CN100500336C - Production method of tungsten carbide base ball shaped thermal spray coating powder - Google Patents

Production method of tungsten carbide base ball shaped thermal spray coating powder Download PDF

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CN100500336C
CN100500336C CN 200510020875 CN200510020875A CN100500336C CN 100500336 C CN100500336 C CN 100500336C CN 200510020875 CN200510020875 CN 200510020875 CN 200510020875 A CN200510020875 A CN 200510020875A CN 100500336 C CN100500336 C CN 100500336C
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powder
spray
spherical
tungsten carbide
production
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CN1686644A (en
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何宪峰
刚 尹
曹万里
李伟勤
石建华
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自贡硬质合金有限责任公司
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Abstract

该发明属于硬质合金生产中的碳化钨基球形热喷涂粉末的生产方法。 The invention is in the production of tungsten carbide based cemented carbide ball thermal spraying method for producing the powder. 包括采用WC为基材、以Co或Co和Cr为粘结相、己烷作球磨介质、石蜡作造粒粘结剂;并通过:湿磨配制料浆、喷雾干燥造粒、筛分干燥粒料、在氢气保护下烧结,最后对烧结的粉料按要求分级,从而获得目的物球形热喷涂粉末。 Using as substrate comprising WC, Co or Co and Cr in the binder phase is hexane as milling media, paraffin as binder granulated; by: wet milling a slurry formulation, spray-dried granulated, sieved and dried granulation material, sintered under hydrogen protection, and finally as required sintered powder classified to obtain the desired product spherical thermal spray powder. 该发明具有工艺流程短,粉末形貌规则、球形化好,生产率可较背景技术提高20倍以上,而设备投资仅为相同规模背景技术的四分之一;生产成本低并可进行大规模工业化生产等特点。 The invention has a short process, powder regular morphology, good spheronization, productivity can be increased by 20 times compared with the background art, only a quarter of the equipment investment on the same scale of the background art; low production cost and large-scale industrialization production and so on. 克服了背景技术设备投资大、而生产率极低、生产成本高且不能用于硬质合金球形热喷涂粉末的生产等缺陷。 BACKGROUND overcome large investment in equipment, and low productivity, high production cost and can not be used for the production of carbide thermal spray powder of spherical defects.

Description

碳化钨基球形热喷涂粉末的生产方法 Based spherical tungsten carbide thermal spray powder production methods

技术领域 FIELD

本发明属于一种热喷涂粉末材料(复合物)的生产方法,特别是一种碳化钨基硬质合金球形热喷涂粉末的生产方法。 The present invention resides in a thermal spray powder material (composite) production methods, and particularly to a tungsten carbide based cemented carbide thermal spray process for producing spherical powders. 采用该方法所生产的球形喷涂粉末可广泛用于高速氧气燃料喷涂,以在基体表面形成具有优越耐磨等性能的致密涂层。 Produced by this method can be used in a spherical spray powder high speed oxygen fuel spraying, to form a dense coating layer having excellent wear-resistant properties of the substrate surface.

背景技术 Background technique

传统的热喷涂用复合粉一般采用机械混合法及烧结破碎法生产。 Conventional thermal spray composite powder is generally mechanical mixing and crushing sintering production method. 碳化钨 Tungsten carbide

基热喷涂粉末是以碳化钨(WC)为基材,以Co或Co和Cr为粘结相的复合粉末。 Based thermal spray powder is tungsten carbide (WC) substrate to a Co or Cr and Co as binder phase in the composite powder. 机械混合法生产碳化钨基热喷涂粉是采用一定比例的碳化钨粉与Co粉或Co和Cr粉通过机械混合而成,其实质仅是一种混合粉,而不能称之为复合粉,该方法虽然具有工艺方法简单、生产成本较低等特点,但却存在WC与Co或Ccr~Cr粉混合的均匀性差、质量不稳定,用于热喷涂后其涂层各部分机械性能一致性差,故目前已很少使用;而烧结破碎法是将WC与Co粉或Co 和Cr粉混合后经烧结成WC基合金后,再经机械破碎而成,采用此方法生产的喷涂粉虽属复合粉,但却存在粉末的形状不规则、流动性差、很难达到喷涂工艺要求;同时该粉末在生产过程中对环境的粉尘和噪音污染严重。 Mechanical mixing of tungsten carbide-based thermal spray powder production is the use of a certain proportion of tungsten carbide powder is mixed with Co powder or Co and Cr powder together by mechanical, its essence is only a mixed powder, the powder can not be called a composite, the Although the method has a simple process, low production cost and the like, but the presence of WC with Co or Ccr ~ Cr powder mixing uniformity is poor, the quality is unstable, after which a thermal spray coating portions of the mechanical properties of consistency is poor, so has been rarely used; sintering crushing method is after sintered WC-based alloy powder after mixing WC powder with Co or Co and Cr, and then is made by mechanical crushing, using this method of producing composite powder spray powder corporations, but irregular shape of powder present, poor fluidity, is difficult to achieve in claim spraying process; while the powder in the production process of serious environmental dust and noise pollution. 为了克服上述热喷涂用复合粉及其生产中存在的缺陷,在美国专利5126104、名称为《制取热喷涂粉末材料的方法》的专利文献中,公开了一种采用Ni^Cr 一B—Si合金粉、Mo粉及Cr3C2/NiCr合金粉,经球磨混合成为流汁性料浆, 采用仲钼酸铵和聚乙烯醇为粘结剂造成团粒,并在800〜95(TC的还原气氛下恒温烧结,其烧结物再置于等离子火焰炉中并在等离子体火焰流中保持足够时间、使烧结物中的所有粉末颗粒基本熔化使之成为球形颗粒,然后再进一步使其金属化,最后经冷却而成。采用该方法虽然具有可获得较理想的粉末形态、粒度,其显微组织及粉末的硬度、耐磨性也较好等特点。但却存在所需等离子火焰炉非常昂贵、设备投资大,而球化产能却极低, 一般生产率仅5kg/小时,生产成本极高;此外,由于等离子火焰流温度极高(其温度截面 To overcome the above composite powder and the thermal spraying defects exist in the production, in U.S. Patent No. 5,126,104, entitled "Preparation methods of thermal spray powder material" in Patent Document discloses a method using a Ni ^ Cr B-Si alloy powder, Mo powder and Cr3C2 / NiCr alloy powder, mixed by a ball mill juice as a flow of slurry of ammonium paramolybdate and using polyvinyl alcohol as the binder resulting pellets, and the temperature (TC reducing atmosphere of 800~95 sintering, the sintering was then placed in a furnace and the like and maintained in the plasma flame for a sufficient time in the plasma flame stream, so that all the powder particles sinter was melted to become substantially spherical particles, and then further metalized, and finally cooled It made. Although this method has achieved an ideal form of powder, grain size, microstructure and hardness of the powder, better wear resistance characteristics. but the presence of the desired plasma flame furnace is very expensive, equipment investment , but the ball is very low capacity, generally production rate 5kg / hr, high production costs; In addition, since a very high temperature plasma flame stream (which is a cross-sectional temperature

最典型的温度区域为5500〜17000°C), WC粉若该在火焰流中加热则烧损严重且易结饼,因而该工艺方法不能用于硬质合金球形喷涂粉末的生产。 The most typical temperature range is 5500~17000 ° C), WC powder, if the stream is heated in a flame burning severe caking and easily, and thus the process is not a method for producing a spherical spray powder of cemented carbide. 发明内容 SUMMARY

本发明的目的是针对背景技术存在的缺陷,在其基础上改进设计一种碳化钨基球形热喷涂粉末的生产方法,以达到简化工艺流程粉末球形化好、形貌规则,降低设备投资、实现大规模工业化生产,提高生产效率及降低生产成本,用于热喷涂其上粉率及涂层的耐磨性好等目的。 Object of the present invention is directed to defects in the background art, an improved design of a production process of spherical tungsten carbide substrate in which the thermal spray powder on the basis of a simplified process flow to achieve a good powder spheroidization, regular morphology, reduced investment in equipment, to achieve large-scale industrial production, improve production efficiency and reduce production costs for thermal spray it on and wear resistance of powder coatings and other purposes.

本发明的解决案是首先根据碳化钩基球形热喷涂粉末的成份要求配料进行湿磨至要求粒度,并加入造粒粘结剂石蜡后制成料浆,再经调节料桨的固液比后将料浆喷雾干燥成球形粉末,然后将该球形粉末直接烧结、最后经分级处理即得目的物,从而实现其目的。 Case solution according to the present invention the first component is a hook-yl spherical carbide thermal spray powder of claim furnish wet milling to the required particle size, slurried and added after granulation binder paraffin, and then the solid-liquid ratio of the pitch conditioner after the slurry was spray-dried into spherical powder, then the powder is directly sintered spherical, the objective was to obtain the final classification treatment, in order to achieve its purpose. 因此,本发明方法包括- Thus, the method of the present invention comprises -

A、 湿磨配制料浆:首先按原料粉重量百分比计将WC粉80〜90wt。 A, wet milling the slurry formulation: First, the raw material powder weight percent of WC powder 80~90wt. /。 /. 和Co 粉或Co和Cr粉10〜20wt。 Co and Cr powder and Co powder or 10~20wt. /。 /. 加入球磨机内,同时加入原料粉总重量20〜23wt% 的己烷,之后,湿磨原料粉至费氏粒度达1.0〜3.0um,然后加入原料粉总重量1. 5〜3. 5wt。 Was added to the ball mill, while adding 20~23wt% of the total weight of the raw material powder hexanes, then, wet grinding the raw material powder to a particle size of Fisher 1.0~3.0um, followed by addition of total weight of the raw material powder 1. 5~3. 5wt. /a的石蜡继续湿磨3〜6小时,配制成混合料浆; / A paraffin continued triturated 3 ~ 6 hours to prepare a mixing slurry;

B、 喷雾干燥造粒:将A所得料浆送入搅拌槽内,再加入己烷将料浆稀释 B, spray drying granulation: A The resulting slurry was stirred into the tank, the slurry was diluted with hexane was added

至固液比为2.5〜3.5:1,搅拌混合均匀后输入喷雾干燥装置内干燥造粒,得球形混合粉料;喷雾干燥装置的喷片孔径为小O. 5〜1. Omm,喷雾压力为0. 8〜 1. 6Mpa,干燥温度为80〜120°C; To a solid-liquid ratio of 2.5~3.5: 1, spray-drying apparatus input granulated after drying evenly stirred and mixed to obtain mixed powder of spherical; sheet discharge aperture for the spray-drying apparatus small O. 5~1 Omm, spraying pressure. 0. 8~ 1. 6Mpa, a drying temperature of 80~120 ° C;

C、 筛分:将由B所得球形混合粉料按产品粒度要求过双层振动筛,筛上物及筛下物均返回B工序重新造粒,筛内物分装于石墨舟皿中; C, screening: B obtained by mixing a spherical powder particle size according to product requirements through double shaker, the oversize and the undersize were regranulated return step B, was dispensed into the graphite boat inner screen;

D、 烧结:将装入粉料的石墨舟皿置于连续烧结炉中,在氢气保护及950〜 115(TC温度下烧结40〜80分钟后,冷却至5(TC以下出炉; D, sintering: The powder was charged in a graphite boat was placed in the continuous sintering furnace, and sintered in a protective hydrogen 950~ 115 (TC temperature at 40~80 min, cooled to. 5 (hereinafter TC released;

E、 分级处理:将上述所得烧结粉料按热喷涂所要求的粒度进行分级,即得目的物。 E, classification treatment: The above-described sintered powder obtained by thermal spraying a desired particle size was classified to obtain the desired product.

上述连续烧结炉为钼丝烧结炉,而氢气流量为1〜3mV小时。 The continuous sintering furnace is a sintering molybdenum wire furnace, and the flow rate of hydrogen 1~3mV hours. 所述分级处理,是将烧结粉料采用双层振动筛进行筛分或采用气流分选。 The classification treatment, the sintered powder is sieved using double vibrating or by an air separation.

本发明由于采用己烷作球磨介质、石蜡作造粒粘结剂,经喷雾干燥造粒后,在氢气保护下直接烧结成球形粉末,最后按要求分级即得成品碳化钨基球形热喷涂粉末,而具有工艺流程短,粉末形貌规则、球形化好,生产率可较背景技术提高20倍以上,而设备投资仅为背景技术的四分之一;且产品用于热喷涂、其上粉率及涂层的耐磨性均较机械混合法及烧结破碎法所得产品大大提高等特点。 The present invention adopts hexane as milling media, paraffin as binder granulated, spray dried after granulated, sintered under hydrogen protection directly into the spherical powder, the final classification as required to obtain the finished thermal spray powder of spherical tungsten carbide substrate, and a short process, powder regular morphology, good spheronization, productivity can be increased by 20 times compared with the background art, while the equipment investment is only a quarter of the background art; and product for thermal spraying, and that the extraction rate the wear resistance of the coating compared with mechanical mixing method and sintering the resulting crushed product greatly improved characteristics.

附图说明 BRIEF DESCRIPTION

图1为实施例1产品形貌400倍扫描电镜照片; 图2为实施例2产品形貌200倍扫描电镜照片。 Example 1 FIG. 1 is a product morphology scanning electron micrograph of 400-fold embodiment; FIG. 2 is a 200 fold Example 2 product morphology photograph of a scanning electron microscope. 实施例1 Example 1

本实施例为以WC为基材,以Co为粘结相的球形热喷涂粉末的生产方法, 其方法为: This embodiment is as the base material of WC to Co binder phase spherical thermally spraying powder production process, which method:

A、 湿磨配制料浆:将符合工业生产国家标准要求纯度的WC粉252kg、 Co粉48kg置于球磨机内,同时加入纯度为99% (工业纯)的己烷67kg,湿30小时至粉料的费氏粒度为1.0〜3.0ixm,然后加入4kg石蜡再湿磨4小时后配成料浆; A, wet milling the slurry formulation: industrial production will meet national standards of purity WC powder 252kg, Co powder 48kg placed in a ball mill, while adding 67kg of hexane purity of 99% (commercially pure), the wet powder to 30 hours the particle size of Fisher 1.0~3.0ixm, followed by addition of 4kg paraffin dubbed again wet-milled slurry after 4 hours;

B、 喷雾干燥造粒:将配制好的料浆送入型号为HC—3000的闭式循环压力喷雾干燥装置的料浆搅拌槽内,再加入33kg己烷将料浆的固液比调至3d, 在搅拌条件下将料浆喷入干燥室内进行干燥、造粒;其中:喷片孔径小0.6mm, 喷雾压力1.2Mpa,干燥温度10(TC,料浆搅拌转速200转/分。 B, spray drying granulation: The prepared slurry is fed to a slurry Model HC-3000 Pressure closed cycle spray-drying apparatus in a stirred tank, added 33kg of hexane slurry of solid-liquid ratio was adjusted to 3d , under stirring the slurry is sprayed into a drying chamber for drying, granulation; wherein: sheet ejection pore size 0.6mm, spray pressure 1.2Mpa, drying temperature 10 (TC, slurry stirring speed 200 rev / min.

C、 筛分:将由B所得粉料过270目及1000目双层振动筛,得《63um、 》10iim的粉料;筛上及筛下物均返回重新造粒; C, screening: B by the resultant powder through a 270 mesh and 1000 mesh Double shaker to give "63um," 10iim powder; undersize and the oversize granules are returned again;

D、 烧结:将上述筛分所得粉料按每个舟皿8kg的量装舟后,置于连续钼丝烧结炉中,在106(TC及氢气保护下烧结60分钟后,冷却至50。C以下,得烧结球形粉料;氢气流量为2mV小时; D, sintering: After sieving the resulting powder after the above-described amount of each boat boat mounted 8kg, molybdenum wire disposed continuous sintering furnace, sintered for 60 minutes (TC protection and hydrogen at 106, cooled to 50.C or less, to obtain a sintered spherical powder; hydrogen flow rate of 2mV hours;

E、筛分:将上述烧结所得球形粉料采用320目和800目双层振动筛筛分, 筛上及筛下物另作它用,即得费氏粒度为15〜45 ii m的WC"Co球形热喷涂粉末; E, screening: The resulting sintered spherical powder above 320 mesh and 800 mesh using double vibrating sieve, and the sieve undersize was used for other purposes, i.e., to give Fisher particle size of 15~45 ii m of WC " Co thermal spray spherical powder;

按GB5242检测本实施例粉末松装密度》3. 8g/cm3,流速<18秒/50g。 GB5242 embodiment according to the present embodiment detects a powder bulk density "3. 8g / cm3, a flow rate of <18 seconds / 50g. 实施例2 Example 2

本实施例为以WC为基材,以Co和Cr为粘结相的球形热喷涂粉末的生产方法,其方法为- This embodiment is as a substrate of WC, Co and Cr to a method for the production of spherical thermal spray powder binder phase, which method -

A、 湿磨配制料浆:将符合工业生产国标要求的WC粉258.45kg及Co粉30. 15kg、 Cr粉11.4kg投入球磨机内,同时加入工业纯的己烷67kg,湿磨31小时至粉料的费氏粒达1. 0〜3. 0 um,然后加入6kg石蜡再湿磨4. 5小时, 配成料浆; A, wet milling the slurry formulation: complies with industrial production requirements of national standard WC powder and Co powder 258.45kg 30. 15kg, Cr 11.4kg powder into a ball mill, while adding 67kg of industrial pure hexane, triturated powder to 31 hours Fibonacci particles of 1. 0~3 0 um, and then wet-milled and then added 6kg paraffin 4.5 hours, dubbed slurry.;

B、 喷雾千燥造粒:将配制好的料浆送入闭式循环压力喷雾干燥装置的料浆搅拌槽内,再加入33kg己垸将其固液比调至3:l,在搅拌条件下将料浆喷入干燥室内干燥、造粒;喷片孔径》0.8mm、喷雾压力1. 3Mpa,干燥温度100 °C,搅拌槽转速200转/分; B, dry in the spray granulation: The prepared slurry is fed into the slurry pressure in closed cycle spray-drying apparatus in a stirred tank, added 33kg embankment which have solid-liquid ratio was adjusted to 3: l, with stirring at the slurry was sprayed into the drying chamber drying, granulation; sheet discharge aperture "0.8mm, spray pressure of 1. 3Mpa, drying temperature 100 ° C, speed of the stirring tank 200 rev / min;

C、 筛分:与实施例l同; C, sieving: Example l with the same embodiment;

D、 烧结:本实施例烧结温度为1100'C,其余亦与实施例l,同; D, sintering: sintering temperature of the present embodiment 1100'C, Example l with the remainder embodiment also, the same;

E、 气流分级:本实施例采用气流分级得费氏粒度为15〜45um的Wc— Co"Cr球形热喷涂粉末;气流分级工艺参数为:风量8mV分,风压0.8Mpa, 进料速度:60kg/小时。 E, air classification: the present embodiment employs air classifier to obtain a Fisher grain size of 15~45um Wc- ​​Co "Cr thermal spray spherical powder; air classifier process parameters: air flow 8mV points, pressure 0.8Mpa, feed rate: 60kg /hour.

本实施例粉末按GB5242检测:松装密度》3.8g/cm3,流速〈18秒/50g。 The powder according to the present embodiment GB5242 detection: Bulk density "3.8g / cm3, a flow rate of <18 seconds / 50g.

Claims (3)

1. 一种碳化钨基球形热喷涂粉末的生产方法,其特征在于该方法包括:A. 湿磨配制料浆:首先按原料粉重量百分比计将WC粉80~90wt%和Co粉或Co和Cr粉10~20wt%加入球磨机内,同时加入原料粉总重量20~23wt%的己烷,之后,湿磨原料粉至费氏粒度达1.0~3.0μm,然后加入原料粉总重量1.5~3.5wt%的石蜡继续湿磨3~6小时,配制成混合料浆;B. 喷雾干燥造粒:将A所得料浆送入搅拌槽内,再加入己烷将料浆稀释至固液比为2.5~3.5∶1,搅拌混合均匀后输入喷雾干燥装置内干燥造粒,得球形混合粉料;喷雾干燥装置的喷片孔径为φ0.5~1.0mm,喷雾压力为0.8~1.6Mpa,干燥温度为80~120℃;C. 筛分:将由B所得球形混合粉料按产品粒度要求过双层振动筛,筛上物及筛下物均返回B工序重新造粒,筛内物分装于石墨舟皿中;D. 烧结:将装入粉料的石墨舟皿置于连续烧结炉中 1. A method of producing spherical tungsten carbide substrate thermal spraying powder, characterized in that the method comprises:. A wet milled slurry formulation: First, the raw material powder weight percent of WC powder and 80 ~ 90wt% Co powder or Co and 10 ~ 20wt% Cr powder was added to the ball mill, while adding the total weight of the starting powder, 20 ~ 23wt% in hexane, then, wet grinding the raw material powder to Fisher particle size of 1.0 ~ 3.0μm, followed by addition of total weight of the raw material powder is 1.5 ~ 3.5wt % paraffin continue triturated 3 to 6 hours to prepare a mixing slurry; spray drying granulation B: a the resulting slurry was stirred into the tank, then diluted with hexane was added to the slurry to solid-liquid ratio of 2.5 to 3.5:1 input stirring and mixing uniformly drying a spray granulation drying apparatus to obtain spherical powder mixture; spray dryer sheet discharge aperture φ0.5 ~ 1.0mm, the spray pressure is 0.8 ~ 1.6Mpa, the drying temperature is 80 ~ 120 ℃; C screening: B obtained by mixing a spherical powder particle size according to product requirements through double shaker, the oversize and undersize are regranulated return step B, the sieve was dispensed into the graphite boat in; D sintering: the powder was charged in a graphite boat was placed in the continuous sintering furnace ,在氢气保护及950~1150℃温度下烧结40~80分钟后,冷却至50℃以下出炉;E. 分级处理:将上述所得烧结粉料按热喷涂所要求的粒度进行分级,即得目的物。 After the sintered under hydrogen protection and temperature 950 ~ 1150 ℃ 40 ~ 80 minutes, and cooled to 50 deg.] C baked; E classification treatment: The above sintered powder obtained by thermal spraying a desired particle size was classified to obtain the desired product .
2. 按权利要求1所述碳化钨基球形热喷涂粉末的生产方法,其特征在于所述连续烧结炉为钼丝烧结炉,而氢气流量为1〜3mV小时。 2. according to claim 1 spherical tungsten carbide based thermal spray powder production methods, wherein said sintering furnace is a continuous sintering molybdenum wire furnace, and the flow rate of hydrogen 1~3mV hours.
3. 按权利要求1所述碳化钨基球形热喷涂粉末的生产方法,其特征在于所述分级处理,是将烧结粉料采用双层振动筛进行筛分或采用气流分选。 3. according to claim 1 spherical tungsten carbide substrate thermal spraying powder production process, characterized in that the classification treatment, the sintered powder is sieved using double vibrating or by an air separation.
CN 200510020875 2005-05-10 2005-05-10 Production method of tungsten carbide base ball shaped thermal spray coating powder CN100500336C (en)

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CN102191447A (en) * 2010-03-09 2011-09-21 中国科学院上海硅酸盐研究所 Tungsten carbide cobalt-copper-molybdenum disulfide self-lubricating wear-resistant coating and preparation method thereof
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CN102554249B (en) * 2012-03-02 2013-04-24 株洲弗拉德科技有限公司 Method for preparing tungsten carbide based thermal spraying alloy powder
CN102876907B (en) * 2012-09-27 2014-02-05 中南大学 Preparation method of tungsten carbide-cobalt or tungsten carbide-cobalt-chromium thermal spraying powder
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