NGHIEN ciiu-TRAO 001 iSU HiNH THANH VA ANH Hl/QNG CUA PHA NANO AI^O, DEN T I N H CHAT CUA VAT LIEU 20% ALO, - Cu NANOCOMPOZIT NGUYEN D i r e DUY NGUYEN QUANG TUAN ("' NGO KIEN CUOfNG NGUYEN DANG THUY T R A N V A N DUNG Dat van de Tom tat Vat lieu nanocompozit (Cu-20% Mp^) da du'oc tong hop cong bang phu'ong phap co - hoa l 99,7%; cd hat 40+50^m; Loba Chemie PVT Ltd, India) Tdng trgng lugng hdn hgp bdt cho mdi lan nghien la 20 gr, bao gdm (14,2649gr Cu + 4,6775gr CuO + l,0576gr Al); ti le rieng phan cua tirng loai bdt hdn hgp bdt ban dau da dugc tinh toan cho ham lugng Al.Oj san pham bdt cudi cung dugc tao la 20% ve thd tich ciia AUO3 (Cu-20% A\p^), theo phan irng sau: IMS-NKL xS.OOk SE(M) (a) (2) 3CuO + xCu + 2A1 = (3 + x)Cu + AI3O3 De khdng che phan irng cha} tu sinh nhiet, phdi lieu bd sung, them bdt Cu nguyen chat da dugc tinh toan theo phan irng (2) Nhu vay, qua trinh phan ung ciia CuO va AI se cd mdt phan phan iing true tiep va mdt phan phan irng nen Cu Qua trinh nghien co- - hda dugc thuc hien tren may nghien canh khuay 60-80 vdi budng nghien hinh tru dudng kinh 60 mm va chieu cao 80 mm Bi nghien hinh cau dudng kinh mm dugc che tao bang thep khdng gl da bien cung Ti le theo khdi lugng bi/bdt la 200/20 Qua trinh gia cdng dugc thuc hien mdi tradng TAP CHi c a KHi VIET NAM V • 1 IMS-NKL x80.0kSE(M) •' 500nm | (b) Hinh 1: Hmh dang miu hon hop hot Cu-CuO-Al truoc (a) va sau nghien voi toe nghidn 620 vg/ph thoi gian 16h (b) Hinh dang, kich thudc hat mau vat lieu bdt trade, sau nghien va cau tnic te vi cua mau khdi dugc quan sat va phan tich tren hien vi dien thir quet (phat xa tmdng HITACHI S-4800) So 1+2-Thang 1+2 nam 2011 NGHIEN cuu-TRAOOOI Ty trgng ciia mau vat lieu Cu-Al^Oj dugc phan tich tren can phan tich dien tir, chinh xac lO^g, dua tren nguyen ly Acsimet Do cirng te vi (Rockwell) cua mau Cu-Al,03 dugc xac dinh b ^ g each sit dung bi thep vdi tai trgng la 100 kO CuO giam dan, va gan nhu khdng the xac dinh thdi gian nghien tang len den 12h Vdi ket qua phan tich phan pha nhu trinh bay tren hinh I cd the khang dinh rang qua trinh nghien phan irng (1) va (2) da xay va tao pha AI.,0 nen Cu 1000 (b) Sau nghien 12h Ket qua va thao luan Trong anh chup hinh dang hdn hgp bdt ban dau (hinh la): hat ddng cd dang hinh nhanh cay, nhdm cd dang cau va CuO cd dang bdng Gia thiet ve ba giai doan tac ddng cua nang Iugng bien dang qua trinh nghien dugc dua nhu sau: Giai doan I - giai doan dau cua qua trinh nghien: dudi tac dung cua irng suat tiep, cac hat kim loai trugt tren cac be mat tiep xiic Hien tugng va ket qua cd the xay nhu sau: I- Cd hien tugng han ngudi giira cac hat Cu vdi tao cac hat Cu ldn hon; 2- Tren be mat tragt giii-a Cu va Al xay qua trinh tao lien kim Cu va Al; 3- Tren be mat tiep xiic giira CuO va Al se xay phan irng theo phuong trinh (1) Giai doan - giai doan nghien dn dinh: ca ba cau tir ban dau CuO, Al va Cu ciing vdi Al^Oj, CuAI va Cu mdi hinh se ket hgp Iai tao mdt hat vdi nen la Cu Tren hinh Ib bieu dien be mat hat sau nghien I6h Dudi tac ddng cua qua trinh bien dang deo manh liet budng nghien, cac be mat tiep xuc mdi dugc hinh mdt hat, qua trinh phan ung xay theo phuang trinh (2) Qua trinh phan irng cd the dugc ggi la phan irng dxi hda ben va bao gdm ca phan ling xay gifla CuAl va CuO Sir xuat hien cua pha Al^Oj hdn hgp bdt nghien chiing td rang qua trinh khuech tan ciia AI va thay the vi tri nguyen tir dxi mang tinh the cua CuO da xa} Qua trinh khuech tan thuc chat la phan img the vi tri nguyen tu- dxi mang tinh the cua Cu bang pha A^Oj • Cu TAI,0, 500 / V J\ < X ã.v,^*^" 5J^'*'A-^-ft,./>^S>-wt*%-W'f,ằ,I^LS-ô-'.^HHW'''fl*"^ ^;^*.-,rtw.^^^.^ão^^*'ã,.^,^ tu 4000 (a) Sau nghien 4h c • Cu •8 3000 • AI2O3 Ol OCuO c o (3 2000 1000 OT O A_._, 20 30 40 50 Goc nhieu xa (2 9) Hinh 2: Bieu nhieu xa ronghen ciia mau sau nghien 4h (a) va 12h (b) H L J T ; ' ^ ^ ' -'/•, 60 3fr'?S -.^^S;: • -'if V • • -J • ( ! » ; ,•: • ; ^ ^ ^ : : • ; : ^ • : •^^•x.r '-%':>••.'•'• s'^WX% '' W •t" -?.fef' 0* Hinh 3: Anh hien vi quang hoc mau Cu-10% (khoi luong) Al,03 sau thieu ket o lOQ^C lrong 3h (X200) Giai doan - giai doan pha hiiy cua hat bdt td hgp Cu-Al^Oj: qua trinh bien dang keo dai sinh xd lech mang la khuyet tat dan den qua trinh pha hii}- cua hat vat lieu to hgp Cu - Alfi^ Cac ket qua phan tich tir gian dd XRD (hinh 2a) cho thay, sau nghien 4h, vdi tdc nghien 620 vg/ ph pha Al^Oj da xuat hien, ciing vdi cac pha Cu, CuO (du) va Al (du) Khi thdi gian nghien keo dai, cac pha Hmh 4: Anh SEM mau Cu-10% (kli5i lucmg) A i p , sau thieu k a a TOCC trona 3h TAP CHi caKHf VIET NAM V So 1+2 - Thang 1+2 nam 2011 CF NGHIEN CUU - TRAO DOI ep so bd nam khoang (200+400) MPa Khi giam ap luc ep thap hon khoang lire tren khd tao sir hen ket giira cac hat dd, xai bdt Cu ngu}-en chat, qua trinh dong banh so bd co the thuc hien a ap lire ep rat thap khoang 40 MPa Mat khae, tang ap luc qua 400 MPa xuat hien hien tugng nut tai chinh giiia khdi Trong ap luc ddng banh cua bdt ddng ngu}en chat cd the tang cao han 600 MPa Ap luc ep dugc hieu la ddng ^•ai trd tao sir bien dang deo cua cac hat bdt Ket qua phan tich td chuc te vi mgt lan niia da tu tao sir bien dang tren be mat tiep xuc xa tao khang dinh su hmh cac hat nano ALO, phan tan nen su mdc ndi giira cac ngu}-en tren be mat na}- Su tren nen Cu Tren hinh v a la anh td chuc te vi cua mau bdt da dugc gia cdng ca - hda \ai che dd nghien tham gia cua ALO, xa t\' trgng lech tang len nhieu 620 vg/ph thdi gian 16h sau dd thieu ket Tren qua Trinh nghien da Iam giam tinh deo cua hdn hgp xa hinh la be mat sau tam thuc \6i phdng dai han che qua trinh hen ket giua cac hat Khoang thieu ket ciing thu hep lai dang ke \di thap, cho ta tha}- rd cac hat \-at lieu td hgp \6i kich cd raong ddi ldn khoang 40 jim, xen giua cac dudng nhiing mau thieu ket -\ oi nhiet 900C thdi gian bien hat la cac Id xdp co kich cd khoang (2+5) |im ni (l+3)h da xuat hien cac xit nirt keo theo \iec tang Pha mau trang cac Id xdp la dung dich tam thuc len cua xdp Hien tugng na} thudng xu}-en xa}- hoac bdt mai khdng dugc lam sach het qua trinh su chenh lech xe he sd gian na nhiet giiia kim loai va chuan bi mau Td chirc te \'i tren mdt hat dugc chup gdm tai nhiet cao tra xe nhiet dd thirdng de lai a phan giai cao bang hien vi dien quet (hinh 4) cac \-et nirt xa Id trdng giira be mat tiep giap Ket qua cho tha}, cd cac pha phan tan A1,0, \di kich cd rat la cimg cua vat lieu cung giam manh Khoang nhiet khoang (50+100) nm, cac hat \a cac \Ting giau xa thai gian thieu ket dn dinh nhat dugc xac dinh tir ALO, \-di kich cd nho hon |im nam phan bd tren nen 700den800"Cvatir den 3h Cu Neu tiep tuc tang nang Iugng nghien trdn thi ham Cac ket qua khao sat tinh kha ep xa kha thieu dugc lugng cua cac hat nano \ L , se phan bd nhieu hon trinh bay tren bang I, bao gdm cac che cdng nghe \-ao nen Cu dd xdp xa cimg Dd xdp dao ddng khoang (20 Pha nano ALO, phan tan nen ddng va qua + 40)% cung tu (70 + 180)HV mau trinh gia cdng co - hda da lam giam manh tinh kha ep va khdi dugc thieu ket tir bdt ddng ngu}'en chat \-di dd xdp kha thieu cua vat lieu Ket qua khao sat qua trinh ep dgc khoang (3 + 5)% cd hat tinh the dudi Ijim cd ciing true cho tha}- khoang ap luc co the ddng banh sau khoang 50 HV [6] &a\ ciing can ghi chu them, qua nghien cac hat tmh the cua cac chat tham gia nho di dan den cudng cua cac dinh deu giam di, va be rdng cua cac dmh tang len Mat khae, nhu tren bieu XRD (hinh 2b), cac dmh cua Cu raang img vdi phuang [111] da bao ca dmh ALO, Vi the khd cd the xac dinh dugc cac dmh cua ALO, thai gian nghien tang len qua 8h Bang 1: Ket qua khao sat che cong nghe xdp xa ciing (Che Ep - Thieu keli Tinh chat T «C T.h R MPa Do xdp % Dd cung HV 700 I 100 34.70 73 900 100 40.40 117 700 j> 100 36.69 900 -1 100 39.98 ' 118 J TAP CHI c a KHI VIET NAM So 1+2-Thang 1-2 nam 2011 84 NGHIEN cuu-TRAODOI Tinh chat Chl E p - Thieu kit 700 300 24.03 176 900 300 29.12 85 700 300 21.78 164 900 300 34.05 120 800 200 26.82 123 800 200 27.82 105 800 200 31.37 138 Bang phuang phap quy hoach tu}-en tinh, su tac ddng cua cac thdng sd cdng nghe den tinh chat cua san pham dugc Iugng hda theo ham muc tieu nhu sau: Ham xop: qua Ket qua da cho phep tac gia tiep tuc cai tien qua trinh tdng hgp va cac che thieu ket, nham dat dugc he vat lieu nanocompozit CU-AUO3 iing dung che tao dien cue