CN105880613B - One kind of powder preparation method of making a special molybdenum for molybdenum electrodes - Google Patents

One kind of powder preparation method of making a special molybdenum for molybdenum electrodes Download PDF

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CN105880613B
CN105880613B CN 201610281360 CN201610281360A CN105880613B CN 105880613 B CN105880613 B CN 105880613B CN 201610281360 CN201610281360 CN 201610281360 CN 201610281360 A CN201610281360 A CN 201610281360A CN 105880613 B CN105880613 B CN 105880613B
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CN 201610281360
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CN105880613A (en )
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赵新瑞
付绍军
张增祥
左翀
程进
陈宇娟
王沛丽
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金堆城钼业股份有限公司
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Abstract

本发明公开了一种用于制作钼焊条的专用钼粉制备方法,将工业二氧化钼和三氧化钼采用固‑固掺杂混合均匀,得到MoO2‑MoO3混合粉末;然后MoO2‑MoO3混合粉末经过高温还原生成钼粉,将钼粉振动打散后先进行200目筛分,然后对200目筛上物进行80目筛分,即得。 The present invention discloses a method for preparing specific method for making molybdenum powder molybdenum welding wire, industrial use of molybdenum trioxide and molybdenum dioxide Solid - Solid doped uniformly mixed to give a mixed powder MoO2-MoO3; MoO2-MoO3 powder mixture then passes molybdenum powder generated high temperature reduction, first at 200 mesh sieve after the vibration molybdenum powder break up, and then on a 200 mesh screen was 80 mesh sieve, to obtain. 本发明制备方法制备的钼粉除去了粒度偏细及偏大部分的颗粒,生产的钼粉颗粒相对均匀,一致性及流动性均稳定良好,满足焊条用粉的技术要求,且成品率较高,可达到70%。 Molybdenum powder produced by the production method of the present invention to remove fine particle size and partial partial majority of the particles, the production of molybdenum powder particles are relatively uniform, stable consistency and flowability are excellent, powders meet the technical requirements of the electrode, and high yield , up to 70%.

Description

一种用于制作钼焊条的专用钼粉制备方法 One kind of powder preparation method of making a special molybdenum for molybdenum electrodes

技术领域 FIELD

[0001]本发明属于钼粉制备技术领域,具体涉及一种用于制作钼焊条的专用钼粉制备方法。 [0001] The present invention belongs to the technical field of the preparation of molybdenum powder, particularly relates to a method for making molybdenum powder special molybdenum welding wire.

背景技术 Background technique

[0002]钼是一种难熔金属,具有较高的高温强度、良好的导电导热性、热膨胀系数与玻璃相似、被广泛用于制造螺旋灯丝的芯线、引线、挂钩、线切割丝,在电子管中用作做栅极和阳极支撑材料,在超大型集成电路中钼用作金属氧化物半导体栅极和各类电极、靶材等,但钼及钼合金熔点高、工件焊接难度大。 [0002] Molybdenum is a refractory metal having a high temperature strength, good electrical and thermal conductivity, coefficient of thermal expansion similar to the glass, it is widely used in the manufacture of the incandescent filament wire, wire, hook, wire cutting wire, in tubes for use as support materials do grid and anode, as in VLSI molybdenum and various metal oxide semiconductor gate electrode, like the target, but the high melting point of molybdenum and molybdenum alloys, large parts difficult to weld.

[0003]目前常规的钼粉生产企业采用的原料为钼酸铵或高纯三氧化钼进行两段或三段氢气还原,将还原钼粉采用一定目数的筛网进行筛分得到最终产品,这种常规方法生产出来的钼粉在制作钼制品、钼丝等产品时表现出了优良的品质,但是在制作钼焊条时由于其颗粒偏细或颗粒均匀度差,导致生产焊条时流动性能不佳、所制作的焊条性能难以均匀,在实际焊接过程中易出现焊道不均匀、气泡等现象,达不到焊接质量。 [0003] The current conventional feed producers use molybdenum powder is high-purity molybdenum trioxide or ammonium molybdate for two or three-stage hydrogen reduction, to restore the molybdenum powder using a certain number of mesh sieved to obtain a final product, such conventional methods of molybdenum powder produced exhibits excellent product quality in the production of molybdenum, molybdenum wire and other products, but in the production of a molybdenum electrode bias due to its fine particle or particles uniformly poor, resulting in the production of electrodes does not flow properties Jia, the prepared electrode performance is difficult to uniformly, unevenness prone bead actual welding process, the phenomenon of air bubbles, reach the welding quality.

发明内容 SUMMARY

[0004] 本发明的目的是提供一种用于制作钼焊条的专用钼粉制备方法,解决了现有方法得到的钼粉制作的焊条,在实际焊接过程中出现焊道不均匀、气泡等问题。 [0004] The object of the present invention is to provide a method for making molybdenum powder dedicated molybdenum welding wire, the method solves the conventional electrodes made of molybdenum powder obtained, unevenness occurs in the actual bead welding process, bubbles in the .

[0005] 本发明所采用的技术方案是,一种用于制作钼焊条的专用钼粉制备方法,将工业二氧化钼和高纯三氧化钼采用固-固掺杂混合均匀,得到M〇02-Mo〇3混合粉末;然后Mo〇2-Mo〇3混合粉末经过高温还原生成钼粉,将钼粉振动打散后先进行200目筛分,然后对200目筛上物进行80目筛分,即得到制作钼焊条的专用钼粉。 [0005] The technical proposal of the present invention, a method of preparing molybdenum powder special electrodes for the production of molybdenum, molybdenum dioxide and the industrial use of high-purity molybdenum trioxide Solid - Solid doped uniformly mixed to give M〇02 -Mo〇3 mixed powder; Mo〇3 then Mo〇2-mixed powder of molybdenum powder generated high temperature reduction, first at 200 mesh sieve after the vibration molybdenum powder break up, and then on a 200 mesh screen was sieved 80 mesh , i.e., to obtain special electrodes made of molybdenum molybdenum powder.

[0006] 本发明的特点还在于, [0006] The features of the present invention is,

[0007] 高纯三氧化钼与二氧化钼的质量比为1:1.5〜1.86。 [0007] The high-purity molybdenum trioxide and molybdenum dioxide mass ratio of 1: 1.5~1.86.

[0008]固-固掺杂混合均匀是将二氧化钼和三氧化钼在双锥混料机中混料4〜5h。 [0008] Solid - Solid dopant is mixed molybdenum dioxide and molybdenum trioxide 4~5h mixing in a double cone blender.

[0009] 高温还原是将Mo02-Mo03混合粉末按照3.0〜4 • 5cm的装舟厚度进行装舟,采用露点为-45°C〜-2(TC氢气逆向流过Mo〇2-Mo〇3混合粉末,高温还原阶段采取阶梯式升温方式,按照第一区保温2〜2 • 5h,还原温度为800°C〜%(TC ;第二区保温2h,还原温度为92(TC〜960 °C ;第三区保温2〜2 • 5h,还原温度为%0°C〜"5°C ;第四区保温2 • 5〜汕,还原温度为98(TC 〜1080。。。 [0009] The high temperature reduction is Mo02-Mo03 mixed powder loaded boat boat according to 3.0~4 • means 5cm thickness, using a dew point of -45 ° C~-2 (TC reverse hydrogen flow through the mixing Mo〇2-Mo〇3 powder, high temperature reduction stages take stepwise heating mode, heat 2~2 • 5h according to the first region, the reduction temperature of 800 ° C~% (TC; second region incubated 2h, the reduction temperature is 92 (TC~960 ° C; third insulation region 2~2 • 5h, temperature reduction% 0 ° C~ "5 ° C; fourth zone incubated 2 • 5~ Shan, reduction temperature 98 (TC ~1080 ...

[0010] 本发明的有益效果是, [0010] Advantageous effects of the present invention is

[0011] (1)本方法对设备没有新的要求,不需要对传统生产线增加或改变任何部分,仅通过工艺调整就可实现该专用钼粉的生产、适合工业化生产。 [0011] (1) This method requires no new equipment is not required for traditional production lines increases or change any part of the dedicated molybdenum powder can be achieved only by the production process adjustment, suitable for industrial production.

[0012] (2)本方法简单易行,不需要生产该规格钼粉的人员进行太多的知识更新、培训, 具备传统钼粉生产技术的人员很快就能够掌握在这种生产方法。 [0012] (2) This method is simple and does not require the specification of molybdenum powder production staff were too much to update their knowledge, training, molybdenum powder production techniques with the traditional personnel will soon be able to grasp in this production method.

[0013] (3)本方法生产的钼粉除去了粒度偏细及偏大部分,生产的钼粉颗粒相对均匀,一致性及流动性稳定良好,满足焊条用粉的技术要求。 [0013] (3) The method for producing the molybdenum powder to remove fine particle size and partial Partial most produce relatively uniform particles of molybdenum powder, good flowability and consistency stability, the electrode powders meet the technical requirements.

[00M] ⑷本方法生产的焊条专用钼粉成品率较高,可达到70%。 [00M] produced by the process of the present high ⑷ special electrodes molybdenum powder yield may reach 70%.

附图说明 BRIEF DESCRIPTION

[0015] 图1是本发明方法得到的钼粉的电镜扫描图。 [0015] FIG. 1 is a scanning electron microscope of FIG molybdenum powder obtained by the method of the present invention.

具体实施方式 detailed description

[0016] 下面结合附图和具体实施方式对本发明进行详细说明。 [0016] The present invention will be described in detail in conjunction with accompanying drawings and specific embodiments.

[0017] 本发明用于制作钼焊条的专用钼粉制备方法,提供一种工艺简单、成品率高、适合工业化生产的钼焊条专用钼粉的生产技术,该方法是采用三氧化钼和工业二氧化钼混合物为原料经一次高温还原,再经两道筛分生产出-80目〜+200目、颗粒均匀、流动性能好的制作钼焊条专用钼粉。 [0017] The present invention is a method for preparing the molybdenum electrodes dedicated molybdenum powder produced is provided a simple process, high yield, suitable for industrial production of molybdenum powder molybdenum electrodes special production technique, which method is the use of molybdenum trioxide and industrial two molybdenum oxide mixture was reduced to a high temperature material, and then sieved by two to produce -80 mesh to + 200 mesh, uniform particles, good flow properties making special molybdenum powder molybdenum electrodes.

[0018] 具体制备步骤如下: [0018] The specific preparation steps are as follows:

[0019] 步骤1,将高纯三氧化钼和工业二氧化钼按质量比为1:1.5〜1.86在双锥混料机中混料4〜5h,得到Mo02-Mo03混合粉末;其中工业二氧化钼费氏粒度为3 • 5〜10.2wn,松装密度0.95〜1.50g/cm3; [0019] Step 1, the high-purity molybdenum trioxide and molybdenum dioxide industrial mass ratio of 1: 1.5~1.86 mixing in a double cone blender 4~5h, Mo02-Mo03 obtain a mixed powder; wherein Dioxide molybdenum Fisher grain size of 3 • 5~10.2wn, bulk density 0.95~1.50g / cm3;

[0020] 步骤2,将步骤1得到的M〇02-M〇03混合粉末按照3.0〜4.5cm的装舟厚度进行装舟, 采用露点为_45°C〜-20°C氢气逆向流过Mo02-Mo03混合粉末,高温还原阶段采取阶梯式升温方式,按照第一区保温2〜2 • 5h,还原温度为800°C〜950°C ;第二区保温2h,还原温度为920 °C〜960°C ;第三区保温2〜2 • 5h,还原温度为950°C〜995。 [0020] Step 2, Step 1 was mixed powder M〇03 M〇02-boat loading apparatus in accordance with the thickness 3.0~4.5cm boat, using a dew point of _45 ° C~-20 ° C the reverse hydrogen flow through Mo02 -Mo03 mixed powder, high temperature reduction stages take stepwise heating mode, heat 2~2 • 5h according to the first region, the reduction temperature is 800 ° C~950 ° C; a second insulation region 2h, the reduction temperature is 920 ° C~960 ° C; third zone incubated 2~2 • 5h, the reduction temperature is 950 ° C~995. (:;第四区保温2.5〜3h,还原温度为980°C〜1080°C,得到钼粉; (:; Fourth region insulation 2.5~3h, reduction temperature is 980 ° C~1080 ° C, to obtain a molybdenum powder;

[0021]步骤3,将步骤2得到的钼粉振动打散后先进行200目筛分,然后对200目筛上物进行80目筛分,即得到制作钼焊条的专用钼粉。 [0021] Step 3, the vibration molybdenum powder obtained in step 2 performed after the first break 200 mesh sieve, and then on a 200 mesh screen was 80 mesh sieve, to obtain special electrodes made of molybdenum molybdenum powder.

[0022]图1是本发明制备方法得到的钼焊条专用钼粉的电镜扫描图,从图1中可以看出, 本发明方法制备的钼粉的颗粒基本为独立的单颗粒分布,颗粒形貌分布较为均匀;在粉末流动性实验中,发现该钼粉具有较好的流动性。 [0022] FIG. 1 is a molybdenum powder molybdenum electrodes dedicated SEM FIG production method of the present invention is obtained, it can be seen from Figure 1, the molybdenum powder particles prepared by the process of the present invention substantially independent single particle distribution, particle shape more uniform distribution; powder flowability test, it was found that molybdenum powder having good flowability.

[0023] 本发明方法中将高纯三氧化钼和工业二氧化钼按质量比为1:1.5〜1.86混合再经过高温还原炉高温还原、筛分得到最终产品,因三氧化钼具有较低的熔融温度,在795°C时均匀分布的三氧化钼会熔融对其周围的二氧化钼进行包裹,这种包裹状态的三氧化钼与二氧化钼混合物经还原后得到均匀团聚态分布的钼粉,但因为三氧化钼与二氧化钼混合物的之间又存在难熔的二氧化钼分割晶界,所以还原生成的团聚态钼粉,呈现以多个独立二氧化钼为核的团聚态钼粉,各个团聚态钼粉界面之间团聚力量较弱,该钼粉经过一定的振动、 拍击,界面之间会分裂、解聚,形成较大颗粒独立钼粉,再对该钼粉再进行过筛,筛次序为先过200目筛网,对200目筛上物再次过80目筛网,得到的钼粉颗粒相对均匀、完整、流动性好, 且按此方法生产的焊接用钼粉品质高、质量稳 [0023] The method of the present invention, in the high purity molybdenum trioxide and molybdenum dioxide industrial mass ratio of 1: 1.5~1.86 mixing and then high-temperature reducing furnace through high temperature reduction, sieved to give the final product, due to having a low molybdenum trioxide melt temperature, molybdenum trioxide is melted at 795 ° C wrapped uniformly distributed around its molybdenum dioxide, molybdenum trioxide after this wrapped state, molybdenum dioxide and molybdenum powder mixture is reduced to give a uniform distribution of the agglomerated state but because of the presence of molybdenum trioxide and molybdenum dioxide and the mixture between refractory grain boundary divided molybdenum dioxide, thus reducing the generated agglomerated state molybdenum powder, molybdenum dioxide presented with a plurality of individual agglomerated state nuclear molybdenum powder , agglomerated state between the respective interfaces is weak agglomeration force molybdenum powder, molybdenum powder through the constant vibration, slap, will split between the interface, depolymerization, forming larger particles separate molybdenum powder, molybdenum powder and then again subjected to the sieve, the order of the first pass through the 200 mesh screen of 200 mesh was again through 80 mesh screen, the resulting molybdenum powder particles are relatively uniform, complete, good fluidity, and this method of producing molybdenum powder welding quality high, stable quality ,成品率可达到70%左右。 Yield can reach 70%.

[0024]本发明之所以选择-80目〜+200目的钼粉,因焊条专用钼粉对钼粉的整体颗粒要求较为严格,要求均匀、流动性好。 [0024] The present invention was chosen + -80 mesh to 200 mesh molybdenum powder, molybdenum powder by special welding molybdenum powder particles overall more stringent requirements, requirements uniform, good fluidity. 本发明在高温还原阶段,采用了三氧化钼熔融包裹二氧化钼的形式,使钼粉颗粒有一定的团聚,增大了钼粉颗粒尺寸,该钼粉的颗粒尺寸基本上都在200目筛网网孔直径以上,80目筛网孔径以下,200目先除去了粒度偏细的部分,80目筛分除去了粒度偏大的部分,产品取200目筛上,8〇目筛下,该阶段钼粉粒度基本均勾、一致性较强且流动性好。 In the present invention, high temperature reduction phase, takes the form of molybdenum trioxide, molybdenum dioxide melt inclusions of the molybdenum powder particles have a certain agglomeration, increasing the molybdenum powder particle size, particle size of the molybdenum powder are substantially 200 mesh mesh diameter than mesh, 80 mesh sieve aperture or less, the particle size of 200 mesh to remove partial small portions, particle size 80 mesh sieve to remove the larger part of the products take a 200 mesh screen, the mesh 8〇 this stage molybdenum powder of essentially uniform particle size of the hook, strong consistency and fluidity.

[0025]采用本发明制备方法制备的钼粉制作焊条时,焊条质地均匀,在焊接时避免了传统钼粉制作的焊条在焊接时焊道不均匀,气泡等现象。 [0025] When using the electrode made of molybdenum powder produced by the production method of the present invention, the electrode uniform texture, molybdenum powder to avoid the traditional making uneven bead electrode welding, welding and so bubbles.

[0026]实施例1 [0026] Example 1

[0027]步骤1,将高纯三氧化钼和工业二氧化钼按质量比为1:1 • 86在双锥混料机中混料4h,得到Mo〇2_Mo〇3混合粉末;其中工业二氧化钼平均费氏粒度为6 • 8um,松装密度1. 〇g/cm3; [0028] 步骤2,将步骤1得到的Mo〇2_Mo〇3混合粉末按照3 • 5cm的装舟厚度进行装舟,采用露点为-45 °C氢气逆向流过M〇〇2_M〇〇3混合粉末,高温还原阶段采取阶梯式升温方式,按照第一区保温2h,还原温度为90(TC;第二区保温2h,还原温度为920°C ;第三区保温2.5h,还原温度为950°C;第四区保温2.5h,还原温度为l〇〇(TC,得到钼粉; [0027] Step 1, the high-purity molybdenum trioxide and molybdenum dioxide industrial mass ratio of 1: 1 • 86 mixing in a double cone blender 4h, to give a mixed powder Mo〇2_Mo〇3; wherein Dioxide the average particle size of molybdenum Fisher 6 • 8um, bulk density 1. 〇g / cm3; [0028] step 2, step 1 Mo〇2_Mo〇3 obtained mixed powder loaded boat boat according to a thickness of 5cm 3 • means of a dew point of -45 ° C using a reverse hydrogen flow through M〇〇2_M〇〇3 mixed powder, a high temperature heating reduction phase stepwise manner taken for 2h according to the first zone, the reduction temperature is 90 (TC; 2h a second insulation region, The reduction temperature is 920 ° C; the third insulation region 2.5h, the reduction temperature is 950 ° C; fourth zone incubated 2.5h, l〇〇 reduction temperature (TC, molybdenum powder obtained;

[0029]步骤3,将步骤2得到的钼粉振动打散后先进行200目筛分,然后对2〇〇目筛上物进行80目筛分,即得到制作钼焊条的专用钼粉。 [0029] Step 3, the vibration molybdenum powder obtained in step 2 performed after the first break 200 mesh sieve, and then was subjected to the 2〇〇 mesh 80 mesh sieve, to obtain special electrodes made of molybdenum molybdenum powder.

[0030] 实施例2 [0030] Example 2

[0031 ]步骤1,将高纯三氧化钼和工业二氧化钼按质量比为1:1.5在双锥混料机中混料5h,得到Mo〇2-M0O3混合粉末;其中工业二氧化钼平均费氏粒度为3.5um,松装密度1.20g/ cm3; [0031] Step 1, the high-purity molybdenum trioxide and molybdenum dioxide industrial mass ratio of 1: 1.5 5h mixing in a double cone mixer to obtain a mixed powder Mo〇2-M0O3; wherein molybdenum dioxide Industrial Average Fisher particle size of 3.5um, bulk density 1.20g / cm3;

[0032]步骤2,将步骤1得到的M〇〇2_Mo〇3混合粉末按照4.5cm的装舟厚度进行装舟,采用露点为_3〇°C氢气逆向流过Mo〇2-Mo〇3混合粉末,高温还原阶段采取阶梯式升温方式,按照第一区保温2 • 5h,还原温度为800°C ;第二区保温2h,还原温度为940°C ;第三g保温2h,还原温度为980°C ;第四区保温3h,还原温度为1 〇80°C,得到钼粉; [0032] Step 2, Step 1 was mixed powder M〇〇2_Mo〇3 means mounted boat boat according to the thickness of 4.5cm, _3〇 ° C using a dew point of the hydrogen gas flowing through the reverse-Mo〇3 mixed Mo〇2 powder, high temperature reduction stages take stepwise heating mode, according to a first insulation region 2 • 5h, the reduction temperature is 800 ° C; a second insulation region 2h, the reduction temperature is 940 ° C; g third insulation 2h, the reduction temperature is 980 ° C; fourth zone incubated 3h, the reduction temperature is 1 〇80 ° C, to obtain a molybdenum powder;

[0033]步骤3,将步骤2得到的钼粉振动打散后先进行200目筛分,然后对2〇〇目筛上物进行80目筛分,即得到制作钼焊条的专用钼粉。 [0033] Step 3, the vibration molybdenum powder obtained in step 2 performed after the first break 200 mesh sieve, and then was subjected to the 2〇〇 mesh 80 mesh sieve, to obtain special electrodes made of molybdenum molybdenum powder.

[0034] 实施例3 [0034] Example 3

[0035]步骤1,将高纯三氧化钼和工业二氧化钼按质量比为1:1.67在双锥混料机中混料4 • 5h,得到Mo〇2_Mo〇3混合粉末;其中工业二氧化钼平均费氏粒度为10 • 2um,松装密度1 • 50g/ cm3; [0035] Step 1, the high-purity molybdenum trioxide and molybdenum dioxide industrial mass ratio of 1: 1.67 in the mixing in a double cone blender 4 • 5h, to obtain a mixed powder Mo〇2_Mo〇3; wherein Dioxide Fisher molybdenum average particle size of 10 • 2um, bulk density 1 • 50g / cm3;

[0036] 步骤2,将步骤1得到的M〇〇2_M〇〇3混合粉末按照3 • Ocm的装舟厚度进行装舟,采用露点为-20°C氢气逆向流过Mo〇2-Mo〇3混合粉末,高温还原阶段采取阶梯式升温方式,按照第一区保温2.2h,还原温度为95(TC ;第二区保温2h,还原温度为9e〇°C ;第三区保温2.3h,还原温度为995°C;第四区保温2.8h,还原温度为l〇2〇°C,得到钼粉; [0036] Step 2, Step 1 was mixed powder M〇〇2_M〇〇3 means mounted boat boat according to the thickness of 3 • Ocm, using a dew point of -20 ° C up reverse hydrogen flow through Mo〇2-Mo〇3 a mixed powder, high temperature reduction stages take stepwise heating mode, in accordance with a first insulation region 2.2h, reduction temperature 95 (TC; second region incubated 2h, reduction temperature 9e〇 ° C; 2.3H third insulation region, reduction temperature to 995 ° C; fourth zone incubated 2.8h, reduction temperature l〇2〇 ° C, to obtain a molybdenum powder;

[0037]步骤3,将步骤2得到的钼粉振动打散后先进行2〇〇目筛分,然后对200目筛上物进行80目筛分,即得到制作钼焊条的专用钼粉。 [0037] Step 3, the vibration molybdenum powder obtained in step 2 performed after the first break 2〇〇 mesh sieve, and then on a 200 mesh screen was 80 mesh sieve, to obtain special electrodes made of molybdenum molybdenum powder.

[0038]实施例4 [0038] Example 4

[0039]步骤i,将高纯三氧化钼和工业二氧化钼按质量比为1:1.75在双锥混料机中混料4 • 5h,得到Mo02-Mo03混合粉末;其中工业二氧化钼平均费氏粒度为8 • 2_,松装密度〇. 95g/ cm3; [0039] Step i, industrial high-purity molybdenum trioxide and molybdenum dioxide mass ratio of 1: 1.75 in the mixing in a double cone blender 4 • 5h, to obtain a mixed powder Mo02-Mo03; wherein molybdenum dioxide Industrial Average Fisher particle size of 8 • 2_, bulk density square 95g / cm3.;

[0040] 步骤2,将步骤!得到的Mo02-Mo〇3混合粉末按照4 _ Ocm的装舟厚度进行装舟,采用露点为-40。 [0040] Step 2, Step! Mo〇3 Mo02-obtained mixed powder loading means boat boat according to the thickness of 4 _ Ocm, using a dew point of -40. (:氢气逆向流过M0O2-M0O3混合粉末,高温还原阶段采取阶梯式升温方式,按照第一区保温2.3h,还原温度为920°C ;第二区保温2h,还原温度为950 °C ;第三区保温2.2h,还原温度为960°C ;第四区保温2.5h,还原温度为980°C,得到钼粉; (: Reverse hydrogen flow through M0O2-M0O3 mixed powder, high temperature reduction stages take stepwise heating mode, in accordance with a first insulation region 2.3h, the reduction temperature is 920 ° C; a second insulation region 2h, the reduction temperature is 950 ° C; first three areas insulation 2.2h, the reduction temperature is 960 ° C; fourth zone incubated 2.5h, the reduction temperature is 980 ° C, to obtain a molybdenum powder;

[0041]步骤3,将步骤2得到的钼粉振动打散后先进行200目筛分,然后对200目筛上物进行80目筛分,即得到制作钼焊条的专用钼粉。 [0041] Step 3, the vibration molybdenum powder obtained in step 2 performed after the first break 200 mesh sieve, and then on a 200 mesh screen was 80 mesh sieve, to obtain special electrodes made of molybdenum molybdenum powder.

Claims (3)

  1. 1. 一种用于制作钼焊条的专用钼粉制备方法,其特征在于,将工业二氧化钼和三氧化钼采用固-固掺杂混合均勾,得到M〇〇2_Mo〇3混合粉末;然后M〇02-Mo〇3混合粉末经过高温还原生成钼粉,将钼粉振动打散后先进行2〇〇目筛分,然后对2〇〇目筛上物进行80目筛分,即得到制作钼焊条的专用钼粉; 所述高温还原是将Mo〇2_Mo03混合粉末按照3.0〜4 • 5cm的装舟厚度进行装舟,采用露点为-45°C〜_20°C氢气逆向流过Mo〇2_Mo〇3混合粉末,高温还原阶段采取阶梯式升温方式,按照第一区保温2〜2 •沾,还原温度为800°C〜%0°C ;第二区保温汍,还原温度为920°C〜960 。 1. A method for preparing special molybdenum electrodes made of molybdenum powder, characterized in that the industrial use of molybdenum trioxide and molybdenum dioxide solid - solid were blended and hook, to give a mixed powder M〇〇2_Mo〇3; and M〇02-Mo〇3 reduced to produce a mixed powder of molybdenum powder at high temperatures, to be 2〇〇 mesh sieve after the vibration molybdenum powder break up, and then the mesh was 2〇〇 80 mesh sieve, to obtain production molybdenum electrodes dedicated molybdenum powder; high-temperature reducing said mixed powder is loaded Mo〇2_Mo03 boat boat according to 3.0~4 • means 5cm thickness, using a dew point of -45 ° C~_20 ° C reverse hydrogen flow through Mo〇2_Mo 〇3 mixed powder, high temperature reduction stages take stepwise heating mode, in accordance with a first insulation region 2~2 • dip, reduction temperature of 800 ° C~% 0 ° C; a second insulation region Wan, reduction temperature of 920 ° C~ 960. (:;第三区保温2〜2.5h,还原温度为950°C〜"5°C ;第四区保温2 • 5〜3h,还原温度为98(TC 〜1080。。。 (:; Third zone insulation 2~2.5h, reduction temperature of 950 ° C~ "5 ° C; fourth zone incubated 2 • 5~3h, reduction temperature 98 (TC ~1080 ...
  2. 2. 根据权利要求1所述的用于制作钼焊条的专用钼粉制备方法,其特征在于,所述三氧化钼与二氧化钼的质量比为1:1.5〜1.86。 The specific method for preparing the molybdenum electrode made of molybdenum powder according to claim 1, wherein said molybdenum trioxide and molybdenum dioxide mass ratio of 1: 1.5~1.86.
  3. 3. 根据权利要求1或2所述的用于制作钼焊条的专用钼粉制备方法,其特征在于,固-固掺杂混合均匀是将二氧化钼和三氧化钼在双锥混料机中混料4〜5h。 The specific method of preparation of molybdenum powder prepared for the molybdenum electrodes to claim 1 or claim 2, characterized in that the solid - solid is uniformly mixed doped molybdenum dioxide and molybdenum trioxide in a double cone blender mixing 4~5h.
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CN101224500A (en) * 2007-12-17 2008-07-23 金堆城钼业股份有限公司 Super particle size molybdenum powder preparing method
CN102601385A (en) * 2012-04-18 2012-07-25 金堆城钼业股份有限公司 Preparation method of molybdenum powder
CN103203455A (en) * 2013-04-12 2013-07-17 金堆城钼业股份有限公司 Method for manufacturing molybdenum powder
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