CN105931935A - High-thermal-conductivity insulating medium fast-heating cathode hot wire assembly and preparation method thereof - Google Patents
High-thermal-conductivity insulating medium fast-heating cathode hot wire assembly and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims description 5
- 238000010438 heat treatment Methods 0.000 title abstract description 49
- 239000000843 powder Substances 0.000 claims abstract description 16
- 239000000919 ceramic Substances 0.000 claims abstract description 15
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 6
- 239000010937 tungsten Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims description 4
- DECCZIUVGMLHKQ-UHFFFAOYSA-N rhenium tungsten Chemical compound [W].[Re] DECCZIUVGMLHKQ-UHFFFAOYSA-N 0.000 claims description 4
- 229910000691 Re alloy Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 3
- 229910052702 rhenium Inorganic materials 0.000 claims description 3
- 238000009849 vacuum degassing Methods 0.000 claims description 2
- 229910017083 AlN Inorganic materials 0.000 claims 3
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims 2
- 229910052786 argon Inorganic materials 0.000 claims 1
- 238000000498 ball milling Methods 0.000 claims 1
- 229910001634 calcium fluoride Inorganic materials 0.000 claims 1
- 239000007789 gas Substances 0.000 claims 1
- 230000014759 maintenance of location Effects 0.000 claims 1
- 238000003801 milling Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 abstract description 14
- 239000002002 slurry Substances 0.000 abstract description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 7
- 239000007787 solid Substances 0.000 abstract description 4
- 238000000280 densification Methods 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract description 2
- 230000035939 shock Effects 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 4
- 229910004261 CaF 2 Inorganic materials 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 229910052575 non-oxide ceramic Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- WMTSAHAFZXEJBV-UHFFFAOYSA-N [Ba].[W] Chemical compound [Ba].[W] WMTSAHAFZXEJBV-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
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- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
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Abstract
一种高导热绝缘介质快热阴极热丝组件制备方法，它包括钨阴极(1)、阴极筒(2)、热丝(3)和绝缘介质(4)，阴极筒(2)和热丝(3)通过绝缘介质(4)紧密封装为一体结构。本发明采用乙醇等有机溶剂和氮化铝粉末混合制得高固含量的陶瓷料浆，料浆浇注入阴极筒并加入热丝，离心处理等成型致密化后经过高温烧结制得所述高导热绝缘介质快热阴极热丝组件。本发明所述高导热绝缘介质快热阴极热丝组件，导热率远高于传统氧化铝陶瓷组件，具有更高的热传递效率，阴极热丝组件预热时间更短，可以在5s内快速达到1050℃的工作温度，该热丝组件高温强度更高，抗震性好，满足高振动冲击下快速启动要求，性能优异，可靠性高、工作寿命长，可广泛应用于快速启动行波管中。
A method for preparing a highly thermally conductive insulating medium fast heating cathode heating wire assembly, which comprises a tungsten cathode (1), a cathode cylinder (2), a heating wire (3) and an insulating medium (4), the cathode cylinder (2) and the heating wire ( 3) tightly packaged as an integral structure through an insulating medium (4). The present invention mixes organic solvents such as ethanol and aluminum nitride powder to prepare ceramic slurry with high solid content. The slurry is poured into the cathode cylinder and a hot wire is added. The high thermal conductivity is obtained by high-temperature sintering after molding and densification by centrifugal treatment. Insulated medium fast heating cathode heating wire assembly. The high thermal conductivity insulating medium fast-heating cathode heating wire assembly of the present invention has a thermal conductivity much higher than that of the traditional alumina ceramic assembly, has higher heat transfer efficiency, and the cathode heating wire assembly has a shorter warm-up time, which can be quickly reached within 5s With a working temperature of 1050°C, the hot wire assembly has higher high-temperature strength, good shock resistance, and meets the requirements of quick start-up under high vibration and impact. It has excellent performance, high reliability, and long working life, and can be widely used in quick-start traveling wave tubes.
Description
技术领域technical field
本发明属于间接式加热快热阴极领域，具体制备一种快热阴极热丝组件。特别是提供了一种高导热氮化铝陶瓷绝缘介质阴极热丝组件制备技术，有助于缩短预热时间，对提升快启行波管关键性能具有非常重要的作用。The invention belongs to the field of indirect heating fast-heating cathodes, and specifically prepares a fast-heating cathode heating wire assembly. In particular, it provides a high thermal conductivity aluminum nitride ceramic insulating dielectric cathode heating wire assembly technology, which helps to shorten the warm-up time and plays a very important role in improving the key performance of the fast-start traveling wave tube.
背景技术Background technique
阴极热丝组件广泛应用于行波管、速调管等微波电子器件，热丝通过电流后急速升温，经绝缘介质和阴极筒使钨阴极快速升温，绝缘介质和阴极筒紧密接触，现有的热量传递介质为氧化铝。现有专利通过采用阴极组件结构设计和优化、在氧化铝中添加烧结助剂等方法缩短预热时间。然而氧化铝导热率限制在20～30W/(m·K)、比热容大、密度高等限制了阴极的升温速率，而添加助剂后导致高温强度不足、氧元素与钨丝高温反应等问题降低了其可靠性和使用寿命。而阴极组件的质量和组件中的热导率是影响热子组件快热的最重要的两个因素，所以因此很有必要在现有基础上发展一种高导热绝缘介质快热阴极热丝组件。The cathode heating wire assembly is widely used in microwave electronic devices such as traveling wave tubes and klystrons. The heating wire heats up rapidly after passing the current, and the tungsten cathode heats up rapidly through the insulating medium and the cathode cylinder. The insulating medium and the cathode cylinder are in close contact. The existing The heat transfer medium is alumina. The existing patent shortens the preheating time by adopting the design and optimization of the structure of the cathode assembly, and adding sintering aids to the alumina. However, the thermal conductivity of alumina is limited to 20-30W/(m K), the large specific heat capacity, and high density limit the heating rate of the cathode, and the addition of additives leads to insufficient high-temperature strength and high-temperature reaction between oxygen and tungsten wire. its reliability and service life. The quality of the cathode assembly and the thermal conductivity in the assembly are the two most important factors affecting the rapid heating of the thermal subassembly, so it is necessary to develop a high thermal conductivity insulating medium fast heating cathode heating wire assembly on the existing basis .
氮化铝陶瓷相比于氧化铝陶瓷密度更低、比热容较小、且导热率可高达120～200W/(m·K)的，且材料中无氧元素，不会与其他材料发生反应，从各方面因素比较其具备有效缩短阴极热丝组件预热时间的能力。采用氮化铝陶瓷作为传热介质的快热阴极热丝组件有更高的热传导效率，可大大提高阴极热子组件预热时间，而氮化铝陶瓷高温下具有更高的强度和稳定性，可大大提高其在振动和高温环境下的可靠性、延长使用寿命。Compared with alumina ceramics, aluminum nitride ceramics have lower density, smaller specific heat capacity, and thermal conductivity as high as 120-200W/(m K), and there is no oxygen element in the material, and it will not react with other materials. Compared with various factors, it has the ability to effectively shorten the warm-up time of the cathode heating wire assembly. The fast-heating cathode heating wire assembly using aluminum nitride ceramics as the heat transfer medium has higher heat conduction efficiency, which can greatly increase the warm-up time of the cathode heating subassembly, while aluminum nitride ceramics have higher strength and stability at high temperatures. It can greatly improve its reliability and prolong its service life under vibration and high temperature environment.
采用非氧化物陶瓷材料氮化铝陶瓷作为绝缘介质，并提供一种采用高固含量氮化铝陶瓷料浆制备高导热绝缘介质的方法，克服了氧化铝陶瓷的不足，提供了一种适合氮化铝陶瓷绝缘介质快热阴极热丝组件的制备方法，解决了氮化铝绝缘介质制备过程中料浆制备、成型致密化、烧结等关键技术要求，获得高可靠性、预热时间短的快热阴极热丝组件。Use non-oxide ceramic material aluminum nitride ceramics as the insulating medium, and provide a method for preparing high thermal conductivity insulating medium by using high solid content aluminum nitride ceramic slurry, overcome the shortcomings of alumina ceramics, and provide a suitable nitrogen The preparation method of aluminum nitride ceramic insulating medium fast-heating cathode hot wire assembly solves key technical requirements such as slurry preparation, molding densification, and sintering in the preparation process of aluminum nitride insulating medium, and obtains high reliability and short warm-up time. Hot cathode filament assembly.
发明内容Contents of the invention
本发明目的为了克服现有技术氧化铝陶瓷热丝组件的不足，采用非氧化物陶瓷材料氮化铝陶瓷作为绝缘介质，并提供一种采用高固含量氮化铝陶瓷料浆制备高导热绝缘介质的方法，最终提供一种高导热绝缘介质快热阴极热丝组件。The object of the present invention is to overcome the shortcomings of the prior art alumina ceramic heating wire assembly, adopt non-oxide ceramic material aluminum nitride ceramics as the insulating medium, and provide a high thermal conductivity insulating medium prepared by using high solid content aluminum nitride ceramic slurry The method finally provides a high-thermal-conductivity insulating medium fast-heating cathode heating wire assembly.
一种高导热绝缘介质快热阴极热丝组件，其特征在于：它包括钨阴极(1)、阴极筒(2)、热丝(3)和绝缘介质(4)，绝缘介质(4)紧密填充在阴极筒(2)和热丝(3)中间。A highly thermally conductive insulating medium fast-heating cathode heating wire assembly is characterized in that it includes a tungsten cathode (1), a cathode cylinder (2), a heating wire (3) and an insulating medium (4), and the insulating medium (4) is tightly packed Between the cathode cylinder (2) and the hot wire (3).
采用高导热氮化铝陶瓷作为绝缘介质，绝缘介质完全填充阴极筒并完全包裹阴极筒内的热丝，界面处无缝隙；热丝采用铼质量分数20～25％的钨铼合金丝。Aluminum nitride ceramics with high thermal conductivity are used as the insulating medium, the insulating medium completely fills the cathode cylinder and completely wraps the hot wire in the cathode cylinder, and there is no gap at the interface;
采用优选方案，制备出低粘度、高固含量的氮化铝料浆，将制得的料浆浇注入阴极筒，放入热丝，料浆完全填充阴极筒并将阴极筒内的热丝完全包裹，采用离心处理或者压滤处理再次提高绝缘介质烧结前致密度。干燥后在钨丝炉中烧结后获得高导热绝缘介质快热阴极热丝组件Adopt the preferred scheme to prepare aluminum nitride slurry with low viscosity and high solid content, pour the prepared slurry into the cathode cylinder, put in the hot wire, completely fill the cathode cylinder with the slurry and completely fill the hot wire in the cathode cylinder Wrapping, using centrifugal treatment or pressure filtration treatment to improve the density of the insulating medium before sintering again. After drying and sintering in a tungsten wire furnace, a high thermal conductivity insulating medium fast heating cathode heating wire assembly is obtained
本发明所述高导热绝缘介质快热阴极热丝组件，对热丝材料和组件进行优化。热丝材料采用铼元素质量分数20～25％的钨铼合金丝，其再结晶温度高、热阻率大、温度系数小、耐冲击性好；热丝结构采用内外双螺旋结构，结构使组件内部温度分布更加均匀。The highly thermally conductive insulating medium fast heating cathode hot wire assembly of the present invention optimizes the material and components of the hot wire. The heating wire material adopts tungsten-rhenium alloy wire with a rhenium mass fraction of 20-25%, which has high recrystallization temperature, high thermal resistance, small temperature coefficient and good impact resistance; the heating wire structure adopts an inner and outer double helix structure, and the structure makes the component The internal temperature distribution is more even.
本发明对钨阴极材料进行优化，采用含铼的钡钨阴极，可以提高其发射性能。The invention optimizes the tungsten cathode material and adopts the barium tungsten cathode containing rhenium to improve its emission performance.
本发明的具体步骤：Concrete steps of the present invention:
1、将高纯AlN粉末，经过高温700～800℃预烧，气流磨破碎后用空气振动筛筛分出5～10μm的粉体；1. The high-purity AlN powder is pre-fired at a high temperature of 700-800 °C, crushed by a jet mill, and then sieved with an air vibrating sieve to obtain a powder of 5-10 μm;
2、用乙醇和乙醚混合液溶解的火棉胶溶液和AlN粉末混合，并添加2～3％Y2O3粉和2～3％CaF2粉，球磨制得均匀流动性好的料浆；2. Mix the collodion solution dissolved in a mixture of ethanol and ether with AlN powder, add 2-3% Y 2 O 3 powder and 2-3% CaF 2 powder, and ball mill to obtain a slurry with good fluidity;
3、料浆经过真空除气，浇注入阴极筒，再将热丝缓慢放入装有料浆的阴极筒，沿阴极筒轴向经过转速2000～6000r/min的离心处理1～10min，放入干燥箱中干燥2小时，干燥温度60～70℃。3. After vacuum degassing, the slurry is poured into the cathode cylinder, and then the hot wire is slowly put into the cathode cylinder containing the slurry, and is centrifuged at a speed of 2000-6000r/min along the axis of the cathode cylinder for 1-10 minutes, and then placed in a drying Dry in the oven for 2 hours at a drying temperature of 60-70°C.
4、将上一步制得的热丝和阴极筒组件放入钨丝炉中，烧结温度1700～1900℃，在氢气、氮气或者氩气气氛下进行烧结，保温时间1～2小时，降温至100℃以下取出，制得封装好的高导热绝缘介质快热阴极热丝组件。4. Put the hot wire and cathode cylinder assembly prepared in the previous step into a tungsten wire furnace, sinter at a temperature of 1700-1900°C, sinter in a hydrogen, nitrogen or argon atmosphere, hold for 1-2 hours, and cool down to 100 The temperature is lower than ℃, and the packaged high thermal conductivity insulating medium fast heating cathode heating wire assembly is obtained.
本发明的优点：Advantages of the present invention:
本发明所述的高绝缘介质快热阴极热丝组件，具有更高的热量传递效率，阴极升温速度快，可以在5s内升温到1050℃的工作温度。本发明所述的高绝缘介质快热阴极热丝组件采用高导热氮化铝陶瓷作为绝缘介质把内外双螺旋结构钨铼丝和阴极筒紧密封装构成一体结构，加热效率更高，预热时间短，高温强度高，稳定性好，具有更高的抗震性能，可靠性高，能更广泛地应用于行波管等真空器件。The high-insulation medium fast-heating cathode heating wire assembly of the present invention has higher heat transfer efficiency, and the cathode heating speed is fast, and the temperature can be raised to a working temperature of 1050° C. within 5 seconds. The high-insulation-medium fast-heating cathode heating wire assembly of the present invention uses aluminum nitride ceramics with high thermal conductivity as the insulation medium to tightly package the inner and outer double-helix structure tungsten-rhenium wires and the cathode cylinder to form an integrated structure, which has higher heating efficiency and short warm-up time. , high temperature strength, good stability, higher shock resistance, high reliability, and can be more widely used in vacuum devices such as traveling wave tubes.
附图说明Description of drawings
图1为本发明所述高导热绝缘介质快热阴极热丝组件结构示意图。Fig. 1 is a schematic structural view of the highly thermally conductive insulating medium fast-heating cathode filament assembly of the present invention.
图2为本发明所述高导热绝缘介质快热阴极热丝组件结构俯视图。Fig. 2 is a top view of the structure of the high thermal conductivity insulating medium fast heating cathode filament assembly of the present invention.
具体实施方式detailed description
实施例1Example 1
1、将高纯AlN粉末，经过高温800℃预烧5小时，气流磨破碎后用空气振动筛筛分出5～10μm的粉体；1. The high-purity AlN powder is pre-fired at a high temperature of 800°C for 5 hours, crushed by a jet mill, and sieved with an air vibrating sieve to obtain a powder of 5-10 μm;
2、用乙醇和乙醚混合液溶解的火棉胶溶液和AlN粉末混合，并添加2％Y2O3粉和2％CaF2粉，球磨制得均匀流动性好的料浆；2. Mix the collodion solution dissolved in a mixture of ethanol and ether with AlN powder, add 2% Y 2 O 3 powder and 2% CaF 2 powder, and ball mill to obtain a slurry with good fluidity;
3、料浆经过真空除气，浇注入阴极筒，再将铼元素质量分数20～25％的钨铼合金热丝缓慢放入装有料浆的阴极筒，沿阴极筒轴向经过转速5000r/min的离心处理5min，放入干燥箱中干燥2小时，干燥温度60℃。3. The slurry is vacuum degassed, poured into the cathode cylinder, and then slowly put the tungsten-rhenium alloy hot wire with a rhenium element mass fraction of 20-25% into the cathode cylinder containing the slurry, and pass through the cathode cylinder axially at a speed of 5000r/min centrifuged for 5 minutes, put into a drying oven to dry for 2 hours, and the drying temperature was 60°C.
4、将上一步制得的热丝和阴极筒组件放入钨丝炉中，烧结温度1800℃，在氢气、氮气或者氩气气氛下进行烧结，保温时间1小时，降温至100℃以下取出，制得封装好的高导热绝缘介质快热阴极热丝组件。4. Put the hot wire and cathode cylinder assembly prepared in the previous step into a tungsten wire furnace at a sintering temperature of 1800°C, sintering in a hydrogen, nitrogen or argon atmosphere, hold for 1 hour, cool down to below 100°C and take it out. A packaged high thermal conductivity insulating medium fast heating cathode heating wire assembly is prepared.
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| CN112490098A (en) * | 2020-12-09 | 2021-03-12 | 成都国光电气股份有限公司 | Mixed filling powder for hot wire component and preparation method thereof |
| CN113053706A (en) * | 2021-03-19 | 2021-06-29 | 安徽华东光电技术研究所有限公司 | Convolution tube hot wire and manufacturing method thereof |
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| CN108321068A (en) * | 2017-12-15 | 2018-07-24 | 南京三乐集团有限公司 | A kind of polymorphic structure cathode and preparation method thereof that traveling wave is effective |
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| CN112490098B (en) * | 2020-12-09 | 2023-03-14 | 成都国光电气股份有限公司 | Mixed filling powder for hot wire component and preparation method thereof |
| CN113053706A (en) * | 2021-03-19 | 2021-06-29 | 安徽华东光电技术研究所有限公司 | Convolution tube hot wire and manufacturing method thereof |
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