臺灣博碩士論文加值系統

本實驗探討不同原子比例的Nd元素添加至Mg-Cu-Y合金基材中，對Mg- Cu-Y-Nd非晶質合金玻璃形成能力和熱性質的影響。在此藉由噴射鑄造法可製作出直徑為3mm~10mm的Mg58Cu31Y1-x Ndx非晶質合金棒材。而在XRD結果表示，這整組Mg58 Cu31Y1-xNdx合金棒材顯示有一非晶質相的寬廣繞射峰，且有一明顯的玻璃轉換溫度(glass transition temperature)和過冷液相區(super cooled region, △Tx about 70 K)。可發現當在Mg58Cu31Y11合金內之Nd元素添量增加時，結晶會從原本單一段變成兩階段的結晶，使得結晶溫度(crystallization temperature)和△Tx會隨著Nd含量的增加而有下降的趨勢。在這合金系統當中以Mg58Cu31Y6Nd5非晶質合金之γ和γm值為最高，分別為0.422和0.758。所以適當的Nd元素添加有助於Mg58Cu31 Y11-x Ndx合金系統的玻璃形成能力。此系統合金的結晶活化能，並不會隨著Nd添加量的增加而有明顯的改變，而Mg58Cu31Y10Nd1(127 kJ/mole)比Mg58Cu31Y6Nd5(125 kJ/ mole)合金之活化能為略高。在晶核飽和點方面，以Mg58Cu31Y10Nd1合金最高為43%，且其在恆溫443 K下的孕核時間為最久約4600秒，表示此成分擁有較佳的熱穩定性。
在機械性質方面，藉由MTS-801萬能試驗機在常溫下壓縮速率5×10-4 s-1下壓縮，Mg58Cu31Y1-x Ndx非晶質合金棒材之壓縮應力值為838 MPa~978 MPa、彈性限度為2 ~2.7%、比強度為254~210 MPa•cm3/g，而硬度值介於282~340 Hv。在熱機械分析(TMA)可知，Mg58Cu31Y6Nd5非晶質合金，在過冷液相區間內會有超塑性變形產生。且黏彈係數介於為106~107 Pa．s。而依據TMA分析結果，藉由MTS高溫壓縮，探討當在不同溫度時(接近Tonset 448 K、453 K、458 K)，經不同壓縮速率條件下(2.5 x 10-3 ~ 1 x 10-2 s-1)其塑性變形行為。結果顯示為均勻塑性變形，使得應變速率敏感化指數(m)約為1。故在過冷液相區內，可發現Mg58 Cu31Y6 Nd5塊狀金屬玻璃，其優異的超塑性能力，且也知其有不錯的加工性。
由XRD和TEM微結構分析，Mg58Cu31Y6 Nd5合金在恆溫熱處理後所產生的結晶相是以Cu2Mg為主相。而在結晶初期會有Cu2Mg析出，之後隨退火時間增加陸續有Cu2Nd、Mg2Cu、CuY和Cu2Y結晶相產生。

The effect of Nd element addition on the glass forming ability and thermal stability for Mg-Cu-Y-Nd amorphous alloy system was deeply studied and discussed in this study. The Mg58Cu31Y11-xNdx (x=0 ~ 11) amorphous alloy rods with 3 ~ 10 mm in diameter were prepared by Cu-mold injection method. The XRD result reveals that these entire Mg58Cu31Y11-xNdx alloy rods exhibit a broaden diffraction pattern of amorphous phase. A clear Tg (glass transition temperature) and supercooled liquid region (about 70 K) were revealed for all of those Mg58Cu31Y11-xNdx amorphous alloy rods. The single stage crystallization of the Mg58Cu31Y11 alloy was found to change into two stages crystallization when large amount of Nd element was added into this alloy. In parallel, the crystallization temperature (Tx) and supercooled region (ΔTx) present a decreasing trend with increasing Nd content. The highest value of γ and γm are 0.422 and 0.758 which occurs at the alloy compositions of Mg58Cu31Y6Nd5 in this alloy system. Therefore, suitable addition of Nd element can obviously increase the glass forming ability for the Mg58Cu31 Y11-x Ndx alloy system. In addition, the highest transition point around 43% crystallization fraction of nucleation-crystal growth occurs and the longest incubation time(namely 4600 s) at isothermal temperature of 443 K was found to occur at the Mg58Cu31 Y10 Nd1 amorphous alloy.
Mechanical properties of the amorphous rods of Mg58Cu31Y1-xNdx alloy were investigated by means of compression test using an MTS-801 material testing system. The fracture strength, elastic elongation limit, and the specific strength of these Mg58Cu31 Y11-x Ndx alloy system are in the range of 838 MPa~978 MPa､2~2.7 % and 254~210 MPa•cm3/g respectively. Based on the thermal mechanical analysis the superplastic deformation with viscosity between 106~107 Pa．s. occurs at the temperature interval of the supercooled liquid region for the Mg58Cu31Y6Nd5 amorphous alloy. According to the result of TMA, the hot deformation behavior for Mg58Cu31Nd5 Y6 BMG rod was investigated by compression test with different strain rate (2.5 x 10-3 ~ 1 x 10-2 s-1) at various temperature near the Tonset (namely 438 K, 448 K, 453 K, and 458 K) in the supercooled liquid region. The results show a superior superplastic forming ability (which has the strain rate sensitivity coefficient (m-value) closed to 1.0) of the Mg58Cu31Nd5 Y6 amorphous alloy occurring within the supercooled liquid region.
After isothermal annealing Mg58Cu31Y6 Nd5 amorphous alloys at 448 K the principal phase of Cu2Mg crystallized firstly at the early stage of crystallization. Then, the Cu2Nd, Mg2Cu, CuY and Cu2Y crystal phase were gradually crystallizw with increasing the annealing time.

中文摘要…………………………………………………………….....................Ⅰ
英文摘要………………………………………………………………………….Ⅲ
誌謝……………………………………………………………………………….Ⅴ
總目錄…………………………………………………………………….............Ⅵ
表目錄…………………………………………………………………………….Ⅹ
圖目錄……………………………………………………………………………………………..…. VI
第一章 前言……………………………………………………………………..1
第二章 理論基礎………………………………………………………...….....3
2-1 非晶質金屬………………………………………………………........ 3
2-1-1序化與非序化…………………………………………………...…..…4
2-2 形成非晶質合金之法則…………………………………………….....5
2-2 塊狀金屬玻璃之發展……………………………………………….....8
2-4 非晶質合金的製造方式…….………………………………………..12
2-5 塊狀非晶質合金的特性……………………………………………...15
2-5-1 機械性質……………………………………………………..16
2-5-2 耐腐蝕性……………………………………...….……………20
2-5-3 磁性質……………………………………………..…………20
2-5-4 其他性質…………………………………………………..…22
2-6 非晶質合金的熱力學..………………………………………….....…22
2-6-1 非晶質合金是平衡的介穩態……………………....................22
2-6-2 玻璃轉換溫度( Tg )……………………………………………24
2-6-3 合金成份與玻璃形成能力的關係…………………………....26
2-6-4 原子相互作用程度與玻璃形成能力的關係………………....26
2-6-5 簡化玻璃溫度Trg…………………………..…………………29
2-6-6 γ值…………………………..…………………………….…29
2-6-7 △Tx………………………..……………………………........29
2-7 非晶質合金的熱穩定性………..………………………………….…..31
2-7-1非晶質合金的壽命..……………………………………….........31
2-7-2 非恆溫方式之活化能計算—Kissinger plot……………...........32
2-7-3 修正之非恆溫分析法…………………………………..............34
2-8 結晶動力學……………………………….……………………............35
2-8-1 恆溫結晶動力學( isothermal crystalline- JMA plot )….............35
2-8-2 結晶成長控制機制……………….…………………….............37
2-9 非晶質之發展近況與應用………….……………………......................39
2-10 Mg58Cu31Y11-xNdx合金元素特性與相圖……………............................40
第三章 實驗步驟…………………………….………………………...............45
3-1 實驗目的………………………….…………………………..................45
3-2 合金配製………………………….…………………………..................47
3-3 合金熔煉…………………….…………………………..........................48
3-3-1電弧熔煉………….…………………………................................48
3-3-2 塊狀非晶質合金棒材和板材之製作……....................................51
3-3-2-1高周波熔煉(induction - melting)…............................................52
3-3-2-2噴射鑄造(injection -casting) …..................................................53
3-4 熱性質分析………………….…………………………..........................48
3-4-1 示差掃描熱量計（DSC）………………...……..........................54
3-4-1-1 非恆溫升溫熱處理…………………...............................54
3-4-1-2 恆溫退火熱處理……………...........................................55
3-5密度量測……………….………………………………............................55
3-6 機械性質分析………….………………………………..........................56
3-6-1硬度量測……….………………………………............................56
3-6-2 熱機械性質分析(TMA)………………….…...............................56
3-6-3壓縮測試 (MTS testing)..…………………...................................56
3-7 微結構分析…………….………………………………..........................57
3-7-1 Ｘ光繞射儀相鑑定（XRD）…………………............................57
3-7-2 掃瞄式電子顯微鏡(SEM) ………………....................................58
3-7-3 穿透式電子顯微鏡(TEM) ……………........................................58
第四章 結果與討論
4-1 熱性質分析(DSC) ….………………………………………...................61
4-1-1 非恆溫熱性質分析………………………………........................61
4-1-2 結晶活化能(Kissinger plot) ……………………..........................65
4-1-3 非恆溫結晶動力學…………………………................................67
4-1-4恆溫結晶動力學…………………………….................................76
4-2 密度量測………….……………………………………..........................83
4-3 機械性質分析…….……………………………………..........................84
4-3-1 熱機械測試(TMA) …………../………………............................85
4-3-2 壓縮測試(MTS) ……...…………………….................................89
4-3-3-1常溫壓縮測試……………………..................................89
4-3-3-2不同溫度下熱壓測試.…………….................................91
4-4 微結構分析……….……………………………………........................100
4-4-1 掃描式電子顯微鏡(SEM)之破斷面觀察.......................100
4-4-2 X光繞射分析…………………………………………...100
4-4-2-1 鑄造後合金之XRD 分析…………………….107
4-4-2-2 Mg58Cu31Y6Nd5合金經恆溫退火熱處理後之
XRD分析…….………………...........................108
4-4-3 穿透式電子顯微鏡分析(TEM) ……………..................115
4-4-3-1 依XRD 和TEM 之結果對Mg58Cu31Y6Nd5 合
金於恆溫退火過程中結晶行為之推………….. 118
第五章 結論…….……………………………………........................................137
參考文獻…………….……………………………..............................................140

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