CN115464136A - Preparation method of high-purity electrode for spherical copper-chromium alloy powder process - Google Patents
Preparation method of high-purity electrode for spherical copper-chromium alloy powder process Download PDFInfo
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- CN115464136A CN115464136A CN202211040843.5A CN202211040843A CN115464136A CN 115464136 A CN115464136 A CN 115464136A CN 202211040843 A CN202211040843 A CN 202211040843A CN 115464136 A CN115464136 A CN 115464136A
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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
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Abstract
The invention discloses a preparation method of a high-purity electrode for a spherical copper-chromium alloy powder process, which comprises the following steps: s1, mixing carbon, S2, sintering and degassing, S3, crushing and pulverizing, S4, mixing copper and chromium, S5, carrying out cold isostatic pressing, S6, alloying a bar stock, and S7, and machining. The invention adopts the powder metallurgy process to prepare the copper-chromium alloy electrode, the gas content is low, the impurities are less, the electrode is uniform and good in consistency, and the prepared electrode bar material is close to the electrode size needed by EIGA and PREP, so the turning amount is extremely small, and the utilization rate of raw materials can be effectively improved.
Description
Technical Field
The invention relates to the technical field of electrode material preparation, in particular to a preparation method of a high-purity electrode for a spherical copper-chromium alloy powder process.
Background
In order to meet the requirements of additive manufacturing equipment and process, the metal powder has to have the characteristics of low oxygen and nitrogen content, good sphericity, narrow particle size distribution interval, high apparent density and the like. The plasma rotating electrode method (PREP), the plasma atomization method (PA), the vacuum induction melting gas atomization (VIGA), the vacuum induction electrode gas atomization (EIGA), and the plasma spheroidization method (PS) are the main methods for preparing metal powder for additive manufacturing at present, and they can all prepare spherical or near-spherical metal powder, wherein the PREP process and the EIGA process both require an electrode as a raw material.
The PREP method is to process metal or alloy into consumable electrode bar stock, heat the end of the bar stock with plasma, rotate the bar stock at high speed, throw out molten metal by centrifugal force to form small liquidity, solidify in inert gas environment and spheroidize under the action of surface tension to form powder.
The EIGA method combines gas atomization technology with electrode induction melting technology, and has the specific principle that alloy is processed into bar stock which is arranged on a feeding device, the whole device is vacuumized and filled with inert protective gas, an electrode bar enters a conical coil below the electrode bar at a certain rotating speed and a certain descending speed, the tip of the bar stock is gradually melted in the conical coil under the induction heating action to form melt liquid flow, the melt liquid flow directly flows into or drips into a non-limiting atomizer below the conical coil under the action of gravity, high-pressure inert gas enters the atomizer through a gas path pipeline, the metal liquid flow is broken into small liquid drops under the gas outlet under the interaction with the metal liquid flow, the small liquid drops are spherical under the action of tension, and then the small liquid drops are solidified into small particles.
Compared with the most widely applied VIGA work meeting at present, the PREP and VIGA processes have the advantages that parts such as a crucible and the like which are in contact with a metal melt are abandoned, the introduction of impurities in the smelting process can be effectively reduced, the degassing of the crucible is avoided, and the safe and clean smelting of active metals is realized. Although the two processes have obvious advantages, the introduction of gas and impurities can be effectively controlled in the atomization powder making process, the preparation process of the electrodes used by the two processes is influenced by smelting, particularly in the high-temperature smelting stage, the quality of the prepared electrodes is reduced due to the fact that a crucible is deflated and falls off, for copper-chromium alloy, inclusions are easy to generate due to corrosion of copper to the crucible, and meanwhile, chromium has extremely strong oxygen absorption performance, so that the quality of a copper-chromium electrode rod prepared by adopting a vacuum induction smelting method is low, in addition, for the copper-chromium electrode added with a special third element, the third element with large difference of melting point, boiling point and density with copper and chromium is difficult to ensure uniform components, the copper-chromium electrode meeting requirements cannot be prepared, and finally, because copper has good heat conductivity, the heat transfer of the cast structure of the copper-chromium electrode can be improved, so that energy consumption is caused in the EIGA powder making process, and energy waste or even energy cannot be smoothly melted to form a liquid flow. However, for the PREP process, it is necessary to have a high strength of the electrode itself to ensure sufficient strength for the rotation process. And finally, the electrode prepared by the smelting method needs to remove a riser shrinkage cavity and a bottom plate, and needs to be subjected to forging deformation treatment so as to achieve the required size, the surface of an ingot is oxidized and cracked in the forging process, surface processing needs to be carried out through a lathe, and the utilization rate of raw materials is greatly reduced in the processes.
The prior art mainly adopts a mode of (1) batching → (2) vacuum induction melting → (3) forging deformation → (4) heat treatment → (5) machining to prepare the electrode material, and has the following defects: 1) In the vacuum induction smelting process, because molten metal formed by heating raw materials is contacted with a crucible, the crucible is deflated and falls off; 2) Because copper has strong corrosivity to the crucible and chromium has strong oxygen absorption capacity, the purity of the material is further reduced, and the quality of the final electrode is reduced; 3) For the copper-chromium electrode needing to add the third element to optimize the performance, the limitation of smelting and the main components of the copper-chromium alloy is adopted, and the components and consistency of the third elements with low boiling points or high melting points or large density difference are difficult to effectively and fully ensure; 4) Because copper has good thermal conductivity, for some copper-chromium electrodes with high copper content, the heat of a smelting area is dissipated due to good heat dissipation characteristics in the EIGA powder making process of the electrodes with cast structures, the melting point temperature cannot be reached, and even the problem that an electrode-free rod cannot be melted to form a metal liquid flow is caused, so that extremely high power output is required, and energy waste is caused; 5) The casting head, the shrinkage cavity and the rough outer wall are generated in the smelting process in the preparation process of the as-cast electrode, the oxide skin and the large machining allowance are generated in the subsequent forging process, the defects are removed through a lathe and a sawing machine, the material waste is caused, and the utilization rate of raw materials is greatly reduced.
Disclosure of Invention
Aiming at the problems pointed out by the background technology, the invention provides a preparation method of a high-purity electrode for a spherical copper-chromium alloy powder process, which comprises the following steps:
s1, mixing carbon:
taking chromium powder and detecting the oxygen content of the chromium powder, carrying out carbon preparation according to the oxygen content of the chromium powder, and carrying out carbon preparation according to a reaction equation of thermal carbon reduction on the basis of O: c, calculating according to the molar ratio of 1:1 to obtain a carbon blending ratio A, adding 50-80% of carbon powder according to the ratio A to ensure that the carbon powder is in a carbon shortage state, then manually mixing the chromium powder and the carbon powder uniformly until the carbon powder is invisible to naked eyes, mixing the powder for 1-3 hours by using a mixer, finally enabling the carbon powder and the chromium powder to collide by using airflow grinding equipment (the airflow grinding equipment adopts the prior art) to be uniformly adhered to the surface of the chromium powder, then sampling to detect the addition ratio B of the carbon in the chromium powder, supplementing the carbon powder of (A-B) x 1.05, manually mixing uniformly, and then adding the carbon powder of (A-B) x 1.05 according to the ratio of the chromium powder: copper ball =100: ball milling and mixing powder for 3-10 h according to the weight ratio of 100, further crushing and dispersing the agglomerated carbon through ball milling and mixing powder, and ensuring the uniformity;
s2, sintering and degassing:
loosely loading the chromium powder uniformly mixed in the step S1 into a graphite crucible, wherein the loose loading can ensure effective pore passage exhaust, and then placing into a vacuum sintering furnace for vacuum sintering degassing to obtain a chromium powder blank;
s3, crushing and pulverizing:
crushing and pulverizing the chromium powder blank subjected to sintering and degassing in the step S2 to obtain high-purity low-gas chromium powder with the particle size of 450-830 microns;
s4, mixing copper and chromium:
and (3) proportioning and mixing the oxygen-free copper powder and the high-purity low-gas chromium powder obtained in the step S3 according to a required proportion to obtain mixed powder A, (if a third element such as Zr, te and the like needs to be added into the electrode material, the third element is added according to the required proportion), and mixing the oxygen-free copper powder and the high-purity low-gas chromium powder according to the ratio of the mixed powder A: copper ball =100: ball milling and mixing the powder for 3-12 h according to the weight ratio of 100 to obtain mixed powder B, wherein the mixing uniformity of the copper powder and the chromium powder and the effectiveness of adding a third element can be ensured through ball milling and mixing the powder;
s5, cold isostatic pressing:
pressing the mixed powder B obtained in the step (4) in a cold isostatic pressing mode to obtain a bar;
s6, alloying the bar stock:
alloying the bar obtained in the step S5 to obtain a high-purity electrode blank for the spherical copper-chromium alloy powder process;
s7, machining:
and (5) processing the electrode material blank prepared in the step (S6) into a required size according to the requirements of a drawing to obtain the high-purity electrode for the spherical copper-chromium alloy powder process.
Further, in the scheme, the particle size of the carbon powder is 1-6.5 microns, so that the chromium powder is effectively ensured to be fully contacted with the carbon powder.
Further, in the above scheme, the vacuum sintering degassing method in step S2 is: vacuumizing until the vacuum degree in the sintering furnace reaches below 1Pa, raising the temperature in the vacuum sintering furnace to 300-600 ℃ at the heating rate of 3-5 ℃/min, preserving the heat for 20-40 min to ensure that the gas adsorbed on the surface of the chromium powder is pumped away, then raising the temperature in the vacuum sintering furnace to 1400-1500 ℃ at the heating rate of 2-3 ℃/min, and preserving the heat for 4-8 h.
Description of the drawings: vacuum sintering refers to a method for performing protective sintering on a blank in a vacuum environment, and the heating mode is more, such as resistance heating, induction heating, microwave heating and the like. The vacuum sintering furnace is a furnace for performing protective sintering on a heated object by utilizing induction heating, and can be divided into types of industrial frequency, medium frequency, high frequency and the like, and the principle is that elements such as water vapor, hydrogen, oxygen, nitrogen and the like in a blank can escape from air holes along the grain boundary of the blank or through crystal grains by means of dissolution and diffusion in the sintering process under the vacuum condition, so that the density of a product is improved. The oxide can be reduced by carbon through vacuum sintering degassing, hot carbon reduction reaction is carried out, low-melting-point impurities and nitrides are removed by high temperature, and the purity of chromium is further improved.
Further, in the above scheme, the method for pulverizing powder in step S3 is: crushing by a jaw crusher, and grinding by a vibration mill or an air flow mill.
Description of the drawings: the working part of the jaw crusher is two jaw plates, one is a fixed jaw plate (fixed jaw), is vertically (or slightly outwards inclined at the upper end) fixed on the front wall of the crusher body, and the other is a movable jaw plate (movable jaw), is inclined in position, and forms a crushing cavity (working cavity) with the fixed jaw plate. The movable jaw is periodically reciprocated, away from and towards the fixed jaw. When the materials are separated, the materials enter the crushing cavity, and finished products are discharged from the lower part; when approaching, the material between the two jaws is squeezed, bent and split to be broken.
The vibration mill utilizes the high-frequency vibration of a cylinder, a steel ball or steel bar medium in the cylinder impacts materials by means of inertia force, and the acceleration of the medium impacting the materials can reach 10g-15g, so that the vibration mill has the advantages of compact structure, small volume, light weight, low energy consumption, high yield, concentrated grinding granularity, simplified process, simplicity in operation, convenience in maintenance, easiness in replacement of lining plate medium and the like, and can be widely applied to powder making in industries such as metallurgy, building materials, mines, fire resistance, chemical engineering, glass, ceramics, graphite and the like.
The jet mill is that compressed air is accelerated into supersonic airflow by Laval nozzle and then injected into crushing area to make the material fluidized (the airflow expands to make fluidized bed suspension boil and collide with each other), so that each particle has the same motion state. In the pulverizing zone, the accelerated particles collide with each other at the point where the nozzles meet to pulverize. The crushed material is conveyed to a grading area by ascending air flow, fine powder meeting the requirement of the granularity is screened out by a horizontally arranged grading wheel, and coarse powder not meeting the requirement of the granularity returns to the crushing area for continuous crushing. The qualified fine powder enters a high-efficiency cyclone separator along with the airflow to be collected, and the dust-containing gas is discharged into the atmosphere after being filtered and purified by a dust collector.
The crushing and grinding process of the jaw crusher, the vibration mill, the jet mill and other equipment is a mechanical crushing process, and impurities are not introduced and powder reaction is not caused.
Further, in the above scheme, in step S4, the ratio of the oxygen-free copper powder to the high-purity low-gas chromium powder is, by weight: cu: cr =99.9:0.1 to 30:70.
further, in the above scheme, in step S5, the cold isostatic pressing is dry bag type cold isostatic pressing, the pressure of the cold isostatic pressing is controlled to be 100 to 280Mpa, and the pressure maintaining time is 3 to 15min.
Description of the drawings: the cold isostatic press is to place the material in sealed elastic mold into liquid or gas container, apply certain pressure to the material with liquid or gas, press the material into solid body and obtain blank in the original shape. And after the pressure is released, taking the die out of the container, demolding, and further shaping the blank body according to requirements. Compare in wet bag formula cold isostatic pressing equipment that drenches, dry bag formula because the mould is in semi-fixity and not with liquid contact, has not only guaranteed the straightness accuracy of suppression bar, can effectively reduce the cutting output of follow-up processing, improves the utilization ratio of material, does not also effectively prevent with liquid contact moreover that aqueous vapor from invading the copper chromium bar, causes the bar pollution.
Further, in the above scheme, in step S6, the alloying treatment of the bar stock is a low-temperature sintering treatment or a hot isostatic pressing treatment.
Alternatively, in the above scheme, the method of the low-temperature sintering treatment is: putting the bar stock obtained in the step S5 into a vacuum sintering furnace, and enabling the vacuum to reach 8 multiplied by 10 -1 Degassing at 300-600 ℃ below pa, then filling inert gases such as argon and the like to micro negative pressure, and preserving the temperature for 2-5 hours at 980-1050 ℃, so as to alloy the bar stock, further remove adsorbed gases and effectively ensure the effective content of volatile third elements.
Description of the drawings: for the electrode for the EIGA process, the method is suitable for alloying the bar stock in a low-temperature sintering treatment mode.
Alternatively, in the above aspect, the hot isostatic pressing treatment is performed by: degassing the bar stock obtained in the step S5 by adopting a sheath, keeping the degassing temperature at 300-600 ℃, and keeping the vacuum degree to 10 in the degassing process -3 And judging that the degassing is finished when the pressure is not changed any more after Pa, then clamping a branch exhaust pipeline for hot isostatic pressing, controlling the temperature to be 1000-1050 ℃, controlling the pressure to be 150-350 Mpa, and keeping the pressure for 1-3 h, so as to alloy and improve the density of the bar stock to ensure that the bar stock has enough strength.
Description of the drawings: and for the electrode for the PREP process, the bar stock alloying is carried out in a mode suitable for hot isostatic pressing treatment.
The hot isostatic pressing process is to place the product inside a sealed container and apply the same pressure and high temperature to the product to sinter and densify the product. Hot isostatic pressing is an indispensable means for high performance material production and new material development; hot isostatic pressing can be carried out by direct powder molding, the powder is filled in a sheath (similar to the action of a mold), the sheath can be made of metal or ceramics (low-carbon steel, ni, mo, glass and the like), and then nitrogen and argon are used as pressurizing media to directly heat, pressurize and sinter the powder; or a molded casting; comprises an aluminum alloy; a titanium alloy; the castings with the shrinkage porosity such as high-temperature alloy and the like are subjected to hot isostatic pressing treatment, so that the castings can achieve 100% densification, and the overall mechanical property of the castings is improved.
Compared with the prior art, the copper-chromium electrode is prepared by adopting a powder metallurgy process, the possibility of introducing crucible inclusions due to high gas content caused by contact of raw materials and a crucible is eliminated, meanwhile, the gas content of the material is further reduced by adopting a hot carbon reduction reaction in the electrode preparation process, in addition, for a third element needing to be added, the problem that the uniform and consistent electrode cannot be prepared due to the difference of melting point, boiling point, density and the like is avoided, finally, because the process adopts different pressing modes in the forming process, the defect of fast heat dissipation of an as-cast electrode for an EIGA (electron cyclotron resonance interference analysis) electrode is overcome, the temperature rise of a heating area can be effectively ensured, a nearly fully-compact structure can be obtained for the electrode for a PREP (pre-press) process through pressing, the required strength is ensured, the size of the prepared bar material is close to that of the EIGA and the required electrode for the PREP is enough, the turning amount is extremely small, and the utilization rate of the raw materials can be effectively improved.
Detailed Description
Example 1
A preparation method of a high-purity electrode for a spherical copper-chromium alloy powder process comprises the following steps:
s1, mixing carbon:
taking chromium powder and detecting the oxygen content of the chromium powder, carrying out carbon preparation according to the oxygen content of the chromium powder, and carrying out carbon preparation on the carbon according to a reaction equation of thermal carbon reduction on O: c, calculating according to the molar ratio of 1:1 to obtain a carbon blending ratio A, adding 50% of carbon powder according to the ratio A to ensure that the carbon powder is in a carbon deficiency state, wherein the particle size of the carbon powder is 1-6.5 microns, then manually mixing chromium powder and the carbon powder uniformly until the carbon powder is invisible to naked eyes, then mixing the powder for 1h by using a mixer, finally enabling the carbon powder and the chromium powder to collide with each other by using airflow milling equipment to uniformly adhere to the surface of the chromium powder, then sampling to detect the addition ratio B of the carbon in the chromium powder, then supplementing the carbon powder of (A-B) x 1.05, manually mixing uniformly, and then adding the carbon powder of (A-B) x 1.05 according to the following ratio: copper ball =100:100 for 3 hours, and further crushing and dispersing agglomerated carbon by ball milling and powder mixing to ensure uniformity;
s2, sintering and degassing:
pouring the chromium powder mixed uniformly with the S1 into a graphite crucible in a loose manner, wherein the loose manner can ensure effective pore passage exhaust, and then placing the mixture into a vacuum sintering furnace for vacuum sintering degassing: vacuumizing until the vacuum degree in the sintering furnace reaches below 1Pa, raising the temperature in the vacuum sintering furnace to 300 ℃ at the heating rate of 3 ℃/min, preserving the heat for 20min to ensure that gas adsorbed on the surface of the chromium powder is extracted, raising the temperature in the vacuum sintering furnace to 1400 ℃ at the heating rate of 2 ℃/min, and preserving the heat for 4h to obtain a chromium powder blank;
s3, crushing and preparing powder:
crushing the chromium powder blank degassed by sintering in the step S2 to prepare powder (crushing by adopting a jaw crusher, and then grinding by adopting a vibration mill or an air flow mill) to obtain high-purity low-gas chromium powder with the particle size of 450-830 mu m;
s4, mixing copper and chromium:
the oxygen-free copper powder and the high-purity low-gas chromium powder obtained in the step S3 are calculated according to the weight proportion, and the proportion of the oxygen-free copper powder to the high-purity low-gas chromium powder is as follows: cu: cr =99.9:0.1, and mixing to obtain mixed powder A (if a third element such as Zr and Te is required to be added to the electrode material, the third element is added according to a required proportion), mixing the components according to the weight ratio of the mixed powder A: copper ball =100: ball milling and mixing the powder for 3 hours according to the weight ratio of 100 to obtain mixed powder B, wherein the mixing uniformity of the copper powder and the chromium powder and the effectiveness of adding a third element can be ensured through ball milling and mixing the powder;
s5, cold isostatic pressing:
pressing the mixed powder B obtained in the step (4) in a cold isostatic pressing mode, wherein the cold isostatic pressing is dry bag type cold isostatic pressing, the pressure of the cold isostatic pressing is controlled to be 100Mpa, and the pressure maintaining time is 3min, so that a bar material is obtained;
s6, alloying the bar stock:
and (3) performing low-temperature sintering treatment on the bar stock obtained in the step (S5): putting the bar stock obtained in the step S5 into a vacuum sintering furnace, and enabling the vacuum to reach 8 multiplied by 10 -1 Degassing at 300 ℃ below pa, then introducing inert gases such as argon and the like to micro negative pressure, and preserving heat at 980 ℃ for 2 hours to obtain the spherical high-purity electrode blank for the copper-chromium alloy powder process;
s7, machining:
and (5) processing the electrode material blank prepared in the step (S6) into a required size according to the requirements of a drawing to obtain the high-purity electrode for the spherical copper-chromium alloy powder process.
Example 2
A preparation method of a high-purity electrode for a spherical copper-chromium alloy powder process comprises the following steps:
s1, mixing carbon:
taking chromium powder and detecting the oxygen content of the chromium powder, carrying out carbon preparation according to the oxygen content of the chromium powder, and carrying out carbon preparation according to a reaction equation of thermal carbon reduction on the basis of O: c, calculating according to the molar ratio of 1:1 to obtain a carbon blending ratio A, adding 60% of carbon powder according to the ratio A to ensure that the carbon powder is in a carbon deficiency state, wherein the particle size of the carbon powder is 1-6.5 microns, then manually mixing chromium powder and the carbon powder uniformly until the carbon powder is invisible to naked eyes, then mixing the powder for 2 hours by using a mixer, finally enabling the carbon powder and the chromium powder to collide with each other by using airflow milling equipment to uniformly adhere to the surface of the chromium powder, then sampling to detect the addition ratio B of the carbon in the chromium powder, then supplementing the carbon powder of (A-B) x 1.05, manually mixing uniformly, and then adding the carbon powder of (A-B) x 1.05 according to the following ratio: copper ball =100:100 for 6 hours, and further crushing and dispersing agglomerated carbon by ball milling and powder mixing to ensure uniformity;
s2, sintering and degassing:
pouring the chromium powder mixed uniformly with the S1 into a graphite crucible in a loose manner, wherein the loose manner can ensure effective pore passage exhaust, and then placing the mixture into a vacuum sintering furnace for vacuum sintering degassing: vacuumizing until the vacuum degree in the sintering furnace reaches below 1Pa, raising the temperature in the vacuum sintering furnace to 500 ℃ at the heating rate of 3 ℃/min, preserving the heat for 30min to ensure that gas adsorbed on the surface of the chromium powder is pumped away, then raising the temperature in the vacuum sintering furnace to 1450 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 6h to obtain a chromium powder blank;
s3, crushing and pulverizing:
crushing the chromium powder blank degassed by sintering in the step S2 to prepare powder (crushing by adopting a jaw crusher, and then grinding by adopting a vibration mill or an air flow mill) to obtain high-purity low-gas chromium powder with the particle size of 450-830 mu m;
s4, mixing copper and chromium:
the method comprises the following steps of (1) weighing the oxygen-free copper powder and the high-purity low-gas chromium powder obtained in the step (S3) according to the weight proportion: cu: cr =50:50, and mixing to obtain mixed powder A (if a third element such as Zr and Te is required to be added into the electrode material, the third element is added according to a required proportion), mixing the mixed powder A: copper ball =100: the weight ratio of 100 is subjected to ball milling and powder mixing for 8 hours to obtain mixed powder B, and the uniformity of mixing copper powder and chromium powder and the effectiveness of adding a third element can be ensured through ball milling and powder mixing;
s5, cold isostatic pressing:
pressing the mixed powder B obtained in the step (4) in a cold isostatic pressing mode, wherein the cold isostatic pressing is dry bag type cold isostatic pressing, the pressure of the cold isostatic pressing is controlled to be 200Mpa, and the pressure maintaining time is 10min, so that a bar is obtained;
s6, alloying the bar stock:
and (3) performing low-temperature sintering treatment on the bar stock obtained in the step (S5): putting the bar stock obtained in the step S5 into a vacuum sintering furnace, and enabling the vacuum to reach 8 multiplied by 10 -1 Degassing at 500 ℃ below pa, introducing inert gases such as argon and the like to micro negative pressure, and preserving heat at 1000 ℃ for 3 hours to obtain the spherical high-purity electrode blank for the copper-chromium alloy powder process;
s7, machining:
and (4) processing the electrode material blank obtained in the step (S6) into a required size according to the drawing requirements to obtain the high-purity electrode for the spherical copper-chromium alloy powder process.
Example 3
A preparation method of a high-purity electrode for a spherical copper-chromium alloy powder process comprises the following steps:
s1, mixing carbon:
taking chromium powder and detecting the oxygen content of the chromium powder, carrying out carbon preparation according to the oxygen content of the chromium powder, and carrying out carbon preparation on the carbon according to a reaction equation of thermal carbon reduction on O: c, calculating according to the molar ratio of 1:1 to obtain a carbon blending ratio A, adding 80% of carbon powder according to the ratio A to ensure that the carbon powder is in a carbon deficiency state, wherein the particle size of the carbon powder is 1-6.5 microns, then manually mixing chromium powder and the carbon powder uniformly until the carbon powder is invisible to naked eyes, then mixing the powder for 3 hours by using a mixer, finally enabling the carbon powder and the chromium powder to collide with each other by using airflow milling equipment to uniformly adhere to the surface of the chromium powder, then sampling to detect the addition ratio B of the carbon in the chromium powder, then supplementing the carbon powder of (A-B) x 1.05, manually mixing uniformly, and then adding the chromium powder according to the following ratio: copper ball =100: ball milling and powder mixing are carried out for 10 hours according to the weight ratio of 100, and the agglomerated carbon is further crushed and dispersed through ball milling and powder mixing, so that the uniformity is ensured;
s2, sintering and degassing:
and (2) loosely loading the chromium powder uniformly mixed in the S1 into a graphite crucible, wherein effective pore passage exhaust can be ensured by loose loading, and then placing the chromium powder into a vacuum sintering furnace for vacuum sintering degassing: vacuumizing until the vacuum degree in the sintering furnace reaches below 1Pa, raising the temperature in the vacuum sintering furnace to 600 ℃ at the heating rate of 5 ℃/min, preserving the heat for 40min to ensure that gas adsorbed on the surface of the chromium powder is extracted, raising the temperature in the vacuum sintering furnace to 1500 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 8h to obtain a chromium powder blank;
s3, crushing and pulverizing:
crushing the chromium powder blank degassed by sintering in the step S2 to prepare powder (crushing by adopting a jaw crusher, and then grinding by adopting a vibration mill or an air flow mill) to obtain high-purity low-gas chromium powder with the particle size of 450-830 mu m;
s4, mixing copper and chromium:
the oxygen-free copper powder and the high-purity low-gas chromium powder obtained in the step S3 are calculated according to the weight proportion, and the proportion of the oxygen-free copper powder to the high-purity low-gas chromium powder is as follows: cu: cr =30:70, and mixing to obtain mixed powder A (if a third element such as Zr, te is required to be added into the electrode material, the third element is added according to a required proportion), mixing the mixed powder A: copper ball =100: the powder is ball-milled and mixed for 12 hours according to the weight ratio of 100 to obtain mixed powder B, and the uniformity of mixing copper powder and chromium powder and the effectiveness of adding a third element can be ensured through ball-milling and mixing the powder;
s5, cold isostatic pressing:
pressing the mixed powder B obtained in the step (4) in a cold isostatic pressing mode, wherein the cold isostatic pressing is dry bag type cold isostatic pressing, the pressure of the cold isostatic pressing is controlled to be 280Mpa, and the pressure maintaining time is 15min, so as to obtain a bar material;
s6, alloying the bar stock:
and (3) performing low-temperature sintering treatment on the bar stock obtained in the step (S5): putting the bar stock obtained in the step S5 into a vacuum sintering furnace, and enabling the vacuum to reach 8 multiplied by 10 -1 Degassing below pa grade at 600 ℃, then introducing inert gases such as argon and the like to micro negative pressure, and preserving heat for 5 hours at 1050 ℃ to obtain a high-purity electrode blank for the spherical copper-chromium alloy powder process;
s7, machining:
and (4) processing the electrode material blank obtained in the step (S6) into a required size according to the drawing requirements to obtain the high-purity electrode for the spherical copper-chromium alloy powder process.
The electrodes prepared in examples 1 to 3 were suitable for the EIGA process.
Example 4
The present embodiment is different from embodiment 1 in that:
in step S6, hot isostatic pressing is performed on the bar obtained in step S5: degassing the bar stock obtained in the step S5 by adopting a sheath, keeping the degassing temperature at 300 ℃, and keeping the vacuum degree to 10 in the degassing process -3 And judging that the degassing is finished when the pressure is not changed any more after Pa, then clamping a branch exhaust pipeline for hot isostatic pressing, controlling the temperature at 1000 ℃, controlling the pressure at 150Mpa, and maintaining the pressure for 1h to obtain the high-purity electrode blank for the spherical copper-chromium alloy powder process.
Example 5
This embodiment is different from embodiment 4 in that:
in step S6, hot isostatic pressing is performed on the bar obtained in step S5: degassing the bar stock obtained in the step S5 by adopting a sheath, keeping the degassing temperature at 500 ℃, and keeping the vacuum degree to 10 in the degassing process -3 And judging that the degassing is finished when the pressure is not changed any more after Pa, then clamping a branch exhaust pipeline for hot isostatic pressing, controlling the temperature at 1020 ℃, controlling the pressure at 250Mpa, and maintaining the pressure for 2h to obtain the high-purity electrode blank for the spherical copper-chromium alloy powder process.
Example 6
The present embodiment is different from embodiment 4 in that:
in step S6, hot isostatic pressing is performed on the bar obtained in step S5: degassing the bar stock obtained in the step S5 by adopting a sheath, keeping the degassing temperature at 600 ℃, and keeping the vacuum degree to 10 in the degassing process -3 And judging that the degassing is finished when the pressure is not changed any more after Pa, then clamping a branch exhaust pipeline for hot isostatic pressing, controlling the temperature at 1050 ℃, controlling the pressure at 350Mpa, and maintaining the pressure for 3h to obtain the high-purity electrode blank for the spherical copper-chromium alloy powder process.
The electrodes prepared in examples 4 to 6 are suitable for the PREP process.
The performance of the electrode materials of examples 1 to 6 was measured, and the results are shown in table 1.
Table 1 results of testing the properties of the electrode materials of examples 1 to 6 and the blank control group
As can be seen from table 1, the gas content of examples 2 and 5 is much lower than that of the control (melting process) process, mainly due to the degassing of chromium in the early stage, and the examples 2 and 5 do not use crucible melting, so that there is no crucible gassing, and the gas content of example 5 is much lower, mainly due to the better degassing of the hot isostatic pressing process.
The data can show that the impurity content of the embodiments 2 and 5 is lower than that of the reference group (smelting method), particularly the content of silicon, calcium and magnesium is obviously reduced, which is mainly that the reference group smelting method needs a crucible as a carrier, and the phenomenon of falling of the crucible exists in the process, so that impurities are introduced. Further, examples 2 and 5 are low in Si/Al because of volatilization.
The data show that the density is more than 85% in examples 1-3, meets the EIGA process, and is more than 98% in examples 4-6, and meets the strength requirement of the PREP powder preparation process.
Claims (9)
1. A preparation method of a high-purity electrode for a spherical copper-chromium alloy powder process is characterized by comprising the following steps:
s1, mixing carbon:
taking chromium powder and detecting the oxygen content of the chromium powder, carrying out carbon preparation according to the oxygen content of the chromium powder, and carrying out carbon preparation on the carbon according to a reaction equation of thermal carbon reduction on O: c, calculating according to the molar ratio of 1:1 to obtain a carbon blending ratio A, adding 50-80% of carbon powder according to the ratio A to ensure that the carbon powder is in a carbon deficiency state, manually mixing chromium powder and the carbon powder, mixing the powder for 1-3 hours by using a mixer, finally enabling the carbon powder and the chromium powder to collide by using airflow mill equipment to be uniformly adhered to the surface of the chromium powder, sampling to detect the addition ratio B of the carbon in the chromium powder, supplementing the carbon powder of (A-B) x 1.05, and manually mixing uniformly according to the following ratio: copper ball =100: ball milling and mixing powder for 3-10 h according to the weight ratio of 100;
s2, sintering and degassing:
loosely loading the chromium powder uniformly mixed in the step S1 into a graphite crucible, and then putting the graphite crucible into a vacuum sintering furnace for vacuum sintering degassing to obtain a chromium powder blank;
s3, crushing and preparing powder:
crushing and pulverizing the chromium powder blank subjected to sintering and degassing in the step S2 to obtain high-purity low-gas chromium powder with the particle size of 450-830 microns;
s4, mixing copper and chromium:
and (3) proportioning and mixing the oxygen-free copper powder and the high-purity low-gas chromium powder obtained in the step (S3) according to a required proportion to obtain mixed powder A, and if third elements such as Zr, te and the like need to be added into the electrode material, adding the oxygen-free copper powder and the high-purity low-gas chromium powder according to the required proportion, wherein the oxygen-free copper powder and the high-purity low-gas chromium powder obtained in the step (A) are prepared by the steps of: copper ball =100: ball-milling and mixing the powder for 3-12 h according to the weight ratio of 100 to obtain mixed powder B;
s5, cold isostatic pressing:
pressing the mixed powder B obtained in the step (4) in a cold isostatic pressing mode to obtain a bar;
s6, alloying the bar stock:
alloying the bar obtained in the step S5 to obtain a high-purity electrode blank for the spherical copper-chromium alloy powder process;
s7, machining:
and (5) processing the electrode material blank prepared in the step (S6) into a required size according to the requirements of a drawing to obtain the high-purity electrode for the spherical copper-chromium alloy powder process.
2. The method for preparing a high-purity electrode for a spherical copper-chromium alloy powder process according to claim 1, wherein the particle size of the carbon powder is 1-6.5 μm.
3. The method for preparing the high-purity electrode for the spherical copper-chromium alloy powder process according to claim 1, wherein the vacuum sintering degassing method in the step S2 comprises the following steps: vacuumizing until the vacuum degree in the sintering furnace reaches below 1Pa, raising the temperature in the vacuum sintering furnace to 300-600 ℃ at the heating rate of 3-5 ℃/min, preserving the heat for 20-40 min to extract the gas adsorbed on the surface of the chromium powder, raising the temperature in the vacuum sintering furnace to 1400-1500 ℃ at the heating rate of 2-3 ℃/min, and preserving the heat for 4-8 h.
4. The method for preparing the high-purity electrode for the spherical copper-chromium alloy powder process according to claim 1, wherein the method for crushing and preparing the powder in the step S3 comprises the following steps: crushing by a jaw crusher, and grinding by a vibration mill or an air flow mill.
5. The preparation method of the high-purity electrode for the spherical copper-chromium alloy powder process according to claim 1, wherein in the step S4, the proportion of the oxygen-free copper powder and the high-purity low-gas chromium powder is as follows according to the weight ratio: cu: cr =99.9:0.1 to 30:70.
6. the method for preparing a high purity electrode for spherical copper-chromium alloy powder process according to claim 1, wherein in step S5, the cold isostatic pressing is dry bag type cold isostatic pressing, the pressure of the cold isostatic pressing is controlled to be 100-280 Mpa, and the pressure holding time is 3-15 min.
7. The method for preparing the high-purity electrode for the spherical Cu-Cr alloy powder process as claimed in claim 1, wherein in step S6, the bar alloying treatment is a low-temperature sintering treatment or a hot isostatic pressing treatment.
8. The preparation method of the high-purity electrode for the spherical copper-chromium alloy powder process according to claim 7, wherein the low-temperature sintering treatment method comprises the following steps: putting the bar stock obtained in the step S5 into a vacuum sintering furnace, and enabling the vacuum to reach 8 multiplied by 10 -1 Degassing at 300-600 ℃ below pa, then filling inert gases such as argon and the like to a micro negative pressure, and preserving heat for 2-5 hours at 980-1050 ℃.
9. The method for preparing the high-purity electrode for the spherical copper-chromium alloy powder process according to claim 7, wherein the hot isostatic pressing treatment is carried out by the following steps: degassing the bar stock obtained in the step S5 by adopting a sheath, keeping the degassing temperature at 300-600 ℃, and keeping the vacuum degree to 10 in the degassing process -3 Judging that the degassing is finished when the pressure is not changed any more after Pa, and then carrying out hot isostatic pressing, wherein the temperature is controlled to be 1000-1050 ℃, the pressure is controlled to be 150-350 Mpa, and the pressure maintaining time is 1-3 h.
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