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Publication numberCN103436013 A
Publication typeApplication
Application numberCN 201310388264
Publication date11 Dec 2013
Filing date30 Aug 2013
Priority date30 Aug 2013
Also published asCN103436013B
Publication number201310388264.4, CN 103436013 A, CN 103436013A, CN 201310388264, CN-A-103436013, CN103436013 A, CN103436013A, CN201310388264, CN201310388264.4
Inventors齐暑华, 张欣欣, 钟晓兰, 何征, 邱华, 黄英
Applicant西北工业大学
Export CitationBiBTeX, EndNote, RefMan
External Links: SIPO, Espacenet
Preparation method of polyaniline/sliver-coated/cobalt ferrite composite material
CN 103436013 A
Abstract
The invention discloses a preparation method of a polyaniline/sliver-coated/cobalt ferrite composite material. The preparation method comprises the following steps: respectively weighing three substances according to a stoichiometric ratio of cobalt nitrate to ferric nitrate to citric acid of 1:2:4: preparing cobalt ferrite (CoFe2O4) by adopting a sol-gel process; carrying out chemical silver-plating onto the prepared CoFe2O4 to obtain wave-absorbing filler with excellent electromagnetic performances; and preparing PANI (Polyaniline)/Ag/CoFe2O4 composite material by using aniline monomer and Ag/CoFe2O4 as raw materials through a chemical in-situ polymerization method. The composite material is combined with the excellent electrical performance of metal single substance Ag, the good magnetic performance of CoFe2O4 as well as good processability, stability and electrical performance of the conductive high polymer polyaniline, is a good microwave-absorbing material, and has an important application value in the microwave-absorbing field. The Ag/CoFe2O4 composite filler obtained by the preparation method disclosed by the invention is combined with the excellent electrical performance of the Ag and the good magnetic performance of the CoFe2O4, and is a good electromagnetic composite material; the PANI/Ag/CoFe2O4 prepared by using the composite material as the filler has good microwave-absorbing performance.
Claims(10)  translated from Chinese
1.ー种聚苯胺/镀银/钴铁氧体复合材料的制备方法,其特征在于步骤如下: 步骤1:以硝酸钴:硝酸铁:柠檬酸的化学计量比为1:2:4分别称取三种物质,分别加入蒸馏水溶解,之后混合;再滴加氨水调节溶液PH值至中性,于80〜120C水浴中加热至溶液呈胶体状,将胶体取出放入烘箱中100〜150C烘干2〜4h,之后取出放入马弗炉中850C下煅烧2〜4h,自然冷却得到钴铁氧体CoFe2O4 ; 步骤2:对CoFe2O4进行预处理,包括粗化、敏化和活化处理; 步骤3:将预处理后的CoFe2O4加入到银氨溶液中,搅拌分散后,滴加甲醛溶液,室温下反应40〜90min后将产物抽滤水洗,并在50〜100C下真空干燥24h得到Ag/CoFe204 ;所述CoFe2O4和AgNO3的质量比为mC()Fe2Q4:mAgN03=l:0.8〜3 ;所述甲醛溶液与银氨溶液的体积比为V甲酸溶液:V银氨溶液=I: 3〜8; 步骤4、采用化学原位聚合法合成PANI/Ag/CoFe204:将苯胺单体加入到盛有盐酸溶液的三ロ烧瓶中,搅拌均匀之后,加入Ag/CoFe204和十六烷基三甲基溴化铵CTAB后超声分散;冰浴条件下缓慢滴加过硫酸铵APS的盐酸溶液,滴加结束后反应6h,将产物先后用丙酮、水洗涤,再用盐酸溶液二次掺杂,在80C条件下真空干燥24h得到聚苯胺/镀银/钴铁氧体复合材料;所述苯胺単体和HCl溶液的体积比为: Vaclga=I: 30〜50;所述苯胺单体和Ag/CoFe204的质量比为m 苯胺:mAg/CoFe204_l: 2〜I ;所述苯胺単体和CTAB的质量比为1: 0.2 ;所述苯胺单体和APS的质量比为111_:1haps=I: 2〜4,苯胺和APS的盐酸溶液的体积比为VJS: Vaps溶液=I: 20〜30。 1. ー kinds of polyaniline / silver / cobalt ferrite preparing a composite material comprising the following steps: Step 1: cobalt nitrate: ferric nitrate: Citric acid stoichiometric ratio of 1: 2: 4 respectively, said Take three substances were dissolved in distilled water was added, followed by mixing; then dropping ammonia solution was adjusted to neutral PH value, and heated at 80~120 C in a water bath until the solution was colloid, the colloid out into the oven 100~150 C drying 2~4h, after removing a muffle furnace at 850 C calcined 2~4h, naturally cooled to obtain cobalt ferrite CoFe2O4; Step 2: CoFe2O4 pretreatment, including roughening, sensitization and activation; Step 3: The CoFe2O4 ammonia solution was added to the silver in the pretreated, after stirring the dispersion was added dropwise formaldehyde solution, the reaction product was suction filtered washed with water after 40~90min at room temperature, and at 50~100 C under vacuum 24h dried to give Ag / CoFe204; quality of the CoFe2O4 and AgNO3 ratio mC () Fe2Q4: mAgN03 = l: 0.8~3; the volume of formaldehyde solution and ammonia solution of silver ratio V formic acid solution: V silver ammonia solution = I: 3~8; step 4, the use of chemical-situ Polymerization PANI / Ag / CoFe204: aniline monomer is added to a solution containing hydrochloric acid three ro flask, stir after adding Ag / CoFe204 and hexadecane trimethyl ammonium bromide after ultrasonic dispersion CTAB; slowly dropped under ice over a hydrochloric acid solution of ammonium APS, after dropping the reaction 6h, the product was washed with acetone, washed with water, and then mixed with hydrochloric acid solution twice miscellaneous, at 80 C and dried under vacuum conditions 24h polyaniline / silver / cobalt ferrite composites; the aniline radiolabeling body and HCl solution volume ratio: Vaclga = I: 30~50; the aniline monomer and Ag / CoFe204 mass ratio m aniline: mAg / CoFe204_l: 2~I; the aniline and CTAB radiolabeling body mass ratio was 1: 0.2; the quality of the aniline monomer and APS ratio 111_: 1haps = I: 2 ~ 4, aniline and APS volume ratio of hydrochloric acid solution V JS: Vaps solution = I: 20~30.
2.根据权利要求1所述聚苯胺/镀银/钴铁氧体复合材料的制备方法,其特征在于:所述步骤2中的粗化是用体积分数为5〜20%的HNO3溶液超声处理10〜30min。 2. 1 The polyaniline / silver / cobalt ferrite composite material preparation method according to claim, characterized in that: the step 2 roughening is the volume fraction of 5~20% HNO3 solution sonication 10~30min.
3.根据权利要求1所述聚苯胺/镀银/钴铁氧体复合材料的制备方法,其特征在于:所述步骤2中的敏化是用10〜50g/L的SnCl2溶液超声处理10〜30min。 According to claim 1 wherein the polyaniline / silver / cobalt ferrite composite material preparation method of claim wherein: the step 2 sensitizing solution is treated with SnCl2 ultrasound 10~50g / L of 10~ 30min.
4.根据权利要求1所述聚苯胺/镀银/钴铁氧体复合材料的制备方法,其特征在于:所述步骤2中的活化是用0.2〜lg/L的PdCl2溶液超声处理30〜60min。 According to claim 1 wherein the polyaniline / silver / cobalt ferrite composite material preparation method of claim wherein: the step 2 activation is treated with PdCl2 solution ultrasonic 0.2~lg / L of 30~60min .
5.根据权利要求1所述聚苯胺/镀银/钴铁氧体复合材料的制备方法,其特征在于:所述步骤3中的银氨溶液要求现配。 5. 1 of the polyaniline / silver / cobalt ferrite composite material preparation method of claim wherein: the step 3 silver ammonia solution requires existing service.
6.根据权利要求1所述聚苯胺/镀银/钴铁氧体复合材料的制备方法,其特征在于:所述AgNO3溶液的浓度为0.01〜0.5mol/L。 6. One of the polyaniline / silver / cobalt ferrite composite material preparation method according to claim, wherein: the concentration of the AgNO3 solution is 0.01~0.5mol / L.
7.根据权利要求1所述聚苯胺/镀银/钴铁氧体复合材料的制备方法,其特征在于:所述甲醛溶液的浓度为40〜100g/L。 7.1 The polyaniline / silver / cobalt ferrite composite material preparation method according to claim, characterized in that: the concentration of formaldehyde solution was 40~100g / L.
8.根据权利要求1所述聚苯胺/镀银/钴铁氧体复合材料的制备方法,其特征在于:所述步骤4中HCl溶液的浓度为0.lmol/L。 1 8. The polyaniline / silver / cobalt ferrite preparing composite material according to claim, characterized in that: the concentration of the HCl solution in step 4 is 0.lmol / L.
9.根据权利要求1所述聚苯胺/镀银/钴铁氧体复合材料的制备方法,其特征在于:所述步骤4中用丙酮、去离子水洗漆时间为15min。 9.1 The polyaniline / silver / cobalt ferrite composite material preparation method according to claim, wherein: the step 4 with acetone, deionized water paint time of 15min.
10.根据权利要求1所述聚苯胺/镀银/钴铁氧体复合材料的制备方法,其特征在于:所述步骤4中HCl溶液浓度为0.lmol/L。 10.1 The polyaniline / silver / cobalt ferrite composite material preparation method according to claim, wherein: the step 4 solution of HCl concentration 0.lmol / L.
Description  translated from Chinese

ー种聚苯胺/镀银/钴铁氧体复合材料的制备方法ー kinds of polyaniline / silver / cobalt ferrite preparing composite materials

技术领域 Technical Field

[0001] 本发明涉及ー种聚苯胺/镀银/钴铁氧体复合材料的制备方法,所制得的复合材料可用于微波吸收领域。 [0001] The present invention relates ー kinds of polyaniline / silver / cobalt ferrite preparation of composite materials, the obtained composite material can be used in microwave absorption fields.

背景技术 Background

[0002] 常用的微波吸收材料包括铁氧体、导电高聚物、碳纳米材料等。 [0002] The conventional microwave absorbing materials include ferrites, conducting polymers, carbon nano-materials. 铁氧体具有较高的饱和磁化強度和磁损耗,是最常用的吸波填料,有着尖晶石结构的钴铁氧体具有较高的饱和磁化強度和矫顽力,是性能优异的磁性材料。 Ferrites have a high saturation magnetization and magnetic loss, is the most common absorbing filler, has a cobalt ferrite spinel structure has a high saturation magnetization and the coercive force of the magnetic material is excellent performance . 导电高聚物主要由聚苯胺、聚吡咯、聚噻吩等,聚苯胺因成本低、合成简便、电导率高、环境稳定性好一集独特的物理、化学、电磁性能备受关注。 Conductive polymer mainly composed of polyaniline, polypyrrole, polythiophene, polyaniline due to low cost, simple synthesis, high conductivity, good environmental stability of a unique set of physical, chemical and electromagnetic properties of concern.

[0003] 吸波材料的基本要求是“薄、轻、宽、高”,即厚度薄、质量轻、频段宽、強度高。 [0003] The basic requirements of absorbing material is "thin, light, wide and high," that is thin, light weight, wide band, high strength. 但是,使用単一填料往往吸收机理単一、微波吸收频段窄,为了解决这些问题,将上述多种吸波填料复合为一体,集各家所长,利于制备具有质轻、宽频、高强的微波吸收复合材料。 However, the use of a filler often radiolabeling absorption mechanism radiolabeling a microwave absorption band is narrow, in order to solve these problems, the above multiple absorbing filler composite as a whole, set each director, which will help prepare a microwave light, broadband, high-strength absorbent composite.

发明内容 DISCLOSURE

[0004] 要解决的技术问题 [0004] The technical problem to be solved

[0005] 为了避免现有技术的不足之处,本发明提出ー种聚苯胺/镀银/钴铁氧体复合材料的制备方法,将聚苯胺、钴铁氧体以及金属单质银复合,制备出兼有良好电性能和磁性能的微波吸收复合材料。 [0005] In order to avoid the shortcomings of the prior art, the present invention proposes ー kinds of polyaniline / silver / cobalt ferrite preparing composite material, polyaniline, cobalt ferrite and metal elemental silver compound was prepared both good electrical properties and magnetic microwave absorbing composite.

[0006] 技术方案 [0006] Technical Solution

`[0007] —种聚苯胺/镀银/钴铁氧体复合材料的制备方法,其特征在于步骤如下: `[0007] - the kind of polyaniline / silver / cobalt ferrite composite material, which is characterized by the following steps:

[0008] 步骤1:以硝酸钴:硝酸铁:柠檬酸的化学计量比为1:2:4分别称取三种物质,分别加入蒸馏水溶解,之后混合;再滴加氨水调节溶液PH值至中性,于80〜120C水浴中加热至溶液呈胶体状,将胶体取出放入烘箱中100〜150C烘干2〜4h,之后取出放入马弗炉中850C下煅烧2〜4h,自然冷却得到钴铁氧体CoFe2O4 ; [0008] Step 1: cobalt nitrate: iron nitrate: citric acid stoichiometric ratio of 1: 2: 4 were weighed three substances were added to distilled water, after mixing; then dropping ammonia solution was adjusted to a value of PH sex, at 80~120 C water bath until the solution was gel-like, out into the colloidal 100~150 C oven drying 2~4h, after removing a muffle furnace at 850 C calcined 2 ~ 4h, naturally cooled to obtain cobalt ferrite CoFe2O4;

[0009] 步骤2:对CoFe2O4进行预处理,包括粗化、敏化和活化处理; [0009] Step 2: CoFe2O4 pretreatment, including roughening, sensitization and activation;

[0010] 步骤3:将预处理后的CoFe2O4加入到银氨溶液中,搅拌分散后,滴加甲醛溶液,室温下反应40〜90min后将产物抽滤水洗,并在50〜100C下真空干燥24h得到Ag/CoFe204 ;所述CoFe2O4和AgNO3的质量比为nwe2Q4:mAgN03=l:0.8〜3 ;所述甲醛溶液与银氨溶液的体 [0010] Step 3: After the pretreatment CoFe2O4 added to the silver ammonia solution, stirred dispersion was added dropwise formaldehyde solution, the reaction product was suction filtered at room temperature 40~90min After washing with water, and 50~100 C under vacuum 24h dried to give Ag / CoFe204; quality of the CoFe2O4 and AgNO3 ratio nwe2Q4: mAgN03 = l: 0.8~3; formaldehyde solution and the ammonia solution of silver body

积比为V甲酸溶液:V银氨溶液=I: 3〜8; Formic acid solution volume ratio V: V silver ammonia solution = I: 3~8;

[0011] 步骤4、采用化学原位聚合法合成PANI/Ag/CoFe204:将苯胺单体加入到盛有盐酸溶液的三ロ烧瓶中,搅拌均匀之后,加入Ag/CoFe204和十六烷基三甲基溴化铵CTAB后超声分散;冰浴条件下缓慢滴加过硫酸铵APS的盐酸溶液,滴加结束后反应6h,将产物先后用丙酮、水洗涤,再用盐酸溶液二次掺杂,在80C条件下真空干燥24h得到聚苯胺/镀银/钴铁氧体复合材料;所述苯胺単体和HCl溶液的体积比为乂_: Vaclga=I: 30〜50;所述苯 [0011] Step 4, the use of chemical-situ Polymerization PANI / Ag / CoFe204: aniline monomer is added to a solution containing hydrochloric acid three ro flask, stir after adding Ag / CoFe204 and Cetyltrimethylammonium After ultrasonic dispersion ammonium bromide CTAB; it was slowly added dropwise under ice-hydrochloric acid solution through the APS ammonium persulfate, after the completion of the reaction dropwise 6h, the product was washed with acetone, washed with water, hydrochloric acid solution and then twice doping, in 80 C under vacuum drying conditions 24h polyaniline / silver / cobalt ferrite composites; the volume of the body and the radiolabeling aniline HCl solution = qe _: Vaclga = I: 30~50; the benzene

胺单体和Ag/CoFe204的质量比为m 苯胺:mAg/CoFe204_l: Amine monomer and Ag / CoFe204 mass ratio m aniline: mAg / CoFe204_l:

2〜I ;所述苯胺单体和CTAB的质量比为1: 0.2 ;所述苯胺単体和APS的质量比为: mAPS=l: 2〜4,苯胺和APS的盐酸溶液的体积比为Vms: Vaps-=I: 20〜30。 2~I; the aniline monomer and CTAB mass ratio of 1: 0.2; the quality of the body and the APS aniline radiolabeling ratio: mAPS = l: 2~4, aniline and APS volume ratio of hydrochloric acid solution Vms: Vaps- = I: 20~30.

[0012] 所述步骤2中的粗化是用体积分数为5〜20%的HNO3溶液超声处理10〜30min。 [0012] The step of roughening is the volume fraction of 5~20% of 2 HNO3 solution sonication 10~30min.

[0013] 所述步骤2中的敏化是用10〜50g/L的SnCl2溶液超声处理10〜30min。 [0013] The sensitizing step 2 is treated with SnCl2 solution ultrasonic 10~50g / L of 10~30min.

[0014] 所述步骤2中的活化是用0.2〜lg/L的PdCl2溶液超声处理30〜60min。 [0014] The activation step 2 is treated with a solution of PdCl2 ultrasonic 0.2~lg / L of 30~60min.

[0015] 所述步骤3中的银氨溶液要求现配。 [0015] The step 3 silver ammonia solution requires existing service.

[0016] 所述AgNO3溶液的浓度为0.01〜0.5mol/L。 [0016] The concentration of the AgNO3 solution was 0.01~0.5mol / L.

[0017] 所述甲醛溶液的浓度为40〜100g/L。 [0017] The concentration of the formaldehyde solution is 40~100g / L.

[0018] 所述步骤4中HCl溶液的浓度为0.lmol/L。 Concentration [0018] The step 4 HCl solution is 0.lmol / L.

[0019] 所述步骤4中用丙酮、去离子水洗涤时间为15min。 [0019] The step 4 with acetone, washed with deionized water, time of 15min.

[0020] 所述步骤4中HCl溶液浓度为0.lmol/L。 [0020] in the step 4 solution of HCl concentration 0.lmol / L.

[0021] 有益效果 [0021] The beneficial effects

[0022] 本发明提出的ー种聚苯胺/镀银/钴铁氧体复合材料的制备方法,按照硝酸钴、硝酸铁、柠檬酸的化学计量比为1:2:4分别称取三种物质,采用溶胶凝胶法制备钴铁氧体(CoFe2O4),在对所制得的CoFe2O4进行化学镀银,从而得到电磁性能优异的吸波填料。 [0022] The present invention proposes ー kinds of polyaniline / silver / cobalt ferrite composite material preparation method, in accordance with cobalt nitrate, iron nitrate and citric acid stoichiometric ratio of 1: 2: 4 are weighed three material prepared by sol-gel cobalt ferrite (CoFe2O4), in the prepared CoFe2O4 for chemical silvering to obtain excellent electromagnetic properties of absorbing filler. 最終以苯胺単体、Ag/CoFe204为原料,采用化学原位聚合法制备PANI/Ag/CoFe204复合材料。 Eventually aniline radiolabeling body, Ag / CoFe204 as raw materials, chemical situ polymerization PANI / Ag / CoFe204 composites. 改复合材料结合了金属单质Ag优异的电性能、CoFe2O4良好的磁性能以及导电高聚物聚苯胺良好的加工性、稳定性及电性能,是ー种很好的微波吸收材料,在微波吸收领域具有重要的应用价值。 Change composite and metallic elemental Ag excellent electrical properties, CoFe2O4 good magnetic and electrically conductive polymer polyaniline good processability, stability and electrical properties, it is ー kind good microwave absorbing materials in the field of microwave absorption It has an important application value. 本发明方法得到的Ag/CoFe204复合填料结合了Ag优异的电性能和CoFe2O4良好的磁性能,是ー种很好的电磁复合材料,将其作为填料制得的PANI/Ag/CoFe204复合材料具有良好的微波吸收性能。 The method of the present invention obtained Ag / CoFe204 composite fillers combined with Ag CoFe2O4 excellent electrical properties and good magnetic properties, is ー kind of good electromagnetic composite material, which is used as a filler obtained PANI / Ag / CoFe204 composites have good microwave absorption.

具体实施方式 DETAILED DESCRIPTION

[0023] 现结合实施例对本发明作进ー步描述: [0023] now with an embodiment of the present invention will be further described into ー:

[0024] 实施例1: [0024] Example 1:

[0025] 制备CoFe2O4:称取5.8210g硝酸钴、16.16g硝酸铁、16.8112g柠檬酸,分别加入蒸馏水中溶解,之后混合,加入氨水调节溶液PH值为7,于90C下水浴加热至溶液呈胶体状,之后将胶体状产物放入烘箱中130C干燥5h,取出产物放入马弗炉中850C煅烧3h,自然冷却即可得到CoFe2O4。 [0025] Preparation CoFe2O4: Weigh 5.8210g of cobalt nitrate, 16.16g ferric nitrate, 16.8112g of citric acid were dissolved in distilled water was added, after mixing, the solution was added ammonia to adjust PH value of 7 at 90 C water bath was heated until the solution was gel-like, after which the gel-like product in 130 C oven drying 5h, remove the product placed in a muffle furnace and calcined 850 C 3h, natural cooling can be obtained CoFe2O4.

[0026] 对CoFe2O4进行化学镀银:将CoFe2O4加入体积分数为10%的HNO3溶液超声处理5min,抽滤水洗至中性;采用浓度为45g/L的SnCl2+HCl溶液超声处理5min,抽滤水洗至中性;采用0.5g/L的PdCl2溶液超声处理15min,抽滤水洗至中性。 [0026] The chemical silvering CoFe2O4: The CoFe2O4 volume fraction of 10% HNO3 solution ultrasonic treatment 5min, filtration and washing to neutral; with a concentration of SnCl2 + HCl solution sonication 45g / L of 5min, water filtration to neutral; PdCl2 solution using ultrasonic 0.5g / L treatment 15min, washed with water to neutral leaching. 称取0.0lmol AgNO3,加入去离子水配成浓度为0.05mol/L的AgNO3溶液,不断搅拌下缓慢滴加氨水制得银氨溶液。 Weigh 0.0lmol AgNO3, adding deionized water to form a concentration of 0.05mol / AgNO3 solution L continuously stirred slowly dropping ammonia to prepare the silver ammonia solution. 将溶液放入烧杯中,加入Ig预处理完成的CoFe2O4,持续电动搅拌,之后缓慢滴加50ml浓度为80g/L的甲醛溶液,反应60min,将产物抽滤水洗,并在80C下进行真空干燥24h。 The solution was placed in a beaker, added CoFe2O4, electric Ig continuous stirring to complete the pretreatment, after the concentration was slowly added dropwise 50ml of 80g / L of formaldehyde solution, the reaction 60min, the product was suction filtered washed with water, and at 80 C under vacuum Drying 24h.

[0027] PANI/Ag/CoFe204的制备:将3ml苯胺单体加入到盛有IOOml0.lmol/L的HCl溶液的三ロ烧瓶中,搅拌均匀。 Preparation [0027] PANI / Ag / CoFe204 of: 3ml of aniline was added to the flask containing three ro IOOml0.lmol / HCl solution of L and stirred evenly. 加入0.6g Ag/CoFe204和0.2gCTAB,超声分散30min,之后在冰浴条件下,缓慢滴加50ml含有9gAPS的HCl (0.lmol/L)溶液,冰浴反应6h,反应结束后分别用丙酮、去离子水洗涤各15min,再用0.lmol/L的HCl溶液二次掺杂1.5h。 Add 0.6g Ag / CoFe204 and 0.2gCTAB, ultrasonic dispersion 30min, then under ice-cooling, was slowly added dropwise 50ml of 9gAPS containing HCl (0.lmol / L) solution, the ice bath was reacted 6h, respectively, after the reaction with acetone, deionized water each 15min, then HCl solution 0.lmol / L of the secondary doping 1.5h. 最终在80C条件下真空干燥24h。 Final conditions at 80 C and dried under vacuum 24h.

[0028] 实施例2: [0028] Example 2:

[0029] CoFe2O4的制备及化学镀银过程同实施例1。 Preparation and silver plating process [0029] CoFe2O4 the same as in Example 1.

[0030] PANI/Ag/CoFe204的制备:将3ml苯胺单体加入到盛有IOOml0.lmol/L的HCl溶液的三ロ烧瓶中,搅拌均匀。 Preparation [0030] PANI / Ag / CoFe204 of: 3ml of aniline was added to the flask containing three ro IOOml0.lmol / HCl solution of L and stirred evenly. 加入1.2g Ag/CoFe204和0.2gCTAB,超声分散30min,之后在冰浴条件下,缓慢滴加50ml含有9gAPS的HCl (0.lmol/L)溶液,冰浴反应6h,反应结束后分别用丙酮、去离子水洗涤各15min,再用0.lmol/L的HCl溶液二次掺杂1.5h。 Add 1.2g Ag / CoFe204 and 0.2gCTAB, ultrasonic dispersion 30min, then under ice-cooling, was slowly added dropwise 50ml of 9gAPS containing HCl (0.lmol / L) solution, the ice bath was reacted 6h, respectively, after the reaction with acetone, deionized water each 15min, then HCl solution 0.lmol / L of the secondary doping 1.5h. 最终在80C条件下真空干燥24h。 Final conditions at 80 C and dried under vacuum 24h.

[0031] 实施例3: [0031] Example 3:

[0032] CoFe2O4的制备及化学镀银过程同实施例1。 Preparation and silver plating process [0032] CoFe2O4 the same as in Example 1.

[0033] PANI/Ag/CoFe204的制备:将3ml苯胺单体加入到盛有IOOml0.lmol/L的HCl溶液的三ロ烧瓶中,搅拌均匀。 Preparation [0033] PANI / Ag / CoFe204 of: 3ml of aniline was added to the flask containing three ro IOOml0.lmol / HCl solution of L and stirred evenly. 加入1.8g Ag/CoFe204和0.2gCTAB,超声分散30min,之后在冰浴条件下,缓慢滴加50ml含有9gAPS的HCl (0.lmol/L)溶液,冰浴反应6h,反应结束后分别用丙酮、去离子水洗涤各15min,再用0.lmol/L的HCl溶液二次掺杂1.5h。 Add 1.8g Ag / CoFe204 and 0.2gCTAB, ultrasonic dispersion 30min, then under ice-cooling, was slowly added dropwise 50ml of 9gAPS containing HCl (0.lmol / L) solution, the ice bath was reacted 6h, respectively, after the reaction with acetone, deionized water each 15min, then HCl solution 0.lmol / L of the secondary doping 1.5h. 最终在80C条件下真空干燥24h。 Final conditions at 80 C and dried under vacuum 24h.

[0034] 实施例4: [0034] Example 4:

[0035] CoFe2O4的制备及化学镀银过程同实施例1。 Preparation and silver plating process [0035] CoFe2O4 the same as in Example 1.

[0036] PANI/Ag/CoFe204的制备:将3ml苯胺单体加入到盛有IOOml0.lmol/L的HCl溶液的三ロ烧瓶中,搅拌均匀。 Preparation [0036] PANI / Ag / CoFe204 of: 3ml of aniline was added to the flask containing three ro IOOml0.lmol / HCl solution of L and stirred evenly. 加入2.4`g Ag/CoFe204和0.2gCTAB,超声分散30min,之后在冰浴条件下,缓慢滴加50ml含有9gAPS的HCl (0.lmol/L)溶液,冰浴反应6h,反应结束后分别用丙酮、去离子水洗涤各15min,再用0.lmol/L的HCl溶液二次掺杂1.5h。 Add 2.4`g Ag / CoFe204 and 0.2gCTAB, ultrasonic dispersion 30min, then under ice-cooling, was slowly added dropwise 50ml of 9gAPS containing HCl (0.lmol / L) solution, the ice bath was reacted 6h, respectively, after the reaction with acetone , washed with deionized water each 15min, then 0.lmol / HCl solution L secondary doping 1.5h. 最终在80C条件下真空干燥24h。 Final conditions at 80 C and dried under vacuum 24h.

[0037] 实施例5: [0037] Example 5:

[0038] CoFe2O4的制备及化学镀银过程同实施例1。 Preparation and silver plating process [0038] CoFe2O4 the same as in Example 1.

[0039] PANI/Ag/CoFe204的制备:将3ml苯胺单体加入到盛有IOOml0.lmol/L的HCl溶液的三ロ烧瓶中,搅拌均匀。 Preparation [0039] PANI / Ag / CoFe204 of: 3ml of aniline was added to the flask containing three ro IOOml0.lmol / HCl solution of L and stirred evenly. 加入3g Ag/CoFe204和0.2gCTAB,超声分散30min,之后在冰浴条件下,缓慢滴加50ml含有9gAPS的HCl (0.lmol/L)溶液,冰浴反应6h,反应结束后分别用丙酮、去离子水洗涤各15min,再用0.lmol/L的HCl溶液二次掺杂1.5h。 Add 3g Ag / CoFe204 and 0.2gCTAB, ultrasonic dispersion 30min, then under ice-cooling, was slowly added dropwise 50ml of 9gAPS containing HCl (0.lmol / L) solution, the ice bath was reacted 6h, respectively, after the reaction with acetone, to washed with deionized water each 15min, then HCl solution 0.lmol / L of the secondary doping 1.5h. 最终在80C条件下真空干燥24h。 Final conditions at 80 C and dried under vacuum 24h.

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