CN112159975A - 在细长玻璃管内镀金属银制备高压电极的方法 - Google Patents
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1875—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment only one step pretreatment
- C23C18/1879—Use of metal, e.g. activation, sensitisation with noble metals
Abstract
本发明公开了一种在细长玻璃管内镀金属银制备高压电极的方法,其是采用添加尿素和NaCl制备的敏化液,及以三乙醇胺为稳定剂、聚乙二醇为助剂制备的镀银试剂,在细长玻璃管内经清洗、敏化、镀银制得一层厚度为0.5~2μm的银镀层,从而以所得含银镀层的玻璃管作为高压电极,制得放电强度均匀、气体流量均匀的放电管,以进而提高臭氧发生器的臭氧产生效率,并同时提高放电电极的可靠性。
Description
技术领域
本发明具体涉及一种在细长玻璃管内镀金属银制备高压电极的方法。
背景技术
臭氧发生器常用的放电方式是管式放电,高压电极在内侧,接地电极在外侧,中间隔着一层介质材料,从而形成介质阻拦放电。采用的介质材料常为玻璃、陶瓷、搪瓷等,其中玻璃由于其易于加工、可靠性高、安装方便等原因逐渐成为主要应用的介质材料。
臭氧发生器的放电管由早期较粗的放电管逐渐发展为较细的放电管,其优点是提高了放电管产生臭氧的效率,并使臭氧发生器小型化。现行的放电管的型式主要是高压电极、介质、接地电极相互独立分离的,即高压电极与介质之间或接地电极与介质之间都有空隙,即使某一电极与介质有接触,也不是紧密接触,这会使气体流经放电管的介质两侧时的气量不均匀,介质两侧的放电强度也不均匀,会对臭氧产生效率有一定影响。
通常介质镀银要经过介质表面清洗、粗化、敏化、活化、化学镀银等步骤,常用于介质外表面或平整介质表面镀银。对于细长玻璃管内壁镀银,由于其结构的特殊性,要求镀银致密均匀,且厚度1μm以上,难度大,目前未见相关报道。
发明内容
本发明的目的在于提供一种在细长玻璃管内镀金属银制备高压电极的方法,其是在介质玻璃管的内侧镀一层导电性能良好的银作为高压电极,使高压电极与玻璃管的间隙消失,放电只在玻璃管和接地电极之间产生,气体也只从玻璃管和接地电极之间的间隙流过,从而得到放电强度均匀、气体流量均匀的放电管,最终提高臭氧产生效率,同时会进一步提高放电电极的可靠性。
为实现上述目的,本发明采用如下技术方案:
一种在细长玻璃管内镀金属银制备高压电极的方法,其包括以下步骤:
1)将细长玻璃管(内径为10~20mm,壁厚为1.0~2.0mm,长度不超过3000mm)清洗干净,晾干备用;
2)将洗净的玻璃管一端封闭,垂直竖立,使封闭端向下,然后将敏化液缓慢倒入玻璃管内,直至加满,静置1h进行敏化;敏化结束后倒出敏化液,用水冲洗玻璃管内壁,洗去残留敏化液,再将玻璃管竖直倒置,控干水分,晾干5~10分钟;
3)将敏化后玻璃管竖立垂直,使封闭端向下固定,然后将镀银试剂缓缓加入玻璃管内(镀银试剂加入量按玻璃管内所需镀银的长度确定);
4)将加入镀银试剂的玻璃管在20~25℃下静置3h,使玻璃管内壁镀上一层厚度为0.5~2μm的光亮银镀层;
5)镀银完成后,倾倒出镀银试剂,用水冲洗玻璃管内壁,晾干,即得所述高压电极。
步骤2)所述敏化液是将30g SnCl2·2H2O、200g NaCl和50g尿素于1000mL水中搅拌溶解,再加入30mL体积浓度为37%的盐酸溶液,搅拌混匀即得。
敏化液通常采用SnCl2加高浓度HCl进行配制,以使介质材料表面吸附二价锡离子,且其水解产物具有还原性,可把银氨络合物还原成金属银。但由于其中二价Sn会被氧化成四价Sn,故这种敏化液不易长时间保存,用于敏化玻璃管效果也不够稳定。本发明在敏化液中添加尿素和NaCl后,可抑制二价Sn的氧化,使敏化液可长期存放使用,并可使敏化效果稳定,且其还能使HCl的用量大大减少,更加安全环保。
步骤3)所述镀银试剂是将A液和B液按体积比1:1混合制得;
所述A液是将20g AgNO3和10g NaOH加入到500mL水中,搅拌混合,再加入30mL质量浓度为28%的氨水溶液,充分搅拌至沉淀溶解制得;
所述B液是将100g酒石酸钾钠加入到500mL水中,搅拌至酒石酸钾钠溶解,再加入50g三乙醇胺、10g聚乙二醇,搅拌溶解制得。
玻璃管内壁镀银的镀层要求致密,厚度2μm,尤其是细长玻璃管内壁要达到要求,对镀液和镀液过程要控制好,首先要求镀液的Ag离子浓度要高,其次要求镀液稳定。在镀银过程中,银要缓慢在玻管壁上析出,并牢固结合。这就需要合适的稳定剂,控制反应条件。反应中银离子的还原剂常用有酒石酸钾钠(罗谢尔盐)、果糖、右旋葡萄糖、葡庚糖酸钠以及葡萄糖醇(山梨醇)等,不同还原剂对银的沉积率有影响。同时,化学镀银液是一个热力学不稳定的体系,由于局部过热、pH过高或某些杂质的影响等原因,不可避免地会在镀液中出现一些活化微粒催化核心,这往往会导致镀液在短时间内发生分解。本发明采用三乙醇胺作为稳定剂,能有效抑制镀液的自发分解,掩蔽这些活性催化核心,使施镀过程在控制下有序进行,提高镀银效果;而适当添加聚乙二醇作为助剂对镀银反应比较有利,可得到表面状况较好的镀层。
本发明的显著优点在于:
1)本发明在细长玻璃管内壁用化学法镀上一层均匀的、厚度在0.5~2μm之间的银镀层,其均匀致密光亮,与玻璃管贴合紧密,用其作为高压电极导电性能优良,电阻率为2.0×10-8Ω m。
2)与常规的臭氧发生器以金属管作内电极相比,本发明省去了金属管内电极的使用,而直接以银镀层为内电极,可节约生产成本。同时,由于省去了金属管內电极,可减轻放电电极的重量,并排除金属管对玻璃(或陶瓷)介质的挤压,提高玻璃(或陶瓷)介质的可靠性,从而可整体提高臭氧发生器的可靠性。
3)以本发明制备的内壁镀银的玻璃管用作臭氧发生器放电管的高压电极,能提高放电管的工作效率,提高臭氧浓度和臭氧产量,使其整体提高效率5~10%。
附图说明
图1为利用实施例制备的高压电极制作的臭氧发生器在放电间隙0.15mm,O2为气源,冷却水温25℃条件下不同进气压力的功率进气比与生成臭氧浓度的关系图。
具体实施方式
为了使本发明所述的内容更加便于理解,下面结合具体实施方式对本发明所述的技术方案做进一步的说明,但是本发明不仅限于此。
实施例
一、清洗
细长玻璃管在镀银之前,先进行清洗,以确保玻璃管内壁干净。即将玻璃管于1N的盐酸溶液中浸泡1小时,取出后用自来水反复冲洗,直至管壁上没有残留的盐酸为止,再将玻璃管晾干,储存在干净的箱子里备用。
二、敏化
1. 称取30g的SnCl2·2H2O,200g的NaCl,50g的尿素,放入3L的烧杯里,并往烧杯里加入1000ml的蒸馏水,用玻棒缓慢搅拌,使各物质溶化,再小心加入30ml体积浓度为37%的HCl溶液,搅拌混合均匀,得敏化液。把配制好的敏化液用储罐装好,密闭,放置阴凉干燥处存放。
2. 将洗净的玻璃管一端封闭,垂直竖立,使封闭端向下,通过漏斗将敏化液缓慢加入玻璃管内,直至加满,然后将玻璃管静置1h进行敏化;敏化结束后,将敏化液回收倒储罐,阴凉干燥处储存,以多次重复利用;敏化后的玻璃管用自来水冲洗内壁,去除残留的敏化液,再将玻璃管竖直倒置,控干自来水,晾干5~10分钟。
三、镀银
1. 将20g AgNO3和10g NaOH加入到玻璃容器中,并加入500mL蒸馏水,搅拌混合,再加入30mL质量浓度为28%的氨水溶液,充分搅拌至沉淀溶解,制得A液;将100g酒石酸钾钠于玻璃容器中,并加入500mL蒸馏水,搅拌至酒石酸钾钠溶解,再加入50g三乙醇胺、10g聚乙二醇,搅拌溶解,制得B液。
2. 将敏化后的玻璃管竖立垂直,使封闭端向下固定,然后将A液和B液混合均匀后,通过漏斗缓缓加入玻璃管内(混合后的镀银试剂应立刻倒入玻璃管内壁进行镀银,最迟应在20分钟内将镀银试剂用完,镀银试剂加入量按玻璃管内所需镀银的长度确定)。
3. 将加入镀银试剂的玻璃管在20~25℃下静置3h,使玻璃管内壁镀上一层厚度约为0.5~2μm的光亮银镀层。
4. 镀银完成后,倾倒出镀银试剂,将玻璃管用自来水冲洗干净,晾干,即得高压电极。
以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。
Claims (5)
1.一种在细长玻璃管内镀金属银制备高压电极的方法,其特征在于:包括以下步骤:
1)将细长玻璃管清洗干净,晾干备用;
2)将洗净的玻璃管一端封闭,垂直竖立,使封闭端向下,然后将敏化液缓慢倒入玻璃管内,直至加满,静置1h进行敏化;敏化结束后倒出敏化液,用水冲洗玻璃管内壁,洗去残留敏化液,再将玻璃管竖直倒置,控干水分,晾干5~10分钟;
3)将敏化后玻璃管竖立垂直,使封闭端向下固定,然后将镀银试剂缓缓加入玻璃管内;
4)将加入镀银试剂的玻璃管在20~25℃下静置3h,使玻璃管内壁镀上一层光亮的银镀层;
5)镀银完成后,倾倒出镀银试剂,用水冲洗玻璃管内壁,晾干,即得所述高压电极。
2.根据权利要求1所述的在细长玻璃管内镀金属银制备高压电极的方法,其特征在于:所述细长玻璃管的内径为10~20mm,壁厚为1.0~2.0mm,长度不超过3000mm。
3. 根据权利要求1所述的在细长玻璃管内镀金属银制备高压电极的方法,其特征在于:步骤2)所述敏化液是将30g SnCl2·2H2O、200g NaCl和50g尿素于1000mL水中搅拌溶解,再加入30mL体积浓度为37%的盐酸溶液,搅拌混匀即得。
4.根据权利要求1所述的在细长玻璃管内镀金属银制备高压电极的方法,其特征在于:步骤3)所述镀银试剂是将A液和B液按体积比1:1混合制得;
所述A液是将20g AgNO3和10g NaOH加入到500mL水中,搅拌混合,再加入30mL质量浓度为28%的氨水溶液,充分搅拌至沉淀溶解制得;
所述B液是将100g酒石酸钾钠加入到500mL水中,搅拌至酒石酸钾钠溶解,再加入50g三乙醇胺、10g聚乙二醇,搅拌溶解制得。
5.根据权利要求1所述的在细长玻璃管内镀金属银制备高压电极的方法,其特征在于:步骤4)所得银镀层的厚度为0.5~2μm。
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