CN100567576C - Method for producing cathode of oxygen generator by dry pressing method - Google Patents
Method for producing cathode of oxygen generator by dry pressing method Download PDFInfo
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Abstract
本发明提出的一种用干压法生产制氧机阴极的方法,属于电化学制氧单元阴极和水中离子膜取氧的技术,它以聚四氟乙烯粉料、碳黑为基料,配入磷片石墨和发泡剂等辅料,按计量配料、搅拌混料、入模干压和焙烧定型的步骤进行生产的制氧单元阴极,具有极佳的透气防水性能和良好的低电阻性能的优点,它同“湿法轧制”方法相比,本发明提出的干压成形技术,明显改进了阴极中嵌装铜网电极引线的工艺操作性,它具有工艺简捷,操作方便,作业效率高,生产成本低的特点,用干压法生产的阴极配装于制氧机,能明显提高产氧量和工作稳定性能,对提高和改善制氧机的产品质量具有良好效果,有极好的推广使用前景。The invention proposes a method for producing the cathode of an oxygen generator by dry pressing, which belongs to the technology of taking oxygen from the cathode of an electrochemical oxygen production unit and ion membrane in water. Phosphorus flake graphite and foaming agent and other auxiliary materials are added, and the cathode of the oxygen making unit is produced according to the steps of metering and batching, stirring and mixing, dry pressing into the mold and roasting and shaping. It has excellent air permeability and waterproof performance and good low resistance performance. Advantages, compared with the "wet rolling" method, the dry pressing forming technology proposed by the present invention significantly improves the process operability of the copper mesh electrode lead embedded in the cathode. It has simple process, convenient operation and high operating efficiency. , the production cost is low, and the cathode produced by the dry pressure method is equipped with the oxygen generator, which can significantly improve the oxygen production and work stability, and has a good effect on improving and improving the product quality of the oxygen generator. Promoting prospects for use.
Description
技术领域: Technical field:
本发明涉及制氧电极材料的生产技术,属于电化学离子膜制氧单元阴极材料和水中离子膜取氧的技术领域,具体地说是一种用干压法生产制氧机阴极的方法。The invention relates to the production technology of oxygen-generating electrode materials, and belongs to the technical field of cathode materials of electrochemical ion membrane oxygen-generating units and ion membrane oxygen extraction in water, and specifically relates to a method for producing cathodes of oxygen generators by dry pressing.
背景技术: Background technique:
我们知道,现有家庭医用制氧机一般分为物理制氧和化学制氧两种方法。物理制氧是用高分子筛变压吸咐分离技术从空气介质中进行氮氧分离制取氧气供吸用,虽然物理制氧机具有取氧资源丰富、产氧数量充足和输氧稳定等优点,但是由于物理制氧机存在结构复杂、压缩机工作噪音大和生产成本高、价格昂贵等缺点,一般家庭难以接受。而化学制氧特别是采用电化学离子膜制氧单元阴极从水中离子膜取氧技术的家庭医用制氧机,由于它具有体积小、重量轻、价格低廉,产氧迅速、输氧效率高、操作使用方便等优点,深受广大用户的青睐。毋庸置疑:电化学离子膜制氧单元阴极是化学制氧机的关键核心技术,离子膜制氧单元阴极材料的质量将直接影响制氧机的工作性能。总的来说:要求制氧单元阴极材料具有低阻值性能和极佳的防水透气性能,并且还要求阴极具有较好的机械强度和外形尺寸稳定性能,在生产过程中具有较好的工艺操作性,能方便于配装电极引线和确保电极引线的牢固可靠性,在使用过程中具有长期稳定工作的性能。现有生产制氧机阴极的方法是将原料经过充分搅拌制成泥状,然后在双辊轧机上反复轧制,再经焙烧定型而成。采用这种“湿法轧制-焙烧定型”的方法所生产的阴极产品存在着如下缺陷:在双辊轧机上配装阴极成品的铜网电极引线的工艺操作性能较差,生产作业效率较低,尤其是在焙烧定型过程中,泥状物料会有大量的液体介质蒸发,不仅影响阴极成品外形尺寸的稳定性能,还会在阴极成品中隐埋下汽泡甚至出现隐性裂缝等质量缺陷,影响阴极成品机械强度和防水透气性能,在实际使用中表现为电极引线的牢固可靠性差,容易出现分层透水,致使阴极导电性能降低,势必影响制氧机的工作效能。这是目前采用湿法轧制方法生产的阴极产品难以克服的致命性技术缺陷。这也正是本发明所要解决的问题。We know that existing home medical oxygen generators are generally divided into two methods: physical oxygen generation and chemical oxygen generation. Physical oxygen generation uses polymer sieve pressure swing adsorption separation technology to separate nitrogen and oxygen from the air medium to produce oxygen for absorption. Although physical oxygen generators have the advantages of rich oxygen resources, sufficient oxygen production and stable oxygen delivery, but Due to the shortcomings of physical oxygen generators such as complex structure, loud compressor operation noise, high production cost, and high price, it is difficult for ordinary families to accept it. The chemical oxygen generator, especially the family medical oxygen generator that adopts the cathode of the electrochemical ion membrane oxygen generator unit to extract oxygen from the ion membrane in water, has the advantages of small size, light weight, low price, rapid oxygen production, high oxygen delivery efficiency, and easy operation. Easy to use and other advantages, favored by the majority of users. There is no doubt that the cathode of the electrochemical ion membrane oxygen generator unit is the key core technology of the chemical oxygen generator, and the quality of the cathode material of the ion membrane oxygen generator unit will directly affect the working performance of the oxygen generator. In general: the cathode material of the oxygen generating unit is required to have low resistance and excellent waterproof and breathable performance, and the cathode is also required to have good mechanical strength and external dimension stability, and have good process operation in the production process It is easy to assemble electrode leads and ensure the firmness and reliability of electrode leads, and has long-term stable working performance during use. The existing method for producing the cathode of an oxygen generator is that the raw materials are fully stirred into a mud, then repeatedly rolled on a double-roll mill, and then roasted and shaped. The cathode products produced by this "wet rolling-roasting and shaping" method have the following defects: the process operation performance of the copper mesh electrode lead wire of the finished cathode product on the twin-roll rolling mill is poor, and the production efficiency is low , especially in the process of roasting and shaping, a large amount of liquid medium will evaporate in the muddy material, which not only affects the stability of the outer dimension of the finished cathode, but also buries bubbles and even hidden cracks in the finished cathode. It affects the mechanical strength and waterproof and breathable performance of the finished cathode. In actual use, it is manifested in the poor reliability of the electrode lead, which is prone to layered water permeability, resulting in a decrease in the electrical conductivity of the cathode, which will inevitably affect the working efficiency of the oxygen generator. This is a fatal technical defect that is difficult to overcome for the cathode products produced by the wet rolling method at present. This is also the problem to be solved by the present invention.
发明内容: Invention content:
本发明的目的旨在针对湿法轧制阴极产品存在的技术缺陷,提出一种用干压法生产制氧机阴极的方法,它是对现有制氧单元阴极材料及其生产方法的进一步改进和完善。The purpose of the present invention aims at the technical defect that wet rolling cathode product exists, proposes a kind of method that produces oxygen generator cathode by dry pressing method, and it is the further improvement to existing oxygen generator unit cathode material and its production method and perfect.
本发明提出的用干压法生产制氧机阴极的方法,它是以聚四氟乙烯粉料和碳黑为基料,其特征在于:它依次按以下步骤进行:The method that the present invention proposes produces the cathode of oxygen generator with dry pressing method, and it is base-material with polytetrafluoroethylene powder and carbon black, it is characterized in that: it carries out according to the following steps successively:
(1)计量配料:按如下重量配比计量备取基料(1) Measuring ingredients: measure and prepare the base material according to the following weight ratio
聚四氟乙烯粉料 1份PTFE powder 1 part
碳黑 0.35~0.45份Carbon black 0.35~0.45 parts
控制基料:聚四氟乙烯粉料的粒径≤1000微米,Control base material: the particle size of polytetrafluoroethylene powder is less than or equal to 1000 microns,
碳黑的粒径≤1000微米,The particle size of carbon black is less than or equal to 1000 microns,
按基料总重量的2.5~5.0%配入石墨,控制石墨的粒度≤200目,Add graphite according to 2.5-5.0% of the total weight of the base material, and control the particle size of the graphite to ≤200 mesh,
按基料总重量的3.5~5.0%配入发泡剂,Add foaming agent according to 3.5-5.0% of the total weight of the base material,
以上所述的石墨是选用具有低阻值高导电性能的磷片石墨产品,The graphite mentioned above is a phosphorus flake graphite product with low resistance and high conductivity.
磷片石墨:粒度≤200目,碳含量≥99%,挥发物含量≤0.25%,选用磷片石墨材料对降低阴极电阻、提高阴极导电性能具有明显效果,Phosphorus flake graphite: particle size ≤ 200 mesh, carbon content ≥ 99%, volatile matter content ≤ 0.25%, the choice of phosphorus flake graphite material has obvious effects on reducing cathode resistance and improving cathode conductivity.
上述所说的发泡剂是选用可市购的由宁夏日盛实业有限公司生产的牌号为ADC型发泡剂。The blowing agent mentioned above is to select commercially available trade mark produced by Ningxia Risheng Industrial Co., Ltd. as ADC type blowing agent.
(2)搅拌混料:将在步骤(1)计量配料中称取的物料放入混料机内进行搅拌混匀,制得混合料,(2) Stir and mix: put the material weighed in the step (1) into the batching mixer and stir and mix to obtain the mix.
所述的搅拌混匀是指:混料机的搅拌转速为1000~1500转/分,连续搅拌时间为:5~10分钟,被搅拌的物料呈现出棉花纤维状时,即制得合格的混合料,使其易于入模干压成形。The stirring and mixing means that the stirring speed of the mixer is 1000-1500 rpm, and the continuous stirring time is 5-10 minutes. When the stirred material appears in the form of cotton fibers, the qualified mixed material, making it easy to enter the mold for dry pressing.
(3)入模干压:将在步骤(2)搅拌混料中制得的混合料加入压模内进行干压成形,制得成形阴极,控制压力为:20~30MPa。(3) Molding and dry pressing: adding the mixed material prepared in step (2) into the pressing mold for dry pressing to obtain a formed cathode, the control pressure is: 20-30 MPa.
所述的压模是按所设计阴极成品外形尺寸工艺要求制成的,入模干压时,用规格为60~100目的筛子过筛混合料,过筛的混合料放进压模内,按设计要求控制放入混合料的物料量,并在中间配装阴极成品的铜网电极引线,然后加压,即可一次性干压制得成形阴极,采用干压成形的方法对确保电极引线的牢固可靠性、防止阴极分层透水具有明显效果。The die is made according to the design process requirements of the finished cathode shape and size. When entering the mold for dry pressing, use a sieve with a specification of 60 to 100 mesh to sieve the mixture, put the sieved mixture into the die, press The design requires the control of the amount of materials put into the mixture, and the copper mesh electrode leads of the finished cathode are installed in the middle, and then pressurized, and the formed cathode can be obtained by one-time dry pressing. The method of dry pressing is used to ensure the firmness of the electrode leads. Reliability, preventing cathode delamination and water penetration have obvious effects.
(4)焙烧定型:将在步骤(3)入模干压中制得的成形阴极进行焙烧,控制焙烧温度为:200~380℃,焙烧时间为:6~8小时,即制得已定型合格的阴极产品。(4) Roasting and finalizing: Roasting the formed cathode prepared in step (3) into the mold and dry pressing, controlling the calcining temperature: 200-380°C, and the calcining time: 6-8 hours, that is, the qualified stereotyped cathode is obtained cathode products.
所述的焙烧是指将成形阴极送入烘箱内进行焙烧定型,控制焙烧温度为:在1~1.5小时内,由室温缓慢升温至200℃;在2~4小时内,由200℃缓慢升温至350℃进行焙烧,可使混合料中的发泡剂逐渐从成形阴极中缓缓挥发,形成均匀致密、防水的透气微孔,对提高阴极的防水透气性能具有明显效果;在370℃~380℃温度下保温2~4小时进行焙烧定型,以稳定阴极成品的尺寸和提高机械强度,然后自然冷却即制得合格的阴极产品。The roasting refers to sending the shaped cathode into an oven for roasting and shaping. The roasting temperature is controlled as follows: within 1 to 1.5 hours, the temperature is slowly raised from room temperature to 200°C; within 2 to 4 hours, the temperature is slowly raised from 200°C to Roasting at 350°C can make the foaming agent in the mixture slowly volatilize from the formed cathode, forming uniform, dense, waterproof and breathable micropores, which has a significant effect on improving the waterproof and breathable performance of the cathode; at 370°C to 380°C Keep the temperature for 2 to 4 hours to bake and set the shape, so as to stabilize the size of the finished cathode and improve the mechanical strength, and then cool naturally to obtain a qualified cathode product.
本发明还有如下技术特征:The present invention also has following technical characteristics:
在计量配料步骤中,在所述的粒径≤1000微米的聚四氟乙烯粉料之中,粒径≤200微米的聚四氟乙烯悬浮细粉按重量计占60~80%。In the step of metering and compounding, among the polytetrafluoroethylene powders with particle diameters ≤ 1000 microns, polytetrafluoroethylene suspended fine powders with particle diameters ≤ 200 microns account for 60-80% by weight.
在粒径≤1000微米的聚四氟乙烯物料之中:粒径≤200微米的为聚四氟乙烯悬浮细粉,其余则为聚四氟乙烯分散细粉。本发明提出的按一定重量比搭配的控制不同粒径的聚四氟乙烯悬浮细粉和聚四氟乙烯分散细粉构成阴极混合料具有独特的技术效果,能明显提高阴极材料的紧密度,有效地改善阴极的工作性能。Among the PTFE materials with a particle size of ≤1000 microns: those with a particle size of ≤200 microns are PTFE suspended fine powder, and the rest are PTFE dispersed fine powder. The polytetrafluoroethylene suspended fine powder and polytetrafluoroethylene dispersed fine powder with different particle sizes matched according to a certain weight ratio to form the cathode mixture has a unique technical effect, which can significantly improve the compactness of the cathode material, effectively improve the performance of the cathode.
本发明的优点表现为:The advantages of the present invention are as follows:
(1)本发明提出的用干压法生产制氧机阴极的方法,工艺流程简捷,操作管理方便,生产作业效率高,可大大降低生产成本,特别是采用独创的干压成形技术,能明显改进和改善阴极中嵌装铜网电极引线的工艺操作性,提高电极引线的牢固可靠性能,对防止电极分层透水、改善阴极工作性能、提高制氧机产品质量具有突出的实质性特点和显著进步;(1) The method for producing the cathode of an oxygen generator by the dry pressing method proposed by the present invention has simple and convenient process flow, convenient operation and management, high production efficiency, and can greatly reduce production costs. In particular, the original dry pressing forming technology can significantly Improve and improve the process operability of copper mesh electrode leads embedded in the cathode, improve the firmness and reliability of the electrode leads, and have outstanding substantive characteristics and significant progress;
(2)用干压法生产的制氧机阴极成品具有极佳的透气防水性能和良好的低电阻性能,阴极工作状态稳定;(2) The finished cathode of the oxygen generator produced by the dry pressure method has excellent air permeability and waterproof performance and good low resistance performance, and the working state of the cathode is stable;
(3)用干压法生产的制氧机阴极产品外形尺寸稳定,具有较好的机械强度,便于组装流程加工作业,在实际生产中,只需更换压模,就能制造各种规格形状的电极成品以满足不同制氧机的需要,适应性强;(3) The cathode product of the oxygen generator produced by dry pressing method has stable appearance and size, good mechanical strength, and is convenient for assembly process and processing operations. In actual production, it is only necessary to replace the die to manufacture various specifications and shapes. The finished electrode can meet the needs of different oxygen generators and has strong adaptability;
(4)用干压法生产的阴极配装于制氧机,能明显提高产氧量,具有长期工作稳定性能,对提高和改善制氧机的工作性能具有积极效果。(4) The cathode produced by the dry pressing method is assembled in the oxygen generator, which can significantly increase the oxygen production, has long-term working stability, and has a positive effect on improving and improving the working performance of the oxygen generator.
具体实施方式: Detailed ways:
实施例一:Embodiment one:
用干压法生产制氧机阴极的方法,它依次按以下步骤进行:The method for producing the cathode of an oxygen generator by a dry pressing method is carried out in the following steps:
(1)计量配料:按如下重量配比计量备取基料(1) Measuring ingredients: measure and prepare the base material according to the following weight ratio
聚四氟乙烯粉料 粒径≤1000微米 8kgPTFE powder particle size ≤ 1000 micron 8kg
碳黑 粒径≤1000微米 3.2kgCarbon black Particle size≤1000 microns 3.2kg
磷片石墨 粒度≤200目 0.32kgPhosphor flake graphite Particle size≤200 mesh 0.32kg
ADC型发泡剂 0.46kgADC type foaming agent 0.46kg
ADC型发泡剂是选用可市购的由宁夏日盛实业有限公司生产的发泡剂成品。The ADC type blowing agent is to select commercially available foaming agent finished products produced by Ningxia Risheng Industrial Co., Ltd.
(2)搅拌混料:将计量称取的物料放入混料机内,启动混料机,按1000转/分的转速高速搅拌6分钟,使被搅拌的物料呈现出棉花纤维状,即制得合格的混合料;(2) Stirring and mixing: put the material weighed into the mixer, start the mixer, and stir at a high speed of 1000 rpm for 6 minutes, so that the stirred material appears in the form of cotton fibers, which is ready-made Qualified mixture;
(3)入模干压:将按所设计阴极成品外形尺寸(例如:长160mm、宽140mm、厚3mm)工艺要求制成的压模安装于干压机内,再将搅拌混料制得的混合料送入规格为80目的筛子进行过筛,过筛的混合料放入压模内,按设计要求准确放入混合料的物料量,并在中间配装阴极成品的铜网电极引线,然后施加26MPa的压力,即可一次性干压制得成形阴极;(3) Die-in dry pressing: Install the die made according to the design process requirements of the finished cathode dimensions (for example: length 160mm, width 140mm, thickness 3mm) in the dry press, and then mix the prepared The mixed material is sent to a sieve with a specification of 80 meshes for sieving, and the sieved mixed material is put into the die, and the amount of the mixed material is accurately put in according to the design requirements, and the copper mesh electrode lead wire of the finished cathode is installed in the middle, and then Applying a pressure of 26MPa, the formed cathode can be obtained by one-time dry pressing;
(4)焙烧定型:将入模干压制得的成形阴极送入电烘箱内进行焙烧定型,精确控制电烘箱内的升温焙烧温度:在1.5小时内缓慢升温至200℃,再在3小时内继续缓慢升温至350℃进行焙烧,再继续升温至380℃焙烧3小时,然后自然冷却即制得符合设计要求的阴极产品。(4) Roasting and shaping: send the formed cathode into the electric oven for roasting and shaping, and precisely control the heating and roasting temperature in the electric oven: slowly heat up to 200 ° C within 1.5 hours, and then continue within 3 hours Slowly raise the temperature to 350°C for calcination, then continue to raise the temperature to 380°C for 3 hours, and then cool naturally to obtain a cathode product that meets the design requirements.
实施例二Embodiment two
用干压法生产制氧机阴极的方法,它依次按以下步骤进行:The method for producing the cathode of an oxygen generator by a dry pressing method is carried out in the following steps:
(1)计量配料:按如下重量配比计量备取基料(1) Measuring ingredients: measure and prepare the base material according to the following weight ratio
聚四氟乙烯悬浮细料粒径≤200微米 5.8kgPTFE suspension fine particle size ≤ 200 microns 5.8kg
聚四氟乙烯分散细料200微米<粒径≤1000微米 2.2kgPTFE dispersion fine material 200 microns < particle size ≤ 1000 microns 2.2kg
碳黑 粒径≤1000微米 2.8kgCarbon black Particle size ≤ 1000 microns 2.8kg
磷片石墨 粒度≤200目 0.29kgPhosphor flake graphite Particle size≤200 mesh 0.29kg
ADC型发泡剂 0.52kgADC type foaming agent 0.52kg
ADC型发泡剂是可市购的,由宁夏日盛实业有限公司生产的发泡剂成品;ADC type foaming agent is commercially available, and is the foaming agent finished product produced by Ningxia Risheng Industrial Co., Ltd.;
(2)搅拌混料:将计量称取的物料放入混料机内,启动混料机,按1200转/分的转速高速搅拌5分钟,使被搅拌的物料呈现出棉花纤维状,即制得合格的混合料;(2) Stirring and mixing: put the material weighed into the mixer, start the mixer, and stir at a high speed of 1200 rpm for 5 minutes, so that the stirred material appears in the form of cotton fibers, which is ready-made Qualified mixture;
(3)入模干压:将按所设计阴极成品外形尺寸工艺要求制成的压模安装于干压机内,再将搅拌混料制得的混合料送入规格为80目的筛子进行过筛,过筛的混合料放入压模内,按设计要求准确放入混合料的物料量,并在中间配装阴极成品的铜网电极引线,然后施加28MPa的压力,即可一次性干压制得成形阴极;,(3) Dry pressing into the mold: Install the mold made according to the design process requirements of the finished cathode shape and size in the dry press, and then send the mixed material prepared by mixing the mixed material into a sieve with a specification of 80 mesh for sieving , the sieved mixture is put into the die, and the amount of the mixture is accurately put in according to the design requirements, and the copper mesh electrode lead wire of the finished cathode is installed in the middle, and then a pressure of 28MPa is applied to dry press it at one time. shaped cathode;
(4)焙烧定型:将入模干压制得的成形阴极送入电烘箱内进行焙烧定型,精确控制电烘箱内的升温焙烧温度:在1小时内缓慢升温至200℃,再在3小时内继续缓慢升温至350℃进行焙烧后,再继续升温至370℃焙烧4小时,然后自然冷却即制得阴极产品。(4) Roasting and shaping: send the formed cathode into the electric oven for roasting and shaping, and precisely control the heating and roasting temperature in the electric oven: slowly increase the temperature to 200°C within 1 hour, and then continue within 3 hours Slowly raise the temperature to 350°C for calcination, then continue to raise the temperature to 370°C for 4 hours, and then cool naturally to obtain the cathode product.
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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US4278525A (en) * | 1978-04-24 | 1981-07-14 | Diamond Shamrock Corporation | Oxygen cathode for alkali-halide electrolysis cell |
US4456521A (en) * | 1980-10-31 | 1984-06-26 | Diamond Shamrock Corporation | Three layer laminate |
US4500647A (en) * | 1980-10-31 | 1985-02-19 | Diamond Shamrock Chemicals Company | Three layer laminated matrix electrode |
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Publication number | Priority date | Publication date | Assignee | Title |
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US4278525A (en) * | 1978-04-24 | 1981-07-14 | Diamond Shamrock Corporation | Oxygen cathode for alkali-halide electrolysis cell |
US4456521A (en) * | 1980-10-31 | 1984-06-26 | Diamond Shamrock Corporation | Three layer laminate |
US4500647A (en) * | 1980-10-31 | 1985-02-19 | Diamond Shamrock Chemicals Company | Three layer laminated matrix electrode |
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