6
Pure&Appl. Chern.,Vol. 62, No. 9, pp. 1751-1756,1990, Printed in Great Britain. @ 1990 IUPAC ECR (electron cyclotron resonance) plasma for thin film technology Satoshi Nakayama Advanced Technology Research Laboratories, Sumitomo Metal Industries, Ltd., 1-3 Nishinagasu-hondori, Amagasaki, Hyogo, 660, Japan Abstract - ECR plasma has been used widely and industrially for CVD and etching in semiconductor processes. In this paper, the progress which has been made i n ECR plasma equipments and processing has been reviewed. ECR plasma source has some excellent features such as low pressure plasma generation, the capability of ion energy control and high ionization effi- ciency. The magnetic plasma control and the high power microwave plasma generation techniques developed in our laboratories have improved uniformi- ty and throughput i n comparison with those i n RF plasma. Satisfactory performances are obtained in various processes, which are interlayer plan- arization, a-Si CVD, tungsten CVD, SiOe and aluminum etchings. 1 INTRODUCTION The ECR plasma source reported by Matsuo has some excellent features such as low pressure plasma generation, high ionization efficiency and effective plasma extraction (ref. 1,2). Some investigators have applied the ECR plasma source to CVD and etching i n semiconductor device fabrication processes. Fundamental properties and the merits of ECR plasma process have been shown in their reports (ref. 3-8). There are, however, two important problems to be overcome in ECR plasma processes: (1) poor plasma uniformity, and (2) low throughput. To overcome these problems, we have newly devel- oped a high performance ECR plasma equipment with a magnetic field controller, a high power microwave generator and a large capacity exhaust. Interlayer planarization in LSI, a-Si CVD, tungsten CVD, A1 and SiOz etchings are performed in this equipment and satisfactory results are obtained. 2 ECR PLASMA EQUIPMENT The high performance ECR equipment developed is shown i n Fig. 1. The equipment has nearly the same concept reported by Matsuo (ref. 1,2). 2.45 GHz microwave is introduced in a plasma chamber through a quartz window. The magnetic flux density is selected to be 0,0875 T in order to satisfy the ECR condition. A divergent magnetic field extracts the plasma from the plasma chamber to the reaction chamber. A wafer is cooled and held by a water cooled elec- trostatic chuck. To improve plasma uniformity we set a dual magnetic coil (DMC) under the substrate stage, the magnetic field just above a wafer can be controlled by DMC. To obtain high throughput, a high power microwave generator (max. 3 kW) and two turbo molecular pumps are used. Source gas or etching gas flow rate can be raised up to more than 200 sccm in 0.133 Pa. 3 MAGNETIC FIELD CONTROL Plasma is generated in the chamber of the ECR plasma source and extracted toward a substrate efficiently by a divergent magnetic field. The density of plasma stream extracted along the magnetic field is significantly high at the center, and is markedly reduced i n near the fringe of the plasma stream, which causes convex distribution of deposition rate or etching rate in ECR plasma processes. The plasma can scarcely diffuse across the magnetic force line, electric particles in the plasma are confined in a magnetic flux tube throughout the extraction, and the plasma density thus correspond to the density of the magnetic flux tube, i.e. magnetic field density (ref.8). The uniformity of the ECR plasma can be improved by a dual magnetic coil (DMC). The DMC consists of inner and outer coils with a cylindrical york located coaxially below the stage. The inner coil generates a cusp field and the outer coil generates a mirror field. The magnetic field modified by the DMC is schematically shown in Fig. 2. There is a low magnetic field core region just above the substrate surrounded by a relatively high field region. The extracted plasma approaches to the substrate, the plasma expands isotropically, but cannot expand beyond the outer relatively high field region. Thus, the uniformity of the plasma density is improved without decreasing in the plasma density. Using the DMC, SiOe films were deposited on 6 inch wafers. The results are shown in Fig. 3. 1751

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Pure&Appl. Chern.,Vol. 62, No. 9, pp. 1751-1756,1990, Printed in Great Britain. @ 1990 IUPAC

ECR (electron cyclotron resonance) plasma for thin film technology

Sa tosh i Nakayama

Advanced Technology Research L a b o r a t o r i e s , Sumitomo Metal I n d u s t r i e s , L td . , 1-3 Nishinagasu-hondori , Amagasaki, Hyogo, 660 , Japan

Abs t r ac t - ECR plasma has been used wide ly and i n d u s t r i a l l y f o r CVD and e t c h i n g i n semiconductor p rocesses . I n t h i s paper , t h e p rogres s which has been made i n ECR plasma equipments and p rocess ing has been reviewed. ECR plasma source has some e x c e l l e n t f e a t u r e s such a s low p r e s s u r e plasma gene ra t ion , t h e c a p a b i l i t y of i o n energy c o n t r o l and h igh i o n i z a t i o n e f f i - c i ency . The magnetic plasma c o n t r o l and t h e h igh power microwave plasma gene ra t ion t echn iques developed i n our l a b o r a t o r i e s have improved uniformi- t y and throughput i n comparison w i t h those i n RF plasma. S a t i s f a c t o r y performances a r e obta ined i n v a r i o u s p rocesses , which a r e i n t e r l a y e r plan- a r i z a t i o n , a-Si CVD, t ungs t en C V D , SiOe and aluminum e tch ings .

1 INTRODUCTION The ECR plasma source r epor t ed by Matsuo has some e x c e l l e n t f e a t u r e s such a s low p r e s s u r e plasma gene ra t ion , h igh i o n i z a t i o n e f f i c i e n c y and e f f e c t i v e plasma e x t r a c t i o n ( r e f . 1 , 2 ) . Some i n v e s t i g a t o r s have app l i ed t h e ECR plasma source t o CVD and e t ch ing i n semiconductor dev ice f a b r i c a t i o n p rocesses . Fundamental p r o p e r t i e s and t h e m e r i t s of ECR plasma p rocess have been shown i n t h e i r r e p o r t s ( r e f . 3-8). There a r e , however, two impor tan t problems t o be overcome i n ECR plasma processes : ( 1 ) poor plasma un i fo rmi ty , and ( 2 ) low throughput . To overcome t h e s e problems, w e have newly devel - oped a h igh performance ECR plasma equipment wi th a magnetic f i e l d c o n t r o l l e r , a h igh power microwave gene ra to r and a l a r g e c a p a c i t y exhaus t . I n t e r l a y e r p l a n a r i z a t i o n i n LSI, a-Si CVD, t ungs t en CVD, A 1 and S i O z e t c h i n g s a r e performed i n t h i s equipment and s a t i s f a c t o r y r e s u l t s a r e ob ta ined .

2 ECR PLASMA EQUIPMENT

The h igh performance ECR equipment developed i s shown i n Fig. 1. The equipment has n e a r l y t h e same concept r epor t ed by Matsuo ( r e f . 1 , 2 ) . 2.45 GHz microwave i s in t roduced i n a plasma chamber through a q u a r t z window. The magnetic f l u x d e n s i t y i s s e l e c t e d t o be 0,0875 T i n o rde r t o s a t i s f y t h e ECR cond i t ion . A d ive rgen t magnetic f i e l d e x t r a c t s t h e plasma from t h e plasma chamber t o t h e r e a c t i o n chamber. A wafer i s cooled and he ld by a water cooled e l e c - t r o s t a t i c chuck. To improve plasma un i fo rmi ty we set a d u a l magnetic c o i l (DMC) under t h e s u b s t r a t e s t a g e , t h e magnetic f i e l d j u s t above a wafer can be c o n t r o l l e d by DMC. To o b t a i n high throughput , a h igh power microwave gene ra to r (max. 3 kW) and two tu rbo molecular pumps a r e used. Source gas o r e t ch ing gas flow r a t e can be r a i s e d up t o more than 200 sccm i n 0.133 Pa.

3 MAGNETIC FIELD CONTROL Plasma i s gene ra t ed i n t h e chamber of t h e ECR plasma source and e x t r a c t e d toward a s u b s t r a t e e f f i c i e n t l y by a d ive rgen t magnetic f i e l d . The d e n s i t y of plasma s t ream e x t r a c t e d a long t h e magnetic f i e l d i s s i g n i f i c a n t l y h igh a t t h e c e n t e r , and i s markedly reduced i n near t h e f r i n g e of t h e plasma s t ream, which causes convex d i s t r i b u t i o n of d e p o s i t i o n r a t e o r e t c h i n g r a t e i n ECR plasma processes . The plasma can s c a r c e l y d i f f u s e a c r o s s t h e magnetic f o r c e l i n e , e l e c t r i c p a r t i c l e s i n t h e plasma a r e conf ined i n a magnetic f l u x tube throughout t h e e x t r a c t i o n , and t h e plasma d e n s i t y t h u s cor respond t o t h e d e n s i t y of t h e magnetic f l u x tube , i . e . magnetic f i e l d d e n s i t y ( r e f . 8 ) . The un i fo rmi ty of t h e ECR plasma can be improved by a d u a l magnetic c o i l (DMC). The DMC c o n s i s t s of i n n e r and o u t e r c o i l s w i th a c y l i n d r i c a l york l o c a t e d c o a x i a l l y below t h e s t a g e . The i n n e r c o i l g e n e r a t e s a cusp f i e l d and t h e o u t e r c o i l g e n e r a t e s a mi r ro r f i e l d . The magnetic f i e l d modified by t h e DMC i s schemat i ca l ly shown i n Fig. 2 . There i s a low magnetic f i e l d co re r eg ion j u s t above t h e s u b s t r a t e surrounded by a r e l a t i v e l y h igh f i e l d r eg ion . The e x t r a c t e d plasma approaches t o t h e s u b s t r a t e , t h e plasma expands i s o t r o p i c a l l y , bu t cannot expand beyond t h e o u t e r r e l a t i v e l y h igh f i e l d reg ion . Thus, t h e un i fo rmi ty of t h e plasma d e n s i t y i s improved wi thout dec reas ing i n t h e plasma d e n s i t y . Using t h e DMC, S i O e f i l m s were depos i t ed on 6 i n c h wafers . The r e s u l t s a r e shown i n F ig . 3 .

1751

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1752 S. NAKAYAMA

- 0 .g 1 - \

4 P) 0 . 9 -

i 0 a

The uniformity of the deposition rate is remarkably improved from 10% to less than 5% with the DMC. The film properties, refractive index and buffered hydrofluoric acid (BHF) etching rate, are not affected by using the DMC. In addition, the deposition rate is increased with the outer coil current, which shows that the plasma is confined inside the relatively high field region.

Outer coil Current lOOA

50 70 '0, *,.-A-A-O-A -04 -

''0-0 0 o.a'?'r,

A-A-A-A \

4 EFFECTS OF HIGH MICROWAVE POWER AND HIGH GAS FLOW RATE

The deposition or etching rates reported previously in ECR plasma process were about 0.2 pm/ min at most. About 1 pm/min rate would be necessary for engineering use. The experimental result in SiOn deposition is shown in Fig. 4 . The deposition rate increases with the in- crease in the gas flow rate and the microwave power, and attains to 1 pm/min rate. The BHF etching rate is very fast in a low microwave power, however, become normal in higher power than about 2 . 5 kW. This result implies there would be no limitation in increasing deposition rate if source gases and microwave power are sufficiently supplied (ref. 5 ) .

Coil Current i Supply

Magnetic Coil

Substrate Stage

I \

Generator L J Fig. 1. Diagram of ECR plasma equipment.

(a) Conventional ECR Magnetic Field

(b) Modified Magnetic Field by DMC

Fig. 2 . Schematic diagram of magnetic force line.

Microwave Power (kW)

Fig. 4 . Deposition rate and BHF etching rate in a SiOn film prepared by ECR plasma CVD. The gas ratio of SiH4 to 02 is 315.

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ECR plasma for thin film technology 7 753

n U U -. 2.0’

* 0 4 x

h U .d

P) Fc m

m rl PA

v 1 . 5 .

3 1.0.

a 0.5.

0 2 15Osccm

0 0.5 1 .0 1.5 2.0 2.5 3 . 0

Microwave Power (kW)

Fig. 5. The dependence of e l e c t r o n temperature and plasma dens i ty on microwave power.

I I I I

0 2 150sccm Micro-wave Power Pressure 0.133Pa

n < v

n

W

z

4

v

0 10 20 30

Ion Energy El (eV)

Fig. 6 . The re la t ionship between ion energy d i s t r i b u t i o n and microwave power.

Fig.

I 7. Cross s e c t i o n a l view of

p lanar iza t ion . I n t e r l a y e r SiOn Microwave power 2.2 kW RF power 1.0 kW

The dependence of plasma dens i ty and e l e c t r o n temperature on microwave power a r e shown i n Fig. 5. The plasma dens i ty increases l i n e a r l y with microwave power and has no s a t u r a t i o n tendency. The e l e c t r o n temperature increases s l i g h t l y with microwave power. Fig. 6 shows t h e i o n energy d i s t r i b u t i o n s f o r microwave powers. The microwave power increase does not change t h e i o n energy d i s t r i b u t i o n and only the number of ions increases . The proper t ies of a deposi ted f i l m a r e scarce ly a f fec ted by ic reas ing microwave power. Deposition under a r e l a t i v e l y low gas pressure is d e s i r a b l e t o obta in good f i lm proper t ies , because they a r e very s e n s i t i v e t o gas pressure. A l a r g e capaci ty exhaust i s needed t o keep a low gas pressure a t high gas flow r a t e . P r a c t i c a l l i m i t of deposi t ion r a t e w i l l be ru led by a capaci ty of a exhaust.

5 EXAMPLES OF APPLICATION I n t e r l a y e r p lanar iza t ion : RF biased ECR plasma CVD i s e f f e c t i v e f o r i n t e r l a y e r p lanar iza t ion i n VLSI ( r e f . 3 ) . By applying an RF b i a s t o the s u b s t r a t e , CVD and s p u t t e r e tching occur simultaneously on t h e surface of the wafer. The sput te r ing e f f ic iency can be increased by i n l e t t i n g A r gas i n addi t ion t o SiH4 and On gases. The p lanar iza t ion of a submicron p a t t e r n with a high aspect r a t i o of 3 i s obtained. A SEM photograph of a c ross s e c t i o n a l view i s shown i n Fig. 7. I t i n d i c a t e s almost a per fec t p lanar iza t ion without a void. A - S i CVD: Hydrogenated amorphous s i l i c o n (a-Si:H) f i lms have been prepared by an RF plasma CVD. It was applied t o many devices such a s photoreceptors and photovol ta ic c e l l s . However, deposi t ion of the RF plasma CVD i s i n t h e range of 0.01 pmlmin t o 0.1 prnlmin and t h e deposi-

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1754 S. NAKAYAMA

10. I I I I I I

microwave power 80Ow - WF6:H2 : A r = 10:50:43sccm

3 - TS=45O0C

2 - 9,

100 - /O -

1- k- 0 -

0 . 5 . ' ' ' ' ' '

10 - 0-0 /O -

1 1 1 1 1 1 1 1

0 5 10 15 20 25

t i o n y i e l d of t h e source gas i s l e s s t h a n 10% ( r e f . 4 ) . We have app l i ed t h e newly developed ECR plasma equipment t o a-Si CVD. The obta ined r e s u l t s a r e shown i n Fig. 8. The d e p o s i t i o n r a t e l i n e a r l y i n c r e a s e wi th t h e i n c r e a s e i n microwave power and h igh d e p o s i t i o n r a t e was achieved a t microwave power of 2.5 kW. I n t h e c a s e of RF plasma CVD, i t i s w e l l known t h a t p h o t o s e n s i t i v i t y i s d e t e r i o r a t e d when d e p o s i t i o n r a t e ex- t remely i n c r e a s e s . Th i s phenomenon d i d not appeared i n t h e ECR plasma CVD. Photoconductiv- i t y ( u p ) i n c r e a s e s wi th t h e i n c r e a s e i n microwave power. e n t of t h e microwave power and keeps low va lue of lo- ' ' S/cm. min have e x c e l l e n t p h o t o s e n s i t i v i t y of log(up/u,,)L6. more than 15%. Tungsten CVD: Tungsten CVD has been app l i ed t o t h e i n t e r c o n n e c t i n g f i l m i n L S I . The tungs t en f i l m depos i t ed by thermal CVD has had some problems such a s h igh i n t e r n a l s t r e s s and i n f e r i o r morphology. On t h e o t h e r hand, meta l CVD by ECR plasma has been thought t o be d i f f i c u l t , because microwave i s r e f l e c t e d by t h e t h i n meta l f i l m depos i t ed on a q u a r t z window. Recent- l y , we succeeded i n p reven t ing t h e format ion of meta l f i l m on t h e q u a r t z window, and a p p l i e d ECR plasma t o tungs t en f i l m depos i t i on . F igure 9 shows t h e r e l a t i o n between gas f low r a t e of SiH4 and f i l m c h a r a c t e r i s t i c s . The f i l m r e s i s t i v i t i e s f o r S i H 4 gas f low r a t e of 0 and 5 sccm a r e l e s s t han 10 pn/cm, which a r e j u s t c l o s e t o t h a t of bu lk tungs t en . The s t r e s s e s of t h e f i l m s a r e low, and a r e between 1 / 2 and 1 / 4 of t h a t i n thermal CVD. A SEM c r o s s s e c t i o n a l view of t h e f i l m i s shown i n F ig . 10 . The step-coverage of f i l m i s ve ry e x c e l l e n t . 1 pm spaces a r e f i l l e d wi thout vo id . The morpholo- gy of t h e f i l m i s smoother t h a n t h a t i n thermal CVD. I n thermal C V D , t ungs t en f i l m can be depos i t ed on ly on S i s u r f a c e and not be depos i t ed on SiOz s u r f a c e . I n ECR plasma C V D , t ungs t en f i l m can be depos i t ed on both s u r f a c e s wi thout any d i f f e r e n c e . E tch ing: The ECR plasma e t ch ing has some advantages , such a s low energy i o n bombardment, plasma g e n e r a t i o n under low p r e s s u r e c o n d i t i o n and t h e c a p a b i l i t y of i o n energy c o n t r o l . E s p e c i a l l y , t h e i n c i d e n t i o n energy can be wide ly c o n t r o l l e d from 10 eV t o 200 eV by us ing RF b i a s c o n t r o l . From t h e s e f e a t u r e s , ECR plasma e t c h i n g can be app l i ed t o f a b r i c a t e f i n e p a t t e r n i n t h e f i l m of v a r i o u s m a t e r i a l s w i th h igh a spec t r a t i o and minimal s u r f a c e damages. The fundamental p r o p e r t i e s and t h e a p p l i c a t i o n t o poly-Si , Molybdenum were p rev ious ly r epor t - ed ( r e f . 6 , 7 ) . Here, w e t r i e d t o e t c h A 1 - S i (1%) and S i O z f i l m s . The e t c h i n g p r o f i l e s ob ta ined a r e shown i n Fig. 11 and 12. It should be noted t h a t l i t t l e r e s i d u e s a r e found i n

Dark conduc t iv i ty (odd) i s independ- The f i l m s depos i t ed a t 1 pm/

The d e p o s i t i o n y i e l d of S i H 4 gas i s

1.0

0 . 8 -

0.6

0.4

0 . 2 -

SiHr Flow R a t e = 1 8 0 (sccm

10-8

-

-

- - ' 0 0.5 1 . 0 1 . 5 2.0 2.5

Microwave Power (kW)

h 5

9 6

20 In

15 ';f w 0 a

*rl b+

10 $

g 5 :;

In 0 a n

0

F i g . 8 . Dependence of a-Si depos i t i on rate and c o n d u c t i v i t y on microwave power. P res su re 0.133Pa, Wafer t empera tu re 200°C.

h

B 2 V

h U .rl > .rl Y

In .rl In d

Fig . 9. Dependence of t ungs t en f i l m r e s i s t i v i t y and stress on SiHs gas flow rate .

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ECR plasma for thin film technology 1755

t h e photograph of A 1 e t c h i n g and t h e r e i s no s i z e change between t h e r e s i s t and t h e SiOz h o l e s i n t h e c o n t a c t h o l e e t ch ing . importance of micro-loading e f f e c t s occur red a t submicron p a t t e r n f a b r i c a t i o n are po in ted ou t r e c e n t l y . plasma, micro-loading e f f e c t i s a l s o minimized a s shown i n Fig. 13.

They were performed by RF-bias i o n energy c o n t r o l .

S ince ECR plasma e t c h i n g i s performed a t t h e p r e s s u r e lower than t h a t of RF

The

0.6 0.8 1.0 2.0 3 .0 4.0

P a t t e r n Width (pm)

Fig. 10. Tungsten f i l m prepared by ECR plasma CVD. WFo:SiH4:Hz:Ar=10:5:50:43 sccm Microwave power 800 W Wafer tempera ture 450°C

Fig. 11. Al-Si a l l o y e t c h i n g p r o f i l e s . P re s su re 0.53 Pa Microwave power 800 W RF power 140 W Etching gas C l z + B C 1 3

F ig . 1 2 . E tch ing p r o f i l e of SiOz c o n t a c t h a l l . P re s su re 0.2 Pa Microwave power 1 kW RF power 400 W Etching gas CHF3+CF4

Fig. 13. Micro load ing e f f e c t i n A1-Si (1%) f i l m e t ch ing . Microwave power 800 W RF power 140 W

Fig. 13. Micro load ing e f f e c t i n Al -Si ( l%) f i l m e t c h i n g . Microwave power 800W, RF Dower 140W

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1756 S. NAKAYAMA

6 CONCLUSION

The un i fo rmi ty and t h e throughput of ECR plasma equipment a r e remarkably improved by us ing a d u a l magnetic c o i l , a h igh power microwave gene ra to r and a l a r g e c a p a c i t y exhaus t . The improved equipment i s s u i t a b l e f o r v a r i o u s k inds of a p p l i c a t i o n . The ECR plasma w i l l p l ay an impor tan t r o l e i n VLSI processes .

REFERENCES

1. S. Matsuo and Y. Adachi, Jpn. J. Appl. Phys. , Zl, L4 (1982). 2. S. Matsuo and M. Kiuchi, Jpn. J . Ap 1. Ph s., 22, L210 (1983). 3. K. Machida and H . Oikawa, J. Vac. SEi. Te:hnolz B 4 , 818 (1986). 4. K. Kobayashi, M. Hayama and S . Kawamoto, J . Appl. Phys. , a, 202 (1987). 5. T. Akahori , T . Suehi ro , T . Tani and S. Nakayama, Microprocess Conf. , 3, 130 (1988). 6. T. Ono, M. Oda, C . Takahashi and S. Matsuo, J . Vac. Sc i . Technol. , B4, 696 (1986). 7. Y. Tobinaga, N. Hayashi, H. Araki and S . Nakayama, J . Vac. S c i . T e c G o l . , B6 (l), 272

(1988). 8. S. Nakamura and S . Nakayama, Proc. Symp. on SIN and SiOn Thin I n s u l a t i n g Films, 285

(1989).