phase control is difficult: slow cooling processes can induce the precipitation of harmful phases (such as σ phase and Laves phase), which reduces the corrosion resistance and strength of the material. Extremely high energy consumption: the thermal efficiency of the smelting furnace is only 30-40%, and the energy consumption of the heat preservation process accounts for more than 60% of the total energy consumption; Flexible production is limited: switching alloy formulas requires furnace cleaning and readjustment, which takes more than 24 hours.
[0003] Although microfluidics technology is mature in the chemical industry, it faces three major technical barriers when applied to molten metals: Blockage problem: The molten metal solidifies rapidly in microchannels (<1mm) (cooling rate >1000℃ / s), causing flow channel blockage (experiments show that Al alloy solidifies in 5 seconds in a 500μm channel). Material corrosion: High-temperature melts (>1000℃) erode the walls of microchannels; quartz glass can only withstand 800℃; Hastelloy has a corrosion rate of >1mm / h in rare earth-containing melts. Temperature and pressure control failure: Temperature gradient >100℃ / mm at the microscale, pressure fluctuation range reaches ±20%, causing uneven mixing or equipment rupture.
[0004] It is evident that there is currently no mature technology that can simultaneously achieve millisecond-level forced mixing of molten metal (≤100ms), coordinated control of high temperature (>1500℃) and high pressure (>5MPa) at the microscale, and stable treatment of highly reactive alloys containing rare earth elements, alkali metals, etc.
[0005] Therefore, in order to overcome the four major problems in the alloying process of existing technologies, namely slow mixing, heavy segregation, high energy consumption, and poor flexibility, it is an urgent technical problem for those skilled in the art to provide a device and method that can achieve millisecond-level atomic-scale homogenization. Summary of the Invention
[0006] In view of this, the present invention provides an alloying method and apparatus for solving segregation.
[0007] To solve the above-mentioned technical problems, the present invention adopts the following technical solution: An alloying apparatus for resolving segregation includes: a multi-component melting unit, a microreactor unit, and an alloy collecting furnace; wherein, The multi-component melting unit includes at least two independent melting furnaces, which respectively melt metals or pre-alloys of different melting point groups; each melting furnace is provided with a molten liquid outlet pipe at the bottom. The inlet end of the microreactor unit is connected to each melt outlet pipe, and is equipped with an external insulation layer and a preheating layer; The alloy collecting furnace is connected to the outlet of the microreactor unit and has a built-in temperature control system.
[0008] External insulation and preheating layers can prevent melt blockage.
[0009] Preferably, the material of the molten liquid outlet pipe at the bottom of each smelting furnace is a high-temperature resistant alloy or ceramic.
[0010] Preferably, the channel width of the microreactor unit is 1mm-50mm and the length is 10cm-50cm.
[0011] Preferably, the structure of the microreactor unit is a multi-Y type mixing unit, with three streams at 60° or four streams at 90° evenly distributed and converging centripetally.
[0012] Preferably, the microreactor unit is made of any one of titanium alloy, Hastelloy, alumina ceramic, or zirconia ceramic.
[0013] Preferably, the temperature control system has a control temperature range of melting point ±20℃.
[0014] The above operations can remove melt pores and suppress secondary segregation.
[0015] Preferably, the roughness Ra of the inner wall of the channel of the microreactor unit is ≤0.8μm to reduce flow resistance; The preheating layer is heated by resistance or induction, and the channel temperature is maintained at or above the lowest melting point group temperature -50°C.
[0016] Preferably, the temperature control system of the alloy collecting furnace includes: a thermocouple array with an accuracy of ±1℃, a PID control module, and an electromagnetic stirrer with a rotation speed of 50-200 rpm.
[0017] The above steps can prevent component segregation.
[0018] An alloying method for resolving segregation, comprising: (1) Melt independently in groups according to melting point: The low-temperature group melts at temperature T1 at 200-500℃. The medium-temperature group melts at temperature T2 (500-800℃). High-temperature components with a melting point > 800℃ will melt at temperature T3, where T3 ≥ melting point + 50℃; (2) The melt is mixed in a microfluidic reactor unit with a residence time ≤ 10 seconds and a mixing shear rate ≥ 1000 s⁻¹; (3) The mixed melt enters the alloy collecting furnace, is kept at the melting point ±20℃ for 1-5 minutes, and is degassed by inert gas; • Control the cooling rate to 1-5℃ / min until solidification.
[0019] Preferably, the method is applicable to alloys prone to segregation, including: Aluminum-tin alloy: Al-20Sn; High density difference alloys: Cu-30Pb, SnAgCu.
[0020] The present invention achieves the following technical effects compared to the prior art: (1) This invention achieves a millisecond-level alloying revolution: through microchannel forced mixing, with a channel size of 50–800 μm, the alloying time is compressed from several hours to several days in the traditional process to ≤100 ms, and the production efficiency is increased by more than 1,000 times; (2) The present invention completely eliminates compositional segregation: microscale turbulent / chaotic convection achieves atomic-level mixing, with an outlet alloy compositional segregation of ≤0.5at%, while the traditional process is >5at%. The present invention improves the uniformity of microstructure at the nanoscale, with a detection variance of <0.3%. (3) The energy consumption of this invention is reduced by 55-65%: the zoned temperature control + multi-layer insulation design makes the heat loss ≤5%, while the heat loss of traditional smelting furnace is >60%, and the comprehensive energy consumption is reduced to 3000-3500 kWh / ton, while the traditional process is ≥8000 kWh / ton; (4) This invention improves the response speed of flexible production: the modular design supports switching alloy formulas within 10 minutes, while traditional production lines require 24 hours of furnace cleaning; this invention is suitable for small-batch, multi-variety production needs. (5) The present invention significantly optimizes material properties: rapid cooling inhibits the precipitation of harmful phases, the σ phase content in high-temperature alloys is <0.1 vol%, and the traditional process is >3 vol%. The present invention increases tensile strength by 15–20% and elongation by 25%. Attached Figure Description
[0021] Figure 1 This is a schematic diagram of the overall structure of the microreactor alloying system of the present invention; Figure 2 This is a cross-sectional view of the microreactor structure of the present invention; (1) Y-type and T-type multichannel microreactors; (2) Caterpillar vortex microreactors. Detailed Implementation
[0022] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0023] This invention discloses an alloying apparatus for solving segregation, comprising: a multi-component melting unit, a microreactor unit, and an alloy collecting furnace; wherein, The multi-component melting unit includes at least two independent melting furnaces, which respectively melt metals or pre-alloys of different melting point groups; each melting furnace is provided with a molten liquid outlet pipe at the bottom. The inlet end of the microreactor unit is connected to each melt outlet pipe, and is equipped with an external insulation layer and a preheating layer; The alloy collecting furnace is connected to the outlet of the microreactor unit and has a built-in temperature control system.
[0024] The molten metal outlet pipes at the bottom of each smelting furnace are made of high-temperature resistant alloys or ceramics.
[0025] The channel width of the microreactor unit is 1mm-50mm and the length is 10cm-50cm.
[0026] The structure of the microreactor unit is a multi-Y type mixing unit, with three streams at 60° or four streams at 90° evenly distributed and converging centripetally.
[0027] The microreactor unit is made of any one of titanium alloy, Hastelloy, alumina ceramic, or zirconia ceramic.
[0028] The temperature control system has a control temperature range of ±20℃ from the melting point.
[0029] The roughness Ra of the inner wall of the channel in the microreactor unit is ≤0.8μm, which reduces flow resistance; The preheating layer uses resistance heating or induction heating to maintain the channel temperature at or above the lowest melting point group temperature -50℃.
[0030] The temperature control system of the alloy collecting furnace includes: a thermocouple array with an accuracy of ±1℃, a PID control module, and an electromagnetic stirrer with a rotation speed of 50-200 rpm.
[0031] This invention also discloses an alloying method for solving segregation, comprising: (1) Melt independently in groups according to melting point: The low-temperature group melts at temperature T1 at 200-500℃. The medium-temperature group melts at temperature T2 (500-800℃). High-temperature components with a melting point > 800℃ will melt at temperature T3, where T3 ≥ melting point + 50℃; (2) The melt is mixed in a microfluidic reactor unit with a residence time ≤ 10 seconds and a mixing shear rate ≥ 1000 s⁻¹; (3) The mixed melt enters the alloy collecting furnace, is kept at the melting point ±20℃ for 1-5 minutes, and is degassed by inert gas; Control the cooling rate to 1-5℃ / min until solidification.
[0032] The method is applicable to easily segregated alloys, including: Aluminum-tin alloy: Al-20Sn; High density difference alloys: Cu-30Pb, SnAgCu.
[0033] Example 1: Aluminum-Tin Alloy Al-20Sn Bearing Material The raw materials were melted separately in groups: the low-temperature group of tin ingots was melted into liquid Sn at 250℃; the medium-temperature group of aluminum ingots was melted into liquid Al at 700℃.
[0034] Two sets of melts are pumped into a counter-jet microfluidic reactor via a delivery module. The reactor employs a 180° counter-jet structure (channel size 400μm) and achieves ultra-fast mixing in 75 milliseconds under the control of a high-pressure pump.
[0035] The Sn distribution was monitored in real time by an online laser spectrometer during the mixing process, and the Sn flow rate was dynamically adjusted by ±0.1 mL / min to ensure uniform dispersion of the Sn phase. The outlet melt is quenched by a twin-roll quenching device at a speed of 1.5 × 10⁻⁶. 5 Forming was performed at a cooling rate of K / s to obtain a foil strip with a thickness of 0.3 mm.
[0036] Results: Sn phase size ≤2μm (≥50μm in traditional casting process), compositional segregation degree 0.28at, friction coefficient 0.12 (40% lower than traditional process), meeting the requirements of high load bearings.
[0037] Example 2: Copper-Lead Alloy Cu-30Pb Self-Lubricating Material Group melting: Low-temperature group lead ingots are melted at 400℃; high-temperature group copper ingots are melted in silicon carbide crucibles at 1150℃.
[0038] Dual-channel gradient control is adopted: the flow rates of inlet A (Cu melt) and inlet B (Pb melt) are adjusted according to an exponential function (Cu from 100%→70%, Pb from 0%→30%), with a flow response time of 0.08 seconds and a multi-pump coordinated phase difference of 0.007 seconds; The mixing process was carried out in a caterpillar-shaped vortex reactor (150 μm in diameter, 50° helix angle), with thermocouples controlling the temperature by ±1.5℃ per 100 mm, and pressure fluctuation ≤0.15 MPa. The gradient melt was rapidly cooled by high-pressure argon atomization (cooling rate 4 × 10⁻⁶). 5 (K / s) grinding.
[0039] Results: The Pb phase exhibited a continuous gradient distribution in the Cu matrix (without interfacial stratification). The lubricating phase size in the 30% Pb region was ≤5 μm, and the wear rate was 2.3 × 10⁻⁶. -6 mm 3 / N·m (conventional sintered alloy 8.1×10 -6 ).
[0040] Example 3: Preparation of modified AZ91 magnesium alloy (narrow range Mg-Al system) Target alloy: AZ91+0.5Cd+0.6MM (solidification range 48.5°C) Technological innovation points: Synergistic refining of cadmium (Cd) and mixed rare earth elements (MM): Cd reduces surface tension, MM inhibits β-Mg 17 Al 12 Phase coarsening Process flow: 1. Third-order melting:
[0041] 2. Microfluidic mixing: • Three-channel 60° counter-jet reactor (600μm diameter), mixing time 100ms • Pressure fluctuation ≤ 0.01 MPa (to avoid oxidation of molten Mg) 3. Dynamic regulation: • The laser spectrometer provides real-time feedback on the Al content, allowing for adjustment of the AZ91 matrix flow rate by ±0.2 mL / min. 4. Rapid cooling and post-treatment: • Argon atomization cooling (rate 3 × 10⁻⁶) 5 K / s) → Hot isostatic pressure (380℃ / 150MPa) result: The solidification range was measured at 49.2°C (the base AZ91 is 128°C). β-Mg 17 Al 12 Phase size ≤3μm (conventional process ~50μm) Tensile strength 348MPa (40% improvement over the basic AZ91) Example 4: Preparation of Au-Cu20 alloy (a typical example of a narrow solidification range) Target alloy: AuCu20 (gold-copper alloy, solidification range <5°C) Process flow: 1. Group melting: • Low-temperature group: Pure copper (melting point 1083℃) melted under argon protection at 1100℃. • High-temperature group: Pure gold (melting point 1064℃) is melted in an alumina crucible at 1150℃. 2. Microfluidic mixing: • Dual-stream melt is pumped into a 180° counter-jet microreactor through an 8mm diameter flow channel at a flow rate accuracy of ±0.05mL / min. • Channel size 300μm, mixing time ≤40ms (gold / copper density difference only 1.7g / cm³) 3 (No gradient control required) 3. Online monitoring and temperature control: • The temperature module maintains the reaction section at 1090℃ (near the eutectic point of 1067℃), with a temperature control accuracy of ±0.5℃. • X-ray fluorescence spectrometer real-time monitoring of component deviation ≤0.03at% 4.Quick cooling forming: • Water-cooled copper rollers at 2×10 5 A 0.2 mm foil strip is produced by a cooling rate of K / s. result: No macroscopic segregation (extremely narrow solidification range inhibits dendrite growth) Microhardness HV 185 (22% higher than traditional casting) Resistivity 1.8 μΩ·cm (99% of theoretical value) Example 5: Preparation of SnAgCu lead-free solder A Sn96.5Ag3.0Cu0.5 solder alloy was prepared. In the low-temperature group, tin and silver were co-melted at 980℃ based on eutectic properties; in the high-temperature group, pure copper was melted in a silicon carbide crucible at 1130℃. The two melts were mixed in a 180° counter-spray microreactor with a channel size of 200 μm and a mixing time of 60 ms. The temperature control module maintains the reaction section at 250℃, and thermocouples are arranged every 100mm to achieve a temperature control accuracy of ±1.8℃; the pressure module stabilizes the differential pressure at 0.3MPa, with fluctuations ≤0.005MPa. The online laser spectrometer dynamically adjusts the silver flow rate by ±0.05 mL / min to ensure an accurate Ag / Cu ratio. The mixed melt is rapidly cooled using a twin-roll casting process at a cooling rate of 2 × 10⁻⁶. 5K / s yielded foil with a β-Sn phase content exceeding 99%. The Ag3Sn compound size was ≤0.5μm, the content was 0.09vol%, the composition deviation was ≤0.1at%, and the wetting angle was reduced by 12° compared to the traditional process.
[0042] The above description is merely a preferred embodiment of the present invention and does not constitute any limitation on the technical scope of the present invention. Therefore, any minor modifications, equivalent changes, and alterations made to the above embodiments based on the technical essence of the present invention shall still fall within the scope of the technical solution of the present invention.
Claims
1. An alloying device for solving segregation, characterized in that, include: Multi-component melting unit, microreactor unit, alloy collecting furnace; among which, The multi-component melting unit includes at least two independent melting furnaces, which respectively melt metals or pre-alloys of different melting point groups; each melting furnace is provided with a molten liquid outlet pipe at the bottom. The inlet end of the microreactor unit is connected to each melt outlet pipe, and is equipped with an external insulation layer and a preheating layer; The alloy collecting furnace is connected to the outlet of the microreactor unit and has a built-in temperature control system.
2. The alloying device for solving segregation according to claim 1, characterized in that, The molten liquid outlet pipes at the bottom of each smelting furnace are made of high-temperature resistant alloys or ceramics.
3. The alloying apparatus for solving segregation according to claim 1, characterized in that, The channel width of the microreactor unit is 1mm-50mm and the length is 10cm-50cm.
4. The alloying apparatus for solving segregation according to claim 1, characterized in that, The structure of the microreactor unit is a multi-Y type mixing unit, with three streams at 60° or four streams at 90° evenly distributed and converging centripetally.
5. An alloying apparatus for solving segregation according to claim 1, characterized in that, The microreactor unit is made of any one of titanium alloy, Hastelloy, alumina ceramic, or zirconia ceramic.
6. An alloying apparatus for solving segregation according to claim 1, characterized in that, The temperature control system has a control temperature range of melting point ±20℃.
7. An alloying apparatus for resolving segregation according to claim 1, characterized in that, The roughness Ra of the inner wall of the channel of the microreactor unit is ≤0.8μm, which reduces flow resistance; The preheating layer is heated by resistance or induction, and the channel temperature is maintained at or above the lowest melting point group temperature -50°C.
8. An alloying apparatus for solving segregation according to claim 1, characterized in that, The temperature control system of the alloy collecting furnace includes: a thermocouple array with an accuracy of ±1℃, a PID control module, and an electromagnetic stirrer with a rotation speed of 50-200 rpm.
9. An alloying method for solving segregation, characterized in that, include: (1) Melt independently in groups according to melting point: The low-temperature group melts at temperature T1 at 200-500℃. The medium-temperature group melts at temperature T2 (500-800℃). High-temperature components with a melting point > 800℃ will melt at temperature T3, where T3 ≥ melting point + 50℃; (2) The melt is mixed in a microfluidic reactor unit with a residence time ≤ 10 seconds and a mixing shear rate ≥ 1000 s⁻¹; (3) The mixed melt enters the alloy collecting furnace, is kept at the melting point ±20℃ for 1-5 minutes, and is degassed by inert gas; Control the cooling rate to 1-5℃ / min until solidification.
10. The alloying method for solving segregation according to claim 9, characterized in that, The method is applicable to easily segregated alloys, including: Aluminum-tin alloy: Al-20Sn; High density difference alloys: Cu-30Pb, SnAgCu.