技术领域technical field
本发明涉及制备球形氮化钛粉末的方法及设备，具体涉及利用射频等离子体粉末生产设备制备球形氮化钛粉末的方法。The invention relates to a method and equipment for preparing spherical titanium nitride powder, in particular to a method for preparing spherical titanium nitride powder by using radio frequency plasma powder production equipment.
背景技术Background technique
金属化合物TiN具有许多优良的物理及化学性能，它抗腐蚀性、抗磨损性及抗氧化性都非常优良，具有较高的熔点(3205℃)和硬度1990(×9.8N/mm2)。TiN沉积在首饰和灯具上既可以达到美观效果，又能增强耐磨性能，是代替目前广泛使用的WC的潜在材料，可以大大降低材料应用的成本。TiN化合物具有较高的生物兼容性，在临床医学和口腔医学方面也具有很高的应用价值。此外TiN也可用作制造坩埚、切削刀具、添加剂等。TiN粉末的应用广度和深度与它所拥有的优异性能极不相称，有待人们研究开发，可以预示，氮化钛粉末将会成为世纪新材料。The metal compound TiN has many excellent physical and chemical properties. It has excellent corrosion resistance, wear resistance and oxidation resistance, and has a high melting point (3205°C) and a hardness of 1990 (×9.8N/mm2 ). TiN deposition on jewelry and lamps can not only achieve aesthetic effect, but also enhance wear resistance. It is a potential material to replace WC, which is widely used at present, and can greatly reduce the cost of material application. TiN compounds have high biocompatibility, and also have high application value in clinical medicine and stomatology. In addition, TiN can also be used to make crucibles, cutting tools, additives, etc. The breadth and depth of application of TiN powder are not commensurate with its excellent properties. It needs to be researched and developed by people. It can be predicted that titanium nitride powder will become a new material of the century.
随着对TiN研究的不断深入，制备TiN粉末的方法也越来越多。传统的TiN粉末制备方法，如：金属钛粉氮化法、二氧化钛碳热还原氮化法、气相法等得到的TiN粉末形状不规则，流动性较差，使用性能大打折扣，而且氮化率不高，氮化时间较长，粒径范围较宽，能源消耗大。到目前为止，还没有行之有效而且含盖以上问题的解决办法。With the continuous deepening of research on TiN, there are more and more methods for preparing TiN powder. Traditional TiN powder preparation methods, such as: metal titanium powder nitriding method, titanium dioxide carbothermal reduction nitriding method, gas phase method, etc., obtain TiN powder with irregular shape, poor fluidity, greatly reduced performance, and low nitriding rate. High, the nitriding time is longer, the particle size range is wider, and the energy consumption is large. So far, there is no effective solution that covers the above problems.
与非球形的氮化钛粉末相比，球形氮化钛的机械性能在各个方向都是一样的，在粉末冶金和3D打印中更容易获得性能优异的产品。因此，急需一种制备工艺简单，球化率高球形氮化钛的制备方法。Compared with non-spherical titanium nitride powder, the mechanical properties of spherical titanium nitride are the same in all directions, and it is easier to obtain products with excellent performance in powder metallurgy and 3D printing. Therefore, there is an urgent need for a method for preparing spherical titanium nitride with simple preparation process and high spheroidization rate.
专利200410072553.4公开了一种反应等离子喷涂纳米晶氮化钛粉末的方法，采用等离子喷枪来进行喷涂，具体包括的主要步骤是：钛粉装入送粉器，送入混合离子气体、向反应室中通氮气，送钛粉粉末进入焰流，向盛水的容器中喷涂和收集，采用该方法，能够得到直径为30～100nm的氮化钛粉末颗粒，但是，该方法采用等离子喷枪来制备氮化钛粉末，送钛粉粉末进入焰流，向盛水的容器中喷涂和收集过程中，其能量损失大。且得到的氮化钛球形度不好，球化率需要进一步的提高。Patent 200410072553.4 discloses a method for reactive plasma spraying nanocrystalline titanium nitride powder, using a plasma spray gun for spraying, specifically including the main steps: titanium powder into the powder feeder, into the mixed ion gas, into the reaction chamber Through nitrogen, titanium powder is sent into the flame flow, sprayed and collected in a container containing water. Using this method, titanium nitride powder particles with a diameter of 30-100 nm can be obtained. However, this method uses a plasma spray gun to prepare nitrided particles. Titanium powder, sending titanium powder into the flame flow, spraying and collecting in the water container, the energy loss is large. Moreover, the sphericity of the obtained titanium nitride is not good, and the spheroidization rate needs to be further improved.
发明内容Contents of the invention
针对以上缺陷，本发明解决的技术问题是提供一种制备工艺简单，球化率高的制备球形氮化钛粉末的方法。In view of the above defects, the technical problem to be solved by the present invention is to provide a method for preparing spherical titanium nitride powder with simple preparation process and high spheroidization rate.
本发明制备球形氮化钛粉末的方法，采用射频等离子体设备制备得到，具体包括如下步骤：The method for preparing spherical titanium nitride powder of the present invention is obtained by using radio frequency plasma equipment, and specifically includes the following steps:
a、起弧：以氩气为电离气体起弧，同时将氮气从射频等离子体设备的保护气体入口处通入；控制射频等离子设备的工作电压为5～15kV，功率为30～200kW，其中，电离气体流量为1～10m3/h，保护气体入口处通入的氮气流量为1～10m3/h；a. Arcing: Argon is used as the ionized gas to start the arc, and nitrogen is introduced from the protective gas inlet of the radio frequency plasma equipment at the same time; the operating voltage of the radio frequency plasma equipment is controlled to be 5-15kV, and the power is 30-200kW, among which, The flow rate of ionized gas is 1~10m3 /h, and the flow rate of nitrogen gas at the inlet of protective gas is 1~10m3 /h;
b、送料：待弧稳定后，由送料装置送入钛粉，得到球形氮化钛。b. Feeding: After the arc is stabilized, titanium powder is fed by the feeding device to obtain spherical titanium nitride.
优选的，a步骤中，待弧稳定后，将电离气体变为氮气。Preferably, in step a, after the arc is stabilized, the ionized gas is changed to nitrogen.
作为优选方案，电离气体的流量为3～4m3/h，保护气体入口处通入的氮气流量为3～6m3/h。As a preferred solution, the flow rate of the ionized gas is 3-4 m3 /h, and the flow rate of nitrogen gas at the inlet of the protective gas is 3-6 m3 /h.
优选的，b步骤中，钛粉的粒径为1～150μm。Preferably, in step b, the particle size of the titanium powder is 1-150 μm.
优选的，所述钛粉采用振动进料，其振幅为10～80％。Preferably, the titanium powder is fed by vibration with an amplitude of 10-80%.
本发明解决的第二个技术问题是提供一种制备球形氮化钛粉末的设备。The second technical problem solved by the present invention is to provide a device for preparing spherical titanium nitride powder.
本发明制备球形氮化钛粉末的设备，包括雾化仓(2)、与雾化仓(2)连接的等离子炬(1)、向等离子炬(1)送料的送料装置(3)、气粉分离装置(8)、与气粉分离装置(8)连接的抽气装置(9)和收粉仓二(7)，其特征在于：所述雾化仓(2)底部连接有收粉仓一(5)，所述雾化仓(2)仓壁连接有排气管(10)，所述排气管(10)与气粉分离装置(8)连接；所述收粉仓一(5)和收粉仓二(7)均设有加热装置。The equipment for preparing spherical titanium nitride powder of the present invention comprises an atomization chamber (2), a plasma torch (1) connected to the atomization chamber (2), a feeding device (3) for feeding the plasma torch (1), a gas powder The separation device (8), the air extraction device (9) connected to the gas-powder separation device (8) and the second powder collection bin (7), are characterized in that: the bottom of the atomization bin (2) is connected with the first powder collection bin (5), the wall of the atomization chamber (2) is connected with an exhaust pipe (10), and the exhaust pipe (10) is connected with the gas powder separation device (8); the powder collection chamber one (5) And the powder collecting bin two (7) are all provided with heating device.
优选的，所述加热装置为电热丝，所述收粉仓一(5)和收粉仓二(7)壳体均为内外双层结构，所述加热丝设置在内外壳体之间。Preferably, the heating device is an electric heating wire, and the housings of the first powder collecting bin (5) and the second powder collecting bin (7) are both inner and outer double-layer structures, and the heating wire is arranged between the inner and outer housings.
优选的，所述排气管(10)呈倒V型。Preferably, the exhaust pipe (10) is in an inverted V shape.
优选的，所述等离子炬(1)为高频等离子炬。Preferably, the plasma torch (1) is a high-frequency plasma torch.
优选的，所述高频等离子炬包括配气座(17)、送料管(13)、中管(14)和放电管(15)；所述配气座(17)设有电离气体入口(12)和保护气体入口(11)，所述送料管(13)、中管(14)和放电管(15)依次由内到外同轴安装在配气座(17)中心，所述送料管(13)贯穿配气座(17)，所述放电管(15)外设有电感线圈(16)，所述中管(14)的腔体为电离气体通道，所述放电管(15)与中管(14)之间的腔体为保护气体通道，所述电离气体入口(12)与电离气体通道相通；所述保护气体入口(11)与保护气体通道相通；所述送料管(13)与送料装置(3)连接。Preferably, the high-frequency plasma torch includes a gas distribution seat (17), a feeding pipe (13), a middle pipe (14) and a discharge tube (15); the gas distribution seat (17) is provided with an ionized gas inlet (12 ) and the protective gas inlet (11), the feed pipe (13), the middle pipe (14) and the discharge tube (15) are coaxially installed in the center of the gas distribution seat (17) from inside to outside in turn, and the feed pipe ( 13) Through the gas distribution seat (17), the discharge tube (15) is provided with an inductance coil (16), the cavity of the middle tube (14) is an ionized gas channel, and the discharge tube (15) and the middle The cavity between the tubes (14) is a protective gas channel, and the ionized gas inlet (12) communicates with the ionized gas channel; the protective gas inlet (11) communicates with the protective gas channel; the feeding pipe (13) communicates with the ionized gas channel; The feeding device (3) is connected.
与现有技术相比，本发明具有如下有益效果：Compared with the prior art, the present invention has the following beneficial effects:
本发明方法，以钛粉为原料，以氮气为反应气体，一步制备得到氮化钛粉末，其工艺流程短、反应时间极短，大大提高了生产效率，获得的产品无杂质污染，制备工艺简单，对原料要求较低，为实现球形氮化钛粉末的工业化生产奠定了基础。制备得到的球形氮化钛粉末，球化率和氮化率都很高。制备原料不需要大量的破碎，其产物粒径小。The method of the present invention uses titanium powder as a raw material and nitrogen as a reaction gas to prepare titanium nitride powder in one step. The process flow is short and the reaction time is extremely short, the production efficiency is greatly improved, the obtained product is free from impurity pollution, and the preparation process is simple. , has lower requirements on raw materials, and lays the foundation for the industrial production of spherical titanium nitride powder. The prepared spherical titanium nitride powder has high spheroidization rate and nitriding rate. The preparation of raw materials does not require a lot of crushing, and the particle size of the product is small.
本发明的设备，收粉仓一和收粉仓二均设有加热装置，冷却后的未充分反应的球形原料粉进入收粉仓后继续与氮气反应，反应更充分，提高了原料的氮化率。同时，收粉仓一用于收集颗粒稍大的氮化钛粉，收粉仓二用于收集较细的氮化钛粉，从而实现氮化钛粉的粗细分选。等离子炬为高频等离子炬，高频等离子炬中心设有送料管，制备出的球形TiN粉颗粒细，无杂质污染。采用本发明的设备，可大大提高了制备氮化钛粉的效率，制备工艺简单，对原料要求较低，球化率和氮化率都有所提高。In the equipment of the present invention, the first powder collecting bin and the second powder collecting bin are equipped with heating devices, and the cooled spherical raw material powder that has not fully reacted enters the powder collecting bin and continues to react with nitrogen, the reaction is more sufficient, and the nitriding of raw materials is improved. Rate. At the same time, the first powder collection bin is used to collect titanium nitride powder with slightly larger particles, and the second powder collection bin is used to collect finer titanium nitride powder, so as to realize the coarse and fine separation of titanium nitride powder. The plasma torch is a high-frequency plasma torch, and the center of the high-frequency plasma torch is equipped with a feeding tube. The prepared spherical TiN powder has fine particles and no impurity pollution. By adopting the equipment of the invention, the efficiency of preparing titanium nitride powder can be greatly improved, the preparation process is simple, the requirement for raw materials is low, and the spheroidization rate and nitriding rate are both improved.
附图说明Description of drawings
图1是本发明的制备球形氮化钛粉末的设备的结构示意图；Fig. 1 is the structural representation of the equipment of preparing spherical titanium nitride powder of the present invention;
图2是高频等离子炬结构示意图；Fig. 2 is a structural schematic diagram of a high-frequency plasma torch;
图中所示：1.等离子炬，2.雾化仓，3.送料装置，4.蝶阀，5.收粉仓一，7.收粉仓二，8.气粉分离装置，9.抽气装置，10.排气管，11.保护气体入口，12.电离气体入口，13.送料管，14.中管，15.放电管，16.电感线圈，17.配气座，18.等离子射流，21.冷却气体口，51.电热丝。As shown in the figure: 1. Plasma torch, 2. Atomization chamber, 3. Feeding device, 4. Butterfly valve, 5. Powder collection chamber 1, 7. Powder collection chamber 2, 8. Air powder separation device, 9. Air extraction Device, 10. exhaust pipe, 11. protective gas inlet, 12. ionized gas inlet, 13. feeding pipe, 14. middle pipe, 15. discharge tube, 16. induction coil, 17. gas distribution seat, 18. plasma jet , 21. Cooling gas port, 51. Heating wire.
图3为本发明制备的球形氮化钛粉末的SEM图。Fig. 3 is a SEM image of the spherical titanium nitride powder prepared in the present invention.
图4为本发明制备的球形氮化钛粉末的XRD图。Fig. 4 is an XRD pattern of the spherical titanium nitride powder prepared in the present invention.
具体实施方式Detailed ways
本发明球形氮化钛的制备方法，采用射频等离子体设备制备得到，具体包括如下步骤：The preparation method of spherical titanium nitride of the present invention is prepared by radio frequency plasma equipment, and specifically comprises the following steps:
a、起弧：以氩气为电离气体起弧，同时将氮气从射频等离子体设备的保护气体入口处通入；控制射频等离子设备的工作电压为5～15kV，功率为30～200kW；其中，电离气体流量为1～10m3/h，保护气体入口处通入的氮气流量为1～10m3/h；a. Arcing: Argon is used as the ionized gas to start the arc, and nitrogen is introduced from the protective gas inlet of the radio frequency plasma equipment at the same time; the operating voltage of the radio frequency plasma equipment is controlled to be 5-15kV, and the power is 30-200kW; among them, The flow rate of ionized gas is 1~10m3/h, and the flow rate of nitrogen gas at the inlet of protective gas is 1~10m3/h;
b、送料：待弧稳定后，由送料装置送入钛粉，在等离子体炬中钛粉球化的同时直接氮化，得到半熔态的氮化钛；然后半熔态的氮化钛在表面张力的作用下，冷却凝固成球形。b. Feeding: After the arc is stable, the titanium powder is fed into the titanium powder by the feeding device, and the titanium powder is spheroidized in the plasma torch while being directly nitrided to obtain semi-molten titanium nitride; then the semi-molten titanium nitride is in the Under the action of surface tension, it cools and solidifies into a spherical shape.
射频等离子体粉末球化技术为现有的技术，其原理是在高频电源作用下，惰性气体被电离，形成稳定的高温惰性气体等离子体；而形状不规则的原料经送料装置送入等离子体炬中，在高温等离子体中吸收大量的热，表面迅速熔化，并以极高的速度进入反应器，在惰性气氛下快速冷却，在表面张力的作用，冷却凝固成球形粉末。而本发明通过控制射频等离子体设备的电压、功率以及通入特定种类的气体和特定的气体流量等参数，实现在等离子体炬中钛粉球化的同时直接氮化，得到球形氮化钛。其反应原理为：The radio frequency plasma powder spheroidization technology is an existing technology. The principle is that under the action of a high frequency power supply, the inert gas is ionized to form a stable high temperature inert gas plasma; and the raw materials with irregular shapes are sent into the plasma through the feeding device. In the torch, a large amount of heat is absorbed in the high-temperature plasma, and the surface is rapidly melted, and enters the reactor at a very high speed, and is rapidly cooled in an inert atmosphere. Under the action of surface tension, it is cooled and solidified into a spherical powder. However, the present invention realizes direct nitriding while titanium powder is spheroidized in the plasma torch to obtain spherical titanium nitride by controlling the voltage and power of the radio frequency plasma equipment, and introducing specific types of gas and specific gas flow. Its reaction principle is:
2Ti+N2＝2TiN2Ti+N2 =2TiN
本发明方法，上述反应均在通入氩气和氮气的射频等离子高温场条件下进行。首先，氩气从射频等离子体设备中心通入，即电离气体入口处通入，而氮气从射频等离子体设备边缘通入，即保护气体入口处通入。这样氩气流易于产生等离子流，将钛物料进行高温分解。氮气从射频等离子体粉末生产设备边缘通入可使氮化反应更加完全。该方法获得的氮化钛球化率和氮化率较高，球化和氮化同时进行，大大提高了生产效率。In the method of the present invention, the above reactions are all carried out under the condition of a high-temperature radio frequency plasma field fed with argon and nitrogen. First, the argon gas is introduced from the center of the radio frequency plasma equipment, that is, the ionized gas inlet, and the nitrogen gas is passed from the edge of the radio frequency plasma equipment, that is, the shielding gas inlet. In this way, the argon flow is easy to generate a plasma flow, and the titanium material is pyrolyzed. Nitrogen is introduced from the edge of the RF plasma powder production equipment to make the nitriding reaction more complete. The titanium nitride spheroidization rate and nitriding rate obtained by the method are high, and the spheroidization and nitriding are carried out simultaneously, which greatly improves the production efficiency.
为了提高球化率，优选的，a步骤中，以氩气为电离气体起弧，得到氩弧，待氩弧稳定后，将电离气体变为氮气，此时，将会形成氮气弧。等离子体炬中的氮气电离作为反应热源的同时又作为反应物，与钛粉在高温下反应直接得到球形氮化钛粉末，不仅可节约反应能源消耗，还能提高产品纯度和球化率。In order to improve the spheroidization rate, preferably, in step a, argon is used as the ionized gas to start the arc to obtain an argon arc. After the argon arc is stabilized, the ionized gas is changed to nitrogen. At this time, a nitrogen arc will be formed. Nitrogen ionization in the plasma torch acts as a reaction heat source and as a reactant at the same time, reacting with titanium powder at high temperature to directly obtain spherical titanium nitride powder, which can not only save reaction energy consumption, but also improve product purity and spheroidization rate.
更优选的，电离气体流量为3～4m3/h，保护气体入口处通入的氮气流量为3～4m3/h。More preferably, the flow rate of the ionized gas is 3-4 m3 /h, and the flow rate of the nitrogen gas at the inlet of the protective gas is 3-4 m3 /h.
常用的钛粉的粒径均适用于本发明，优选的，b步骤中，钛粉的粒径为1～150μm。The particle size of the commonly used titanium powder is suitable for the present invention. Preferably, in step b, the particle size of the titanium powder is 1-150 μm.
作为优选方案，所述钛粉采用振动进料，其振幅为10～80％，这样可以使得钛粉的反应更加完全，提高氮化率。As a preferred solution, the titanium powder is fed by vibration with an amplitude of 10-80%, which can make the reaction of the titanium powder more complete and increase the nitriding rate.
一种制备球形TiN粉的设备，如图1所示，包括雾化仓2、与雾化仓2连接的等离子炬1、向等离子炬1送料的送料装置3、气粉分离装置8、与气粉分离装置8连接的抽气装置9和收粉仓二7，所述雾化仓2底部连接有收粉仓一5，所述雾化仓2仓壁连接有排气管10，所述排气管10与气粉分离装置8连接；所述收粉仓一5和收粉仓二7均设有加热装置。A kind of equipment for preparing spherical TiN powder, as shown in Figure 1, comprises atomizing bin 2, plasma torch 1 connected with atomizing bin 2, feeding device 3 for feeding plasma torch 1, gas-powder separation device 8, and gas The air extraction device 9 connected to the powder separation device 8 and the powder collecting bin 2 7, the bottom of the atomizing bin 2 is connected with the powder collecting bin 1 5, the wall of the atomizing bin 2 is connected with an exhaust pipe 10, and the exhaust pipe 10 The air pipe 10 is connected to the gas-powder separation device 8; the first powder collection bin 5 and the second powder collection bin 7 are both equipped with heating devices.
等离子炬1可选直流等离子炬或高频等离子炬等，等离子炬1可为一个或多个。等离子炬1与雾化仓2连接，即等离子炬1可安装在雾化仓2内，也可以是等离子炬1射流口直接连通雾化仓2。气粉分离装置8可以选旋风分离器，布袋除尘器等，优选旋风分离器。抽气装置9可以选气泵、风机等，雾化仓2底部连接有收粉仓一5，用于收集颗粒较大的球形TiN粉。图1中，雾化仓2底部呈锥形设置，收粉仓一5位于雾化仓1下方，以便于粉料的收集。雾化仓2仓壁连接有排气管10，雾化仓2与气粉分离装置8通过排气管10连通，排气管10呈倒V型。排气管10呈倒V型，可防止TiN粉沉积在管道中。设备工作时，原料由送料装置3送入等离子炬1，原料熔融雾化并与氮气反应，从雾化仓冷却气体口21通入冷却氮气快速冷却，制的球形TiN粉。较大TiN粉下沉进入收粉仓一5中，较细的TiN粉经排气管10进入到气粉分离装置8分离后由收粉仓二7收集。通过上述方式，可实现对TiN粉的粗细分选。收粉仓一5和收粉仓二7设有加热装置，通过加热装置加热保持粉仓一5和收粉仓二7温度等于或高于800℃，从而使从雾化仓2球化后冷却的未反应的原料进入收粉仓后，在收料仓中能再次与氮气反应生成TiN，从而提高原料氮化率。加热装置可以为鼓风机，利用鼓风机对保温室5壳体鼓人高温气体加热，也可选电热丝，利用电加热。The plasma torch 1 can be a DC plasma torch or a high-frequency plasma torch, etc., and the plasma torch 1 can be one or more. The plasma torch 1 is connected to the atomization chamber 2, that is, the plasma torch 1 can be installed in the atomization chamber 2, or the jet port of the plasma torch 1 can be directly connected to the atomization chamber 2. The gas-powder separation device 8 can be selected from a cyclone separator, a bag filter, etc., preferably a cyclone separator. The suction device 9 can be an air pump, a blower fan, etc. The bottom of the atomization chamber 2 is connected with a powder collection chamber 15, which is used to collect spherical TiN powder with larger particles. In Fig. 1, the bottom of the atomization chamber 2 is set in a conical shape, and the powder collection chamber 1 5 is located below the atomization chamber 1, so as to facilitate the collection of powder. An exhaust pipe 10 is connected to the chamber wall of the atomization chamber 2, and the atomization chamber 2 communicates with the gas-powder separation device 8 through the exhaust pipe 10, and the exhaust pipe 10 is in an inverted V shape. The exhaust pipe 10 is in an inverted V shape, which can prevent TiN powder from depositing in the pipe. When the equipment is working, the raw material is sent into the plasma torch 1 by the feeding device 3, the raw material is melted and atomized and reacts with nitrogen gas, and the cooling nitrogen gas is introduced from the cooling gas port 21 of the atomization chamber for rapid cooling to produce spherical TiN powder. Larger TiN powder sinks into the powder collection bin one 5, and the finer TiN powder enters the gas powder separation device 8 through the exhaust pipe 10 and is separated by the powder collection bin two 7 for collection. Through the above method, the coarse and fine classification of TiN powder can be realized. Powder collection bin 1 5 and powder collection bin 2 7 are equipped with heating devices, and the temperature of powder collection bin 1 5 and powder collection bin 2 7 is kept equal to or higher than 800°C by heating the heating device, so that the atomization bin 2 is spheroidized and then cooled After the unreacted raw materials enter the powder collection bin, they can react with nitrogen again in the collection bin to form TiN, thereby increasing the nitriding rate of raw materials. The heating device can be a blower, and utilizes the blower to heat the high-temperature gas of the housing of the heat preservation chamber 5, and also selects an electric heating wire, and utilizes electric heating.
采用鼓风机对收粉仓壳体鼓人高温气体加热，会产生大量废气，优选的，加热装置为电热丝51，收粉仓一和收粉仓二壳体均为内外双层结构，加热丝51设置在内外壳体之间。收粉仓壳体为内外双层结构，加热丝51设置在内外壳体之间，可防止收粉仓内的粉末附着在电热丝51上。Using a blower to heat the high-temperature gas in the shell of the powder collection bin will generate a large amount of exhaust gas. Preferably, the heating device is an electric heating wire 51. It is arranged between the inner and outer shells. The shell of the powder collecting bin has an inner and outer double-layer structure, and the heating wire 51 is arranged between the inner and outer shells, which can prevent the powder in the powder collecting bin from adhering to the heating wire 51 .
由于高频等离子炬具有无电极污染、弧区大、温度相对均匀、能提供纯净热源，材料处理快，尤其在高熔点粉末球化方面展现出独特的优势。优选的，等离子炬为高频等离子炬。Due to the high-frequency plasma torch has no electrode pollution, large arc area, relatively uniform temperature, can provide a pure heat source, and can process materials quickly, especially showing unique advantages in the spheroidization of high melting point powder. Preferably, the plasma torch is a high-frequency plasma torch.
如图2所示的一种高频等离子炬结构示意图，图中：高频等离子炬包括配气座17、送料管13、中管14和放电管15；配气座17设有电离气体入口12和保护气体入口11，所述送料管13、中管14和放电管15依次由内到外同轴安装在配气座17中心，送料管13管穿配气座17，放电管15外设有电感线圈16，中管14的腔体为电离气体通道，放电管15与中管14之间的腔体为保护气体通道，电离气体入口12与电离气体通道相通；保护气体入口11与保护气体通道相通；送料管13与送料装置3连接。送料管13设置在高频等离子炬中心，有利于原料送达等离子体弧芯部高温区，利于原料的融洽和球化，也利于原料与氮气反应，提高原料氮化率。通过调节电离气体的进气量，可调节等离子射流的焓值和喷射强度，从而实现不同效果熔融和球化效果。保护气体入口11可通入氮气，在高频等离子炬放电管14管壁形成一层冷气膜，对放电管14进行冷却和防止受热熔融的原料和TiN粘附在放电管14内壁上。A structural schematic diagram of a high-frequency plasma torch as shown in Figure 2, in the figure: the high-frequency plasma torch includes a gas distribution seat 17, a feeding pipe 13, a middle tube 14 and a discharge tube 15; the gas distribution seat 17 is provided with an ionized gas inlet 12 And the protective gas inlet 11, the feed pipe 13, the middle pipe 14 and the discharge tube 15 are coaxially installed in the center of the gas distribution seat 17 from the inside to the outside in turn, the feed pipe 13 passes through the gas distribution seat 17, and the discharge tube 15 is provided with The inductance coil 16, the cavity of the middle tube 14 is an ionized gas channel, the cavity between the discharge tube 15 and the middle tube 14 is a protective gas channel, the ionized gas inlet 12 communicates with the ionized gas channel; the protective gas inlet 11 and the protective gas channel Communication; feeding pipe 13 is connected with feeding device 3 . The feeding pipe 13 is arranged in the center of the high-frequency plasma torch, which is conducive to the delivery of raw materials to the high-temperature area of the plasma arc core, the harmony and spheroidization of raw materials, and the reaction between raw materials and nitrogen to increase the nitriding rate of raw materials. By adjusting the intake volume of the ionized gas, the enthalpy and jet intensity of the plasma jet can be adjusted to achieve different melting and spheroidizing effects. The protective gas inlet 11 can be fed with nitrogen to form a layer of cold gas film on the tube wall of the high-frequency plasma torch discharge tube 14 to cool the discharge tube 14 and prevent heated and melted raw materials and TiN from adhering to the discharge tube 14 inner wall.
下面结合实施例对本发明的具体实施方式做进一步的描述，并不因此将本发明限制在所述的实施例范围之中。The specific implementation of the present invention will be further described below in conjunction with the examples, and the present invention is not limited to the scope of the examples.
实施例1Example 1
采用图1所示的射频等离子体粉末生产设备生产球形氮化钛粉末。设置射频等离子体粉末生产设备的进料装置的振幅为20％，工作电压10.5KV，功率32kW。“边气”(即保护气体入口)通入氮气，“中气”(即电离气体入口)通入氩气，氮气流量为3m3/h，氩气流量为3m3/h，其中氮气为反应气，氩气为离化气体。送料反应5min收料，制备得到球形氮化钛粉末。其SEM图如图3所示，其XRD图谱见图4，图4上面的曲线为实施例1中制备的最终产品TiN，下面的曲线为含Ti的TiN粉。该方法球化率达到91％，氮化率为87％。Spherical titanium nitride powder was produced using the RF plasma powder production equipment shown in Fig. 1. The amplitude of the feeding device of the radio frequency plasma powder production equipment is set at 20%, the operating voltage is 10.5KV, and the power is 32kW. "Side gas" (that is, the protective gas inlet) is fed with nitrogen, and "middle gas" (that is, the ionized gas inlet) is fed with argon gas. The flow rate of nitrogen gas is 3m3 /h, and the flow rate of argon gas is 3m3 /h. Argon is an ionizing gas. The feeding reaction was carried out for 5 minutes, and the materials were collected to prepare spherical titanium nitride powder. Its SEM image is shown in FIG. 3 , and its XRD spectrum is shown in FIG. 4 . The upper curve in FIG. 4 is the final product TiN prepared in Example 1, and the lower curve is the TiN powder containing Ti. The spheroidization rate of this method reaches 91%, and the nitriding rate reaches 87%.
其中，球化率采用扫描电镜进行形貌观察球化数量获得。氮化率采用能谱仪测定样品表面并结合X射线衍射仪分析结果获得。Among them, the spheroidization rate is obtained by observing the spheroidization number by scanning electron microscope. The nitriding rate is obtained by measuring the surface of the sample with an energy spectrometer and combining with the analysis results of an X-ray diffractometer.
实施例2Example 2
采用图1所示的射频等离子体粉末生产设备生产球形氮化钛粉末。设置射频等离子体粉末生产设备的进料装置的振幅为22％，工作电压11.5kV，功率54kW。“边气”(即保护气体入口)通入氮气，“中气”(即电离气体入口)先通入氩气起弧，待弧稳定后关闭氩气通入氮气，调节“中气”流量为3m3/h，“边气”流量为3m3/h，送料反应5min收料，测得氮化钛粉末质量为27g。其SEM图与图3类似，其XRD图谱与图4上面的曲线类似。该方法球化率达到92％，氮化率为86％。Spherical titanium nitride powder was produced using the RF plasma powder production equipment shown in Fig. 1. The amplitude of the feeding device of the radio frequency plasma powder production equipment is set at 22%, the operating voltage is 11.5kV, and the power is 54kW. "Side gas" (that is, the protective gas inlet) is fed with nitrogen gas, and "middle gas" (that is, the ionized gas inlet) is first fed with argon gas to start the arc. After the arc is stable, close the argon gas and feed nitrogen gas, and adjust the flow rate of "middle gas" to 3m3 /h, the flow rate of "edge gas" is 3m3 /h, the feeding reaction is 5min and the material is collected, and the measured mass of titanium nitride powder is 27g. Its SEM picture is similar to that of Figure 3, and its XRD pattern is similar to the curve above Figure 4. This method achieves a spheroidization rate of 92% and a nitriding rate of 86%.
实施例3Example 3
采用图1所示的射频等离子体粉末生产设备生产球形氮化钛粉末。设置射频等离子体粉末生产设备的进料装置的振幅为24％，工作电压13kV，功率62kW。“边气”通入氮气，“中气”先通入氩气起弧，待弧稳定后关闭氩气通入氮气，调节“中气”流量为4m3/h，“边气”流量为4m3/h，送料反应5min收料，测得氮化钛粉末质量为28g。其SEM图与图3类似，其XRD图谱与图4上面的曲线类似。该方法球化率达到90％，氮化率为85％。Spherical titanium nitride powder was produced using the RF plasma powder production equipment shown in Fig. 1. The amplitude of the feeding device of the radio frequency plasma powder production equipment is set at 24%, the operating voltage is 13kV, and the power is 62kW. The "edge gas" is fed with nitrogen, and the "middle gas" is first fed with argon to start the arc. After the arc is stable, close the argon and feed nitrogen. Adjust the flow rate of "middle gas" to 4m3 /h, and the flow rate of "edge gas" to 4m3 /h, feeding reaction 5min receiving, the measured mass of titanium nitride powder is 28g. Its SEM picture is similar to that of Figure 3, and its XRD pattern is similar to the curve above Figure 4. The spheroidization rate of this method reaches 90%, and the nitriding rate reaches 85%.
实施例4Example 4
采用图1所示的射频等离子体粉末生产设备生产球形氮化钛粉末。设置射频等离子体粉末生产设备的进料装置的振幅为80％，工作电压5kV，功率30kW。“边气”通入氮气，“中气”先通入氩气起弧，待弧稳定后关闭氩气通入氮气，调节“中气”流量为4m3/h，“边气”流量为4m3/h，送料反应5min收料，测得氮化钛粉末质量为28g。其SEM图与图3类似，其XRD图谱与图4上面的曲线类似。该方法球化率达到77％，氮化率为83％。Spherical titanium nitride powder was produced using the RF plasma powder production equipment shown in Fig. 1. The amplitude of the feeding device of the radio frequency plasma powder production equipment is set to 80%, the working voltage is 5kV, and the power is 30kW. The "edge gas" is fed with nitrogen, and the "middle gas" is first fed with argon to start the arc. After the arc is stable, close the argon and feed nitrogen. Adjust the flow rate of "middle gas" to 4m3 /h, and the flow rate of "edge gas" to 4m3 /h, feeding reaction 5min receiving, the measured mass of titanium nitride powder is 28g. Its SEM picture is similar to that of Figure 3, and its XRD pattern is similar to the curve above Figure 4. This method achieves a spheroidization rate of 77% and a nitriding rate of 83%.
实施例5Example 5
采用图1所示的射频等离子体粉末生产设备生产球形氮化钛粉末。设置射频等离子体粉末生产设备的进料装置的振幅为10％，工作电压11kV，功率48kW。“边气”通入氮气，“中气”先通入氩气起弧，待弧稳定后关闭氩气通入氮气，调节“中气”流量为4m3/h，“边气”流量为4m3/h，送料反应5min收料，测得氮化钛粉末质量为28g。其SEM图与图3类似，其XRD图谱与图4上面的曲线类似。该方法球化率达到91％，氮化率为89％。Spherical titanium nitride powder was produced using the RF plasma powder production equipment shown in Fig. 1. The amplitude of the feeding device of the radio frequency plasma powder production equipment is set to be 10%, the working voltage is 11kV, and the power is 48kW. The "edge gas" is fed with nitrogen, and the "middle gas" is first fed with argon to start the arc. After the arc is stable, close the argon and feed nitrogen. Adjust the flow rate of "middle gas" to 4m3 /h, and the flow rate of "edge gas" to 4m3 /h, feeding reaction 5min receiving, the measured mass of titanium nitride powder is 28g. Its SEM picture is similar to that of Figure 3, and its XRD pattern is similar to the curve above Figure 4. This method achieves a spheroidization rate of 91% and a nitriding rate of 89%.
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| Date | Code | Title | Description |
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| PB01 | Publication | ||
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| SE01 | Entry into force of request for substantive examination | ||
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| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication | Application publication date:20180629 |