CN102294490B - A method of preparing a crude powder of molybdenum - Google Patents

A method of preparing a crude powder of molybdenum Download PDF

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CN102294490B
CN102294490B CN 201110220800 CN201110220800A CN102294490B CN 102294490 B CN102294490 B CN 102294490B CN 201110220800 CN201110220800 CN 201110220800 CN 201110220800 A CN201110220800 A CN 201110220800A CN 102294490 B CN102294490 B CN 102294490B
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powder
molybdenum
step
molybdenum powder
crude
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CN102294490A (en )
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何庆春
温宁兵
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成都虹波实业股份有限公司
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本发明公开了一种制取粗钼粉的方法,将钼粉∶氧化钼粉末按重量比为(4~0.67)∶1的比例混合后,按照(4ml~8ml)/100g混合粉末的比例向混合粉末中喷洒去离子水,搅拌均匀后再混合30min~60min;将混合物采用等静压压制成坯;压制坯经破碎后筛选得到(-20目,+180目)预制粉末;预制粉末进行氢气还原,还原温度为750℃~970℃;还原时间为10h~12h,氢气流量:20L/h-30L/h;按照球料体积比为1.1~2.0,对所制钼粉球磨30min~60min后,筛分得到所需产品。 The present invention discloses a molding method for obtaining a crude molybdenum powder, molybdenum powder: the weight ratio of molybdenum oxide powder (4 to 0.67) to 1 mixing ratio, in proportion / 100g powder mixture (4ml ~ 8ml) to the mixed powder is sprayed with deionized water, mixed well and then stirred for 30min ~ 60min; the mixture into a compact using isostatic pressing; the obtained compact was broken filter (-20 mesh, +180 mesh) preformed powder; powder preform hydrogen reduction, the reduction temperature is 750 ℃ ​​~ 970 ℃; reduction time 10h ~ 12h, hydrogen flow rate: 20L / h-30L / h; the ball feed volume ratio of 1.1 ~ 2.0, 30min ~ after molybdenum powder milling prepared 60min, sieved to obtain the desired product. 本发明方法生产成本低、工艺简单,所制备的钼粉使用性能好。 The method of the present invention is low cost, simple process, good performance molybdenum powder prepared.

Description

一种制取粗钼粉的方法 A method of preparing a crude powder of molybdenum

技术领域 FIELD

[0001]本发明涉及一种钼粉的制备方法,特别涉及一种预压制粒制取粗颗粒钼粉的方法。 Take coarse particles of molybdenum powder method [0001] The molybdenum powder is directed to a method of preparing the present invention, particularly to a pre-compression tablets prepared.

背景技术 Background technique

[0002]众所周知,除少数贵金属外,金属材料会与周围介质发生化学反应和电化学反应而遭受腐蚀。 [0002] is well known, except for a few noble metal material and a chemical reaction will be subject to corrosion electrochemical reaction with the surrounding medium. 此外,金属表面受各种机械作用而引起的磨损也极为严重。 In addition, wear metal surface by a variety of mechanical action caused extremely serious. 因此,发展金属表面防护和强化技术,是各国普遍关心的重大课题。 Therefore, the development and strengthening of metal surface protection technology, is a major issue of universal concern. 钼以其优良的耐磨性、抗腐蚀性和抗拉伤性能等而广泛应用于现代汽车工业中。 Molybdenum its excellent wear resistance, corrosion resistance and like properties strain widely used in modern automotive industry. 直接采用钼制造这类零部件价格昂贵,而在工程材料表面上制备钼系涂层,既满足了性能要求,又降低了成本。 Direct molybdenum manufacturing such parts is expensive, and the preparation of molybdenum-based coating on the surface engineering materials, both to meet the performance requirements of, and reducing costs. 在汽车工业发展过程中,有许多型号的涂层被用来提高变速器同步环、内燃机活塞环的耐磨性能,钼系涂层就是被广泛应用的涂层之一。 In the course of development of automobile industry, there are many types of coatings are used to improve the transmission of the synchronizer ring, wear resistance, molybdenum coating is one of the internal combustion engine a piston ring coating is widely used. 钼系涂层的制备在我国部分企业一直沿用火焰喷涂的方法。 Preparation of molybdenum-based coatings in our part of the business has been in use flame spraying method. 钼丝火焰喷涂设备简单,但沉积颗尺寸不一,氧化烧损严重,涂层疏松且因钼丝加工而成本高昂,严重制约其广泛应用。 Molybdenum wire flame spraying equipment is simple, but the deposition of particles of varying size, severe oxidation loss, and osteoporosis due to coating of molybdenum wire processing and high cost, which severely restricts widely. 近年来,用钼粉作原料的等离子喷涂方法随着啧涂设备、喷涂粉末生产技术的改进得以推广。 In recent years, plasma spraying with molybdenum powder as a raw material with Tut coating equipment, spraying powder production technology to improve promotion. 钼粉成本仅为钼丝的50%左右,为满足不同的性能要求,可方便地在钼粉中添加各种合金元素,以形成所期望的涂层。 Molybdenum powder molybdenum wire cost is only about 50%, to meet the different performance requirements, may be conveniently added various alloying elements in the molybdenum powder to form the desired coating.

[0003]等离子喷涂钼涂层的工艺特点要求喷涂钼粉粒度较粗(超过ΙΟμπι)、有适当的粒度分布范围和良好的流动性。 [0003] Plasma sprayed coatings of molybdenum of molybdenum powder spraying process characteristics required coarser (than ΙΟμπι), appropriate particle size distribution and good flowability. 普通钼粉粒度较小且分布宽、流动性差,不能满足等离子喷涂工艺和涂层性能要求。 Common molybdenum powder and small particle size distribution is broad, poor fluidity, can not meet the plasma spraying process and the coating performance requirements. 同时,为使涂层具备特定的性能,还须对喷涂钼粉的化学成分进行严格控制,如钼粉中的氧、碳、氮含量等杂质将对涂层的硬度、耐磨性等起重作用。 Meanwhile, as the coating with specific properties, the chemical composition of the spray must be strictly controlled molybdenum powder, molybdenum powder, such as oxygen, carbon and nitrogen impurities such coatings will hardness, wear resistance, such as lifting effect.

[0004]影响钼粉颗粒度的工艺因素,可以用下列关系式表示: [0004] Process Factors of molybdenum powder by influence, it can be expressed by the following relationship:

[0005] d = f(T,AT,h,Q,t) [0005] d = f (T, AT, h, Q, t)

[0006]式中;d为粉末粒度;T为还原温度;AT为温度梯度;h为舟皿内料层厚度;Q为氢气流量;t为还原时间。 [0006] wherein; d is a powder particle size; T is the temperature reduction; the AT is the temperature gradient; H boat within a material thickness; Q is a hydrogen flow rate; t is the reduction time.

[0007]还原温度越高、钼粉粒度越大、料层厚度越大、氢气渗入和水蒸气逸出将越困难,实际上相当于增加了水蒸气的分压,促进钼粉末挥发一一沉积长大,使颗粒变粗;氢气流量越大,水蒸气逸出速度加快,则钼粉粒度越细。 [0007] The higher reduction temperature, the larger the particle size of molybdenum powder, the greater thickness of material, hydrogen and steam penetration will be more difficult to escape, actually corresponds to an increase of partial pressure of water vapor, volatile eleven promote Mo powder deposited up, coarsening the particles; the greater the hydrogen gas flow rate, steam escape faster, finer the particle size of the molybdenum powder. 还原时间长,钼粉末反复氧化-还原长大、聚集再结晶长大的几率就大,钼粉末颗粒就越大。 Reducing long time, Mo powder of repeated oxidation - reduction grow, collective recrystallization big chance to grow, the greater the molybdenum powder particles.

[0008]上述工艺因素对钼粉颗粒长大的贡献是有限的,尤其是粒度大于20μπι的钼粉是无法用上述方式获得。 [0008] The above-described process of molybdenum powder particle growth factor contribution is limited, especially molybdenum powder 20μπι particle size greater than the above-described manner can not be obtained.

[0009]目前,为了适应等离子喷涂钼涂层的工艺特点要求,主要采用以下两种方法制备钼粉: [0009] Currently, in order to adapt the characteristics of plasma spraying molybdenum and other process requirements of the coating, molybdenum powder prepared mainly by the following two methods:

[0010]第一种方法是高温烧结破碎: [0010] A first method is a high-temperature sintering crushing:

[0011] (I)选择合适的常规钼粉。 [0011] (I) selecting suitable conventional molybdenum powder. 钼粉的粒度和密度适中,化学成分均匀、合格,钼粉形貌较为规则,无过多的搭接。 Molybdenum powder particle size and moderate density, uniform chemical composition, qualified, molybdenum powder morphology more regular, without excessive overlap.

[0012] (2)压坯成型。 [0012] (2) forming compacts. 采用足够吨位的液压机和模具,将钼粉压制成坯。 Using sufficient tonnage hydraulic press and die, pressed into the molybdenum powder compact.

[0013] (3)烧结。 [0013] (3) sintering. 选择800 °C -1200 °C的温度,将压制的钼坯放入烧结炉内烧结I _5h。 And a temperature 800 ° C -1200 ° C, and the pressed molybdenum billet into the sintering furnace the sintered I _5h.

[0014] (4)破碎和筛分。 [0014] (4) crushing and screening. 采用机械破碎的方法将经过烧结的坯料进行破碎并筛分。 Mechanical disruption method using the sintered blank be crushed and sieved.

[0015]上述第一种方法因烧结后坯料较硬,机械破碎需要增加专用设备投入,设备投入较大,生产成本高;所制备的粉末因粉碎工序导致杂质含量较高,颗粒形貌不规则,粉末流动性能较差,严重影响粉末的使用性能。 [0015] In the first method because hard sintered billet, mechanical disruption is necessary to increase investment in special equipment, large equipment investment, high production costs; powder prepared by pulverizing step leads to a higher content of impurities, particle shape irregular , poor powder flow properties, seriously affect the properties of the powder.

[0016]第二种方法是粘结制粒: [0016] The second method is a bonded granulation:

[0017] (I)将钼粉与PEG、PVA和乙醇和纯化水化浆配制成钼粉料; [0017] (I) The molybdenum powder with PEG, PVA and ethanol, and the purified pulp formulated hydrated molybdenum powder;

[0018] (2)将配制的钼粉料浆进行喷雾干燥造粒; [0018] (2) The molybdenum powder prepared slurry was spray-dried granules;

[0019] (3)得到的钼粉颗粒进行排胶、过筛、高温烧结; [0019] (3) molybdenum powder particles obtained debinding, sieving, high temperature sintering;

[0020] (4)将经过高温烧结的钼粉在高效球磨机中球磨,过筛分级后得到喷涂钼粉。 [0020] (4) After the high temperature sintering of molybdenum powder milled in a ball mill efficiency after spraying molybdenum powder obtained was sieved.

[0021 ]上述第二种方法生产工序复杂,要配置专用设备增加投资,生产成本高;调浆过程中加入的PEG和PVA等物质,烧结过程中分解出的碳、氧等杂质难以除尽,影响粉末的使用性能;高温烧结后的料硬度大,球磨硬料会增加粗钼粉中的杂质。 [0021] The second method of production process is complicated, to increase the investment in special equipment arranged, high production costs; mashing process by adding substances such as PEG and PVA, during sintering decomposition of carbon, oxygen and other impurities difficult divisible, affect the properties of the powder; large material hardness after high-temperature sintering, milling hard materials will increase the impurities in the crude molybdenum powder.

发明内容 SUMMARY

[0022]本发明的目的在于针对现有技术中制备钼粉的方法生产成本高、工艺复杂,钼粉使用性能不佳的问题,提供一种制取粗钼粉的方法。 [0022] The object of the present invention is directed to a method of preparing molybdenum powder prior art high production cost, process complexity, poor performance problems molybdenum powder, a method of preparing a crude molybdenum powder.

[0023]为实现上述目的,本发明解决其技术问题所采用的技术方案如下: [0023] To achieve the above object, the present invention is to solve the technical problem The technical solution adopted is as follows:

[0024] A、将普通钼粉与氧化钼(MoO3或MoO2)粉末按重量比(4〜0.67):1的比例混合,特别是(4〜1.5): I的比例混合后,再按照每100克混合粉末添加4ml〜8ml去离子水的比例,向混合粉末中喷洒去离子水,搅拌均勾后再混合30min〜60min; [0024] A, the ratio (4~0.67) by weight of molybdenum powder, molybdenum oxide general (of MoO3 or MoO2) powder: 1 ratio, in particular (4~1.5): I ratio after mixing, and then at every 100 ratio of the mixed powder grams of deionized water was added 4ml~8ml, sprayed with deionized water to this mixed powder, and then mixed with stirring are hook 30min~60min;

[0025] B、将步骤A获得的混合物采用等静压压制成坯; [0025] B, the mixture obtained in Step A using isostatic pressing into a billet;

[0026] C、将步骤B中所得的压制坯经破碎后筛选得到(-20目,+180目)预制粉末; [0026] C, obtained in Step B was press-crushed and screened to obtain a blank (-20 mesh, + 180 mesh) powder preform;

[0027] D、将步骤C中所得的预制粉末进行氢气还原,还原温度为750°C〜970°C;还原时间为1h〜12h,氢气流量:20L/h〜30L/h ; [0027] D, Step C, the resulting powder is hydrogen reduction pre-reduction temperature is 750 ° C~970 ° C; reduction time 1h~12h, hydrogen flow rate: 20L / h~30L / h;

[0028] E、将步骤D中所得的粉末料送入球磨机,球磨机中加入玛瑙球,球料体积比为1.1〜2.0,球磨30min〜60min后,筛分得到所需产品。 [0028] E, Step D the resulting material into a powder mill, a ball mill was added agate ball feed volume ratio of 1.1~2.0, after ball milling 30min~60min, sieved to obtain the desired product.

[0029]作为优选方式,所述步骤B中,等静压压制的压力值为SOMPa〜lOOMPa,保压时间为10s〜120s。 [0029] As a preferred embodiment, the step B, the isostatic pressing pressure value is SOMPa~lOOMPa, dwell time 10s~120s.

[0030]作为优选方式,所述步骤C中,筛选后,+20目的筛上物返回继续破碎,-180目的筛下物返回等静压压制。 [0030] As a preferred embodiment, the step C, after screening, + 20 mesh sieve is returned to continue the crushing, the -180 mesh sieve is returned isostatic pressing.

[0031]作为优选方式,所述步骤A中,普通钼粉的费氏粒度为2.Ιμπι〜3.5μηι,松装比重为 [0031] As a preferred embodiment, the step A, Fisher ordinary molybdenum powder particle size of 2.Ιμπι~3.5μηι, bulk specific gravity

0.8g/cm3〜1.lg/cm3 ; 0.8g / cm3~1.lg / cm3;

[0032] M0O2粉末的费氏粒度为5.Ομπι〜7.Ομπι,松装比重为0.6g/cm3〜I.2g/cm3 ; [0032] M0O2 Fisher particle size of the powder 5.Ομπι~7.Ομπι, bulk specific gravity of 0.6g / cm3~I.2g / cm3;

[0033] M0O3粉末的费氏粒度为5.7μηι〜7.8μηι,松装比重为0.7g/cm3〜I.2g/cm3。 [0033] M0O3 Fisher particle size of the powder 5.7μηι~7.8μηι, bulk specific gravity of 0.7g / cm3~I.2g / cm3.

[0034]本发明方法以钼粉和氧化钼粉为原料,以水作为钼粉和氧化钼颗粒之间的润滑剂,将三者混合,在等静压设备中进行预压制,获得具有一定强度的预压坯料。 [0034] The method of the present invention to molybdenum powder and molybdenum powder as raw material with water as a lubricant between the molybdenum powder and molybdenum oxide particles, mixing the three, the pre-isostatic pressing apparatus to obtain a certain strength preload blank. 坯料经适度破碎、筛分后,根据用户对粗钼粉的要求,选取(-20目,+ 180目)预制粒的粉末,对超出粒度范围的过粗钼粉进行球磨处理,对过细的钼粉可作为预压制粒的原料重复使用。 Moderate blank by crushing, sieving, according to user requirements crude molybdenum powder, selecting (-20 mesh, +180 mesh) pre-granulated powder of particle size outside the range for molybdenum powder is too coarse milling process, too small of molybdenum powder can be reused as a pre-pressed grain material. 在现有钼粉还原设备允许的条件范围内,在氢气气氛中还原成钼粉,钼粉经筛分分级,可以制取满足用户要求的粗钼粉(例如粒度费氏粒度超过ΙΟμίΉ,甚至高达20μπΐ左右的大颗粒钼粉)。 Within the conditions existing device allows reduction of molybdenum powder, reduced in a hydrogen atmosphere into the molybdenum powder, molybdenum powder by sieve classification, can meet user requirements preparing crude molybdenum powder (e.g. Fisher particle size exceeds ΙΟμίΉ, even up to 20μπΐ large particles of about molybdenum powder).

[0035]在本发明技术方案中,添加钼粉作为氧化钼(如MoO3)粉末还原时挥发一一沉积长大的核心,通过两种物质热力学性能的不同,从而促进氧化一一还原反应的反复进行。 [0035] In the aspect of the present invention, the addition of molybdenum powder as a repeated oxidation-reduction reaction of volatile eleven eleven grew when molybdenum oxide is deposited the core (e.g., of MoO3) powder was reduced by the different thermal properties of the two substances, thereby promoting get on. 虽然MoO3颗粒与Mo粉颗粒接触区域有中间氧化物的生成,但MoO3颗粒与Mo颗粒接触区域总向MoO3侧迀移,Mo团聚体长大。 Although Mo MoO3 particles and toner particles with a contact area of ​​the intermediate oxide generated, but the particle-particle contact area MoO3 total Mo to MoO3 side shift Gan, Mo agglomerates grow. 加入去离子水,预压时作为钼粉和三氧化钼颗粒之间的润滑剂,有利于预压成坯;氢气还原时,增大了水蒸气的分压,加速钼粉与三氧化钼界面反应生成钼粉的迀移,促进钼粉颗粒挥发一一沉积长大,有利于粉末颗粒团聚紧密。 Deionized water was added as a lubricant between molybdenum trioxide and molybdenum powder particles, into a compact beneficial preload when the preload; when reduced with hydrogen, water vapor partial pressure is increased to accelerate the powder and molybdenum trioxide interface Gan generated shift reaction molybdenum powder, molybdenum powder particles to promote the deposition of the volatiles eleven grew, agglomerated powder particles facilitate tight. 因此,钼粉中加入一定量的MoO3,再进行“加湿”预制粒后,通过氢气热处理,可得到粗钼粉。 Thus, the molybdenum powder was added an amount of MoO3, then after the "humidification" preformed particles through hydrogen heat treatment to obtain a crude molybdenum powder.

[0036]本发明方法避免了因机械破碎或添加粘结剂从而增加所制钼粉的杂质含量,可制备出杂质含量低,粒度较大的粗颗粒钼粉。 Method [0036] The present invention avoids the coarse particles of molybdenum powder by mechanical disruption or by adding a binder to increase the impurity content of molybdenum powder prepared can be prepared a low impurity content, a larger particle size. 这种方法相比预烧结后破碎制备粗钼粉的方法降低了制备难度和生产成本,简化了制备过程。 This method is compared with the pre-sintering crushing method for the preparation of a crude preparation of the reduced molybdenum powder production costs and difficulty, simplifies the manufacturing process. 通过钼粉中添加的适量的氧化钼和去离子水(由于还原过程中的气体交换,如果氧化钼添加过多就会导致所制粉末颗粒团疏松),在氢气还原与烧结过程中有利于提高钼粉团聚体的强度。 Molybdenum oxide and a suitable amount of deionized water was added by molybdenum powder (due to reduction of the gas exchange process, if too much is added molybdenum will cause the produced powder particles loose group), in the hydrogen reduction process and help to improve the sintering strength of from molybdenum powder agglomeration. 通过本发明方法制备出的粉末粒度在ΙΟμπι以上,甚至高达20μηι左右,松装比重大于1.5g/cm3。 Powder size prepared by the methods of the present invention ΙΟμπι above, even up to about 20μηι, bulk specific gravity of greater than 1.5g / cm3.

附图说明 BRIEF DESCRIPTION

[0037]图1为本发明工艺流程图。 [0037] FIG. 1 process flow diagram of the present invention.

具体实施方式 detailed description

[0038]本说明书中公开的所有特征,或公开的所有方法或过程中的步骤,除了互相排斥的特征和/或步骤以外,均可以以任何方式组合。 [0038] All of the features disclosed in this specification, or all of the methods disclosed processes or steps, except the mutually exclusive features and / or steps, can be combined in any manner.

[0039]实施例1:如图1所示,一种制取粗颗粒钼粉的方法,包括如下步骤: 1 [0039] Example: in FIG. A coarse molybdenum powder preparation method shown in FIG. 1, comprising the steps of:

[0040] A、将普通钼粉:MoO3粉按重量比1.5:1比例混合后,按照4ml去离子水/10g混合粉末的比例向混合粉末中喷洒去离子水,搅拌均匀后再混合60min ; [0040] A, ordinary molybdenum powder: 1.5 weight ratio of MoO3 powder: 1 ratio of the mixed powder after mixing ratio according 4ml deionized water / 10g spraying powder mixture of deionized water, mixing well and then stirred for 60min;

[0041] B、将步骤A的混合物采用等静压压制成坯,等静压压制的压力值为lOOMPa,保压时间为10s; [0041] B, the mixture of step A into a billet using isostatic pressing, isostatic pressing pressure value Loompa, dwell time of 10s;

[0042] C、将步骤B中所得的压制坯经破碎后筛选得到(-20目,+ 180目)预制粉末;筛选后,+20目的筛上物返回继续破碎,-180目的筛下物返回等静压压制。 [0042] C, obtained in Step B was press-crushed and screened to obtain a blank (-20 mesh, + 180 mesh) powder preform; After screening, + 20 mesh sieves is returned to continue the crushing, the -180 mesh sieve is returned isostatic pressing.

[0043] D、将步骤C中所得的预制粉末进行氢气还原,还原温度为750°C;还原时间为12h,氢气流量:20L/h; [0043] D, Step C, the resulting powder is hydrogen reduction pre-reduction temperature of 750 ° C; reduction time 12h, hydrogen flow rate: 20L / h;

[0044] E、将步骤D中所得的粉末料送入球磨机,球磨机中的玛瑙球与混合料的体积比为2.0:1,对所制钼粉球磨30min后,筛分得到所需产品费氏粒度为14.5μηι,松装比重为1.90g/ [0044] E, Step D the resulting material into a powder mill, the volume ratio of agate ball mill and the mix is ​​from 2.0: 1, the molybdenum powder prepared 30min milling, sieving to give the desired product Fisher particle size of 14.5μηι, bulk specific gravity of 1.90g /

Cm30 Cm30

[0045]实施例2:如图1所示,一种制取粗颗粒钼粉的方法,包括如下步骤: A method of preparing coarse particles of molybdenum powder shown in Figure 1, comprising the steps of: 2 [0045] Example:

[0046] A、将普通钼粉与MoO2粉按重量比4:1混合后,按照8ml去离子水/10g混合粉末的比例向混合粉末中喷洒去离子水,搅拌均匀后再混合30min ; [0046] A, MoO2 ordinary powder and molybdenum powder weight ratio 4: 1 ratio after mixing, deionized water according 8ml / 10g powder mixture is sprayed into the mixed powder of deionized water, mixing well and then stirred for 30 min;

[0047] B、将步骤A的混合物采用等静压压制成坯,等静压压制的压力值为lOOMPa,保压时间为114s; [0047] B, the mixture of step A into a billet using isostatic pressing, isostatic pressing pressure value Loompa, 114S dwell time;

[0048] C、将步骤B中所得的压制坯经破碎后筛选得到(-20目,+ 180目)预制粉末;筛选后,+20目的筛上物返回继续破碎,-180目的筛下物返回等静压压制。 [0048] C, obtained in Step B was press-crushed and screened to obtain a blank (-20 mesh, + 180 mesh) powder preform; After screening, + 20 mesh sieves is returned to continue the crushing, the -180 mesh sieve is returned isostatic pressing.

[0049] D、将步骤C中所得的预制粉末进行氢气还原,还原温度为970°C;还原时间为10h,氢气流量:20L/h; [0049] D, Step C, the resulting powder is hydrogen reduction pre-reduction temperature of 970 ° C; 10H reduction time, the hydrogen gas flow rate: 20L / h;

[0050] E、将步骤D中所得的粉末料送入球磨机,向球磨机中加入玛瑙球,球料体积比为1.5:1,对所制钼粉球磨601^11后,筛分得到所需产品费氏粒度为15.24111,松装比重为2.138/ [0050] E, Step D the resulting material into a powder mill, a ball mill was added to the agate ball, the ball feed volume ratio of 1.5: 1, the molybdenum powder prepared by milling 601 ^ 11, sieved to give the desired product 15.24111 Fisher particle size, bulk specific gravity of 2.138 /

Cm30 Cm30

[0051 ]实施例3:—种制取粗颗粒钼粉的方法,包括如下步骤: Preparation species coarse molybdenum powder, comprising the steps of: -: 3 [0051] Example

[0052] A、将普通钼粉:MoO3粉按重量比4:1比例混合后,按照8ml去离子水/10g混合粉末的比例向混合粉末中喷洒去离子水,搅拌均匀后再混合30min ; [0052] A, ordinary molybdenum powder: weight ratio of MoO3 powder 4: 1 ratio of the mixing ratio, in accordance with deionized water 8ml / 10g powder mixture is sprayed into the mixed powder of deionized water, mixing well and then stirred for 30 min;

[0053] B、将步骤A的混合物采用等静压压制成坯,等静压压制的压力值为lOOMPa,保压时间为114s; [0053] B, the mixture of step A into a billet using isostatic pressing, isostatic pressing pressure value Loompa, 114S dwell time;

[0054] C、将步骤B中所得的压制坯经破碎后筛选得到(-20目,+ 180目)预制粉末;筛选后,+20目的筛上物返回继续破碎,-180目的筛下物返回等静压压制。 [0054] C, obtained in Step B was press-crushed and screened to obtain a blank (-20 mesh, + 180 mesh) powder preform; After screening, + 20 mesh sieves is returned to continue the crushing, the -180 mesh sieve is returned isostatic pressing.

[0055] D、将步骤C中所得的预制粉末进行氢气还原,还原温度为970°C;还原时间为12h,氢气流量:20L/h; [0055] D, Step C, the resulting powder is hydrogen reduction pre-reduction temperature of 970 ° C; reduction time 12h, hydrogen flow rate: 20L / h;

[0056] E、将步骤D中所得的粉末料送入球磨机,球磨机中的玛瑙球与粉末料的体积比为1.5: I,对所制钼粉球磨30min后,筛分得到所需产品费氏粒度为22.Ομπι,松装比重为2.23g/ [0056] E, Step D the resulting material into a powder mill, the volume ratio of the powder material with an agate ball mill is from 1.5: I, after 30min molybdenum powder prepared milled and sieved to give the desired product Fisher particle size of 22.Ομπι, bulk specific gravity of 2.23g /

Cm30 Cm30

[0057]实施例4: 一种制取粗颗粒钼粉的方法,包括如下步骤: [0057] Example 4: Preparation method of coarse particles of molybdenum powder, comprising the steps of:

[0058] A、将普通钼粉:MoO3粉按重量比0.67:1比例混合后,按照6ml去离子水/10g混合粉末的比例向混合粉末中喷洒去离子水,搅拌均匀后再混合40min ; [0058] A, ordinary molybdenum powder: of MoO3 powder weight ratio 0.67: 1 ratio of the mixing ratio, in accordance with deionized water 6ml / 10g powder mixture is sprayed into the mixed powder of deionized water, mixing well and then stirred for 40min;

[0059] B、将步骤A的混合物采用等静压压制成坯,等静压压制的压力值为80MPa,保压时间为120s; [0059] B, the mixture of step A into a billet using isostatic pressing, isostatic pressing pressure is 80MPa, dwell time of 120s;

[0060] C、将步骤B中所得的压制坯经破碎后筛选得到(-20目,+ 180目)预制粉末;筛选后,+20目的筛上物返回继续破碎,-180目的筛下物返回等静压压制。 [0060] C, obtained in Step B was press-crushed and screened to obtain a blank (-20 mesh, + 180 mesh) powder preform; After screening, + 20 mesh sieves is returned to continue the crushing, the -180 mesh sieve is returned isostatic pressing.

[0061] D、将步骤C中所得的预制粉末进行氢气还原,还原温度为970°C;还原时间为12h,氢气流量:30L/h; [0061] D, Step C, the resulting powder is hydrogen reduction pre-reduction temperature of 970 ° C; reduction time 12h, hydrogen flow rate: 30L / h;

[0062] E、将步骤D中所得的粉末料送入球磨机,球磨机中的玛瑙球与粉末料的体积比为 [0062] E, Step D the resulting powder material into the mill, and the volume ratio of the powder material agate ball mill is from

1.1:1,对所制钼粉球磨30min后,筛分得到所需产品费氏粒度为13.4μπι,松装比重为1.78g/ 1.1: 1, the molybdenum powder prepared 30min milling, sieving to obtain desired particle size of the product Fisher 13.4μπι, bulk specific gravity of 1.78g /

Cm30 Cm30

[0063] 上述四项实施例中,普通钼粉的费氏粒度为2.1口111〜3.54111,松装比重为0.88/0113〜I.lg/cm3;Mo02粉末的费氏粒度为5.(^111〜7.(^111,松装比重为0.68/0113〜1.Sg/cnAMoCb粉末的费氏粒度为5.7μηι〜7.8μηι,松装比重为0.7g/cm3〜1.2g/cm3。上述实施例中,球磨所用的玛瑙球也可以根据需要采用钢球进行研磨。 [0063] In the above-described four embodiments, Fisher ordinary molybdenum powder particle size of 2.1 111~3.54111, bulk specific gravity of 0.88 / 0113~I.lg / cm3; Mo02 powder Fisher particle size of 5 (111 ^. ~ 7. (^ 111, bulk specific gravity of 0.68 / 0113~1.Sg / cnAMoCb Fisher particle size of the powder 5.7μηι~7.8μηι, bulk specific gravity of 0.7g / cm3~1.2g / cm3. the above-described embodiment , agate ball milling used may be ball milled according to need.

[0064]采用上述实施例的本发明方法生产成本低、工艺简单,所制备的钼粉使用性能好。 [0064] Low method of the above-described embodiments of the present invention, production cost, simple process, good performance molybdenum powder prepared.

[0065]本发明并不局限于前述的具体实施方式。 [0065] The present invention is not limited to the foregoing specific embodiments. 本发明扩展到任何在本说明书中披露的新特征或任何新的组合,以及披露的任一新的方法或过程的步骤或任何新的组合。 The present invention extends to any novel features disclosed in this specification, or any novel combination, or any novel combination, and any steps disclosed a new method or process.

Claims (5)

  1. 1.一种制取粗钼粉的方法,其特征在于包括如下步骤: A、将普通钼粉:氧化钼粉末按重量比(4〜1.5):1的比例混合后,再按照每100克混合粉末添加4 m I〜8 m I去离子水的比例,向上述混合粉末中喷洒去离子水,搅拌均匀后再混合30min〜60min; B、将步骤A获得的混合物经等静压压制成坯; C、将步骤B所获得的压制坯经破碎后筛选,得到粉末粒度为一20目〜+180目的预制粒粉末; D、将步骤C中所获得的预制粒粉末进行氢气还原,还原温度为750°C〜970°C;还原时间为1h〜12h,氢气流量:20L/h〜30L/h ; E、将步骤D所获得的粉末料送入球磨机,向球磨机中加入玛瑙球,球料体积比为(1.1〜2.0): I,球磨30min〜60min后,筛分得到所需粗钼粉。 1. A method of preparing a crude molybdenum powder, comprising the steps of: A, ordinary molybdenum powder: powder ratio of molybdenum oxide (4~1.5) by weight: 1 ratio after mixing, and then at every mixing 100 grams powder is added 4 ratio m I~8 m I of deionized water, sprayed with deionized water to the mixed powder, and then homogeneously mixed with stirring 30min~60min; B, step a obtained mixture was isostatically pressed into a billet; C, the pressed blank step B obtained after crushing screening, the powder particle size of -20 mesh to +180 object preform granulated powder; D, the pre-granulation powder in step C obtained is reduced with hydrogen, the reduction temperature is 750 ° C~970 ° C; reduction time 1h~12h, hydrogen flow rate: 20L / h~30L / h; E, the powder material obtained in the step D into a ball mill, a ball mill was added to the agate ball, the ball feeder volume ratio It is (1.1~2.0): I, milled 30min~60min, sieved to give the desired crude molybdenum powder.
  2. 2.如权利要求1所述的制取粗钼粉的方法,其特征在于:所述氧化钼为MoO3或MoO2。 2. The system as claimed in claim 1. A method for obtaining a crude molybdenum powder, characterized in that: said molybdenum oxide MoO3 or MoO2.
  3. 3.如权利要求1所述的制取粗钼粉的方法,其特征在于:所述步骤B中,等静压压制的压力值为80MPa〜lOOMPa,保压时间为10s〜120s。 Prepared according to a method for obtaining a crude molybdenum powder as claimed in claim 3, wherein: said step B, the isostatic pressing pressure value is 80MPa~lOOMPa, dwell time 10s~120s.
  4. 4.如权利要求1所述的制取粗钼粉的方法,其特征在于:所述步骤C中,筛选后,+20目的筛上物返回继续破碎,一180目的筛下物返回等静压压制。 Hydrostatic the step C, after screening, + 20 mesh sieves is returned to continue crushing, under a 180-mesh screen is returned and the like: 4. The system according to claim 1 for obtaining a crude method of molybdenum powder, characterized in that suppress.
  5. 5.如权利要求2所述的制取粗钼粉的方法,其特征在于: 所述普通钼粉的费氏粒度为2.Ιμπι〜3.5μηι,松装比重为0.8g/cm3〜1.lg/cm3 ; M0O2粉末的费氏粒度为5.Ομπι〜7.Ομπι,松装比重为0.6g/cm3〜1.2g/cm3 ; M0O3粉末的费氏粒度为5.7μηι〜7.8μηι,松装比重为0.7g/cm3〜1.2g/cm3。 5. The system according to claim 2 Methods crude molybdenum powder, characterized in that: the normal Fisher molybdenum powder particle size of 2.Ιμπι~3.5μηι, bulk specific gravity of 0.8g / cm3~1.lg / cm3; M0O2 Fisher particle size of the powder 5.Ομπι~7.Ομπι, bulk specific gravity of 0.6g / cm3~1.2g / cm3; M0O3 Fisher particle size of the powder 5.7μηι~7.8μηι, bulk specific gravity of 0.7 g / cm3~1.2g / cm3.
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