摘(zhai) 要： 目(mu)的(de)(de)在氧化(hua)(hua)(hua)鋁(lv)陶(tao)瓷表(biao)(biao)面(mian)(mian)(mian)(mian)化(hua)(hua)(hua)學鍍(du)金屬(shu)鎳(nie)鍍(du)層(ceng)(ceng), 研究施(shi)(shi)鍍(du)時(shi)(shi)(shi)間(jian)(jian)對氧化(hua)(hua)(hua)鋁(lv)陶(tao)瓷表(biao)(biao)面(mian)(mian)(mian)(mian)化(hua)(hua)(hua)學鍍(du)鎳(nie)層(ceng)(ceng)的(de)(de)表(biao)(biao)面(mian)(mian)(mian)(mian)形貌(mao)、組織(zhi)結(jie)(jie)構、顯(xian)微(wei)(wei)硬(ying)度(du)、表(biao)(biao)面(mian)(mian)(mian)(mian)粗糙度(du)和(he)鍍(du)鎳(nie)層(ceng)(ceng)結(jie)(jie)合(he)力(li)的(de)(de)影響。方法 所(suo)用(yong)鍍(du)液組成及工藝(yi)參數為(wei):NiSO4·6H2O25g/L, NaH2PO2·H2O 22g/L, Na3C6H5O7·2H2O 64g/L, (NH4) SO4 62g/L, pH=5.06.0, 水浴加熱至90℃, 施(shi)(shi)鍍(du)時(shi)(shi)(shi)間(jian)(jian)14h。采用(yong)NovaNanoSEM50型(xing)(xing)場發射掃描電(dian)子顯(xian)微(wei)(wei)鏡(jing)觀(guan)察鍍(du)層(ceng)(ceng)的(de)(de)表(biao)(biao)面(mian)(mian)(mian)(mian)微(wei)(wei)觀(guan)形貌(mao), 采用(yong)TH765型(xing)(xing)自動顯(xian)微(wei)(wei)硬(ying)度(du)儀測(ce)試(shi)鍍(du)層(ceng)(ceng)硬(ying)度(du), 采用(yong)OLS4000型(xing)(xing)三維形貌(mao)測(ce)量儀測(ce)量鍍(du)層(ceng)(ceng)表(biao)(biao)面(mian)(mian)(mian)(mian)粗糙度(du), 采用(yong)壓入法和(he)熱震試(shi)驗評價(jia)鍍(du)層(ceng)(ceng)的(de)(de)結(jie)(jie)合(he)性(xing)能。結(jie)(jie)果(guo) 施(shi)(shi)鍍(du)時(shi)(shi)(shi)間(jian)(jian)為(wei)14h時(shi)(shi)(shi), 1h鍍(du)層(ceng)(ceng)表(biao)(biao)面(mian)(mian)(mian)(mian)金屬(shu)光(guang)(guang)澤性(xing)好, 呈銀白色(se), 4h鍍(du)層(ceng)(ceng)表(biao)(biao)面(mian)(mian)(mian)(mian)更為(wei)細(xi)膩(ni), 但(dan)表(biao)(biao)面(mian)(mian)(mian)(mian)光(guang)(guang)澤性(xing)較差。隨著施(shi)(shi)鍍(du)時(shi)(shi)(shi)間(jian)(jian)的(de)(de)增(zeng)長, 氧化(hua)(hua)(hua)鋁(lv)陶(tao)瓷表(biao)(biao)面(mian)(mian)(mian)(mian)化(hua)(hua)(hua)學鍍(du)鎳(nie)層(ceng)(ceng)表(biao)(biao)面(mian)(mian)(mian)(mian)越光(guang)(guang)滑, 顯(xian)微(wei)(wei)硬(ying)度(du)越大。不同施(shi)(shi)鍍(du)時(shi)(shi)(shi)間(jian)(jian)下的(de)(de)化(hua)(hua)(hua)學鍍(du)層(ceng)(ceng)均沒有(you)出(chu)現(xian)起(qi)泡(pao)、片狀剝落或者與氧化(hua)(hua)(hua)鋁(lv)基體分(fen)離等現(xian)象。結(jie)(jie)論 施(shi)(shi)鍍(du)時(shi)(shi)(shi)間(jian)(jian)為(wei)14h時(shi)(shi)(shi), 在溫(wen)度(du)和(he)pH不變的(de)(de)情況(kuang)下, 隨著施(shi)(shi)鍍(du)時(shi)(shi)(shi)間(jian)(jian)增(zeng)加, 化(hua)(hua)(hua)學鍍(du)鎳(nie)層(ceng)(ceng)厚(hou)度(du)變化(hua)(hua)(hua)不大, 但(dan)是鍍(du)層(ceng)(ceng)顆粒更細(xi)小, 顯(xian)微(wei)(wei)硬(ying)度(du)明(ming)顯(xian)提高, 表(biao)(biao)面(mian)(mian)(mian)(mian)粗糙度(du)降低, 鍍(du)層(ceng)(ceng)結(jie)(jie)合(he)力(li)良好。
陶(tao)瓷(ci)(ci)具(ju)有高硬度、高耐蝕(shi)性(xing)、高介(jie)電性(xing)等諸(zhu)多優(you)點。隨著(zhu)材料科學和(he)工藝的發展, 陶(tao)瓷(ci)(ci)材料已(yi)從傳統的硅酸鹽材料, 發展成為除了要求力學性(xing)能外, 還要求聲、光、熱、電等方面性(xing)能的現代陶(tao)瓷(ci)(ci)材料[1-3], 其用(yong)途也(ye)越(yue)(yue)來越(yue)(yue)廣。陶(tao)瓷(ci)(ci)應用(yong)時(shi), 往往要進(jin)行(xing)部分或全部的表(biao)面金(jin)屬(shu)化處理, 以使陶(tao)瓷(ci)(ci)更容易電鍍加(jia)工、生產, 增加(jia)其可焊性(xing), 增強其與金(jin)屬(shu)間的結合力, 并且使其表(biao)面具(ju)有金(jin)屬(shu)光澤[4-7]。
陶(tao)瓷(ci)(ci)化學鍍(du)是實現陶(tao)瓷(ci)(ci)材料表面金屬化的一(yi)種重(zhong)要(yao)手段(duan), 鍍(du)后能進一(yi)步擴大其用途, 使(shi)其在電(dian)子電(dian)路、裝飾材料等(deng)方面得到應(ying)用。化學鍍(du)不需要(yao)外(wai)加電(dian)源(yuan), 操作方便, 工藝簡單(dan), 鍍(du)層(ceng)均(jun)勻, 孔隙率低(di), 外(wai)觀良好, 能在塑料、陶(tao)瓷(ci)(ci)等(deng)多種非金屬基體上沉(chen)積, 包(bao)覆性(xing)優良 (不用外(wai)加電(dian)源(yuan), 凡(fan)鍍(du)液能浸到的部位(wei), 即使(shi)是復雜零件的微小孔、盲孔都可以(yi)獲得均(jun)勻鍍(du)層(ceng)) , 附著力、抗腐蝕性(xing)、耐(nai)磨性(xing)好, 功能性(xing)優異, 以(yi)上優點使(shi)其得到了迅速發(fa)展和(he)廣泛應(ying)用[8-11]。
目(mu)前(qian), 陶(tao)瓷(ci)表面(mian)(mian)金屬(shu)化(hua)主(zhu)要(yao)應用于(yu)電子(zi)元件制(zhi)造(zao)、電磁屏蔽和室內裝(zhuang)飾等(deng)領(ling)域。國內已有不少關于(yu)陶(tao)瓷(ci)表面(mian)(mian)金屬(shu)化(hua)的(de)報道(dao)。崔永麗(li)等(deng)[12]為(wei)提高陶(tao)瓷(ci)金屬(shu)化(hua)層的(de)焊(han)接性(xing)能, 提出了(le)(le)(le)一種陶(tao)瓷(ci)二次(ci)金屬(shu)化(hua)鍍(du)鎳工(gong)藝(yi), 介(jie)紹(shao)了(le)(le)(le)鍍(du)鎳液的(de)配(pei)方(fang)(fang)、工(gong)藝(yi)條件及具(ju)體工(gong)藝(yi)流程, 探討了(le)(le)(le)鍍(du)鎳層常見缺陷(xian)的(de)原因并提出了(le)(le)(le)解決方(fang)(fang)法。張德庫[13]研究了(le)(le)(le)硫酸鎳濃度、次(ci)亞磷酸鈉(na)濃度、施鍍(du)溫度、施鍍(du)時間等(deng)對鍍(du)層沉積速率的(de)影響, 對鍍(du)層進行(xing)了(le)(le)(le)金相分析, 從而(er)得到了(le)(le)(le)化(hua)學(xue)(xue)鍍(du)鎳的(de)優化(hua)工(gong)藝(yi)。但有關施鍍(du)時間對陶(tao)瓷(ci)表面(mian)(mian)化(hua)學(xue)(xue)鍍(du)鎳層性(xing)能影響的(de)報道(dao)較少。
本文采用化(hua)學鍍的(de)方法在氧化(hua)鋁陶瓷(ci)表(biao)(biao)(biao)面制(zhi)備金屬(shu)鎳(nie)(nie)鍍層(ceng)。研究了不同(tong)施鍍時(shi)間對氧化(hua)鋁陶瓷(ci)表(biao)(biao)(biao)面化(hua)學鍍鎳(nie)(nie)層(ceng)的(de)表(biao)(biao)(biao)面形貌、組織結(jie)構、顯微(wei)硬度(du)、表(biao)(biao)(biao)面粗糙度(du)以及鍍鎳(nie)(nie)層(ceng)結(jie)合力的(de)影(ying)響。
1 實驗
1.1 實驗材料
選取Al2O3陶(tao)瓷片(pian)作為基材試(shi)樣, 試(shi)樣原(yuan)始形貌見圖(tu)1, 尺寸為25.0mm×25.0mm×2.0mm。采用XRD衍射儀對試(shi)樣進行(xing)相(xiang)分(fen)析, 樣品為純度(du)99%的α-Al2O3陶(tao)瓷, 衍射圖(tu)譜見圖(tu)2。
圖1 未經任何處(chu)理的原始(shi)試(shi)樣(yang)
圖2 試樣的XRD圖譜
1.2 化學鍍液制備
化(hua)學(xue)鍍液主要包括鎳鹽、還(huan)原劑和絡合(he)劑三種(zhong)成分, 陶瓷表(biao)面(mian)化(hua)學(xue)鍍鎳配方及工藝條件見表(biao)1。
表(biao)1 氧化鋁陶瓷表(biao)面化學鍍鎳配方(fang)及工藝條(tiao)件
1.3 陶瓷表面化(hua)學鍍鎳工藝流程
化(hua)(hua)學鍍(du)之前, 要對氧化(hua)(hua)鋁陶(tao)(tao)瓷表面進(jin)(jin)行預處(chu)理(li)。工(gong)藝流程為(wei)(wei):除(chu)(chu)油→很聲(sheng)(sheng)波(bo)(bo)清(qing)(qing)洗→脫(tuo)水(shui)烘(hong)干(gan)(gan)→粗化(hua)(hua)→很聲(sheng)(sheng)波(bo)(bo)清(qing)(qing)洗→脫(tuo)水(shui)烘(hong)干(gan)(gan)→敏化(hua)(hua)→活(huo)化(hua)(hua)→水(shui)洗→化(hua)(hua)學鍍(du)鎳。上述水(shui)洗工(gong)序均采(cai)用去離子水(shui), 很聲(sheng)(sheng)波(bo)(bo)清(qing)(qing)洗均采(cai)用無水(shui)乙(yi)醇, 目(mu)的(de)(de)是(shi)徹底(di)清(qing)(qing)除(chu)(chu)含(han)(han)在陶(tao)(tao)瓷微孔中的(de)(de)除(chu)(chu)油液(ye)(ye)。脫(tuo)水(shui)烘(hong)干(gan)(gan)是(shi)為(wei)(wei)了(le)將陶(tao)(tao)瓷含(han)(han)浸(jin)的(de)(de)水(shui)徹底(di)脫(tuo)掉(diao), 一般在200~400℃下進(jin)(jin)行烘(hong)干(gan)(gan)。采(cai)用氫氟(fu)酸進(jin)(jin)行化(hua)(hua)學粗化(hua)(hua), 使用氟(fu)化(hua)(hua)物處(chu)理(li)液(ye)(ye)是(shi)為(wei)(wei)了(le)溶(rong)解陶(tao)(tao)瓷中的(de)(de)二氧化(hua)(hua)硅, 從(cong)而(er)使表面具有一定(ding)的(de)(de)粗糙(cao)度。陶(tao)(tao)瓷的(de)(de)敏化(hua)(hua)與活(huo)化(hua)(hua), 分(fen)別采(cai)用氯(lv)(lv)化(hua)(hua)亞錫(xi)溶(rong)液(ye)(ye)、氯(lv)(lv)化(hua)(hua)鈀溶(rong)液(ye)(ye)作為(wei)(wei)敏化(hua)(hua)液(ye)(ye)和活(huo)化(hua)(hua)液(ye)(ye)。完(wan)成以上表面預處(chu)理(li)后, 陶(tao)(tao)瓷進(jin)(jin)入鍍(du)槽開始化(hua)(hua)學鍍(du)鎳[14-17]。
1.4 測試與表征
采用(yong)美國FEI公司生產(chan)的Nova Nano SEM50型(xing)(xing)場發射(she)高分(fen)辨掃描(miao)電子顯微(wei)鏡 (FE-SEM) 觀察鍍層的表面微(wei)觀形貌, 采用(yong)日本奧(ao)林巴斯公司生產(chan)的OLS4000型(xing)(xing)三維(wei)形貌測量儀(yi)測試鍍層表面粗(cu)糙度。采用(yong)TH765型(xing)(xing)自動顯微(wei)硬度儀(yi)測試鍍層硬度, 載荷100g, 保持10 s, 每種鍍層測4個位置, 計算平均值。
采(cai)(cai)用WGL-230B型電熱鼓風(feng)干燥箱進行熱震實驗(yan), 測(ce)(ce)試(shi)鍍層(ceng)的結合(he)性能, 溫(wen)度設定為 (250±10) ℃, 保溫(wen)30min, 然(ran)后迅(xun)速(su)將試(shi)樣放(fang)入(ru)室溫(wen)的水中驟冷, 反(fan)復進行25次。采(cai)(cai)用北(bei)京時代四合(he)科(ke)技有限公司生產的THR-150D型洛氏硬度計, 進行壓入(ru)法(fa)鍍層(ceng)結合(he)力(li)測(ce)(ce)試(shi):120°圓錐(zhui)金(jin)剛石壓頭, 施加壓力(li)60kg, 保持30s, 出現明顯(xian)壓痕(hen)。采(cai)(cai)用Nova Nano SEM50型場發射掃描電子顯(xian)微(wei)鏡 (FE-SEM) 觀察壓痕(hen)微(wei)觀形貌(mao)及裂痕(hen)。采(cai)(cai)用蘭(lan)州微(wei)納儀器科(ke)技有限公司生產的MFT-4000型多(duo)功(gong)能材(cai)料表面性能試(shi)驗(yan)儀, 測(ce)(ce)量(liang)不同鍍層(ceng)破壞(huai)的臨界(jie)載荷(he), 加載速(su)度60N/m, 劃痕(hen)長(chang)度10mm。
2 結果與討論
2.1 化學鍍鎳層(ceng)的表面形貌
圖3為(wei)不同施鍍時間下氧化(hua)鋁(lv)陶瓷(ci)表(biao)面(mian)化(hua)學鍍鎳的SEM圖。從圖3a可知, 施鍍1h時, 鍍層表(biao)面(mian)
圖(tu)3 氧化鋁陶瓷(ci)表面化學鍍鎳層的微觀形貌
較(jiao)(jiao)平(ping)整, 鍍(du)層(ceng)結合致密, 覆層(ceng)顆(ke)粒(li)(li)較(jiao)(jiao)為粗大(da), 鍍(du)層(ceng)表面(mian)(mian)(mian)無孔(kong)洞。隨著施(shi)(shi)鍍(du)時(shi)間(jian)的(de)(de)延長, 鍍(du)層(ceng)表面(mian)(mian)(mian)平(ping)整度無明(ming)顯變化, 但在高倍電鏡下可觀察(cha)到覆層(ceng)顆(ke)粒(li)(li)變得多而細小, 呈葡萄狀排布, 致密無間(jian)隙。對(dui)比不同(tong)施(shi)(shi)鍍(du)時(shi)間(jian)下氧(yang)化鋁陶瓷表面(mian)(mian)(mian)化學(xue)鍍(du)鎳的(de)(de)組織形(xing)貌, 發現(xian)施(shi)(shi)鍍(du)1h鍍(du)層(ceng)的(de)(de)表面(mian)(mian)(mian)金(jin)屬光澤性好, 呈銀(yin)白色, 施(shi)(shi)鍍(du)4 h鍍(du)層(ceng)的(de)(de)表面(mian)(mian)(mian)更為細膩, 但表面(mian)(mian)(mian)光澤性較(jiao)(jiao)差。
2.2 化(hua)學鍍鎳(nie)層(ceng)的表(biao)面粗糙度(du)
圖(tu)4為施鍍(du)(du)時間對氧(yang)(yang)化鋁(lv)陶瓷(ci)表(biao)(biao)面化學鍍(du)(du)鎳(nie)層(ceng)(ceng)表(biao)(biao)面粗糙度(du)的影響。由(you)圖(tu)可知, 隨著施鍍(du)(du)時間的增長, 氧(yang)(yang)化鋁(lv)陶瓷(ci)表(biao)(biao)面化學鍍(du)(du)鎳(nie)層(ceng)(ceng)表(biao)(biao)面粗糙度(du)越小。施鍍(du)(du)2h時, 表(biao)(biao)面粗糙度(du)開始有(you)明(ming)顯改善(shan);施鍍(du)(du)3 h時, 表(biao)(biao)面粗糙度(du)變化不大;施鍍(du)(du)4 h時, 表(biao)(biao)面較光(guang)滑, Ra為0.668μm, 且較其(qi)他施鍍(du)(du)時間, 表(biao)(biao)面粗糙度(du)改善(shan)幅度(du)較為明(ming)顯。這(zhe)是(shi)因為隨著施鍍(du)(du)時間的增長, 鍍(du)(du)層(ceng)(ceng)顆粒逐漸變細小, 晶粒排布更致密, 從而(er)使得氧(yang)(yang)化鋁(lv)陶瓷(ci)表(biao)(biao)面化學鍍(du)(du)鎳(nie)層(ceng)(ceng)的表(biao)(biao)面粗糙度(du)變小, 表(biao)(biao)面變光(guang)滑。
圖4 施鍍時間(jian)與表面粗糙度的關系(xi)
2.3 化學鍍鎳層的(de)顯(xian)微(wei)硬度
圖5為氧(yang)化(hua)鋁陶(tao)瓷(ci)表面(mian)化(hua)學鍍鎳(nie)層顯(xian)微(wei)硬(ying)(ying)(ying)度(du)(du)與(yu)施鍍時(shi)(shi)間(jian)(jian)的(de)(de)關系(xi)。由圖可知, 隨著施鍍時(shi)(shi)間(jian)(jian)增長, 氧(yang)化(hua)鋁陶(tao)瓷(ci)表面(mian)化(hua)學鍍鎳(nie)層的(de)(de)顯(xian)微(wei)硬(ying)(ying)(ying)度(du)(du)逐漸增大。施鍍4h時(shi)(shi), 硬(ying)(ying)(ying)度(du)(du)較大。這與(yu)施鍍時(shi)(shi)間(jian)(jian)對鍍層微(wei)觀組織的(de)(de)影響(xiang)有密切關系(xi), 沉積層的(de)(de)顯(xian)微(wei)硬(ying)(ying)(ying)度(du)(du)主要受(shou)晶(jing)(jing)粒尺(chi)寸、內應(ying)力(li)以及可動位(wei)錯密度(du)(du)的(de)(de)影響(xiang), 氧(yang)化(hua)鋁陶(tao)瓷(ci)表面(mian)化(hua)學鍍鎳(nie)層亦如(ru)此(ci), 其顯(xian)微(wei)硬(ying)(ying)(ying)度(du)(du)H與(yu)晶(jing)(jing)粒尺(chi)寸d之間(jian)(jian)的(de)(de)關系(xi)可用Hall-Petch公(gong)式H=H0+k/d描述。其中, H0和k是(shi)大于零的(de)(de)常數。顯(xian)然, H與(yu)1/d呈線性(xing)關系(xi), 即鍍層的(de)(de)顯(xian)微(wei)硬(ying)(ying)(ying)度(du)(du)隨晶(jing)(jing)粒尺(chi)寸的(de)(de)減小而提高(gao)[17]。
圖5 不同施鍍時間下(xia)所得氧化(hua)(hua)鋁陶瓷表面化(hua)(hua)學鍍鎳層顯微硬度(du)
2.4 化學鍍鎳(nie)層的結(jie)合(he)力
采用壓入法和熱震(zhen)試驗評(ping)價鍍(du)(du)層(ceng)的(de)結(jie)合力。圖6為熱震(zhen)實驗后, 不同(tong)施(shi)鍍(du)(du)時間下(xia)氧(yang)化(hua)(hua)鋁(lv)陶瓷表面化(hua)(hua)學(xue)鍍(du)(du)鎳層(ceng)的(de)表面形貌。可以看出, 經熱震(zhen)實驗后, 不同(tong)施(shi)鍍(du)(du)時間下(xia)所制(zhi)備的(de)化(hua)(hua)學(xue)鍍(du)(du)層(ceng)均沒有出現起泡、片狀(zhuang)剝落或者(zhe)與氧(yang)化(hua)(hua)鋁(lv)基體分離(li)等現象, 即(ji)鍍(du)(du)層(ceng)結(jie)合力良好, 無明顯宏觀變化(hua)(hua)。
圖7為(wei)(wei)采用(yong)壓(ya)入(ru)法后(hou)所形(xing)成壓(ya)痕及周(zhou)圍裂(lie)(lie)紋(wen)(wen)(wen)的(de)(de)微觀形(xing)貌(mao), 裂(lie)(lie)紋(wen)(wen)(wen)在圖中用(yong)箭頭標(biao)出, 并用(yong)數字進行了編號, 便于(yu)記錄(lu)裂(lie)(lie)紋(wen)(wen)(wen)數量。圖7b、d、f、h分別為(wei)(wei)圖7 a、c、e、g中白色方框(kuang)區域的(de)(de)放大照片。由圖可以(yi)看出, 施鍍(du)1h時(shi), 壓(ya)痕周(zhou)圍有明顯片狀剝(bo)落(luo), 裂(lie)(lie)紋(wen)(wen)(wen)較(jiao)(jiao)(jiao)少且較(jiao)(jiao)(jiao)為(wei)(wei)粗(cu)大;施鍍(du)2h時(shi), 壓(ya)痕較(jiao)(jiao)(jiao)為(wei)(wei)平(ping)整, 無明顯剝(bo)落(luo)痕跡(ji), 裂(lie)(lie)紋(wen)(wen)(wen)較(jiao)(jiao)(jiao)少且較(jiao)(jiao)(jiao)為(wei)(wei)粗(cu)大;施鍍(du)3、4h時(shi), 裂(lie)(lie)紋(wen)(wen)(wen)明顯增多(duo)且細長, 有向外延(yan)伸的(de)(de)趨(qu)勢。施鍍(du)時(shi)間(jian)為(wei)(wei)1h和2h時(shi), 裂(lie)(lie)紋(wen)(wen)(wen)較(jiao)(jiao)(jiao)少, 說明鍍(du)層結合力更好。
圖6 氧化(hua)鋁(lv)陶瓷表面(mian)化(hua)學鍍鎳層熱(re)震實驗后表面(mian)形貌(mao)
圖7 氧(yang)化鋁陶瓷表面化學鍍鎳層壓痕及(ji)裂紋(wen)的(de)微觀形貌
上述兩種方法(fa)可定性(xing)檢(jian)測鍍鎳(nie)層與基(ji)體的(de)結(jie)合(he)強度, 對(dui)于不同(tong)施(shi)鍍時(shi)間(jian)(jian)對(dui)結(jie)合(he)強度的(de)影(ying)響并不能(neng)用(yong)數值來反應出結(jie)果, 為此(ci)采(cai)用(yong)劃痕法(fa)來測量(liang)不同(tong)施(shi)鍍時(shi)間(jian)(jian)下, 氧化(hua)鋁陶(tao)瓷表面鍍鎳(nie)層結(jie)合(he)力(li)大小(xiao)。
圖8為(wei)氧化(hua)(hua)鋁陶(tao)(tao)(tao)瓷化(hua)(hua)學鍍(du)鎳(nie)層表(biao)面劃(hua)(hua)痕的宏觀(guan)形貌, 圖9為(wei)氧化(hua)(hua)鋁陶(tao)(tao)(tao)瓷化(hua)(hua)學鍍(du)鎳(nie)層的劃(hua)(hua)痕實驗曲線(xian)和(he)劃(hua)(hua)痕的微(wei)觀(guan)形貌。從(cong)圖9a中可(ke)以看到, 載荷約(yue)11.5N處(chu)(chu)出現了(le)顯著(zhu)聲發射信號(hao), 而且摩擦(ca)力和(he)摩擦(ca)系數(shu)也在此處(chu)(chu)發生了(le)明(ming)顯變化(hua)(hua), 此時對應(ying)的劃(hua)(hua)痕距(ju)離約(yue)1.3mm。觀(guan)察(cha)該處(chu)(chu)的形貌 (圖9b) 可(ke)以看到鍍(du)層已(yi)發生破壞, 暴(bao)露出了(le)陶(tao)(tao)(tao)瓷基(ji)體(ti), 說(shuo)明(ming)該處(chu)(chu)信號(hao)對應(ying)鍍(du)層與基(ji)體(ti)結(jie)合失效。一般用臨(lin)界(jie)(jie)載荷的大(da)(da)小來表(biao)征鍍(du)層的結(jie)合強(qiang)度, 劃(hua)(hua)痕法測得(de)的不同施鍍(du)時間樣品的臨(lin)界(jie)(jie)載荷見圖10。由圖可(ke)以看出, 隨著(zhu)施鍍(du)時間的增(zeng)(zeng)長, 臨(lin)界(jie)(jie)載荷越(yue)來越(yue)小, 且施鍍(du)3h和(he)施鍍(du)4h時的差(cha)別不大(da)(da), 與壓入法測得(de)的結(jie)果(guo)一致。這是因為(wei)隨著(zhu)施鍍(du)時間的增(zeng)(zeng)長, 氧化(hua)(hua)鋁陶(tao)(tao)(tao)瓷表(biao)面鍍(du)鎳(nie)層的硬度增(zeng)(zeng)大(da)(da), 鍍(du)鎳(nie)層脆性增(zeng)(zeng)大(da)(da)。
圖8 氧化(hua)鋁陶瓷化(hua)學(xue)鍍(du)鎳層表面劃痕的宏觀形貌
圖9 氧(yang)化鋁陶瓷(ci)表面(mian)化學鍍(du)鎳(nie)層(ceng)劃痕形(xing)貌與劃痕實驗(yan)曲線
圖(tu)10 氧化鋁陶瓷表面(mian)化學鍍鎳(nie)層(ceng)臨界(jie)載荷(he)與(yu)施鍍時間(jian)的關系
3 結論
采用(yong)化學(xue)鍍(du)制(zhi)備氧(yang)(yang)化鋁陶瓷表面(mian)(mian)(mian)鍍(du)鎳層(ceng)(ceng)(ceng), 鍍(du)層(ceng)(ceng)(ceng)組織(zhi)致(zhi)密, 表面(mian)(mian)(mian)平整, 無孔洞(dong)。施(shi)(shi)(shi)(shi)鍍(du)時(shi)間為(wei)1~4h時(shi), 隨著(zhu)施(shi)(shi)(shi)(shi)鍍(du)時(shi)間增長(chang), 表面(mian)(mian)(mian)越來越光(guang)滑, 但金屬光(guang)澤性逐漸(jian)降(jiang)低。施(shi)(shi)(shi)(shi)鍍(du)時(shi)間對氧(yang)(yang)化鋁陶瓷表面(mian)(mian)(mian)鍍(du)鎳層(ceng)(ceng)(ceng)的顯微硬度有影(ying)響, 施(shi)(shi)(shi)(shi)鍍(du)時(shi)間越長(chang), 鍍(du)層(ceng)(ceng)(ceng)維氏硬度越大(da), 但施(shi)(shi)(shi)(shi)鍍(du)3h后, 鍍(du)層(ceng)(ceng)(ceng)硬度變化不(bu)明顯, 隨施(shi)(shi)(shi)(shi)鍍(du)時(shi)間延(yan)長(chang), 鍍(du)層(ceng)(ceng)(ceng)結合(he)強(qiang)度下降(jiang)。施(shi)(shi)(shi)(shi)鍍(du)時(shi)間為(wei)2h時(shi), 氧(yang)(yang)化鋁陶瓷表面(mian)(mian)(mian)化學(xue)鍍(du)鎳層(ceng)(ceng)(ceng)的結合(he)強(qiang)度、表面(mian)(mian)(mian)粗(cu)糙度和(he)光(guang)澤度較優, 工藝參數為(wei):Ni SO4·6H2O 25g/L, Na H2PO2·H2O22g/L, Na3C6H5O7·2H2O 64g/L, (NH4) SO462g/L, p H=5.0~6.0, 水浴加熱至90℃。
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