•MiMJi[»WCONG NGHE rr zo li -/ir KHAO SAT HINH THAI HOC VAOQ NHAM TE VI CUA LdP M A N G CUfNG CrN CHE TAO BANG PHI/0NG P H A P LANG DONG VAT LY Tir PHA HOI TRONG MOI TRl/OFNG C H A N KHONG INVESTIGATION INTO MORPHOLOGY AND MICRO/NANO-ROUGHNESS OF CrN HARD COATING FABRICATED BY USING PHYSICALVAPOR DEPOSITION TECHNIQUE Tran Van D u a , Pham Dvtc Cudng, Oao Huy Hoang, Dao Duy Trung hinh dang hinh hoe cua be mat dUOc phd, nhung lai eo nhOng dae tinh cOly-hoa tUdng tU nhU vat lieu khoi (bulk bam dinh, tang tuoi tho lam viec cua chi tiet va dung cu Hinh ^ a i hoc va nham te vi ciJa ^ mang CrN materials) dung detao ehung Vi the dong mot vai tro quan trpng tdi dac tinh ma sat va mai mon ciia ^ mang CrN Bai bao gidi thieu tdm tat Idp phii rat thich hop d l bao ve be mat ket qua nghien cdu tao Idp mang CrN bang phifOng phap lang dong vat ly ti^ pha hi^ moi tnfdng chan mem hon hoac cho cac be mat can cac khong tren mau thep 5KD11 va khao sat hinh thai hpc be mat va dp nham te vi cua Idp mang CrN tao du'oc yeu cau ky thuat cu the ma khong can Ket qui thu du'oc la cd sd de tiep tuc nghien cdu tao Idp mang CrN cd cac dac tinh phu hop dng dung phai che tao ca khoi vat lieu, cho hiSu linhvilccflkhichetao qua kinh te cao, dac biet la vdi eSc va! Ti^ khda: M^ng cdng, PVD, ON, Hlnh thai hoc, Do nham te vi lieu hiem va dat tien Ldp mang CrN co cac dac diem sau: Abstract CO cang eao (khoang 1800-210C Tlie Cr-based hard coating is often used to protea the surface from scratching and abrasion, reduce HV), he so ma sat nhd (khoang 0,5), kh3 friction and surface adhesion, and therefore increase the lifetime of parts and tools Morphology and nang chju nhiet tot (lam viee on dlnl' micro/nanoroughness of the CrN coating play an important role in determining the friction and wear tdi nhiet 700°C), kha nang chju ma properties ofthe coating This paper briefly introduces the results of fabricating CrN coating on SKD11 steel mon va eao xUdc tot, CrN la vat lieu tre substrates using physical vapor deposition (PVD) technique and investigates rtie surface morphology and (khong phan ufng vdi hau het eac ho; micro/nanoroughness ofthe coating The results are ftindamental for further study in order to fabricate chat) va on dmh, khS nang bam dinf CrN coaling for industrial applications rat manh - tao lien ket phan tCf vci Keywords: Hard coating, PVD, CrN, Morphology, Micro/nano roughness vat lieu nen, co the diing de phu ler TtiS.Tran Vanflua.TS.Ptiamflu'c Cudng, KS Dao Huy Hoang rat nhieu loai vat lieu nen khae nfiau Tnrtingfiaihoc C6ng nghiep Ha Noi Ngaynhanbai: 10/03/2014 Ben canh dd, CrN la vat lieu khong i36i TS Dao Duy Trung - Viln Nghien cQu Co Ngay chap nhan dang: 16/05/2014 nen ed the phu cho cac dung cy diini Email; duatv79@yahoo.com giai phau hoac cac thiet bj sai xuat thu'c pham 1.GldlTH|U be mat eua vat lieu nhSm mue dich bao Hinh thai hpc va nham be mSt I Mang eiJffig la mot hoac nhieu ldp ve be mat khdi sJ cao xade, dong thdi mong (ehieu day bang nanomet CO kha nang cSi thien cac dac tinh co- mpt thdng sd quan trpng cua chi tie Snh hu'dng tdi cac dac tinh lam viecVc hoae mieromet) b^ng kim loai hoac ly-hoa khac cac chi tiet/ be mat co cd ehuy^ hap chat co goc kim loai (kim loai 6uge Cae ldp mang ciJrng khong lam thay nitrit hoa, cae bit hoa, ) dUdc phO len doi cau true eixa vat lieu khoi cung nhii ddng taong doi doi vdi cae chi tiet/b Tom t^t Mang culig goc Crom thucmg duoc su'dung bao ve be mat khoi sif cao xUdc va mai mon, giam ma sat chong TapchiKHOAHOC&CONGNGHE So 2 SCIENCETECHNOLOGY mat khae, viec g i i m dp nham cua Idp be mat co y nghia quan trpng doi vdi kha nang lam viec, dac tinh ma sat va mai mon eua ehi tiet Khi phij mang len, chat laong eua mang (dp nham be mat va eac dac tinh khac cCia mang) se true tiep quyet djnh chat lupng eua chi tiet Hien nay, mot nhCrng iJng dung ehu yeu cua mang edng cO la phu len cac dung cu gia cong elt got, len be mat khuon mau hay cac chi tiet may nhSm giam mai mon tang tuoi thp cua cac chi tiet mat phu Trong eae phuong phap PVD thi phuong phap phun xa (sputtering) dupc sCf dung kha bien nghien cdu lain eac u'ng dung thiic te Trong Phuong phap phun xa (cd nguyen ly nha hinh 1): eac ion nang luong cao Ar+ tradng plasma b i n pha be mat bia Crom (target) "lay" eac phan td vat lieu eua bia Cac phan tCf sau dd se lang dpng tren be mat nen (substrate) tao Idp mang Spurtrrlng Trong nghien edu nay, chung tdi tien h^nh ehe tao eae mau thep, tif SKD11, tien hanh phCi Idp mang CrN va khao sat danh gia hlnh thai hoc va dp nham te vi cua be mat mau thep trudc va sau phu sCf dung kinh hien vi quang hpc va thiet bl hien vi luc nguyen ttf (Atomic Force IWierosope-AFM) L ^ - M O T A V A C H U A N BjTHf N G H I E M •••; ) J ~- Hinh Nguyen ly cua phuong phap PVD 2.1 Phucrng phap PVD PVD (Physical Vapour Deposition) la t h u i t ngQ chung dung de chi cac phuang phap tao mang mdng bang sU lang dpng vat ly cua vat lieu d pha hoi len be mat mau hoac ehi tiet mdi trudng chan khdng Qua trinh PVD bao gom ba giai doan chinh: Bay hoi (Evaporation): tach hole lay vat lieu tii bia hay dich (target, source); Chuyen chd (Transportation): di chuyen vat lieu tdi be mat can phu (substrate); va Lang dpng (Deposition/ Condensation): tao Idp mang len be Hlnh2.MauthepSKD11 2.2 Chuan bj m l u thi nghiem Thep hpp kim SKD11 dUOc sd dung de tao mang CrN Mau phai dat eac yeu Bang Quy trinh cong nghe che tao mau Thong s6 ciia phoi TI Kich Nguyen cong thirdc Do 0° cijrng nham R, 3,2 3,2 1,6 (HRC) Tien 16x5,5 28-30 Oanh so 16x5,5 28-^30 Mai phang 16x5,3 28+30 Nhiet luyen 16x5,3 58+60 Mai phang 16x5,1 58+60 0,8 16x5,0 58+60 0,1 Danh bang mau Dung cu, trang thiet bj -May tien, may do c^g -Bg danh so -Maymaiph^ng - Thiet hi nhiet luyen, may do ciJng -May mai phang - May danh bong, giay rap cacloai, dung dich AI2O) 0,5pm, dung dich hat kim cuong 0,1pm cau ve dp nham be mat, cdng be mat va kich thadc phCi hop vdi cac thiet bi va thi nghiem phan tich danh gia (hinh2), bang la quy trinh eong nghe sd tao mau • Yeu cdu cho mdu thi nghiem: -Kich thudc it)15xL5mm -Vatmau:ThepSKD11 -DdeUng:55-^60HRC - Da mai phang va danh bdng dat dp nhan bdng cap 11-13 -Sai sddo phlng 0,005 • Ldm sach mdu trUdc tgo mdng: Cac chi tiet sau ehe tao co duoc gia edng co hpc be mat trade ma Cd nhieu phaong phap gia cdng be mat: mai va danh bdng, quay, xdc, phun nham loai bd het gi, oxit, chat ban, ba via va dat dUOc nhan bdng theo yeu eau Tuy nhien, qua trinh gia cdng cac phuang phap gia eong van de lai tren be mat eua chi tiet cac vet dau md va eac Idp oxit Xd ly be mat la mot khau quan trpng, then chdt quy trinh ma, nd quyet djnh nhieu den chat lapng Idp ma va dp bam dinh cua Idp ma vdi Idp nen Cae vet dau md va cae Idp oxit can phai dapc loai bd XCf iy be mat kim loai bang phaong phap hda hpc cd the thac hien duoc nhufng dieu dd, Phaong phap hda hoc de tay rda be mated hai qua trinh: -Tayrdadaumd -Tay gi:Tay cac Idp oxit bam tren be mat • Cdc budc Idm sach hda hgc: Qua trinh lam sach de thdng thadng dapc chia lam 11 bade (hinh 3): - eadc (Be I): Day la bade lam sach dau tien, d bade hau het cac chat ban dupc loai bd - BUdc (Be 2): Rda bang nadc Dl, han che qua trinh mang ehat ban t d be sang be - BUde (Be 3): BSy la qua trinh tay rda bo sung eho budc 1, ngoai be cd the sd dung chat tay rda cd tinh axit de tay cac chat oxy hda be mat So 2 Tap dii KHOA HOC & CONG NGHE •!^!MJirtTdc6NGNGHE - BUde (Be 4): Rda bSng nUde Dl, lam sach be mat eac chi tiet can lam nadc Dl han ehe qua trinh mang chat ban td be sach Loai cd ngudn goc dpng thUe vat - BUdc (Be 7): Dung axit HCl de tiy sang be ed the tac dung vdi xut xa phdng Idp oxit, nong axit 10%, tdc dp th cua HCl chu yeu phu thupc vao nfing - Budc (Be 5): Thadng la chat kiem, tan dUpc nUde sd dung dung dich NaOH de tiep tuc - Budc (Be 6): Rda lai ehi tiet bSng dp, ft phu thupc vao nhiet do v$y khong daoc tay HCl d nhi#t d6 cao hpn 40''C tranh bdc hoi HCl gSy dpc hai - BUdc (Be 8): RCfa lai b^ng nadc Dl - Budc (Be 9): Rda chi tiet bSng nUde Dl dadi vdi nadc chay - Budc 10: Xi khd va say khd chl tilt - Budc 11: Bao quan hoac ga l^n bg ga va dUa vao buong chan khdng 2.3 Mo ta thiet bj tao mang va thiet bj cto kiem nham Qua trinh lang dong mang m6ng CrN bang phaong phap phun xa xung dapc thae hien tren thiet bj chSn khdng cd kich thadc buong vdi dudng kinh 0300 x 600 mm, he bom chSn khdng sd dung la bom cP hpc vi bom khuech tan Oau phun xa magnetron l i p bia Crom (99,99%) kich thKdc 0100x10 mm, cdng tac sd dung gom hai loai: Ar 99,99% va N, 99,99% Lupng dUa vao buong chan khong dapc dieu khien b^ng hai thiet bj Mass Flow Control 2179A eua hang MKS Nguon dien ap xung sddung la thiet bj Pinnacle™ plus co tan so td O-BSOKHz, cdng suat 5kW cda hang Advance Energy, Inc - USA Cac thdng so cong nghe tao mang CrN dupe tham khioHi eac nghien cdu trudc da dupe edng b6 Khoang each de - bia: 100 mm, ddng phun xa A, tan sd xung: 100 kH^ lau lupng Ar: 10 seem, luu lapng kW N^: seem, nhiet dp de: 300"C Oe thep SKD 11 (Cl ,5%, Si 0,6%, Mn 0,6%, Cr 12%, Mo 0,85%, V 1,1%, Co 1%, P 0,3%) dadng kinh 020 x5 mm Thiet bj kh^o sat hinh thai hpc va iJ6 nham te vi be mat: kinh hien vi Olympus CX200, kinh hien vi lae nguyen tdAFM (Atomic Force Microscope) Hlnh Quy trinh thirc hien cac biro'c lam sach mlu bang phu'Ong phap hoa hoc apdiiKHOA HOC&CONG NGHE So 2 2.4 Tao mang CrN tren de th^p SKD11 • BUdc Ldm sach bemgtdeth^^' SClENCETECHNOLOGYl - Hut chan khdng den 10'^Pa • Su'd'c Ldm sach debdng plasma -Nhiet buong ehan khdng: 300°C/ thdi gian tri 30 phut - Ap suat eo ban: x l ^ Pa - Luu lapng 0^: 40 seem/ ap suat buong Pa -Bien ap lam sach: kV -Ddng lam sach: 2A -Thdi gian lam sach: 30 phut • Budc Mg Idp chuyen tiip Cr - Dieu khien Ar vao buong chan khong vdi lau laong 10 seem Hinh Cac mau trudc tao mang CrN tren be mat lUaii I Udii -Dieu ehinh ddng phun xa IA -Thdi gian ma phut • BUdc Mg ldp phu CrN - Dieu khien khf Ar vao budng chan khdng vdi luu laong 10 seem Mau Hinh Cac mau sau tao mang CrN tren be mat Mail I - Dieu khien N^ vao buong ehan khdng vdi lUu lUOng seem -Dieu ehinh ddng phun xa IA -Thdi gian ma 150 phut • Budc Chd ngudi vd lay mdu - Chd nhiet buong xudng lOO^C - X I va lay ehi ti€t khdi buong chan khdng Mail Hlnh Anh be mat cua cac mau sau nhiet luyen va mai - Kiem tra va danh gia Idp phu: quan sat dudi kinh hien vi, do cdng Mail I Mail K I T QUA VA THAO LUAN Hlnh va la anh chup cac mau SKD11 trade va sau tao mang Ket qua khao sat ban dau eho thay, mang CrN tao dong deu va bam dinh tdt tren nen thep SKD11, khdng cd vet nijft, rd, bong trdc tren be mat 3.1 Khao sat hinh thai hoc be mat ciia m l u sd dung phUtfng phap quang hoc Win Hinh Anh be mat ciia cac mau sau nhiet luyen, mai va danh bong ; Ma„ I Mail Man '• Hinh Anh be mat 1^ mang CrN tren mau thep SKD11 ( Theo cac bade lam sach chi tiet Mdu -I buong chan khdng b^ng phaong phap hda hpc (nhu trinh - Dieu chinh khoang each t d dau j bay phia tren) phdn xa den d^: SO mm • Budc Hut chdn khong cabdn vd - Hut chan khdng den ap suat 10'Pa 11 gia nhiet di ' ^^^ nguon nung de, dat nhiet dp: - Ga chi tiet len bp ga quay 300°C Cac mau khao sat: -ThepSKDIl - Mang CrN tren thep SKDl Anh be mat cua mdt so mau thep SKDII sau dupc nhiet luyen + mai (hlnh 6) va nhiet luyen -i- mai -i- danh bdng (hinh 7), chup bdi kinh hien vi Olympus CX200 Be mat cac mau chua danh bdng xuat hien nhieu vet xudc dpc theo S o 2 •TapchiKHOAHOC&CONGNGHE IMiWJilltMeONG NGHE hinh thai hpc be mat d cap dp microm e t Uu diem eua phuong phap quang hpc la cho ket quei nhanh va tuong doi ehinh xac, nhien phUOng phap khdng the danh gia chfnh xae daoc cae nhap nhd te vi d cap dp nano-met tren be mat, khdng danh gia dapc cac khuyet tat te vi tren be mat mau hoac eae khuyet tat gay qua trinh tao mang 3.2 KhSo sat hinh thai hoc be mat va nham t^ vi cua mau trUdc va sau phu mang CrN sdr dung thiet bjAFM Hinh la anh AFM be mat eae mau trade va sau ddOC phu Dien tich quet (khSo sat) la 30x30 am^ Sd dung phaong phap AFM cho ta hlnh anh ehinh xae ve hlnh thai hpe b^ mat cua ldp mang d cap dp nano-met, be mat Idp mang g^n nhu chep lai be mat mau nen tren be mat mang ta cung ed the thay eac dudng gach song song chinh la cac vet gia cong tren be mat nen Ket qua do nham te vi tren mau thep SKD11 (hinh 10) va tren be mat mang CrN (hinh 11) Cac mau daoc vdi - dien tich quet = 30x30 \XTnh Mail (Mail dd phu) Mail I (Mail cia phu) Mail (Mail da phu) Mau (Mdu da phu) ifinh ifinh thai hoc be mat cua cac mau cl cap nano met khao sat bang AFM phaong ehay dao doc eua da mai ehdng td nham cdn rat ldn, dd eae mau 6uac danh bdng cd be mat trpn mm, cae vet xUde xuat hien rat It va cd chieu sau nhd hOn Hinh la anh cua be mat mang CrN tren cac mau sau phu Cd the thay rang hinh thai hpe be mat eua mau trudc va sau phu la giong nhau, hay ndi mdt each khac, Idp mang CrN khdng lam thay doi hinh dang hlnh hpc cua be mat dapc phu Ket qua thi nghiem cho thay, sd dung kinh hien vi Olympus CX200 cd the danh gia daoc TapchiKHOAHOC&CONGNGHE S o 2 Ket qua cho thay, nham te vi be mat ldp mang khoang (R^ =12,53 -^ 35,91 nm) So sanh nham dUtfC tren Idp mang CrN va mau thep DKDll (hinh 10 va hinh 11) cho thay dd nham cua Idp mang CrN sau phu Icffi hcJn dp nham be mat mau thep SKDl l.Dleu c6 the giai thieh bdi cac hat/khol hat vat lieu CrN cd kich thUde khac l^ng dpng cCia len be mat cda mau thep, tao nen sU thay doi nhd ve dp nham te vi KET LUAN Ket qua nghien cdu da che tao cac mau thep SKDl va xay ddng qui trmh lam sach be mat mau bang phaong phap hda hoe trUdc phd Idp manaj CrN nham nang cao khii nang bam dinh CLia Idp phu vdi Idp nen Sau d6 thue hien tao mang CrN tren mau thep SKD11 va da tien hanh khao sat danh SClENCETECHNOLOGYl Hlnh 10 Ket qua So nham te vi be mat mang CrN Hlnh Ket qu^ nham te vi be mat mau thep SKDII gia h i n h thai h o c v a d o n h a m t e v i I d p m a n g CrN T d cae k e t q u a d a t d u p c , dUa n h d n g ket luan sau: 179,9-10,2010 thude khae Hudng nghidn cdu tiep theo se tap [2] B Warcholinski, A Gilewicz, Tnbologycal trung vao dieu chinh eac thdng so cdng properties of CrN_ coatings JAMME, P498-504, nghe de tao dupe Idp mang ed eac dac 12/2009 - Ldp mang CrN bam dinh tdt tren tinh phii hop Thd nghiem cac dac tfnh [3] A,6.Cnst6bal, J.J Damborenea, TJ Tate, nen thep SKDII, khdng cd eae vet ro, cua mang dieu kien phdng thi Recent advances in the chmmium nitride PVD process nut tren be mat mang nghiem eung nhd dieu kien lam viec for forming and machining surface protection JMPT, cua Idp phu de danh gia khS nang dng P415-421,12/2005 - Thiet bi hi^n vi luc nguyen t d la edng eu manh eho phep nghien cdu dung thuc te [4] Jianliang Lin, John J Moore, Zhili Wu, hinh thai hoc va dp nham be mat d cap dp nano-met Brajendra Mistira, Process, structure and properties of PliAn bien khoa hoc: PGS.TS Hoang Van Gfft - Op nham te vi cua mau sau phu Idp mang CrN Idn hon so vdi dp nham CrN coatings deposited using Modulated Pulse Power (MPP) Sputtering - Be mat Idp mang CrN gan nhu chep lai b^ mat cCia de thep SKDl [5] GFE Schmalkalden e.V, Principles of coating technology TAILIEUTHAMKHAO Dobrzanski, [6] M Polok-Rubiniec, LA Dobrzanski, M cua Idp mau thep SKDl 1, cd the sU Comparision of tde CrN anclTiN/(TiAI)N PVD coatings Admiak, The properties and wear resistance os the lang dpng eda cac hat vat lieu vdi kich deposited onto plasma nitrited steel JAMME, P172- [1) M Polok-Rubiniec, L A CrN PVD coatings JAMME, P165-171,10/2008 Hdi T H A O KHOA HOC QUOC GIA Sang 16/5/2014, tai co sd 2, trifcmg Bai hgc Cong nghiep Ha Noi to chisc dien cho doanh nghiep, nha sis dung lao dpng Ve phia Nha tririmg, dai dien buoi Hpi thao khoa hoc quoc gia "Dao tao ly thuyet gan lien v ^ thiic tien cho Ban lanh dao Nha tnidng cdTS Ha Xuan Quang, TS Nguyen Anh Tuan -Pho ' ngdnh Qu^n tri kinh doanh va Tai chmh ngSn hang" vd\ i\S tham dii ci^a Hieu trudng ciing tru'dng, phd cac khoa va cac giao vien, glSng vien cfia Khoa c k nha khoa hoc d^n tir cac trifdng Dai hoc Quoc gia Ha Moi, Sai hgc Kinh te Quan ly kinh doanh quoc dan, 6ai hgcThifcmg mai, Bai hgc Lao dgng - Xa hgi; cac doanh nhan - dai Hien nay, tyle smh vien (SV) tnfdng tim du'oc viec lam phii hpp, dap dng du'oc cac yeu cau cua cdng viec cdn kha han che Nganh QuSn tri kinh doanh va Tai chinh ngan hang [QTKD va TCNH) cung khong phSi ngoai le C6 nhieu nguyen nhan de gi^i thich van de nay, nguydn nhSn quan trgng la SV mdi tftiisnq chi cd nhiilig kien thdc ly thuyet co ban ma chira diu^ cd nhQng kinh nghiem, ky nang in} ly cac cong viec phat sinh trang thi/c te Sau nghe cac bai tham luan la cac cong trinh nghien cdu cua ck nha khoa hoc, cac dai bleu da thSo luan ba ngi dung: -Tam quan Uong cua gSn ket ly thuyet vdi thifc tien giang day SV nganh QTKD va TCNH tai tru'dng Bai hpc Cdng nghiep Ha Npi - PhUtfng phip giang day cd the ap dung doi vdi cac hgc phan, dac biet la hpc phan chuyen nganh cua sinh vien QTKD va TCNH - Hlnh he thdng cac nguyen t3c va tif xay difng bd quy tac chuan dio giang vien giang day tren Idp So 2 •TapdiiKHOAHOC&CONGNGHE 1£ ... cua phuong phap PVD 2.1 Phucrng phap PVD PVD (Physical Vapour Deposition) la t h u i t ngQ chung dung de chi cac phuang phap tao mang mdng bang sU lang dpng vat ly cua vat lieu d pha hoi len... Idp nen Cae vet dau md va cae Idp oxit can phai dapc loai bd XCf iy be mat kim loai bang phaong phap hda hpc cd the thac hien duoc nhufng dieu dd, Phaong phap hda hoc de tay rda be mated hai qua... tien hanh phCi Idp mang CrN va khao sat danh gia hlnh thai hoc va dp nham te vi cua be mat mau thep trudc va sau phu sCf dung kinh hien vi quang hpc va thiet bl hien vi luc nguyen ttf (Atomic