CN112091224A - Method for preparing metal chromium powder by ultralow temperature grinding - Google Patents

Method for preparing metal chromium powder by ultralow temperature grinding Download PDF

Info

Publication number
CN112091224A
CN112091224A CN202011250219.9A CN202011250219A CN112091224A CN 112091224 A CN112091224 A CN 112091224A CN 202011250219 A CN202011250219 A CN 202011250219A CN 112091224 A CN112091224 A CN 112091224A
Authority
CN
China
Prior art keywords
powder
grinding
chromium
chromium powder
blocks
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202011250219.9A
Other languages
Chinese (zh)
Other versions
CN112091224B (en
Inventor
聂红锋
闫利平
孙刚刚
王文斌
梁建斌
梁鹏帅
宋新华
冯亚红
朱金泽
翟荣荣
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sirui Advanced Copper Alloy Co ltd
Original Assignee
Sirui Advanced Copper Alloy Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sirui Advanced Copper Alloy Co ltd filed Critical Sirui Advanced Copper Alloy Co ltd
Priority to CN202011250219.9A priority Critical patent/CN112091224B/en
Publication of CN112091224A publication Critical patent/CN112091224A/en
Application granted granted Critical
Publication of CN112091224B publication Critical patent/CN112091224B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/10Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00Other disintegrating devices or methods
    • B02C19/18Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
    • B02C19/186Use of cold or heat for disintegrating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
    • B02C23/08Separating or sorting of material, associated with crushing or disintegrating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • B22F1/142Thermal or thermo-mechanical treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • B22F1/145Chemical treatment, e.g. passivation or decarburisation
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/041Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3244Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/612Machining

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Food Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a method for preparing metal chromium powder by ultra-low temperature grinding, which relates to the technical field of metal powder preparation and comprises the following steps: s1, crushing, namely crushing the original chromium block by a crusher, and ensuring that the particle size of the crushed chromium block is less than 10 mm; s2, ultra-low temperature grinding, namely grinding the crushed chromium blocks at low temperature to prepare powder, introducing a protective medium, and controlling the temperature to be-150-0 ℃; s3, drying, namely performing vacuum drying treatment on the chromium powder after low-temperature grinding, and controlling the temperature to be 60-100 ℃; s4, screening, namely screening and grading the dried chromium powder, and selecting a target screen to obtain the target particle size; the metal chromium powder prepared by the invention has low impurity element content and low gas content, and the appearance of chromium particles is irregular.

Description

Method for preparing metal chromium powder by ultralow temperature grinding
Technical Field
The invention relates to the technical field of metal powder preparation, in particular to a method for preparing metal chromium powder by ultralow temperature grinding.
Background
Chromium is an important alloy element, and is widely applied to the fields of metallurgy, chemical industry, cast iron, fire resistance, high-precision science and technology and the like because of the excellent characteristics of hardness, brittleness, corrosion resistance and the like.
The metal chromium powder is widely applied to copper chromium contacts, vacuum sputtering coating targets, high-temperature alloy materials, 3D printing materials, high-performance welding materials, chromium-containing powder metallurgy products and the like.
At present, the method for producing chromium powder at home and abroad is a mechanical grinding method.
Mechanical grinding method: a method for producing a metal or alloy powder by mechanical pulverization. The method mainly comprises a ball milling method and a fluidized bed airflow milling method.
Ball milling method: this is usually done by charging the material into a ball mill. In the ball milling process, materials are among the grinding balls which are stirred intensively and are subjected to repeated actions of impact force, grinding force, shearing force and pressure, so that the materials are continuously deformed, crushed and cold welded. The method can be directly used for producing brittle and hard metal or oxide powder; meanwhile, the method can also be used for treating the agglomeration of metal powder, atomized powder or electrolytic powder by a reduction method.
Fluidized bed jet milling: the material particles are accelerated by the compressed gas in the fluidized bed and are micronized by the collision of the high velocity particles with the particles.
Ball milling method: the impurity content and the gas content of the chromium powder are obviously increased after ball milling.
Fluidized bed jet milling: the prepared chromium powder has excessively fine particle size and excessively high surface adsorbed gas content.
Disclosure of Invention
In order to solve the technical problem, the invention provides a method for preparing metal chromium powder by ultralow temperature grinding.
The technical scheme of the invention is as follows: a method for preparing metal chromium powder by ultra-low temperature grinding comprises the following steps:
s1: crushing
Selecting original chromium blocks, then putting the selected chromium blocks into liquid nitrogen for freezing for 1h, crushing the frozen metal chromium blocks by a crusher, filtering the crushed chromium particles by a screen, wherein the size of the aperture of the screen is 10mm, secondarily crushing the particles left on the screen, and refrigerating the particles passing through the screen;
s2: ultra-low temperature grinding
Placing the refrigerated particles into a grinder, adding grinding medium, introducing protective medium liquid nitrogen, controlling the grinding temperature at-150-0 deg.C, controlling the flow rate of liquid nitrogen at 5-10 m/h, grinding for 2-5h, collecting the powder, elutriating with gasoline, wherein the liquid level of gasoline is higher than that of chromium powder, and adding nano Al during elutriation2O3And ZrO2Mixing to obtain high-toughness ceramic blocks, wherein the particle diameter of the high-toughness ceramic blocks is 0.5-1cm, fishing the ceramic blocks by using a screen after the elutriation is finished, and then filtering out chromium powder by using filter cloth;
s3: drying by baking
Putting the chromium powder obtained in the step S2 into a drying device, drying at 60-100 ℃ for 0.5-0.8h, stirring at the stirring speed of 10-20r/min during drying, recovering evaporated gasoline during drying, reusing, vacuumizing the drying device at the vacuum degree of 6-7Pa, and airing at low temperature for 20-30min after drying;
s4: sieving
And (3) grading and screening the clean chromium powder obtained in the step (S3), carrying out multi-stage screening according to the particle size of the chromium powder, carrying out middle-stage screening to obtain low-grade powder and high-grade powder, simultaneously subdividing the high-grade chromium powder and the low-grade chromium powder, collecting powder which does not reach the standard in the low-grade powder, and repeating the steps (S2) -S4).
Further, in the step S2, when grinding, the power of the grinder is first adjusted to the ball-milling rotation number of 100r/min, and after 1 hour, the ball-milling rotation number is then adjusted to 500r/min, and the grinding is continued to be performed to be powder.
Further, standing the gasoline washed in the step S2 for 12-18h, taking a hose, introducing the supernatant onto industrial anti-static filter cloth by using a siphon principle, collecting the filtrate below the filter cloth by using a barrel, repeating the steps for three times, and recycling the gasoline.
Further, the chromium powder obtained in the step S4 is led into a microwave heating furnace for decarburization treatment, the heating temperature is 450-610 ℃, the heating time is 30min, after heating is finished, the temperature is cooled to room temperature, and graphite particles are separated to obtain the decarburized chromium powder.
Further, the decarburized chromium powder is introduced into a ceramic container provided with a hydrogen plasma radio frequency device, the decarburized chromium powder is subjected to reduction deoxidation by using hydrogen as reducing gas, and a cooling device is arranged in the container.
Further, in the step S2, the grinding medium in the grinder is tungsten steel, the lining is made of zirconia, liquid nitrogen is used as temperature-controlled gas during grinding, helium is introduced as protective gas, the gas flow is 10-25m for cultivation/h, and the ball-to-material ratio is 10: 1.
Further, sampling and detecting the chromium powder after deoxidation, wherein the detection items comprise carbon content, oxygen content, color and chemical components, and the chromium powder qualified in detection is subjected to bag-dividing vacuum packaging and then enters a storage link.
Further, in the elutriation in step S2, the magnet is added to the chromium powder, the elutriation is performed by electromagnetic stirring, and the iron powder on the magnet is cleaned after the elutriation is completed.
Further, the nano Al2O3And ZrO2The preparation method of the high-toughness ceramic block prepared by mixing comprises the following steps:
s2-1: mixing nano Al2O3Powder and ZrO2Mixing the powder according to the weight ratio of 1:1, and uniformly mixing in an electromagnetic stirring device to obtain a mixed additive;
s2-2: breaking the porcelain stone to 1-2cm3Grinding the materials in a grinding device to obtain grinding powder, elutriating the grinding powder, removing impurities, adding the mixed additive obtained in S2-1, wherein the weight ratio of the mixed additive to the grinding powder is 1:20, stirring elutriation liquid, uniformly stirring, precipitating for 24 hours, and filtering precipitate liquid to obtain soft mud blocks;
s2-3: and drying the soft mud blocks to obtain hard mud blocks, cutting the hard mud blocks into a specified size, and firing to obtain the finished high-toughness ceramic blocks.
The invention has the beneficial effects that:
(1) the method can reduce impurities in the chromium powder through elutriation, can also remove iron elements in the chromium powder, can reduce the oxygen content in the chromium powder through deoxidation treatment, and can effectively reduce the carbon content in the chromium powder through a carbon removal process.
(2) The metal chromium powder prepared by the invention has the advantages that: the increment of impurity elements is low, the gas content is low, and the shape of chromium particles is irregular.
Detailed Description
Example 1:
a method for preparing metal chromium powder by ultra-low temperature grinding comprises the following steps:
s1: crushing
Selecting original chromium blocks, then putting the selected chromium blocks into liquid nitrogen for freezing for 0.5h, crushing the frozen metal chromium blocks by a crusher, filtering the crushed chromium particles by a screen, wherein the aperture of the screen is 10mm, secondarily crushing the particles left on the screen, and refrigerating the particles passing through the screen;
s2: ultra-low temperature grinding
Put cold-stored granule into the machine of grinding, add grinding medium, and let in protection medium liquid nitrogen, grinding temperature control is at-150 ℃, the liquid nitrogen velocity of flow is 5m for thin year/h, it is 2h to grind duration, earlier when grinding machine power adjustment ball-milling revolution number 100r/min, last 1h back, again will grind ball-milling revolution number and transfer to 500r/min and continue to grind to powdered, grinding medium in the machine of grinding is the tungsten steel, the inside lining is the zirconia material, liquid nitrogen is as accuse temperature gas in the course of grinding, let in addition and let in the helium as protective gas, gas flow is 10m mansion/h, the ball material ratio is 10:1, collecting the powder obtained after grinding, elutriating by adopting gasoline, wherein the liquid level of the gasoline is higher than that of the chromium powder, and adding nano Al during elutriation2O3And ZrO2Mixing the prepared high-toughness ceramic blocks, wherein the particle diameter of each high-toughness ceramic block is 0.5cm, fishing the ceramic blocks by using a screen after elutriation is finished, filtering out chromium powder by using filter cloth, standing the elutriated gasoline for 12 hours, taking a hose, introducing a supernatant onto industrial anti-static filter cloth by using a siphon principle, collecting a filtrate below the filter cloth by using a barrel, repeating the process for three times, recycling the gasoline, adding a magnet into the chromium powder during elutriation, elutriating by using an electromagnetic stirring mode, and cleaning iron powder on the magnet after elutriation is finished;
s3: drying by baking
Putting the chromium powder obtained in the step S2 into a drying device, drying at 60 ℃ for 0.5h, stirring at the stirring speed of 10r/min during drying, recovering evaporated gasoline during drying, recycling, vacuumizing the drying device at the vacuum degree of 6Pa, and airing at the low temperature of 4 ℃ for 20min after drying;
s4: sieving
Classifying and screening the clean chromium powder obtained in the step S3, performing multi-stage screening according to the particle size of the chromium powder, performing intermediate-stage screening to obtain low-grade powder and high-grade powder, subdividing the high-grade chromium powder and the low-grade chromium powder simultaneously, collecting substandard powder in the low-grade powder, repeating the steps S2-S4, introducing the obtained chromium powder into a microwave heating furnace for decarburization treatment, heating at 450 ℃ for 30min, cooling to room temperature after heating is completed, separating graphite particles to obtain decarburized chromium powder, introducing the decarburized chromium powder into a ceramic container provided with hydrogen plasma radio frequency equipment, reducing and deoxidizing the decarburized chromium powder by using hydrogen as reducing gas, installing a cooling device in the container, sampling and detecting the decarburized chromium powder, wherein detection items comprise carbon content, oxygen content, color and luster and chemical components, and qualified detected chromium powder, performing bag-dividing vacuum packaging, and then entering a storage link;
the nano Al2O3And ZrO2The preparation method of the high-toughness ceramic block prepared by mixing comprises the following steps:
s2-1: mixing nano Al2O3Powder and ZrO2Mixing the powder according to the weight ratio of 1:1, and uniformly mixing in an electromagnetic stirring device to obtain a mixed additive;
s2-2: breaking the porcelain stone to 1cm3Grinding the materials in a grinding device to obtain grinding powder, elutriating the grinding powder, removing impurities, adding the mixed additive obtained in S2-1, wherein the weight ratio of the mixed additive to the grinding powder is 1:20, stirring elutriation liquid, uniformly stirring, precipitating for 24 hours, and filtering precipitate liquid to obtain soft mud blocks;
s2-3: and drying the soft mud blocks to obtain hard mud blocks, cutting the hard mud blocks into a specified size, and firing to obtain the finished high-toughness ceramic blocks.
Example 2:
a method for preparing metal chromium powder by ultra-low temperature grinding comprises the following steps:
s1: crushing
Selecting original chromium blocks, then putting the selected chromium blocks into liquid nitrogen for freezing for 0.7h, crushing the frozen metal chromium blocks by a crusher, filtering the crushed chromium particles by a screen, wherein the aperture of the screen is 10mm, secondarily crushing the particles left on the screen, and refrigerating the particles passing through the screen;
s2: ultra-low temperature grinding
Grinding the refrigerated granulesGrinding the mixture into powder, wherein the grinding medium is added into a grinding machine, liquid nitrogen serving as a protective medium is introduced into the grinding machine, the grinding temperature is controlled to be-100 ℃, the flow speed of the liquid nitrogen is 7.5 m/h, the grinding time is 3.5h, the power of the grinding machine is adjusted to the grinding rotation number of 100r/min during grinding, the grinding rotation number of the grinding ball is adjusted to 500r/min after the grinding is continued for 1h, the grinding is continued to be ground into powder, the grinding medium in the grinding machine is tungsten steel, the lining is made of zirconium oxide, liquid nitrogen serves as temperature control gas during grinding, helium serves as protective gas is introduced into the grinding machine, the gas flow is 18m of profile/h, the ball-to-material ratio is 10:1, the powder obtained after grinding is collected and elutriated by adopting gasoline, the liquid level of2O3And ZrO2Mixing the prepared high-toughness ceramic blocks, wherein the particle diameter of each high-toughness ceramic block is 0.7cm, fishing out the ceramic blocks by using a screen after elutriation is finished, filtering out chromium powder by using filter cloth, standing the elutriated gasoline for 15 hours, taking a hose, introducing a supernatant onto industrial anti-static filter cloth by using a siphon principle, collecting a filtrate below the filter cloth by using a barrel, repeating the process for three times, recycling the gasoline, adding a magnet into the chromium powder during elutriation, elutriating by using an electromagnetic stirring mode, and cleaning iron powder on the magnet after elutriation is finished;
s3: drying by baking
Putting the chromium powder obtained in the step S2 into a drying device, drying at 80 ℃ for 0.6h, stirring at the stirring speed of 15r/min during drying, recovering evaporated gasoline during drying, recycling, vacuumizing the drying device at the vacuum degree of 6.5Pa, and airing at the low temperature of 5 ℃ for 25min after drying is finished;
s4: sieving
Classifying and screening the clean chromium powder obtained in the step S3, performing multi-stage screening according to the particle size of the chromium powder, performing intermediate-stage screening to obtain low-grade powder and high-grade powder, subdividing the high-grade chromium powder and the low-grade chromium powder simultaneously, collecting substandard powder in the low-grade powder, repeating the steps S2-S4, introducing the obtained chromium powder into a microwave heating furnace for decarburization treatment at the heating temperature of 550 ℃ for 30min, cooling to room temperature after heating is completed, separating graphite particles to obtain decarburized chromium powder, introducing the decarburized chromium powder into a ceramic container provided with hydrogen plasma radio frequency equipment, reducing and deoxidizing the decarburized chromium powder by using hydrogen as reducing gas, arranging a cooling device in the container, sampling and detecting the decarburized chromium powder, wherein detection items comprise carbon content, oxygen content, color and luster and chemical components, and qualified detected chromium powder, performing bag-dividing vacuum packaging, and then entering a storage link;
nano Al2O3And ZrO2The preparation method of the high-toughness ceramic block prepared by mixing comprises the following steps:
s2-1: mixing nano Al2O3Powder and ZrO2Mixing the powder according to the weight ratio of 1:1, and uniformly mixing in an electromagnetic stirring device to obtain a mixed additive;
s2-2: breaking the porcelain stone to 1cm3Grinding the materials in a grinding device to obtain grinding powder, elutriating the grinding powder, removing impurities, adding the mixed additive obtained in S2-1, wherein the weight ratio of the mixed additive to the grinding powder is 1:20, stirring elutriation liquid, uniformly stirring, precipitating for 24 hours, and filtering precipitate liquid to obtain soft mud blocks;
s2-3: and drying the soft mud blocks to obtain hard mud blocks, cutting the hard mud blocks into a specified size, and firing to obtain the finished high-toughness ceramic blocks.
Example 3:
a method for preparing metal chromium powder by ultra-low temperature grinding comprises the following steps:
s1: crushing
Selecting original chromium blocks, then putting the selected chromium blocks into liquid nitrogen for freezing for 1h, crushing the frozen metal chromium blocks by a crusher, filtering the crushed chromium particles by a screen, wherein the size of the aperture of the screen is 10mm, secondarily crushing the particles left on the screen, and refrigerating the particles passing through the screen;
s2: ultra-low temperature grinding
Placing the refrigerated particles into a grinder, adding grinding medium, introducing protective medium liquid nitrogen, controlling the grinding temperature at 0 deg.C, and performing thin film seed bearing at a flow rate of 10 m/h during grindingThe length of the grinding process is 5 hours, the power of a grinding machine is firstly adjusted to the ball milling revolution number of 100r/min during grinding, the grinding process lasts for 1 hour, then the ball milling revolution number is adjusted to 500r/min, the grinding process is continued to be ground into powder, a grinding medium in the grinding machine is tungsten steel, a lining is made of zirconia, liquid nitrogen is used as temperature control gas during the grinding process, helium is introduced as protective gas, the gas flow is 25m year/h, the ball material ratio is 10:1, the powder obtained after grinding is collected and elutriated by adopting gasoline, the liquid level of the gasoline is higher than that of chromium powder, and nano Al is added during elutriation2O3And ZrO2Mixing the prepared high-toughness ceramic blocks, wherein the particle diameter of each high-toughness ceramic block is 1cm, fishing the ceramic blocks by using a screen after elutriation is finished, filtering out chromium powder by using filter cloth, standing the elutriated gasoline for 18 hours, taking a hose, introducing a supernatant onto industrial anti-static filter cloth by using a siphon principle, collecting a filtrate below the filter cloth by using a barrel, recycling the gasoline after repeating the filtrate for three times, adding a magnet into the chromium powder during elutriation, elutriating by using an electromagnetic stirring mode, and cleaning iron powder on the magnet after elutriation is finished;
s3: drying by baking
Putting the chromium powder obtained in the step S2 into a drying device, drying at 100 ℃ for 0.8h, stirring at the stirring speed of 20r/min during drying, recovering evaporated gasoline during drying, recycling, vacuumizing the drying device at the vacuum degree of 7Pa, and airing at the low temperature of 5 ℃ for 30min after drying;
s4: sieving
Classifying and screening the clean chromium powder obtained in the step S3, performing multi-stage screening according to the particle size of the chromium powder, performing intermediate-stage screening to obtain low-grade powder and high-grade powder, subdividing the high-grade chromium powder and the low-grade chromium powder simultaneously, collecting substandard powder in the low-grade powder, repeating the steps S2-S4, introducing the obtained chromium powder into a microwave heating furnace for decarburization treatment at the heating temperature of 550 ℃ for 30min, cooling to room temperature after heating is completed, separating graphite particles to obtain decarburized chromium powder, introducing the decarburized chromium powder into a ceramic container provided with hydrogen plasma radio frequency equipment, reducing and deoxidizing the decarburized chromium powder by using hydrogen as reducing gas, arranging a cooling device in the container, sampling and detecting the decarburized chromium powder, wherein detection items comprise carbon content, oxygen content, color and luster and chemical components, and qualified detected chromium powder, performing bag-dividing vacuum packaging, and then entering a storage link;
nano Al2O3And ZrO2The preparation method of the high-toughness ceramic block prepared by mixing comprises the following steps:
s2-1: mixing nano Al2O3Powder and ZrO2Mixing the powder according to the weight ratio of 1:1, and uniformly mixing in an electromagnetic stirring device to obtain a mixed additive;
s2-2: breaking the porcelain stone to 1-2cm3Grinding the materials in a grinding device to obtain grinding powder, elutriating the grinding powder, removing impurities, adding the mixed additive obtained in S2-1, wherein the weight ratio of the mixed additive to the grinding powder is 1:20, stirring elutriation liquid, uniformly stirring, precipitating for 24 hours, and filtering precipitate liquid to obtain soft mud blocks;
s2-3: and drying the soft mud blocks to obtain hard mud blocks, cutting the hard mud blocks into a specified size, and firing to obtain the finished high-toughness ceramic blocks.
The chromium powder produced in the three examples was tested using the chromium blocks used in the three examples as the same batch of chromium blocks, and the test results are shown in table 1:
TABLE 1 impurity content of chromium powder produced in three examples
Examples Carbon content Oxygen content Iron content
Example 1 0.008% 0.01% 0.02%
Example 2 0.005% 0.008% 0.025%
Example 3 0.003% 0.005% 0.01%
As can be seen from the data in Table 1, the content of impurity elements in the chromium metal powder prepared by the method of the present invention is low, and the comparison of the above experimental data shows that example 2 is the best scheme.

Claims (9)

1. A method for preparing metal chromium powder by ultra-low temperature grinding is characterized by comprising the following steps:
s1: crushing
Selecting original chromium blocks, then putting the selected chromium blocks into liquid nitrogen for freezing for 0.5-1h, crushing the frozen metal chromium blocks by a crusher, filtering the crushed chromium particles by a screen, wherein the aperture of the screen is 10mm, secondarily crushing the particles left on the screen, and refrigerating the particles passing through the screen;
s2: ultra-low temperature grinding
Placing the refrigerated particles into a grinder, adding grinding medium, introducing protective medium liquid nitrogen, controlling the grinding temperature at-150-0 deg.C, controlling the flow rate of liquid nitrogen at 5-10 m/h, grinding for 2-5h, collecting the powder, elutriating with gasoline, wherein the liquid level of gasoline is higher than that of chromium powder, and adding nano Al during elutriation2O3And ZrO2Mixing to obtain high-toughness ceramic blocks, wherein the particle diameter of the high-toughness ceramic blocks is 0.5-1cm, fishing the ceramic blocks by using a screen after the elutriation is finished, and then filtering out chromium powder by using filter cloth;
s3: drying by baking
Putting the chromium powder obtained in the step S2 into a drying device, drying at 60-100 ℃ for 0.5-0.8h, stirring at the stirring speed of 10-20r/min during drying, recovering evaporated gasoline during drying, reusing, vacuumizing the drying device at the vacuum degree of 6-7Pa, and airing at low temperature for 20-30min after drying;
s4: sieving
And (3) grading and screening the clean chromium powder obtained in the step (S3), carrying out multi-stage screening according to the particle size of the chromium powder, carrying out middle-stage screening to obtain low-grade powder and high-grade powder, simultaneously subdividing the high-grade chromium powder and the low-grade chromium powder, collecting powder which does not reach the standard in the low-grade powder, and repeating the steps (S2) -S4).
2. The method for preparing chromium metal powder through ultra-low temperature grinding as claimed in claim 1, wherein in the step S2, the power of the grinder is firstly adjusted to 100r/min for 1h, and then the grinding is continued to be powdered after the grinding ball rotation number is adjusted to 500 r/min.
3. The method for preparing chromium metal powder through ultra-low temperature grinding as claimed in claim 1, wherein the gasoline washed in step S2 is firstly stood for 12-18h, the supernatant is introduced into an industrial antistatic filter cloth by using a hose and using a siphon principle, the filtrate is collected by a barrel below the filter cloth, and after the process is repeated three times, the gasoline is recycled.
4. The method for preparing metallic chromium powder through ultra-low temperature grinding as claimed in claim 1, wherein the chromium powder obtained in S4 is subjected to decarburization treatment in a microwave oven at a temperature of 450-610 ℃ for 30min, and after completion of heating, it is cooled to room temperature, and graphite particles are separated to obtain decarburized chromium powder.
5. The method for preparing metallic chromium powder through ultra-low temperature grinding as claimed in claim 4, wherein the decarburized chromium powder is introduced into a ceramic container equipped with a hydrogen plasma radio frequency device, and the decarburized chromium powder is deoxidized by reduction using hydrogen as a reducing gas, and a cooling device is installed in the container.
6. The method of claim 1, wherein in step S2, the grinding medium in the grinding machine is tungsten steel, the lining is zirconia, liquid nitrogen is used as temperature-controlled gas during grinding, helium is introduced as protective gas, the gas flow is 10-25m top-dressing/h, and the ball-to-material ratio is 10: 1.
7. The method for preparing metallic chromium powder through ultra-low temperature grinding as claimed in claim 5, wherein the chromium powder after deoxidation is sampled and tested, the test items include carbon content, oxygen content, color and chemical composition, and the qualified chromium powder is packaged in bags in vacuum and then enters the storage link.
8. The method for preparing metallic chromium powder through ultra-low temperature grinding as claimed in claim 1, wherein the magnet is added into the chromium powder during elutriation in step S2, the elutriation is performed by means of electromagnetic stirring, and the iron powder on the magnet is cleaned after the elutriation is completed.
9. The method for preparing metallic chromium powder by ultra-low temperature grinding as claimed in claim 1, wherein said nano Al is2O3And ZrO2The preparation method of the high-toughness ceramic block prepared by mixing comprises the following steps:
s2-1: mixing nano Al2O3Powder and ZrO2Mixing the powder according to the weight ratio of 1:1, and uniformly mixing in an electromagnetic stirring device to obtain a mixed additive;
s2-2: breaking the porcelain stone to 1-2cm3Size in the grinding deviceGrinding the materials to obtain grinding powder, elutriating the grinding powder, removing impurities, adding the mixed additive obtained in S2-1, wherein the weight ratio of the mixed additive to the grinding powder is 1:20, stirring the elutriation liquid, uniformly stirring, precipitating for 24 hours, and filtering the precipitation liquid to obtain soft mud blocks;
s2-3: and drying the soft mud blocks to obtain hard mud blocks, cutting the hard mud blocks into a specified size, and firing to obtain the finished high-toughness ceramic blocks.
CN202011250219.9A 2020-11-11 2020-11-11 Method for preparing metal chromium powder by ultralow temperature grinding Active CN112091224B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011250219.9A CN112091224B (en) 2020-11-11 2020-11-11 Method for preparing metal chromium powder by ultralow temperature grinding

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011250219.9A CN112091224B (en) 2020-11-11 2020-11-11 Method for preparing metal chromium powder by ultralow temperature grinding

Publications (2)

Publication Number Publication Date
CN112091224A true CN112091224A (en) 2020-12-18
CN112091224B CN112091224B (en) 2021-02-09

Family

ID=73785116

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011250219.9A Active CN112091224B (en) 2020-11-11 2020-11-11 Method for preparing metal chromium powder by ultralow temperature grinding

Country Status (1)

Country Link
CN (1) CN112091224B (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112719275A (en) * 2021-04-06 2021-04-30 西安斯瑞先进铜合金科技有限公司 Method for preparing titanium-silicon metal powder by low-temperature grinding
CN112846199A (en) * 2021-01-08 2021-05-28 新乡医学院 Method for preparing ultrathin bismuth-alkene nanosheets by heating, freezing, grinding and ultrasonic
CN112974810A (en) * 2021-05-07 2021-06-18 陕西斯瑞新材料股份有限公司 Preparation method of high-performance copper-chromium alloy contact
CN114012100A (en) * 2021-11-09 2022-02-08 宁波新睦科技有限公司 Raw material powder preparation process for powder metallurgy
CN115194165A (en) * 2022-09-14 2022-10-18 四川泽丰锂能新能源科技有限公司 Low-temperature brittle metal powder grinding device
CN116571753A (en) * 2023-07-13 2023-08-11 长春黄金研究院有限公司 Preparation method of flaky metal powder

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1031400A (en) * 1987-08-05 1989-03-01 北京有色金属研究总院 The production method of hypoxemia chromium powder
JPH05263179A (en) * 1992-03-17 1993-10-12 Kubota Corp Chromium base heat resistant sintered alloy and its manufacture
CN104070172A (en) * 2014-06-23 2014-10-01 陕西斯瑞工业有限责任公司 Method for preparing spherical chromium powder
CN104070171A (en) * 2014-06-12 2014-10-01 陕西斯瑞工业有限责任公司 Preparation method for superfine chromium powder
CN104099478A (en) * 2014-07-28 2014-10-15 李平 Method for recycling and preparing metal chromium
CN104550903A (en) * 2014-12-11 2015-04-29 陕西斯瑞工业有限责任公司 Hydrogen plasma deoxidation method for chromium powder
CN110202159A (en) * 2019-06-21 2019-09-06 西安斯瑞先进铜合金科技有限公司 A kind of preparation method of high-performance CuCr electrical contact special-purpose metal chromium powder
CN111531164A (en) * 2020-04-15 2020-08-14 河南中钻新材料有限公司 Method for reducing oxygen and nitrogen contents in chromium powder particles at low cost

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1031400A (en) * 1987-08-05 1989-03-01 北京有色金属研究总院 The production method of hypoxemia chromium powder
JPH05263179A (en) * 1992-03-17 1993-10-12 Kubota Corp Chromium base heat resistant sintered alloy and its manufacture
CN104070171A (en) * 2014-06-12 2014-10-01 陕西斯瑞工业有限责任公司 Preparation method for superfine chromium powder
CN104070172A (en) * 2014-06-23 2014-10-01 陕西斯瑞工业有限责任公司 Method for preparing spherical chromium powder
CN104099478A (en) * 2014-07-28 2014-10-15 李平 Method for recycling and preparing metal chromium
CN104550903A (en) * 2014-12-11 2015-04-29 陕西斯瑞工业有限责任公司 Hydrogen plasma deoxidation method for chromium powder
CN110202159A (en) * 2019-06-21 2019-09-06 西安斯瑞先进铜合金科技有限公司 A kind of preparation method of high-performance CuCr electrical contact special-purpose metal chromium powder
CN111531164A (en) * 2020-04-15 2020-08-14 河南中钻新材料有限公司 Method for reducing oxygen and nitrogen contents in chromium powder particles at low cost

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112846199A (en) * 2021-01-08 2021-05-28 新乡医学院 Method for preparing ultrathin bismuth-alkene nanosheets by heating, freezing, grinding and ultrasonic
CN112719275A (en) * 2021-04-06 2021-04-30 西安斯瑞先进铜合金科技有限公司 Method for preparing titanium-silicon metal powder by low-temperature grinding
CN112719275B (en) * 2021-04-06 2021-07-16 西安斯瑞先进铜合金科技有限公司 Method for preparing titanium-silicon metal powder by low-temperature grinding
CN112974810A (en) * 2021-05-07 2021-06-18 陕西斯瑞新材料股份有限公司 Preparation method of high-performance copper-chromium alloy contact
CN114012100A (en) * 2021-11-09 2022-02-08 宁波新睦科技有限公司 Raw material powder preparation process for powder metallurgy
CN115194165A (en) * 2022-09-14 2022-10-18 四川泽丰锂能新能源科技有限公司 Low-temperature brittle metal powder grinding device
CN116571753A (en) * 2023-07-13 2023-08-11 长春黄金研究院有限公司 Preparation method of flaky metal powder
CN116571753B (en) * 2023-07-13 2023-10-20 长春黄金研究院有限公司 Preparation method of flaky metal powder

Also Published As

Publication number Publication date
CN112091224B (en) 2021-02-09

Similar Documents

Publication Publication Date Title
CN112091224B (en) Method for preparing metal chromium powder by ultralow temperature grinding
KR102490248B1 (en) Powder metallurgy sputtering target and its production method
He et al. Synthesis of nanostructured WC-12 pct Co coating using mechanical milling and high velocity oxygen fuel thermal spraying
CN109108273B (en) Preparation method of NbZrTiTa refractory high-entropy alloy powder and NbZrTiTa refractory high-entropy alloy powder
Wang et al. The preparation and the properties of microcrystalline and nanocrystalline CuCr contact materials
WO2019024421A1 (en) Method for preparing target material and target material
CN109868405B (en) High-entropy alloy CoCrFeMnNi and atomization powder preparation method thereof
CN111910160B (en) Preparation method of aluminum-scandium target material
CN110428947B (en) Rare earth permanent magnetic material and raw material composition, preparation method and application thereof
KR20090049590A (en) Metal alloy powders production
TW201533248A (en) High-purity tantalum powder and preparation method therefor
CN111621650B (en) Method for extracting metallic nickel from laterite-nickel ore
CN113528925A (en) High-entropy alloy high-powder-yield mechanical alloying and sintering forming method
CN109837441B (en) Novel tungsten nickel cobalt material and preparation method thereof
CN114367669B (en) Preparation method of TaW10 alloy spherical powder for 3D printing
US2892697A (en) Method of producing powdered titanium and titanium alloys
CN113496817B (en) Mass production method of nanocrystalline composite permanent magnet powder containing SmCo
CN113308688A (en) Nano bulk crystal metal material and preparation method thereof
US2368489A (en) Production of metal powder
US3238039A (en) Process for separating non-molten slag from nickel chromium-containing iron ores
Kim et al. Heat treatment effect on the behavior of oxide particles in mechanically alloyed oxide dispersion strengthened powders
CN114959412B (en) Method for improving structure and performance of additive manufacturing alloy steel
CN114309627B (en) Preparation method of low-oxygen-content refractory high-entropy alloy powder
CN111906295B (en) Spherical hard alloy powder and preparation method thereof
CN114042921B (en) Chromium-silicon alloy powder and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant