CN111822725B - Preparation method of alloy powder for recycling copper-chromium alloy - Google Patents
Preparation method of alloy powder for recycling copper-chromium alloy Download PDFInfo
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- 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
- B22F2009/0824—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 with a specific atomising fluid
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- 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
- B22F2009/0848—Melting process before atomisation
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Abstract
The invention provides a preparation method of alloy powder for recycling copper-chromium alloy, which specifically comprises the following steps: medicine for treating acute respiratory syndromeWashing and drying; vacuum induction melting: placing the CuCr alloy leftovers into a crucible of a smelting chamber until the vacuum degree reaches 10‑1Pa or less, starting heating; the heating power is increased in a gradient manner, 40kW is kept for 3-5 minutes, 60kW is kept for 3-5 minutes, and finally the heating power is increased to 80kW, when the CuCr alloy in the crucible begins to melt, a vacuum system is closed, and then argon is filled to the standard atmospheric pressure; then, increasing the power to 100-150 kW to melt the CuCr alloy to obtain a completely melted CuCr alloy melt; refining and impurity removal; atomizing to prepare powder; screening to obtain CuCr alloy powder with different particle sizes; the method has simple process and low manufacturing cost, can efficiently recover the copper-chromium alloy waste, and prepares the CuCr alloy powder with low gas content and high purity.
Description
Technical Field
The invention relates to the technical field of alloy powder preparation, in particular to a preparation method of alloy powder for recycling copper-chromium alloy.
Background
The copper-chromium alloy is a series of alloys formed by adding chromium and other trace alloy elements on the basis of copper, and has high strength and hardness, good electric and thermal conductivity and corrosion resistance after heat treatment, so that the copper-chromium alloy is widely applied to various industries.
The existing copper-chromium alloy recovery is generally to cut and grind copper-chromium alloy waste, then to press the obtained copper-chromium alloy scraps into consumable electrodes, and then to adopt electrode induction gas atomization to prepare powder; the prefabricated bar is zone refined under the condition of protective gas, the metal liquid continuously and vertically passes through the nozzle and flows downwards, when the metal liquid passes through the nozzle, the metal liquid is atomized and broken into a large number of fine liquid drops by high-pressure gas flow, and the fine liquid drops are solidified into particles in flight.
The prior art has the following defects that firstly, alloy scraps are easy to oxidize in the cutting and grinding process, impurities in the alloy scraps are increased due to the abrasion of materials such as props in the process, and meanwhile, a large amount of energy is consumed in the cutting, grinding and scrap making process of the lump materials, so that waste is caused; secondly, the copper-chromium alloy scraps are difficult to densify in the pressing process due to high strength, and extremely high pressing force is required, so that extremely strict requirements are provided for equipment and a die; thirdly, electrode induction gas atomization is used for preparing powder, materials cannot be fully smelted, the content of impurities and gas of the electrode materials cannot be reduced, the electrode densification degree is low, and gas is easy to bleed and short-circuit in the electrode induction gas atomization process, so that continuous production cannot be realized; fourthly, electrode induction gas atomization powder preparation needs to consume a large amount of energy and protective gas, and the production cost is far higher than the cost of raw materials, so that the method cannot be industrially applied in batches.
Disclosure of Invention
Aiming at the problems, the invention provides a method for preparing alloy powder by recycling copper-chromium alloy, which can efficiently recycle copper-chromium alloy waste and prepare CuCr alloy powder with low gas content and high purity; compared with the electrode induction gas atomization powder preparation process, the invention effectively reduces the energy consumption and the gas consumption in the atomization process, greatly reduces the manufacturing cost and can realize batch production.
The technical scheme of the invention is as follows: a preparation method of alloy powder for recycling copper-chromium alloy specifically comprises the following steps:
s1: cleaning and drying
Cleaning and drying the CuCr alloy leftovers;
s2: vacuum induction melting
Step S1 is obtainedThe CuCr alloy leftovers are put into a crucible of a smelting chamber, wherein the crucible is any one of a magnesia material crucible, a calcium oxide material crucible and a zirconia material crucible; until the vacuum degree reaches 10-1Pa, starting heating; the heating power is increased in a gradient manner, 40kW is kept for 3-5 min, 60kW is kept for 3-5 min, and finally the heating power is increased to 80kW, when the CuCr alloy in the crucible begins to melt, the vacuum system is closed, the heating power is reduced to 20kW, and then argon is filled to the standard atmospheric pressure; heating power is increased to 100-150 kW, so that the CuCr alloy is melted, and a completely melted CuCr alloy molten liquid is obtained;
s3: refining to remove impurities
Then reducing the heating power to 60-100 kW, waiting until impurities float on the surface of the CuCr alloy molten liquid, and removing surface impurities by using a slag remover;
s4: atomized powder
Heating power is increased to 100-150 kW, and when the superheat degree of the CuCr alloy molten liquid reaches 50-200 ℃, vacuum atomization is carried out in an atomization chamber to prepare powder, so that CuCr alloy atomized powder is obtained; the vacuum atomization powder preparation method comprises the following specific steps: enabling the CuCr alloy molten liquid to flow out downwards through a flow guide nozzle, atomizing and crushing the CuCr alloy molten liquid into a large number of fine liquid drops through a nozzle by using high-pressure inert gas flow of 2-10 Mpa, and then cooling to obtain CuCr alloy atomized powder;
s5: sieving
And (4) screening the atomized CuCr alloy powder obtained in the step (S4) to obtain the CuCr alloy powder with the required granularity.
Further, in the step S1, firstly, high-pressure water flow is adopted to wash impurities adhered to the surface of the CuCr alloy leftovers, then an ultrasonic cleaning method is adopted to remove oil stains and oxide layers on the surface, and finally drying is carried out; external impurities on the surfaces of the CuCr alloy leftovers can be washed away through high-pressure water flow, and further ultrasonic cleaning is performed, so that an oxide film on the surfaces of the CuCr alloy leftovers can fall off, and the purity of the powder preparation is effectively improved.
Further, after the argon is filled into the vacuum induction melting in the step S2, preheating the tundish, and keeping the power of a heating device at 7-30 kW; the refractory material of the tundish substrate can be prevented from being damaged due to thermal shock through preheating, and the phenomenon of blockage of the metal solution due to too fast cooling is avoided.
Further, step S4 atomizing and pulverizing the nozzle melt flow is 5-25L/min, the alloy melt diameter is 5mm, the improvement of the powder particle size is realized by controlling the nozzle melt flow and the melt diameter, and the atomizing and pulverizing quality is favorably improved.
Further, the atomized powder preparation in the step S4 adopts hot gas atomization, and inert gas is heated to 300 ℃; the pressure of the inert gas is 3 MPa; the atomization efficiency can be effectively improved through hot gas atomization, the deviation of the average particle size can be reduced, and the gas consumption can be reduced.
Further, in the step S5, a 230-mesh screen is used for screening, so as to obtain CuCr alloy powder with a particle size of less than 60 μm.
Further, collecting CuCr alloy powder sieved in the step S5, and performing ball milling treatment by adopting a vibration ball mill; during ball milling treatment, 0.3 wt% of process control agent is added, wherein the process control agent is stearic acid; the grinding medium is 20mm quenched steel balls, and the filling rate is 65%; the ball milling treatment time is 12h, the ball material ratio is 5: 1, ball milling at a rotating speed of 130 r/min; the powder with the off-standard granularity is corrected through ball milling treatment, and the yield of powder preparation by recycling CuCr alloy leftovers is effectively improved.
Furthermore, liquid nitrogen is introduced for cooling during ball milling treatment, and liquid nitrogen is introduced for cooling and dry milling, so that the ball milling process time can be reduced, and the ball milling efficiency is improved.
Compared with the prior art, the invention has the beneficial effects that: the method can efficiently recover the copper-chromium alloy waste material and prepare the CuCr alloy powder with low gas content and high purity; compared with an electrode induction gas atomization powder preparation process, the invention effectively reduces the energy consumption and gas consumption in the atomization process, greatly reduces the manufacturing cost and can realize batch production; according to the invention, through hot gas atomization, the atomization efficiency can be effectively improved, the argon consumption is reduced, and the deviation of average particle size can be reduced; powder with substandard granularity is ball-milled through ball milling treatment to meet the granularity requirement, and the yield of powder preparation by recycling CuCr alloy leftovers is effectively improved.
Drawings
FIG. 1 is an SEM microstructure of CuCr alloy powder prepared in example 1 of the invention.
Detailed Description
Example 1: a preparation method of alloy powder for recycling copper-chromium alloy comprises the following steps:
s1: cleaning and drying
Firstly, washing impurities adhered to the surface of the CuCr alloy leftovers by adopting high-pressure water flow, then removing oil stains and oxide layers on the surface by using an ultrasonic cleaning method, and finally drying;
s2: vacuum induction melting
Placing the CuCr alloy leftovers obtained in the step S1 into a crucible of a smelting chamber, wherein the crucible is made of magnesium oxide; until the vacuum degree reaches 10-1Pa, starting heating; the heating power is increased in a gradient manner, 40kW is kept for 3min, 60kW is kept for 3min, and finally the heating power is increased to 80kW, when the CuCr alloy in the crucible begins to melt, the vacuum system is closed, the heating power is reduced to 20kW, and then argon is filled to the standard atmospheric pressure; preheating the tundish, keeping the power of a heating device at 7kW, and increasing the heating power to 100kW to melt the CuCr alloy to obtain a completely molten CuCr alloy melt;
s3: refining to remove impurities
Then reducing the heating power to 60kW, waiting until impurities float on the surface of the CuCr alloy molten liquid, and removing surface impurities by using a slag remover;
s4: atomized powder
Heating power is increased to 100kW, and when the superheat degree of the CuCr alloy molten liquid reaches 50 ℃ through detection of an infrared temperature measuring instrument, powder preparation is carried out through vacuum atomization in an atomization chamber, so that CuCr alloy atomized powder is obtained; the method comprises the following specific steps of preparing powder by vacuum atomization: the CuCr alloy molten liquid flows downwards through a flow guide nozzle, is atomized and crushed into a large number of fine liquid drops through a nozzle by 2MPa high-pressure inert gas flow, and is cooled to obtain CuCr alloy atomized powder; wherein the flow rate of the nozzle melt is 5L/min, and the diameter of the alloy melt is 5 mm;
s5: sieving
And (4) screening the CuCr alloy atomized powder obtained in the step (S4) by adopting a 230-mesh screen to obtain the CuCr alloy powder with the particle size of less than 60 mu m.
Example 2: a preparation method of alloy powder for recycling copper-chromium alloy comprises the following steps:
s1: cleaning and drying
Firstly, washing impurities adhered to the surface of the CuCr alloy leftovers by adopting high-pressure water flow, then removing oil stains and oxide layers on the surface by using an ultrasonic cleaning method, and finally drying;
s2: vacuum induction melting
Placing the CuCr alloy leftovers obtained in the step S1 into a crucible of a smelting chamber, wherein the crucible is made of calcium oxide; until the vacuum degree reaches 10-1Pa, starting heating; the heating power is increased in a gradient manner, 40kW is kept for 4min, 60kW is kept for 4min, and finally the heating power is increased to 80kW, when the CuCr alloy in the crucible begins to melt, the vacuum system is closed, the heating power is reduced to 20kW, and then argon is filled to the standard atmospheric pressure; preheating the tundish, keeping the power of a heating device at 18kW, and then increasing the heating power to 125kW to melt the CuCr alloy to obtain a completely molten CuCr alloy molten liquid;
s3: refining to remove impurities
Then reducing the heating power to 80kW, waiting until impurities float on the surface of the CuCr alloy molten liquid, and removing surface impurities by using a slag skimmer;
s4: atomized powder
Heating power is increased to 125kW, and the CuCr alloy atomized powder is obtained by carrying out vacuum atomization powder preparation in an atomization chamber through detection of an infrared temperature measuring instrument until the superheat degree of the CuCr alloy molten liquid reaches 125 ℃; the method comprises the following specific steps of preparing powder by vacuum atomization: the CuCr alloy molten liquid flows downwards through a flow guide nozzle, is atomized and crushed into a large number of fine liquid drops through a nozzle by 6MPa high-pressure inert gas flow, and is cooled to obtain CuCr alloy atomized powder; wherein the flow rate of the nozzle melt is 12.5L/min, and the diameter of the alloy melt is 5 mm;
s5: sieving
And (4) screening the CuCr alloy atomized powder obtained in the step (S4) by adopting a 230-mesh screen to obtain the CuCr alloy powder with the particle size of less than 60 mu m.
Example 3: a preparation method of alloy powder for recycling copper-chromium alloy comprises the following steps:
s1: cleaning and drying
Firstly, washing impurities adhered to the surface of the CuCr alloy leftovers by adopting high-pressure water flow, then removing oil stains and oxide layers on the surface by using an ultrasonic cleaning method, and finally drying;
s2: vacuum induction melting
Placing the CuCr alloy leftovers obtained in the step S1 into a crucible of a smelting chamber, wherein the crucible is made of zirconia; until the vacuum degree reaches 10-1Pa, starting heating; the heating power is increased in a gradient manner, 40kW is kept for 5min, 60kW is kept for 5min, and finally the heating power is increased to 80kW, when the CuCr alloy in the crucible begins to melt, the vacuum system is closed, the heating power is reduced to 20kW, and then argon is filled to the standard atmospheric pressure; preheating the tundish, keeping the power of a heating device at 30kW, and then increasing the heating power to 150kW to melt the CuCr alloy to obtain a completely melted CuCr alloy melt;
s3: refining to remove impurities
Then reducing the heating power to 100kW, waiting until impurities float on the surface of the CuCr alloy molten liquid, and removing surface impurities by using a slag skimmer;
s4: atomized powder
Heating power is increased to 150kW, and when the superheat degree of the CuCr alloy molten liquid reaches 200 ℃ through detection of an infrared temperature measuring instrument, powder preparation is carried out through vacuum atomization in an atomization chamber, so that CuCr alloy atomized powder is obtained; the method comprises the following specific steps of preparing powder by vacuum atomization: the CuCr alloy molten liquid flows downwards through a flow guide nozzle, is atomized and crushed into a large number of fine liquid drops through a nozzle by high-pressure inert gas flow of 10MPa, and is cooled to obtain CuCr alloy atomized powder; wherein the flow rate of the nozzle melt is 25L/min, and the diameter of the alloy melt is 5 mm;
s5: sieving
And (4) screening the CuCr alloy atomized powder obtained in the step (S4) by adopting a 230-mesh screen to obtain the CuCr alloy powder with the particle size of less than 60 mu m.
Example 4: the difference from example 1 is: step S4, adopting hot gas atomization to prepare powder, and heating inert gas to 300 ℃; the pressure of the inert gas is 3 MPa.
Example 5: the difference from example 1 is: collecting CuCr alloy powder sieved in the step S5, performing ball milling treatment by adopting a vibration ball mill, and introducing liquid nitrogen for cooling; wherein 0.3% wt of a process control agent is added, said process control agent being stearic acid; the grinding medium is 20mm quenched steel balls, and the filling rate is 65%; the ball milling treatment time is 12h, the ball material ratio is 5: 1, the ball milling rotating speed is 130 r/min.
Test example:
the CuCr alloy powder produced by the powder making method for recycling copper-chromium alloy in examples 1 to 5 and the CuCr alloy powder produced by the conventional recycling method were subjected to the test of the relevant performance parameters, and the test methods were as follows:
according to GB/T5314-;
measuring the apparent density of the CuCr alloy powder according to the GB/T1479.1-2011 method for measuring the apparent density of the metal powder;
measuring the flow rate of the CuCr alloy powder according to the standard of GB/T1482-;
measuring the granularity of the CuCr alloy powder according to the standard GB/T1480-2012 'granularity determination by dry sieving method for metal powder';
measuring the mass loss of the CuCr alloy powder after the hydrogen reduction process according to the GB/T5158.2-2011 Standard of 'measuring oxygen content by a metal powder reduction method';
the specific surface area of the CuCr alloy powder was measured according to the GB/T13390-2008 "determination of specific surface area of Metal powder".
The test results are shown in table 1:
table 1: CuCr alloy powder test results of examples 1 to 5 and comparative example
| Examples | Bulk Density (g/cm)3） | Deviation in particle size (um) | Flow rate (s/50 g) | Hydrogen loss (%) | Specific surface area (m)2/g） | Sphericity ratio (%) |
| 1 | 4.2 | 2.2 | 27.8 | 0.15 | 0.9 | 96 |
| 2 | 4.6 | 2.1 | 25.9 | 0.14 | 1.2 | 97 |
| 3 | 4.3 | 2.3 | 26.8 | 0.15 | 1.0 | 96 |
| 4 | 4.9 | 2.1 | 25.2 | 0.09 | 1.0 | 98 |
| 5 | 5.1 | 1.5 | 25.3 | 0.13 | 2.8 | 98 |
| Comparative example | 3.9 | 2.8 | 28.1 | 0.16 | 0.8 | 95 |
And (4) conclusion: as can be seen from the data in Table 1: compared with the detection results of comparative examples, the hydrogen loss of the CuCr alloy powder prepared by the method is smaller than that of the alloy powder prepared by the traditional method, which shows that the CuCr alloy powder has low gas content and high purity; the sphericity rate and the flow rate of the CuCr alloy powder prepared by the method are superior to those of the alloy powder prepared by the traditional method, which shows that the milling quality of the method is superior to that of the traditional method;
the particle size deviation of the embodiment 5 is far smaller than that of other embodiments, which indicates that the addition of the vibration ball mill to perform ball milling treatment on the CuCr alloy powder is beneficial to controlling the particle size of the alloy powder, reducing the particle size deviation and improving the powder preparation quality;
the hydrogen loss of the embodiment 4 is far less than that of other embodiments, which shows that the powder preparation by hot gas atomization can effectively reduce gas impurities in the powder in the atomization process and improve the purity of the powder.
Claims (3)
1. The preparation method of the alloy powder for recycling the copper-chromium alloy is characterized by comprising the following steps of:
s1: cleaning and drying
Cleaning and drying the CuCr alloy leftovers;
s2: vacuum induction melting
Placing the CuCr alloy leftovers obtained in the step S1 into a crucible of a smelting chamber; until the vacuum degree reaches 10-1Pa, starting heating; heating power gradient increase: keeping 40kW for 3-5 minutes, keeping 60kW for 3-5 minutes, and finally increasing to 80kW, closing the vacuum system when the CuCr alloy in the crucible begins to melt, and then filling argon to the standard atmospheric pressure; preheating the tundish, and keeping the power of a heating device at 7-30 kW; heating power is increased to 100-150 kW, so that the CuCr alloy is melted, and a completely melted CuCr alloy molten liquid is obtained;
s3: refining to remove impurities
Then reducing the heating power to 60-100 kW, waiting until impurities float on the surface of the CuCr alloy molten liquid, and removing surface impurities by using a slag remover;
s4: atomized powder
Heating power is increased to 100-150 kW, and when the superheat degree of the CuCr alloy molten liquid reaches 50-200 ℃, vacuum atomization is carried out in an atomization chamber to prepare powder, so that CuCr alloy atomized powder is obtained; the vacuum atomization powder preparation method comprises the following specific steps: the CuCr alloy molten liquid flows downwards through a flow guide nozzle, is atomized and crushed into a large number of fine liquid drops through a nozzle by 3MPa high-pressure inert gas flow, and is cooled to obtain CuCr alloy atomized powder; wherein, hot gas atomization is adopted, and inert gas is heated to 300 ℃; the flow rate of the nozzle melt is 5-25L/min, and the diameter of the alloy melt is 5 mm;
s5: sieving
Screening the CuCr alloy atomized powder obtained in the step S4 to obtain CuCr alloy powder with required granularity;
s6: ball milling treatment
Collecting CuCr alloy powder sieved in the step S5, and performing ball milling treatment by adopting a vibration ball mill; during ball milling treatment, 0.3 wt% of process control agent is added, wherein the process control agent is stearic acid; the grinding medium is 20mm quenched steel balls, and the filling rate is 65%; the ball milling treatment time is 12h, the ball material ratio is 5: 1, ball milling at a rotating speed of 130 r/min; and introducing liquid nitrogen for cooling during ball milling treatment.
2. The method for preparing alloy powder for recycling of copper-chromium alloy according to claim 1, wherein in step S1, high-pressure water is used to wash out the impurities adhered to the surface of the CuCr alloy scraps, then ultrasonic cleaning is used to remove oil stains and oxide layers on the surface, and finally drying is performed.
3. The method for preparing alloy powder for recycling of copper-chromium alloy according to claim 1, wherein in the step S5, a 230-mesh screen is adopted for screening to obtain CuCr alloy powder with the particle size of less than 60 mu m.
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