新型化学镀法制备木质电磁屏蔽材料的研究
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摘要
木材化学镀是木材功能性改良的一种重要手段,在保留木材优异特性基础上赋予其良好的导电及电磁屏蔽性能,拓展了木材的应用领域。目前,木材化学镀尚存在镀铜还原剂的有毒性、活化工艺成本过高及镀层颜色单一等问题。本研究针对以上问题,开展新型木材化学镀制备电磁屏蔽材料的相关研究。
以桦木、水曲柳为基材,以表面电阻率及金属沉积率为主要指标探讨最佳施镀效果。主要包括四部分内容：(1)探讨以离子钯活化、乙醛酸为还原剂的全新的镀铜镀液及施镀条件；(2)研究活化与施镀一浴完成的新型非钯活化木材表面化学镀铜的镀液体系及条件；(3)通过彩化处理,赋予镀层丰富的颜色,探索彩化工艺条件及颜色形成机理；(4)以XPS、SEM-EDS、XRD对镀层成分、形貌和结构进行表征,并对导电性、电磁屏蔽性能、色度、光泽度、润湿性、结合强度进行测定。
研究得出的结论归纳如下：
(1)乙醛酸为还原剂的木材化学镀铜,离子钯活化最佳条件为壳聚糖8g/L,处理时间8min,壳聚糖吸附氯化钯时间8min,2g/L次亚磷酸钠处理时间8min；适合桦木的镀液及条件为：硫酸铜20g/L,EDTA-2Na40g/L,乙醛酸7.5g/L,联吡啶0.01g/L,添加剂L为0.015g/L, pH值12,温度55℃,施镀时间30min；适合水曲柳的镀液及条件为：硫酸铜12g/L, EDTA·2Na40g/L,乙醛酸10.5g/L,联吡啶0.01G/L,添加剂L为0.01g/L, pH值12,温度50℃,施镀时间30min。
EDS和XPS结果表明镀层由单质铜组成,与乙醛酸还原机理吻合,XRD分析表明镀层铜为晶态结构,SEM观察发现镀铜单板表面镀覆均匀并具有金属光泽。桦木、水曲柳镀铜单板电磁屏蔽效能在9kHz～1.5GHz频段分别达到55dB和50dB以上；镀层的结合强度分别超过1.08Mpa和1.49Mpa；涂饰使单板的导电性和电磁屏蔽效能略有下降,最低值仍大于44dB,完全满足实际应用需要；经化学镀铜的单板表面由亲水性变为疏水性；施镀后单板颜色在CIEL*a*b*色空间的分布中,a*值变化最为显著；在孟塞尔色系统中桦木和水曲柳单板颜色标注分别为9.8R6.9/10.6和9.8R7.1/10.1,为明度、饱和度较高的橙红色。镀铜桦木和水曲柳单板表面光泽度参数GZL、GZT分别为7.75%、5.21%、和6.15%、3.38%,较素材有所提高。
(2)非钯活化木材化学镀铜,适合桦木的镀液及条件：NaBH4处理液浓度3g/L,处理时间8min；硫酸铜20g/L、硫酸镍0.55g/L,乙醛酸8.5g/L, EDTA·2Na39g/L,联吡啶0.014g/L,添加剂L0.011g/L, pH值12.25,温度60℃,施镀时间50min；适合水曲柳的镀液及条件：NaBH4处理液3g/L,处理时间10min,硫酸铜18g/L,硫酸镍0.5g/L,乙醛酸8.5g/L, EDTA·2Na39g/L,联吡啶0.008g/L,添加剂L0.011g/L, pH值12.25,温度60℃,施镀时间50min。
EDS和XPS分析表明,镀层内部为单质铜；XRD结果显示铜镀层为面心立方结构,无Ni的化合物和Cu-Ni合金的形成。桦木、水曲柳单板电磁屏蔽效能在频率9kHz～1.5GHz范围内分别达到60dB及50dB以上；镀层与木材结合强度超过1.22Mpa和1.03Mpa；涂饰使单板导电性和电磁屏蔽效能略有下降,但仍分别大于49dB和37dB,超过实际应用所需标准；镀铜使单板表面具有较好的疏水性；桦木、水曲柳镀铜单板颜色标注分别为9.8R6.2/9.8和9.7R5.9/9.5,颜色为较饱满的橙红色；镀铜单板表面光泽度参数GZL.GZT分别为5.33%、4.35%、水曲柳为3.35%、2.56%,较素材有小幅下降,光泽柔和。
(3)在彩化过程中,钼酸铵0.25g/L～0.35g/L.次亚磷酸钠0.8g/L～1.0g/L范围内,浓度变化对镀层表面电阻率无明显影响,随着二者浓度的增加,单板表面颜色逐渐变暗,颜色向红色、蓝色过渡较为明显；温度对彩化后镀镍单板表面电阻率没有明显影响,温度升高对彩化反应有一定促进作用,单板明度降低；彩化过程中期,单板整体颜色最暗,饱和度最低,约25min之后颜色饱和度逐渐增大,颜色较为稳定,呈现无明显规律的彩虹颜色。
XPS和XRD分析结果表明,镍镀层表面经彩化处理生成钼的氧化物膜使镀层产生不同颜色,钼的氧化物未形成结晶,镀层中的Ni仍为晶态结构,SEM表明彩化后单板表面依然被镀层完全覆盖,光泽比彩化前稍有减弱。彩化使单板电磁屏蔽效能下降至40dB左右；涂饰后电磁屏蔽效能下降,最低值仍达到35dB以上；彩化后镀层结合力良好,结合强度均超过2.06MPa；彩化处理使镀镍单板表面的疏水性提高；彩化使单板颜色由中等明度的中性色变为不规律的彩虹颜色,几乎不具有重现性且光泽度下降,光泽各向异性程度降低；涂饰使单板颜色变暗,整体色彩变得柔和。
通过研究新型木材化学镀制备电磁屏蔽材料及其性能,解决了目前木材化学镀中的镀液组成、活化工艺、镀层颜色等方面存在的相关问题,所得材料具备环境友好、颜色丰富、性能良好等特性,对木材化学镀的工业化生产及实际应用提供了理论依据与实践指导。
Electroless plating on wood surface is an important method for wood functional modification, which can endow wood perfect electro-conductivity and electromagnetic shielding based on maintaining its own special properties. It can enlarge the application field for wood. In present, there exist some problems for electroless plating on wood, such as toxic reducing agent in copper plating on wood, high cost of activation process, and monotonous color of the coatings. In order to overcome those problems, novel electroless plating on wood were conducted for preparing electromagnetic shielding wood-based material.
The birch and ash veneers were used as the substrate to investigate the suitable plating conditions according to surface resistivity and metal deposition. Four parts were carried out as follows:1) investigating the components of the plating solution and plating conditions for electroless copper plating by using glyoxylic acid as reductant under Pd2+activation;2) discussing the components of the plating solution and plating conditions for electroless copper plating under Pd-free activation that the activation and plating are combined in one bath;3) Endowing colorful surface to the coatings by coloring process for studying the conditions and the coloring mechanism;4) XPS, SEM-DES and XRD analysis were used to characterize the coating component, morphology and structure, respectively. The electro-conductivity, electromagnetic shielding performance, shade of the color, gloss, wettability, and adhesion strength were measured.
The conclusions were summarized as below:
(1) In the process of electroless copper plating by using glyoxylic acid as reductant, the suitable activation conditions are8g/L of chitosan treating for8min, Pd2+adsorption for8min and reduce in2g/L of sodium hypophosphite solution for8min. The plating solution composition and conditions for birch veneer are as follows:CuSO420g/L, EDTA·2Na40g/L, glyoxylic acid7.5g/L, Dipyridyl O.Olg/L, additive L0.015g/L, pH value12,55℃for30min. Those for ash veneer are as follows:CuSO412g/L, EDTA·2Na40g/L, glyoxylic acid10.5g/L, Dipyridyl O.Olg/L, additive L O.OlOg/L, pH value12,50℃for30min.
The EDS and XPS results showed that the coating consists of native copper, which accords with the reducing mechanism of glyoxylic acid. The XRD analysis indicated that the coating is crystalline. SEM observation showed that the coatings with metallic luster covered the surface of wood uniformly. The electromagnetic shielding effectiveness (ESE) of plated birch and ash veneers are55dB and50dB in the frequencies from9kHz to1.5GHz, respectively. The adhesion strength is1.08Mpa and1.49Mpa. Surface decoration made the ESE decrease to44dB, which can still meet the practical application. The surface changed from hydrophilic to hydrophobic after electroless copper plating. In CIEL*a*b*color system, the change a*value of veneers before and after plated is significant. In Munsell system, the color code are9.8R6.9/10.6and9.8R7.1/10.1, indicating that orange-red with high lightness and saturation. The GZL and GZT parameters in gloss measurement of copper plated birch and ash veneers are7.75%,5.21%and6.15%,3.38%, respectively. They are higher than those of pristine wood veneers.
(2) In the process of electroless copper plating by using Pd free activation, the pretreatment for birch veneer is that the veneers were immersed in3g/L of NaBH4solution for8min. The plating solution composition and conditions for birch veneer are as follows:CuSO420g/L, NiSO40.55g/L, glyoxylic acid8.5g/L, EDTA·2Na39g/L, Dipyridyl0.014g/L, additive L0.011g/L, pH value12.25,60℃for50min. Those for ash veneer are as follows:the pretreatment in3g/L of NaBH4solution for10min, CUSO418g/L, NiSO40.50g/L, glyoxylic acid8.5g/L, EDTA·2Na39g/L, Dipyridyl0.008g/L, additive L0.011g/L, pH value12.25,60℃for50min.
The EDS, XPS and XRD results showed that the coating consists of native copper with the face-centre cubic structure, which no Ni and N-Cu alloy mixed. The ESE of plated birch and ash veneers are60dB and50dB in the frequencies from9kHz to1.5GHz, respectively. The adhesion strength is more than1.22Mpa and1.03Mpa. Surface decoration made the ESE decrease to49dB and37dB, which can still meet the practical application. The plated veneers have good hydrophobic property. The color codes are9.8R6.9/10.6and9.8R7.1/10.1for plated birch and ash veneers, which indicated full orange-red color. The GZL and GZT parameters in gloss measurement of copper plated birch and ash veneers are5.33%,4.35%and3.35%, 2.56%, respectively. They are lower than those of pristine wood veneers. The sheen is mild.
(3) In the coloring process, the concentration of ammonium molybdate (0.25-0.35g/L) and sodium hypophosphite (0.8-1.Og/L) had no obvious effects on the surface resistivity of the colored veneer. The color of the veneer became darker and transited to red or blue. The temperature didn't affect the surface resistivity of the colored veneer. However, temperature increase could promote the coloring reaction in some extents. In the middle of the color process, the color and the saturation of the veneer was the darkest and lowest. After25min of coloring process, the saturation gradually increased and the color was tending towards stable iridescence.
The XPS and XRD results indicated that molybdenum oxide membrane formed and made the coating colorful after coloring process. Molybdenum oxide did not form crystalline structure. But nickel in the coating was still in crystalline style. It was observed by SEM photographs that the veneer surface was still covered by the coating with lower sheen. Coloring process made the ESE decrease, but it was still higher than40dB. Surface decoration made the ESE decrease to35dB, which can still reach the application standard. The adhesion strength is more than2.06Mpa. Coloring treatment made the coating more hydrophobic. The color changed from neutral color with moderate intensity to irregular iridescence before and after coloring process, which showed bad reproducibility. The sheen decreased and the anisotropic property faded down. Decoration made the colored veneer darker and the whole shade became pastel.
The study of preparing wood-based electromagnetic shielding material and the properties by using novel electoless plating has resolved the key problems in the solution composition, activation conditions and coating colors. The obtained materials are environment friendly, colorful and with good properties, which offered the theory base and practical instruction for commercial produce and application.
以桦木、水曲柳为基材,以表面电阻率及金属沉积率为主要指标探讨最佳施镀效果。主要包括四部分内容：(1)探讨以离子钯活化、乙醛酸为还原剂的全新的镀铜镀液及施镀条件；(2)研究活化与施镀一浴完成的新型非钯活化木材表面化学镀铜的镀液体系及条件；(3)通过彩化处理,赋予镀层丰富的颜色,探索彩化工艺条件及颜色形成机理；(4)以XPS、SEM-EDS、XRD对镀层成分、形貌和结构进行表征,并对导电性、电磁屏蔽性能、色度、光泽度、润湿性、结合强度进行测定。
研究得出的结论归纳如下：
(1)乙醛酸为还原剂的木材化学镀铜,离子钯活化最佳条件为壳聚糖8g/L,处理时间8min,壳聚糖吸附氯化钯时间8min,2g/L次亚磷酸钠处理时间8min；适合桦木的镀液及条件为：硫酸铜20g/L,EDTA-2Na40g/L,乙醛酸7.5g/L,联吡啶0.01g/L,添加剂L为0.015g/L, pH值12,温度55℃,施镀时间30min；适合水曲柳的镀液及条件为：硫酸铜12g/L, EDTA·2Na40g/L,乙醛酸10.5g/L,联吡啶0.01G/L,添加剂L为0.01g/L, pH值12,温度50℃,施镀时间30min。
EDS和XPS结果表明镀层由单质铜组成,与乙醛酸还原机理吻合,XRD分析表明镀层铜为晶态结构,SEM观察发现镀铜单板表面镀覆均匀并具有金属光泽。桦木、水曲柳镀铜单板电磁屏蔽效能在9kHz～1.5GHz频段分别达到55dB和50dB以上；镀层的结合强度分别超过1.08Mpa和1.49Mpa；涂饰使单板的导电性和电磁屏蔽效能略有下降,最低值仍大于44dB,完全满足实际应用需要；经化学镀铜的单板表面由亲水性变为疏水性；施镀后单板颜色在CIEL*a*b*色空间的分布中,a*值变化最为显著；在孟塞尔色系统中桦木和水曲柳单板颜色标注分别为9.8R6.9/10.6和9.8R7.1/10.1,为明度、饱和度较高的橙红色。镀铜桦木和水曲柳单板表面光泽度参数GZL、GZT分别为7.75%、5.21%、和6.15%、3.38%,较素材有所提高。
(2)非钯活化木材化学镀铜,适合桦木的镀液及条件：NaBH4处理液浓度3g/L,处理时间8min；硫酸铜20g/L、硫酸镍0.55g/L,乙醛酸8.5g/L, EDTA·2Na39g/L,联吡啶0.014g/L,添加剂L0.011g/L, pH值12.25,温度60℃,施镀时间50min；适合水曲柳的镀液及条件：NaBH4处理液3g/L,处理时间10min,硫酸铜18g/L,硫酸镍0.5g/L,乙醛酸8.5g/L, EDTA·2Na39g/L,联吡啶0.008g/L,添加剂L0.011g/L, pH值12.25,温度60℃,施镀时间50min。
EDS和XPS分析表明,镀层内部为单质铜；XRD结果显示铜镀层为面心立方结构,无Ni的化合物和Cu-Ni合金的形成。桦木、水曲柳单板电磁屏蔽效能在频率9kHz～1.5GHz范围内分别达到60dB及50dB以上；镀层与木材结合强度超过1.22Mpa和1.03Mpa；涂饰使单板导电性和电磁屏蔽效能略有下降,但仍分别大于49dB和37dB,超过实际应用所需标准；镀铜使单板表面具有较好的疏水性；桦木、水曲柳镀铜单板颜色标注分别为9.8R6.2/9.8和9.7R5.9/9.5,颜色为较饱满的橙红色；镀铜单板表面光泽度参数GZL.GZT分别为5.33%、4.35%、水曲柳为3.35%、2.56%,较素材有小幅下降,光泽柔和。
(3)在彩化过程中,钼酸铵0.25g/L～0.35g/L.次亚磷酸钠0.8g/L～1.0g/L范围内,浓度变化对镀层表面电阻率无明显影响,随着二者浓度的增加,单板表面颜色逐渐变暗,颜色向红色、蓝色过渡较为明显；温度对彩化后镀镍单板表面电阻率没有明显影响,温度升高对彩化反应有一定促进作用,单板明度降低；彩化过程中期,单板整体颜色最暗,饱和度最低,约25min之后颜色饱和度逐渐增大,颜色较为稳定,呈现无明显规律的彩虹颜色。
XPS和XRD分析结果表明,镍镀层表面经彩化处理生成钼的氧化物膜使镀层产生不同颜色,钼的氧化物未形成结晶,镀层中的Ni仍为晶态结构,SEM表明彩化后单板表面依然被镀层完全覆盖,光泽比彩化前稍有减弱。彩化使单板电磁屏蔽效能下降至40dB左右；涂饰后电磁屏蔽效能下降,最低值仍达到35dB以上；彩化后镀层结合力良好,结合强度均超过2.06MPa；彩化处理使镀镍单板表面的疏水性提高；彩化使单板颜色由中等明度的中性色变为不规律的彩虹颜色,几乎不具有重现性且光泽度下降,光泽各向异性程度降低；涂饰使单板颜色变暗,整体色彩变得柔和。
通过研究新型木材化学镀制备电磁屏蔽材料及其性能,解决了目前木材化学镀中的镀液组成、活化工艺、镀层颜色等方面存在的相关问题,所得材料具备环境友好、颜色丰富、性能良好等特性,对木材化学镀的工业化生产及实际应用提供了理论依据与实践指导。
Electroless plating on wood surface is an important method for wood functional modification, which can endow wood perfect electro-conductivity and electromagnetic shielding based on maintaining its own special properties. It can enlarge the application field for wood. In present, there exist some problems for electroless plating on wood, such as toxic reducing agent in copper plating on wood, high cost of activation process, and monotonous color of the coatings. In order to overcome those problems, novel electroless plating on wood were conducted for preparing electromagnetic shielding wood-based material.
The birch and ash veneers were used as the substrate to investigate the suitable plating conditions according to surface resistivity and metal deposition. Four parts were carried out as follows:1) investigating the components of the plating solution and plating conditions for electroless copper plating by using glyoxylic acid as reductant under Pd2+activation;2) discussing the components of the plating solution and plating conditions for electroless copper plating under Pd-free activation that the activation and plating are combined in one bath;3) Endowing colorful surface to the coatings by coloring process for studying the conditions and the coloring mechanism;4) XPS, SEM-DES and XRD analysis were used to characterize the coating component, morphology and structure, respectively. The electro-conductivity, electromagnetic shielding performance, shade of the color, gloss, wettability, and adhesion strength were measured.
The conclusions were summarized as below:
(1) In the process of electroless copper plating by using glyoxylic acid as reductant, the suitable activation conditions are8g/L of chitosan treating for8min, Pd2+adsorption for8min and reduce in2g/L of sodium hypophosphite solution for8min. The plating solution composition and conditions for birch veneer are as follows:CuSO420g/L, EDTA·2Na40g/L, glyoxylic acid7.5g/L, Dipyridyl O.Olg/L, additive L0.015g/L, pH value12,55℃for30min. Those for ash veneer are as follows:CuSO412g/L, EDTA·2Na40g/L, glyoxylic acid10.5g/L, Dipyridyl O.Olg/L, additive L O.OlOg/L, pH value12,50℃for30min.
The EDS and XPS results showed that the coating consists of native copper, which accords with the reducing mechanism of glyoxylic acid. The XRD analysis indicated that the coating is crystalline. SEM observation showed that the coatings with metallic luster covered the surface of wood uniformly. The electromagnetic shielding effectiveness (ESE) of plated birch and ash veneers are55dB and50dB in the frequencies from9kHz to1.5GHz, respectively. The adhesion strength is1.08Mpa and1.49Mpa. Surface decoration made the ESE decrease to44dB, which can still meet the practical application. The surface changed from hydrophilic to hydrophobic after electroless copper plating. In CIEL*a*b*color system, the change a*value of veneers before and after plated is significant. In Munsell system, the color code are9.8R6.9/10.6and9.8R7.1/10.1, indicating that orange-red with high lightness and saturation. The GZL and GZT parameters in gloss measurement of copper plated birch and ash veneers are7.75%,5.21%and6.15%,3.38%, respectively. They are higher than those of pristine wood veneers.
(2) In the process of electroless copper plating by using Pd free activation, the pretreatment for birch veneer is that the veneers were immersed in3g/L of NaBH4solution for8min. The plating solution composition and conditions for birch veneer are as follows:CuSO420g/L, NiSO40.55g/L, glyoxylic acid8.5g/L, EDTA·2Na39g/L, Dipyridyl0.014g/L, additive L0.011g/L, pH value12.25,60℃for50min. Those for ash veneer are as follows:the pretreatment in3g/L of NaBH4solution for10min, CUSO418g/L, NiSO40.50g/L, glyoxylic acid8.5g/L, EDTA·2Na39g/L, Dipyridyl0.008g/L, additive L0.011g/L, pH value12.25,60℃for50min.
The EDS, XPS and XRD results showed that the coating consists of native copper with the face-centre cubic structure, which no Ni and N-Cu alloy mixed. The ESE of plated birch and ash veneers are60dB and50dB in the frequencies from9kHz to1.5GHz, respectively. The adhesion strength is more than1.22Mpa and1.03Mpa. Surface decoration made the ESE decrease to49dB and37dB, which can still meet the practical application. The plated veneers have good hydrophobic property. The color codes are9.8R6.9/10.6and9.8R7.1/10.1for plated birch and ash veneers, which indicated full orange-red color. The GZL and GZT parameters in gloss measurement of copper plated birch and ash veneers are5.33%,4.35%and3.35%, 2.56%, respectively. They are lower than those of pristine wood veneers. The sheen is mild.
(3) In the coloring process, the concentration of ammonium molybdate (0.25-0.35g/L) and sodium hypophosphite (0.8-1.Og/L) had no obvious effects on the surface resistivity of the colored veneer. The color of the veneer became darker and transited to red or blue. The temperature didn't affect the surface resistivity of the colored veneer. However, temperature increase could promote the coloring reaction in some extents. In the middle of the color process, the color and the saturation of the veneer was the darkest and lowest. After25min of coloring process, the saturation gradually increased and the color was tending towards stable iridescence.
The XPS and XRD results indicated that molybdenum oxide membrane formed and made the coating colorful after coloring process. Molybdenum oxide did not form crystalline structure. But nickel in the coating was still in crystalline style. It was observed by SEM photographs that the veneer surface was still covered by the coating with lower sheen. Coloring process made the ESE decrease, but it was still higher than40dB. Surface decoration made the ESE decrease to35dB, which can still reach the application standard. The adhesion strength is more than2.06Mpa. Coloring treatment made the coating more hydrophobic. The color changed from neutral color with moderate intensity to irregular iridescence before and after coloring process, which showed bad reproducibility. The sheen decreased and the anisotropic property faded down. Decoration made the colored veneer darker and the whole shade became pastel.
The study of preparing wood-based electromagnetic shielding material and the properties by using novel electoless plating has resolved the key problems in the solution composition, activation conditions and coating colors. The obtained materials are environment friendly, colorful and with good properties, which offered the theory base and practical instruction for commercial produce and application.
引文
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