CN103785843B - The preparation method of the spherical agglomerated powder of a kind of super fine titanium carbonitride based ceramic metal - Google Patents
The preparation method of the spherical agglomerated powder of a kind of super fine titanium carbonitride based ceramic metal Download PDFInfo
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Abstract
The invention discloses the preparation method of the spherical agglomerated powder of a kind of super fine titanium carbonitride based ceramic metal, taking paraffin as powder adhesive, alcohol is solvent medium, adopt spray granulation to process super fine titanium carbonitride based ceramic metal powder and form reunion powder, this reunion powder has even particle size distribution and is spherical, the feature of mobile performance excellence, and it is simple that this preparation method has technique, production efficiency is high, is applicable to the features such as mass production.
Description
Technical field
The present invention relates to metal ceramic powder processability and improve field, especially relate to a kind of the super of high fluidity that haveThe preparation method of the spherical agglomerated powder of thin titanium carbonitride (Ti (C, N)) based ceramic metal.
Background technology
Titanium carbonitride (Ti (C, N)) base metal-ceramic material is widely used in machinery because having good combination propertyCutter material in processing. In recent years, Ti (C, N) based ceramic metal is sent out to crystalline grains ultra and a nanometer trend that material strengthensExhibition, ultra-fine or nano level powder stock is the basis of preparing ultra-fine crystal particle cermet material. Adopt at present suitable ball millingProcess can be prepared high-quality superfine powder, and superfine powder is because particle diameter is little, specific area is large, and surface can be high, very easily sends outRaw agglomeration, makes powder flowbility poor, is difficult for filling mould, and in pressing process, dress powder speed is slow, and easily produces " archBridge effect ", cause pressed compact size or density not to be inconsistent requirement, even occur affecting product quality by cracking phenomena. How to improve ultra-fineThe mobility of Ti (C, N) based ceramic metal powder, improves compressing performance, becomes Investigation for Super-fine Cermets material and realizes raw in batchesProduce problem demanding prompt solution.
The mobile performance that improves superfines mainly adopts prilling to realize, and adopts certain method by fine powder groupBe polymerized to thicker powder particle, reunion powder particle diameter increases, and its mobility is improved significantly. Prilling is mainly paddling processTwo kinds of granulation and mist projection granulatings, paddling process granulation is undertaken by disc type or roller pelletizer, and suitable binding agent is mixed with powderAnd agitation as appropriate, produce bonding and form agglomerated particle, the method use equipment simple, output is larger, but after its granulationGrain lack of homogeneity, particle shape is irregular, and the raising of flow of powder performance is limited. Spray granulation passes through mist projection granulating equipment willPowder slurries and binding agent carry out atomization drying processing, form reunion powder, because of the agglomerated particle size distribution after its granulation equalEven and most shapes spherical in shape, have excellent mobile performance. Therefore, spray granulation becomes gradually and improves various superfine powder streamOne of effective ways of moving performance.
The disclosed spray granulation of prior art mainly contains: (Lu Youjun, Wu Laner, the red .SiC spray of Chen Yu such as Lu YoujunThe technology controlling and process [J] of mist pelletizing. Chinese powder technology, 2008 (13): 84-85) taking ethanol as solvent, phenolic resins is bondingAgent is prepared mobility high under suitable mist projection granulating parameter, spherical solid and be suitable for the SiC pelletizing of moulding. Lin ZhenhanDeng (Lin Zhenhan, Wu Liang, Lin Gang, etc. prepare the pattern research [J] of PSZ23Y powder particle by spray drying process. rare metal,2003,27 (1): 144-147). The patent application that adopts spray granulation to improve superfines aspect of performance focuses mostly at oxygenChange metal or the ceramic ultrafine powder body aspects such as zirconium, carbide and carbide alloy. Such as: Zhuan Yufeng (make by zirconic wet sprayGrain technique, publication number CN1413764A, 2003.04.30), a kind of zirconic wet spray granulating technology having been proposed, can makeFor going out Zirconia particles of uniform size, effectively reduce defect ware rate and make constant product quality. Wu Guoping be (boron carbide powderSpray drying granulation method, publication number CN102503428A, 2012.06.20) make moulding by spray drying granulation methodThe boron carbide powder that performance is good, its suitable high performance boron carbide ceramics of high-compactness of preparing. (a kind of ultra-fine hard closes Li KelinGold and its preparation method and application, publication number CN101629263A, 2010.01.20) by ultra-fine cemented carbide powder good wet-millingEnd slurry carries out mist projection granulating, to reach compressing requirement.
Be applied to the patent application situation aspect aspect cermet, Zhai Changsheng, Lu's peace, Wang Jun etc. at mist projection granulating(large granular spherical metal ceramic nano composite spraying powder, publication number CN1793048A, 2006.06.28) adopts wet method ballMill-mist projection granulating-vacuum heat treatment process is prepared the powder of 20～75 microns of spherical in shape or subsphaeroidal structure, has improvedProduct quality, but this Patent Application Publication technology is mainly used in thermal spraying industry, does not relate to cutting material field, and its granulationThe object of processing is titanium diboride based ceramic metal powder. An Nikakaopi, Wu Erfu especially Si Telun (manufacture hard closeThe method of golden or cermet agglomerated mixture of powders, publication number CN101081739A, 2007.12.05) powder slurries is sprayedPenetrate and be dried to conglomeration powder, it can be used for manufacturing cutting element and wear part etc., but this Patent Application Publication technology is mainly specialLevy and be the pressure of powder slurries, the component prescription of plastic polymer bonding agent, do not relate to technological parameter and the stream of mist projection granulatingMoving property improvement content.
Summary of the invention
The object of the invention is to overcome the deficiency of prior art, provide a kind of super fine titanium carbonitride based ceramic metal sphericalThe preparation method of reunion powder, is taking paraffin as powder adhesive, adopts spray granulation to process super fine titanium carbonitride fundBelong to ceramic powders and form reunion powder, this reunion powder has even particle size distribution and is spherical, the spy of mobile performance excellencePoint, it is simple that this preparation method has technique, and production efficiency is high, is applicable to the features such as mass production.
The technical solution adopted for the present invention to solve the technical problems is: a kind of super fine titanium carbonitride based ceramic metal is sphericalThe preparation method of reunion powder, comprises the steps:
A. add binding agent step: this step is taking paraffin as powder adhesive, by super fine titanium carbonitride based ceramic metal1～15wt.% of powder weight takes paraffin, and paraffin and super fine titanium carbonitride based ceramic metal powder are together put into ball grinderIn;
B. prepare powder slurries step: this step is taking alcohol as solvent medium, in the ratio of 5～50g/100ml to ShengHave in the ball grinder of super fine titanium carbonitride based ceramic metal powder and corresponding proportion paraffin and add spirit solvent, by ratio of grinding media to material 5:1Add carbide alloy abrading-ball, the rotating speed ball milling with 100r/min in planetary ball mill is prepared ultra-fine carbon nitrogenize after 5 hoursTitanium-based metal ceramic powders slurry;
C. mist projection granulating step: this step is to adopt high speed centrifugation Spray Grain-make Drier to super fine titanium carbonitride Base MetalCeramic powders slurry carries out mist projection granulating processing, thereby obtains the spherical agglomerated powder of super fine titanium carbonitride based ceramic metal powder;Wherein, in mist projection granulating process, inlet temperature is made as 80～300 DEG C, and outlet temperature is made as 60～200 DEG C, and atomizer rotating speed is establishedBe 5～20kr/min, charging pump rotating speed is made as 20～80r/min.
The preparation method of the spherical agglomerated powder of a kind of super fine titanium carbonitride based ceramic metal of the present invention is to adopt spraying to makeGrain technology, taking paraffin as powder adhesive, alcohol is solvent medium, its preparation technology's flow process is: super fine titanium carbonitride Base MetalCeramic powders → add binding agent → prepare powder slurries → mist projection granulating → reunion powder body material. The present invention adopts mist projection granulatingLegal system is for the spherical agglomerated powder of super fine titanium carbonitride based ceramic metal powder, by the parameter control in mist projection granulating process, and canPrepare varigrained spherical agglomerated powder.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention adopts spray granulation to prepare the spherical agglomerated powder of super fine titanium carbonitride based ceramic metal powder, by sprayParameter control in mist granulation process, can prepare varigrained spherical agglomerated powder, can obviously improve powder flowbility, aobviousWork improves the suppression performance of powder, and technique is simple, and production efficiency is high, is applicable to mass production.
Below in conjunction with drawings and Examples, the present invention is described in further detail; But the ultra-fine carbon nitrogenize of one of the present inventionThe preparation method of titanium-based metal ceramic spherical reunion powder is not limited to embodiment.
Brief description of the drawings
Fig. 1 is process chart of the present invention;
Fig. 2 is superfines shape appearance figure;
Fig. 3 is the reunion morphology microstructure figure after mist projection granulating;
Fig. 4 is the particle size distribution figure of reunion powder.
Detailed description of the invention
Embodiment mono-,
The preparation method of the spherical agglomerated powder of a kind of super fine titanium carbonitride based ceramic metal of the present invention is to adopt spraying to makeGrain technology, taking paraffin as powder adhesive, alcohol is solvent medium, its preparation technology's flow process is: super fine titanium carbonitride Base MetalCeramic powders → add binding agent → prepare powder slurries → mist projection granulating → reunion powder body material. The present invention adopts mist projection granulatingLegal system is for the spherical agglomerated powder of super fine titanium carbonitride based ceramic metal powder, by the parameter control in mist projection granulating process, and canPrepare varigrained spherical agglomerated powder.
Shown in Figure 1, the preparation method of the spherical agglomerated powder of a kind of super fine titanium carbonitride based ceramic metal of the present invention,Comprise the steps:
A. add binding agent step: this step is taking paraffin as powder adhesive, by super fine titanium carbonitride based ceramic metalThe 15wt.% of powder weight takes paraffin, and paraffin and super fine titanium carbonitride based ceramic metal powder are together put into ball grinder;Super fine titanium carbonitride based ceramic metal powder morphology as shown in Figure 2;
B. prepare powder slurries step: this step is taking alcohol as solvent medium, super to filling in the ratio of 50g/100mlIn the ball grinder of thin base titanium carbonitride powder and corresponding proportion paraffin, add spirit solvent, by ratio of grinding media to material, 5:1 addsCarbide alloy abrading-ball, the rotating speed ball milling with 100r/min in planetary ball mill is prepared super fine titanium carbonitride base after 5 hoursMetal ceramic powder slurry;
C. mist projection granulating step: this step is to adopt high speed centrifugation Spray Grain-make Drier to super fine titanium carbonitride Base MetalCeramic powders slurry carries out mist projection granulating processing, thereby obtains the spherical agglomerated powder of super fine titanium carbonitride based ceramic metal powder;Wherein, in mist projection granulating process, inlet temperature is made as 280 DEG C, and outlet temperature is made as 180 DEG C, and atomizer rotating speed is made as 20kr/Min, charging pump rotating speed is made as 70r/min;
Pattern and the granularity of the spherical agglomerated powder of super fine titanium carbonitride based ceramic metal powder of preparing by above techniqueDistribute as shown in Figure 3 and Figure 4, reunion powder good sphericity, narrow particle size distribution is and even, and its average grain diameter is 87.8 μ m, pine dressDensity is 1.43g/cm3, tap density is 1.67g/cm3。
Embodiment bis-,
Shown in Figure 1, the preparation method of the spherical agglomerated powder of a kind of super fine titanium carbonitride based ceramic metal of the present invention,Comprise the steps:
A. add binding agent step: this step is taking paraffin as powder adhesive, by super fine titanium carbonitride based ceramic metalThe 12wt.% of powder weight takes paraffin, and paraffin and super fine titanium carbonitride based ceramic metal powder are together put into ball grinder;
B. prepare powder slurries step: this step is taking alcohol as solvent medium, super to filling in the ratio of 25g/100mIn the ball grinder of thin base titanium carbonitride powder and corresponding proportion paraffin, add spirit solvent, by ratio of grinding media to material, 5:1 addsCarbide alloy abrading-ball, the rotating speed ball milling with 100r/min in planetary ball mill is prepared super fine titanium carbonitride base after 5 hoursMetal ceramic powder slurry;
C. mist projection granulating step: this step is to adopt high speed centrifugation Spray Grain-make Drier to super fine titanium carbonitride Base MetalCeramic powders slurry carries out mist projection granulating processing, thereby obtains the spherical agglomerated powder of super fine titanium carbonitride based ceramic metal powder;Wherein, in mist projection granulating process, inlet temperature is made as 200 DEG C, and outlet temperature is made as 120 DEG C, and atomizer rotating speed is made as 12kr/Min, charging pump rotating speed is made as 55r/min;
The reunion powder average grain diameter of preparing by above technique is 102.3 μ m, and apparent density is 1.23g/cm3, vibration densityDegree is 1.47g/cm3, reunion morphology microstructure and Fig. 3 are similar.
Embodiment tri-,
Shown in Figure 1, the preparation method of the spherical agglomerated powder of a kind of super fine titanium carbonitride based ceramic metal of the present invention,Comprise the steps:
A. add binding agent step: this step is taking paraffin as powder adhesive, by super fine titanium carbonitride based ceramic metalThe 10wt.% of powder weight takes paraffin, and paraffin and super fine titanium carbonitride based ceramic metal powder are together put into ball grinder;
B. prepare powder slurries step: this step is taking alcohol as solvent medium, super to filling in the ratio of 10g/100mlIn the ball grinder of thin base titanium carbonitride powder and corresponding proportion paraffin, add spirit solvent, by ratio of grinding media to material, 5:1 addsCarbide alloy abrading-ball, the rotating speed ball milling with 100r/min in planetary ball mill is prepared super fine titanium carbonitride base after 5 hoursMetal ceramic powder slurry;
C. mist projection granulating step: this step is to adopt high speed centrifugation Spray Grain-make Drier to super fine titanium carbonitride Base MetalCeramic powders slurry carries out mist projection granulating processing, thereby obtains the spherical agglomerated powder of super fine titanium carbonitride based ceramic metal powder;Wherein, in mist projection granulating process, inlet temperature is made as 100 DEG C, and outlet temperature is made as 80 DEG C, and atomizer rotating speed is made as 8kr/min,Charging pump rotating speed is made as 25r/min;
The reunion powder average grain diameter of preparing by above technique is 121.3 μ m, and apparent density is 1.15g/cm3, vibration densityDegree is 1.27g/cm3, reunion morphology microstructure and Fig. 3 are similar.
In sum, three kinds of spherical agglomerated morphology microstructures of super fine titanium carbonitride based ceramic metal powder that embodiment is preparedSimilar, difference is the difference along with technological parameter, and the performance such as size distribution, pine dress/tap density of reunion powder is poor to some extentDifferent. The present invention, by the parameter control of mist projection granulating, can prepare the spherical agglomerated powder body material that different grain size distributes, and equal toolHave that apparent density is high, the feature of good fluidity. The present invention adopts ball milling to prepare powder slurry to carry out powder in conjunction with spray granulationThe method of granulation, preparation technology is simple, and production efficiency is high, is easy to mass production.
It is spherical agglomerated that above-described embodiment is only used for further illustrating a kind of super fine titanium carbonitride based ceramic metal of the present inventionThe preparation method of powder, but the present invention is not limited to embodiment, and every foundation technical spirit of the present invention is to above embodimentAny simple modification, equivalent variations and the modification done, all fall in the protection domain of technical solution of the present invention.
Claims (1)
1. a preparation method for the spherical agglomerated powder of super fine titanium carbonitride based ceramic metal, is characterized in that: comprise following stepRapid:
A. add binding agent step: this step is taking paraffin as powder adhesive, by super fine titanium carbonitride based ceramic metal powder1～15wt.% of weight takes paraffin, and paraffin and super fine titanium carbonitride based ceramic metal powder are together put into ball grinder;
B. prepare powder slurries step: this step is taking alcohol as solvent medium, super to filling in the ratio of 5～50g/100mlIn the ball grinder of thin base titanium carbonitride powder and corresponding proportion paraffin, add spirit solvent, by ratio of grinding media to material, 5:1 addsCarbide alloy abrading-ball, the rotating speed ball milling with 100r/min in planetary ball mill is prepared super fine titanium carbonitride base after 5 hoursMetal ceramic powder slurry;
C. mist projection granulating step: this step is to adopt high speed centrifugation Spray Grain-make Drier to super fine titanium carbonitride based ceramic metalPowder slurries carries out mist projection granulating processing, thereby obtains the spherical agglomerated powder of super fine titanium carbonitride based ceramic metal powder; Wherein,In mist projection granulating process, inlet temperature is made as 80～300 DEG C, and outlet temperature is made as 60～200 DEG C, and atomizer rotating speed is made as 5～20kr/min, charging pump rotating speed is made as 20～80r/min.
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| CN105328200A (en) * | 2014-07-15 | 2016-02-17 | 昆山玛冀电子有限公司 | Atomization pelleting method for soft magnetic powder |
| CN109336612B (en) * | 2018-09-20 | 2021-05-07 | 成都美奢锐新材料有限公司 | Preparation method of superfine titanium carbonitride powder |
| CN110615438A (en) * | 2018-10-10 | 2019-12-27 | 西南交通大学 | Ti3C2Method for preparing powder |
| CN111455253A (en) * | 2020-03-25 | 2020-07-28 | 成都美奢锐新材料有限公司 | Titanium carbide-based metal ceramic thermal spraying powder and preparation method thereof |
| CN115196970B (en) * | 2022-08-08 | 2023-07-04 | 四川大学 | Preparation method of high-fluidity AlON spherical powder |
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