CN102161098A - Method for preparing low-oxygen content superfine pre-alloyed powder through ultrahigh pressure water and gas combined atomization - Google Patents
Method for preparing low-oxygen content superfine pre-alloyed powder through ultrahigh pressure water and gas combined atomization Download PDFInfo
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Abstract
The invention relates to a method for preparing low-oxygen content superfine pre-alloyed powder through ultrahigh pressure water and gas combined atomization. The method comprises the following process flows of: pre-alloy smelting, ultrahigh pressure water and gas combined atomization, quick solidification, cooling, corrosion inhibition treatment on powder, collection, drying, performance detection, finished product package and the like. The method has the advantages that: the product is low in oxygen content, small in particle size, controllable in particle shape and uniform in components; the components have no segregation; power elements are pre-alloyed; and the equipment and process in a production process are simple and are convenient to operate.
Description
Technical field
The present invention relates to the preparing technical field of metal powder material, specifically a kind of super-pressure aqueous vapor combination atomizing prepares the method for the fine pre-alloyed powder of low oxygen content.
Background technology
Begin to have produced since the atomized iron powder during World War II, the powder by atomization technology has obtained development rapidly, becomes one of most important method of present preparation powder.Atomization can be produced elemental metals powder such as lead, tin, aluminium, zinc, copper, nickel, cobalt, also can produce pre-alloyed powders such as bronze, brass, steel alloy, stainless steel.Compare with electrolysis, reducing process, mechanical crushing mixing method, atomization has guaranteed the pre-alloyed fully of metallic element because of fusion process, eliminated the composition segregation, added that the composition prescription is easy to adjust, so atomization is the most effective production method of preparation pre-alloyed powder.Most of elemental metals that uses in the modern powder metallurgy industry and pre-alloyed powder all are to adopt atomization technique to produce.According to the difference of atomizing medium, atomization can be divided into aerosolization method and water atomization.
Although existing conventional aerosolization method and water atomization are to prepare the method that metal dust extensively adopts, but still there are a lot of weak points on the metal dust quality of its preparation and the performance, be mainly reflected in the following aspects: (1) oxygen content in power height, about 2000～5000ppm; (2) average grain diameter is thick, about 50～100 μ m; (3) powder morphology is restive, the main attitude spherical in shape of powder morphology that the aerosolization method is produced, and the powder morphology of water atomization preparation is irregular attitude, and a cover atomization plant is difficult to carry out according to user's requirement the adjustment of product particle pattern; (4) the secondary oxidation pollution takes place in Zhi Bei powder easily in storage, use, greatly reduces the serviceability of powder.
Along with the continuous development of modern science and technology and new material, more and more harsher to the requirement of aspects such as the kind of dusty material, performance, cost, the preparation of metal dust towards high-purity, fine, composition and pattern is controlled and cheaply direction develop.Closely during the last ten years, powder metallurgy new technology fast developments such as metal injection moulding, thermal spraying, metal are shaped fast, surface mount, the powder metallurgy industry has proposed higher and stricter requirement to the metal dust raw material, be badly in need of that oxygen content is low, granularity is fine, uniform ingredients segregation-free, controlled high-performance elemental metals and the prealloy powder powder stock of granule-morphology, the metal of existing conventional atomization process and the preparation of other processes and pre-alloyed powder more and more are difficult to adapt to the needs of modern powder metallurgy industry development.
Summary of the invention
Problem at above-mentioned existence, the objective of the invention is to overcome above shortcoming, provide a kind of super-pressure aqueous vapor combination atomizing to prepare the method for the fine pre-alloyed powder of low oxygen content, its technology path is advanced reliable, process equipment is simple, and continuity is strong, and production cost is low, good product performance is suitable for suitability for industrialized production and can be widely used in the powder metallurgy industry.
For achieving the above object, the present invention takes following design:
Super-pressure aqueous vapor combination atomization prepares the basic principle of the fine pre-alloyed powder method of low oxygen content: impact melt metal or alloy melt by the ultra-high pressure water fluid jet medium fluid that water atomization power set and atomizer eject, overcome the bonding force between the melt metallic atom, make the kinetic energy of adjusting medium fluid be converted into metal bath increase total surface area the surface can, and realize the metal or alloy melt cracked be the process of powder.The ultra-high pressure water fluid jet medium fluid is different from the conical jet of traditional water atomizing in this law, and it does not concentrate on the geometrical focus of nozzle, but forms the cavity near focus, and forms the jet that circles round symmetrically after gathering into necking down.The pressure of conventional water atomization water jet is: 8～20MPa, the atomization process cooldown rate is: 102～104K/s, the pressure of super-pressure aqueous vapor combination atomized water jet is: 70～150MPa, the atomization process cooldown rate is: the liquid metal fluid that the ultra-high pressure water fluid jet that 104～106K/s produces by atomizer will flow out fistulae is ground into the drop of fine metal, and by convection type heat radiation and rapidly cooled and solidified becomes low oxygen content, granularity is fine, the metal dust that pattern is controlled, the water jet medium of super-pressure is the power source that metal liquid stream is smashed, it simultaneously is again the cooling agent of preparation metal dust, the powder of preparation adopts the TZYJ corrosion inhibiter after further inhibition is handled, powder surface forms the fine and close continuously hydrophobic film of one deck, can prevent that powder from storing, the secondary oxidation in the use pollutes.The process flow formula of the fine pre-alloyed powder of super-pressure aqueous vapor combination atomizing preparation low oxygen content is seen Fig. 1.
A kind of super-pressure aqueous vapor combination atomizing prepares the method for the fine pre-alloyed powder of low oxygen content, it is characterized in that having following technical process:
(1) fusion process adds the inertia protective medium to prevent the oxidation of alloy at melting process, and the degree of superheat of metal bath is: 80～150 ℃.
(2) atomization process hydraulic pressure is: 70～150MPa, discharge to the ratio of metal flow is: 2: 1～7: 1, the atomizing cooldown rate is: 104～106K/s, the angular range that circles round of water jet medium was: 0.2～0.70rad.
(3) the atomizing bucket adopts double-layer stainless steel water jacket cooling structure, adopts recirculated water cooling staving.
(4) the nodularization time and the setting time of control pre-alloyed powder reach the purpose for preparing the different-shape pre-alloyed powder.When nodularization time during greater than setting time, metal drop has little time balling-up and has just solidified, and powder particle is irregular form; When nodularization time during less than setting time, metal drop has sufficient time nodularization, powder particle attitude spherical in shape before solidifying; When nodularization time and setting time near the time, powder particle is the spherical attitude of class.
(5) powder of atomizing preparation is that powder surface formed the fine and close continuously hydrophobic film of one deck, can prevent the secondary oxidation pollution of powder in deposit and use after drying was handled in about 0.4% TZYJ corrosion inhibitor solution inhibition through concentration.
The present invention has the following advantages:
(1) the obvious refinement of powder size.Because degree of supercooling is big before the forming core, has improved nucleation rate greatly, nucleus is solidifying not as good as fully growing up, so the average grain diameter of powder is fine, only is 10～20 μ m, and the powder average grain diameter that conventional atomizing is produced is 50～100 μ m.
(2) uniform ingredients can be eliminated powder composition segregation phenomena.Under chilling and rapid solidification condition, alloying element has little time enrichment and solidifies rapidly, has eliminated the composition segregation phenomena, has significantly improved the functioning efficiency of alloying element.
(3) oxygen content of powder reduces greatly.Adopt super-pressure aqueous vapor combination atomization powder-making technique, because chilling and the rapid solidification of powder in atomization process, powder is crystallite and amorphous state, greatly reduces the oxidation of powder in atomization process.The oxygen content of conventional atomized powder is 2000～5000ppm, adopts the oxygen content in power of super-pressure aqueous vapor combination atomization powder-making technique preparation to be lower than 800ppm.
(4) degree of supersaturation of powder metallurgy element and solid solubility obviously improve.Because the setting rate that super-pressure aqueous vapor combination atomization process chilling causes is much larger than equilibrium freezing speed, so alloy powder has little time in process of setting according to equilbrium phase diagram by diffuseing to form second phase or generating other equilibrium phases, thereby degree of supersaturation and the solid solubility of alloying element in solid solution is greatly improved, so the quick cooling alloy powder has good solid solution strengthening effect.
(5) the powder particle pattern is controlled.By regulating technological parameters such as atomizing nozzle structure form, melt overheat degree and melt-flow diameter, the particles of powder pattern can be chosen as spherical attitude, the spherical attitude of class or irregular form according to customer requirements.
Description of drawings
Fig. 1 is the process chart of the fine pre-alloyed powder of super-pressure aqueous vapor combination atomizing preparation low oxygen content
Fig. 2 is the spherical attitude pre-alloyed powder SEM shape appearance figure of super-pressure aqueous vapor combination atomizing preparation
Fig. 3 is the irregular form pre-alloyed powder SEM shape appearance figure of super-pressure aqueous vapor combination atomizing preparation.
The specific embodiment
Embodiment 1:
Percentage meter by weight, the batching composition is Cr:19%, Ni:10%, Mn:1.5%, Si:0.8%, Fe: surplus.The weighing double centner joins in the intermediate frequency (IF) smelting stove and heats up, and treats alloy raw material fusing and overheated 150 ℃.Pour motlten metal into the bottom pour ladle crucible, when molten metal bath leaks eye and flow path atomizer by the pottery at the bottom of the bottom pour ladle, control jet hydraulic pressure is: 110～120MPa, discharge to the metal flow ratio is: 5.0～5.2, the process cooldown rate is: 104～105K/s, the angular range that circles round of water jet is: 0.60～0.65rad, and the super-pressure current that liquid metal is come out by nozzle ejection smash into droplet, and the prealloy drop is frozen into powder in atomizing collecting vessel water subsequently.Through concentration is after 0.4% TZYJ corrosion inhibiter inhibition is handled, and powder is dry under 80～120 ℃ of temperature, analyze after testing qualified after, vacuum packaging is the finished product powder.The pre-alloyed powder that makes, oxygen content is low, and the powder meso-position radius is about 15 μ m, even particle size distribution, scope is narrower, granule-morphology attitude (see figure 2) spherical in shape.Products obtained therefrom can be used as powder injection forming stainless steel pre-alloyed powder.
Embodiment 2:
Percentage meter by weight, the batching composition is Cu:30%, Fe:15%, Co:35%, Sn:10%, Zn%.The weighing double centner joins in the intermediate frequency (IF) smelting stove and heats up, and treats alloy raw material fusing and overheated 80～100 ℃.Pour motlten metal into the bottom pour ladle crucible, when molten metal bath leaks eye and flow path atomizer by the pottery at the bottom of the bottom pour ladle, control jet hydraulic pressure is: 100～105MPa, discharge to the metal flow ratio is: 5.4～5.5, the process cooldown rate is: 104～106K/s, the angular range that circles round of water jet is: 0.40～0.45rad, and the super-pressure current that liquid metal is come out by nozzle ejection smash into droplet, and the prealloy drop is frozen into powder in atomizing collecting vessel water subsequently.Through concentration is after 0.4% TZYJ corrosion inhibiter inhibition is handled, and powder is dry under 80～120 ℃ of temperature, analyze after testing qualified after, vacuum packaging is the finished product powder.The pre-alloyed powder that makes, oxygen content is low, and the powder meso-position radius is about 14 μ m, even particle size distribution, scope is narrower, and particle is irregular form (see figure 3).Products obtained therefrom can be used as artificial diamond's stone manufacture carcass pre-alloyed powder.
Claims (6)
1. a super-pressure aqueous vapor combination atomizes and prepares the method for the fine pre-alloyed powder of low oxygen content, and it is characterized in that: may further comprise the steps: (1) is melt into liquid metals with the intermediate frequency (IF) smelting stove with raw metal in the inertia protective medium; (2) molten metal liquid is poured into the bottom pour ladle crucible, when the leakage eye at the bottom of molten metal liquid is by bottom pour ladle was flowed through atomizer, the injected super-pressure current that come out smashed into droplet; (3) molten drop in atomizing bucket in the dropping process rapid solidification be cooled to powdered form, fall into atomizing bucket bottom water and also further be cooled to normal temperature; (4) the powder employing TZYJ corrosion inhibiter with cooling carries out the inhibition processing, makes the surface of powder form the fine and close continuously hydrophobic film of one deck, prevents that powder from producing secondary oxidation in storage and use; (5) with the powder for drying processing and after testing, the vacuum-packed storage.
2. super-pressure aqueous vapor combination atomizing according to claim 1 prepares the method for the fine pre-alloyed powder of low oxygen content; it is characterized in that: fusion process adds the inertia protective medium; prevent the oxidation of alloy at fusion process, the degree of superheat of metal liquid is: 80～150 ℃.
3. super-pressure aqueous vapor combination atomizing according to claim 1 prepares the method for the fine pre-alloyed powder of low oxygen content, it is characterized in that: atomization process hydraulic pressure remains on: 70～120MPa, discharge to the ratio of metal flow is: 2: 1～7: 1, the atomizing cooldown rate is: 104～106K/s, the angular range that circles round of water jet is: 0.2～0.70rad.
4. make up the method that atomizing prepares the fine pre-alloyed powder of low oxygen content according to right 1 described super-pressure aqueous vapor, it is characterized in that: the atomizing bucket adopts a double-layer stainless steel water jacket cooling structure, employing recirculated water cooling staving.
5. make up the method that atomizing prepares the fine pre-alloyed powder of low oxygen content according to right 1 described super-pressure aqueous vapor, it is characterized in that: the nodularization time and the setting time of control pre-alloyed powder reach the purpose for preparing the different-shape pre-alloyed powder;
When nodularization time during greater than setting time, metal drop has little time balling-up and has just solidified, and it is irregular that powder particle is; When nodularization time during less than setting time, metal drop has sufficient time nodularization, powder particle attitude spherical in shape before solidifying; When nodularization time and setting time near the time, powder particle is the spherical attitude of class.
6. the method for preparing the fine pre-alloyed powder of low oxygen content according to right 1 described super-pressure aqueous vapor combination atomization, it is characterized in that: the powder of atomizing preparation, through concentration is after drying is handled in about 0.4% TZYJ buffer agent solution inhibition, powder surface forms the fine and close continuously hydrophobic film of one deck, can prevent that the secondary oxidation of powder in deposit and use from polluting.
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| CN103056374A (en) * | 2011-10-22 | 2013-04-24 | 湖南省冶金材料研究所 | Method for preparing prealloy powder for low-oxygen-content micro-diamond product and using ultrahigh-pressure water atomization |
| CN103111626A (en) * | 2013-02-26 | 2013-05-22 | 连云港倍特超微粉有限公司 | Miniature alloy steel shot preparation method |
| CN103111625A (en) * | 2013-03-19 | 2013-05-22 | 南京理工大学 | Method of improving sphericity degree of metal powder prepared through water atomization |
| CN103752822A (en) * | 2014-02-20 | 2014-04-30 | 西华大学 | Composite powder and preparing method thereof |
| CN104596244A (en) * | 2015-02-02 | 2015-05-06 | 苏州化联高新陶瓷材料有限公司 | Resistance furnace for continuously melting gas-atomized ceramic material and production application method thereof |
| CN105108166A (en) * | 2015-09-29 | 2015-12-02 | 四川有色金源粉冶材料有限公司 | Method for preparing iron-base alloy powder used for injection molding |
| CN106001590A (en) * | 2016-07-24 | 2016-10-12 | 刘志强 | Iron-based intermetallic compound prealloy atomized powder new material |
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| CN103056374A (en) * | 2011-10-22 | 2013-04-24 | 湖南省冶金材料研究所 | Method for preparing prealloy powder for low-oxygen-content micro-diamond product and using ultrahigh-pressure water atomization |
| CN103111626A (en) * | 2013-02-26 | 2013-05-22 | 连云港倍特超微粉有限公司 | Miniature alloy steel shot preparation method |
| CN103111625A (en) * | 2013-03-19 | 2013-05-22 | 南京理工大学 | Method of improving sphericity degree of metal powder prepared through water atomization |
| CN103752822B (en) * | 2014-02-20 | 2016-11-02 | 西华大学 | A kind of composite granule and preparation method thereof |
| CN103752822A (en) * | 2014-02-20 | 2014-04-30 | 西华大学 | Composite powder and preparing method thereof |
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| CN104596244A (en) * | 2015-02-02 | 2015-05-06 | 苏州化联高新陶瓷材料有限公司 | Resistance furnace for continuously melting gas-atomized ceramic material and production application method thereof |
| CN105108166A (en) * | 2015-09-29 | 2015-12-02 | 四川有色金源粉冶材料有限公司 | Method for preparing iron-base alloy powder used for injection molding |
| CN106001590A (en) * | 2016-07-24 | 2016-10-12 | 刘志强 | Iron-based intermetallic compound prealloy atomized powder new material |
| JP2019011483A (en) * | 2017-06-29 | 2019-01-24 | 福田金属箔粉工業株式会社 | Copper-based alloy powder for powder metallurgy and sintered body formed of copper-based alloy powder |
| CN107876786A (en) * | 2017-10-27 | 2018-04-06 | 湖南博锋新材料有限公司 | A kind of method of oxidization of metal powder in reduction water atomization pulverization |
| CN110653377A (en) * | 2019-10-18 | 2020-01-07 | 郑州机械研究所有限公司 | Gas-water coupling preparation method of metastable silicon brass particles |
| CN112430763A (en) * | 2020-10-29 | 2021-03-02 | 桂林金格电工电子材料科技有限公司 | Al (aluminum)2O3Preparation method of dispersion-strengthened copper-based composite material |
| CN112430763B (en) * | 2020-10-29 | 2021-09-21 | 桂林金格电工电子材料科技有限公司 | Al (aluminum)2O3Preparation method of dispersion-strengthened copper-based composite material |
| CN112676562A (en) * | 2020-12-17 | 2021-04-20 | 安徽奥微新材料有限公司 | Preparation method of high-performance metal prefabricated powder added with rare earth |
| CN113500198A (en) * | 2021-07-08 | 2021-10-15 | 河南黄河旋风股份有限公司 | Preparation method of high-zinc alloy powder |
| CN114558337A (en) * | 2022-03-15 | 2022-05-31 | 广东长信精密设备有限公司 | Metal atomization powder process production facility |
| CN114558337B (en) * | 2022-03-15 | 2023-12-01 | 广东长信精密设备有限公司 | Metal atomizing powder process production facility |
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Application publication date: 20110824 |