Vapor-Phase Epitaxy of Group III-V Compound Optoelectronic Devices

12

Vapor-Phase Epitaxy of Group III-V Compound Optoelectronic Devices

Downloaded by UNIV OF CALIFORNIA SAN DIEGO on January 23, 2017 | http://pubs.acs.org Publication Date: October 2, 1985 | doi: 10.1021/bk-1985-0290.ch012

G. H. Olsen Epitaxx, Inc., Princeton, NJ 08540

The major types of VPE growth systems throughout the world are reviewed. Growth parameters and equipment sketches are included. Limitations and solutions to the "preheat problem" are discussed. Multibarrel reactors, which allow multilayer heteroepitaxial layers to be grown without interruption of c r y s t a l growth are also described. Novel growth phenomena such as "non-planar" VPE lasers, l a t e r a l growth over d i e l e c t r i c layers, growth on (311) and (511) InP substrates and combined VPE/LPE growth are discussed. I n - s i t u laser diagnostic probing and device results -- including the use of VPE for v i s i b l e lasers -- are also reviewed.

The vapor phase epitaxy (VPE) of III-V compounds -- whereby s o l i d e p i t a x i a l layers are deposited by passing chemical vapors over a substrate -- i s of great use i n the optoelectronics area. Commerc i a l devices which are synthesized by t h i s process include GaAsP LEDs, GaAs photocathodes, 1.06 µm InGaAs LEDs and lasers, 1.3 µm InGaAsP LEDs, 1.3 µm InGaAsP cw lasers and 0.9-1.7 µm InGaAs PIN detectors (1) (another important class of VPE grown components (2) -microwave devices -- w i l l not be discussed i n t h i s review). Annual sales of optoelectronic devices made by the VPE process undoubtedly run into the tens of millions of d o l l a r s . The two methods f o r the VPE growth o f I I I - V compounds have been the s o - c a l l e d " c h l o r i d e " method, whereby a group V c h l o r i d e ( e . g . , A s C l ) passes o v e r a m e t a l t o form t h e group I I I c h l o r i d e ( e . g . G a C l ) , whereas i n t h e s o - c a l l e d " h y d r i d e " t e c h n i q u e , t h e group V element i s i n t r o d u c e d as a h y d r i d e ( e . g . , A S H 3 ) and HC1 gas i s passed over a m e t a l t o form the group I I I c h l o r i d e . S t r i c t l y s p e a k i n g , t h e term " h a l i d e " s h o u l d be used r a t h e r t h a n " c h l o r i d e , " s i n c e I and B r have a l s o been used as t r a n s p o r t a g e n t s . The main advantage o f the c h l o r i d e system i s t h a t i t has produced v e r y low (— H

2

+ AsH

3

+PH

3

F i g u r e 3. VPE r e a c t o r d e s c r i b e d by Z i n k i e w i c z ( c o u r t e s y o f L. M. Z i n k i e w i c z ) .

Stroeve; Integrated Circuits: Chemical and Physical Processing ACS Symposium Series; American Chemical Society: Washington, DC, 1985.

12.

OLSEN

Group III-

V Compound

Optoelectronic

227

Devices

connected t o a s i n g l e l a r g e r growth tube. A l l gas f l o w s are cont r o l l e d a t the i n l e t end by e l e c t r o n i c mass-flow c o n t r o l l e r s . AsH and P H f l o w d i r e c t l y i n t o the growth tube w h i l e the HC1 i s passed over g r a p h i t e b o a t s c o n t a i n i n g l i q u i d i n d i u m and l i q u i d g a l l i u m . Dopants a r e added t h r o u g h the f o u r t h tube. M i x i n g o f the m e t a l c h l o r i d e s and the h y d r i d e s i s d e l a y e d by p a s s i n g the h y d r i d e gases through a n o z z l e . T h i s reduces w a l l d e p o s i t s upstream from the subs t r a t e , which may cause changes i n growth r a t e and c o m p o s i t i o n . The n o z z l e t i p i s p e r f o r a t e d t o enhance a c t i v e gax m i x i n g j u s t b e f o r e f l o w i n g over the s u b s t r a t e . The s u b s t r a t e i s pushed i n from the exhaust end t o a p o i n t about 5 cm downstream from the n o z z l e . The r e a c t o r i s mounted i n a h o r i z o n t a l f u r n a c e and heated t o a temperat u r e o f 840°C a t the source zone and 700°C a t the growth zone. 3


3

The system o f Sugiyama e t a l (18) i s shown i n F i g . 5. A s C l i s used as an HC1 s o u r c e . A r e s i d e n c e time o f over 4 s i s c l a i m e d between the m e t a l s and HC1 gas. No p r o v i s i o n f o r p-type doping i s specified. 3

The system o f Enda (8) employs a s e a l e d p r e h e a t chamber i n which the s u b s t r a t e temperature can be brought up t o growth temperature i n a group V h y d r i d e ambient (see F i g . 6 ) . The system o f Susa e t a l ( 1 9 ) , p r i m a r i l y f o r InP and InGaAs growth, uses A s C l as an HC1 source and a l s o uses a s l i d i n g q u a r t z boat t o p r o t e c t s u b s t r a t e s from d e c o m p o s i t i o n . Improved c r y s t a l l i n e q u a l i t y was a t t r i b u t e d t o t h i s b o a t . 3

V o h l (20) has grown a l l o y s by the t r i c h l o r i d e method which uses P C 1 and A s C l as s o u r c e s f o r P and As. Three compound s o u r c e s , InP, InAs, and GaAs — each i n a s e p a r a t e tube — a r e r e a c t e d w i t h a gas m i x t u r e c o n t a i n i n g the same group V element. Each r e a c t i o n i s independently c o n t r o l l e d . The d e p o s i t i o n o f the a l l o y s i s regarded as the d e p o s i t i o n o f a m i x t u r e o f GaAs, InP, and InAs. The a l l o y c o m p o s i t i o n i s o b t a i n e d by a d j u s t i n g the r e l a t i v e amounts o f the t h r e e compounds t h a t are d e p o s i t e d on the s u b s t r a t e . A s k e t c h o f the f u r n a c e i s shown i n F i g . 7. 3

3

L i m i t a t i o n s Imposed by the P r e h e a t P r o c e s s One drawback o f the s i n g l e - b a r r e l VPE p r o c e s s i s the p r e h e a t cycle. Here, s u b s t r a t e w a f e r s a r e heated up t o 650-700°C, p r i o r t o growth, u s u a l l y w i t h o u t d e p o s i t i o n o r e t c h i n g t a k i n g p l a c e . This temperature range e q u a l s o r exceeds the congruent e v a p o r a t i o n tempera t u r e (25) f o r most I I I - V compounds, and some p r e f e r e n t i a l evaporat i o n o f the group V clement i s bound t o t a k e p l a c e . InP i s p a r t i c u l a r l y s u s c e p t i b l e t o t h i s phenomenon, s i n c e i t s d e c o m p o s i t i o n tempera t u r e i s o n l y around 400°C. The damage can be reduced by p r e h e a t i n g


CHEMICAL AND PHYSICAL PROCESSING OF INTEGRATED CIRCUITS

HCI(5%)

-AsH •-PH - H


EXHAUST

SUBSTRATE

^

Go

3

3

2

Zn

t

MFC

t HCI(2%)

F i g u r e 4. VPE r e a c t o r o f Johnston and Strege ( c o u r t e s y o f W. D. J o h n s t o n , J r . ) .

F i g u r e 5. VPE r e a c t o r o f Sugiyama e t a l . ( c o u r t e s y o f K. Sugiyama).


12.

OLSEN

Group III-V

Compound

Optoelectronic

CHAMBER

229

Devices

SUBSTRATE

EXHAUST

j|

P U S H ROD


HCl+H2HCl+H2-

F i g u r e 6.

VPE r e a c t o r o f Enda ( c o u r t e s y o f H. Enda).

-6a

As r-InAs

F i g u r e 7.

VPE r e a c t o r of Vohl ( c o u r t e s y o f P. V o h l ) .


230


the s u b s t r a t e i n the a p p r o p r i a t e PH ).

group V h y d r i d e

(1)

(i.e.,

ASH3

or


3

A l t h o u g h the s u r f a c e morphology of a p r e h e a t e d l a y e r i s o b v i o u s l y degraded by the p r e h e a t d e c o m p o s i t i o n , the m i c r o s t r u c t u r e o f the m a t e r i a l a l s o s u f f e r s . A h i g h d e n s i t y o f d e f e c t loops has been o b s e r v e d , (1) v i a t r a n s m i s s i o n e l e c t r o n m i c r o s c o p y , near the a c t i v e r e g i o n s of InGaP/GaAsP l a s e r s . The d i s l o c a t i o n l o o p s can be e l i m i nated by u s i n g h i g h f l o w s of the group V c a r r i e r - g a s and lower temperatures d u r i n g p r e h e a t . However, an excess p o i n t - d e f e c t concent r a t i o n may always be p r e s e n t t o some e x t e n t , and s h o u l d be viewed as a p o t e n t i a l f a i l u r e mechanism i n any I I I - V compound l i g h t - e m i t t i n g device prepared at elevated temperatures. Preheat decomposition can be reduced w i t h the use o f the " s l i d e r - b o a t " s u b s t r a t e h o l d e r whereby a q u a r t z " s l i d e r " i s used t o s h i e l d the s u b s t r a t e from gaseous ambients ( 1 0 ) . The NTT v e r s i o n (19) a l l o w s group V gases t o be t r a p p e d a l o n g w i t h the s u b s t r a t e . However, m i c r o s c o p i c d e c o m p o s i t i o n s t i l l p r o b a b l y o c c u r s .

M u l t i b a r r e l VPE

Reactors

The p r e h e a t problem, d i s c u s s e d i n the l a s t s e c t i o n , can be s o l v e d by e l i m i n a t i n g the need f o r i t . The use o f m u l t i b a r r e l r e a c t o r s a l l o w s s u c c e s s i v e h e t e r o e p i t a x i a l l a y e r s t o be grown by moving the s u s b s t r a t e from one growth chamber t o another w i t h o u t i n t e r r u p t i n g growth. A dual-growth-chamber GaAs VPE r e a c t o r was proposed by Watanabe e t a l (26) i n 1977 t o produce abrupt changes i n doping p r o f i l e . T h i s system was upgraded i n t o a GalnAsP d u a l - g r o w t h chamber r e a c t o r by M i z u t a n i e t a l ( 1 3 ) . Other types of m u l t i b a r r e l r e a c t o r s were i n d e p e n d e n t l y c o n c e i v e d t o grow (Ga,In)(As,P) by O l s e n and Zamerowski (15) (the " d o u b l e - b a r r e l " r e a c t o r ) and by Beuchet e t a l (7) (the f o u r - b a r r e l "multichamber" r e a c t o r ) . The t h r e e types of r e a c t o r s are shown i n F i g s . 8, 9, and 10. The "dual-growth-chamber" r e a c t o r o f M i z u t a n i (13) ( F i g . 8) c o n s i s t s of one h o r i z o n t a l chamber t o grow InP and another p a r a l l e l chamber t o grow a l l o y s o f ( G a , I n ) ( A s , P ) . The s u b s t r a t e i s supported by a rod mounted on a f l e x i b l e rubber b e l l o w s so t h a t t r a n s f e r between chambers i s a c c o m p l i s h e d by w i t h d r a w i n g and s h i f t i n g the rod. T r a n s f e r can be e f f e c t e d w i t h i n 2 s and h e t e r o i n t e r f a c e t r a n s i t i o n w i d t h s l e s s t h a n 50-60 & are c l a i m e d . A l t h o u g h ( i n the form shown) g a l l i u m - b e a r i n g a l l o y s can o n l y be grown i n one of the chambers, and no p r o v i s i o n s have been made f o r p-type doping, h i g h - q u a l i t y 1.3 |Jm cw l a s e r s have been s y n t h e s i z e d i n the system (Cd was d i f f u s e d i n a f t e r growth f o r p - c o n t a c t ) .

sists

The "multichamber" r e a c t o r of Beuchet e t a l (7) ( F i g . 9) cono f f o u r p a r a l l e l t u b e s , each w i t h a s p e c i f i c f u n c t i o n . The


OLSEN

Group III- V Compound

r

Optoelectronic

Devices

H2/HCl r HH2 2/ /HHCCi i RUBBER

r H 2 2//«s AsH n 33 /* P H ,

I

BELLOWS

-In -Go


-In 800°C

850°C

660-700°C

^ H ip2//r H C t H

2

/PH

3

/H

2

S

EXHAUST

F i g u r e 8, "Dual-growth-chamber" VPE r e a c t o r of M i z u t a n i ( c o u r t e s y o f T. M i z u t a n i ) .

F i g u r e 9. "Multichamber" VPE r e a c t o r o f Beuchet G. B e u c h e t ) .

(courtesy

InP SUBSTRATE HOLDER InGaAsP

H

T=700 ±0.5°C

F i g u r e 10. RCA " d o u b l e - b a r r e l " VPE r e a c t o r .


232


system has been automated e f f e c t e d w i t h i n 1 s. The first: second: third: fourth:

so t h a t i n t e r c h a m b e r t r a n s f e r can be purpose o f each chamber i s as f o l l o w s :

p r e h e a t and s u b s t r a t e e t c h , growth o f n-InP growth o f n-GalnAs growth o f p-InP

M e t a l l i c z i n c i s used f o r p-type d o p i n g w h i l e H S dopant. Downloaded by UNIV OF CALIFORNIA SAN DIEGO on January 23, 2017 | http://pubs.acs.org Publication Date: October 2, 1985 | doi: 10.1021/bk-1985-0290.ch012

2

i s the n-type

The " d o u b l e - b a r r e l " VPE r e a c t o r (15) d e s i g n e d a t RCA i s shown i n F i g s . 10. The concept i n v o l v e s the use o f two c o n v e n t i o n a l VPE systems p l a c e d i n p a r a l l e l and f e e d i n g i n t o a s i n g l e - g r o w t h chamber. W i t h t h i s c o n s t r u c t i o n , d i f f e r e n t gases can be run t h r o u g h each t u b e , so t h a t d o u b l e - h e t e r o s t r u c t u r e l a s e r s ( e . g . , InP/InGaAsP/InP/InGaAsP) can be p r e p a r e d by s i m p l y s w i t c h i n g the s u b s t r a t e from one tube t o the o t h e r , thus removing the need f o r p r e h e a t c y c l e s , which may l i m i t d e v i c e performance s i n c e t h e y can i n t r o d u c e i n t e r f a c i a l d e f e c t s . I t i s i m p o r t a n t t o note here t h a t c r y s t a l growth i s not i n t e r r u p t e d d u r i n g the the s w i t c h o v e r from one l a y e r t o a n o t h e r . The substrate can e i t h e r be h e l d j u s t i n f r o n t of each t u b e , o r i n s e r t e d i n t o the tube i f any m i x i n g problems o c c u r . C o n v e r s e l y , by h o l d i n g the s u b s t r a t e a t the end of the q u a r t z p l a t e and r o t a t i n g i t , e x t r e m e l y t h i n m u l t i l a y e r s can be grown. I t i s e s t i m a t e d t h a t by r o t a t i n g the s u b s t r a t e a t 200-300 rpm under normal VPE growth c o n d i t i o n s , s i n g l e atomic l a y e r s o f each m a t e r i a l c o u l d be d e p o s i t e d . F i g u r e 11 c o n t a i n s an SEM photo o f a s t a i n e d a n g l e - l a p p e d s e c t i o n from a 5 0 - l a y e r InAsP/InP m u l t i l a y e r s t r u c t u r e — each w i t h a 200 X t h i c k n e s s . A l t h o u g h e x c i t i n g fundamental s t u d i e s may be performed w i t h s t r u c t u r e s p r e p a r e d i n the d o u b l e - b a r r e l r e a c t o r , i t s main p r a c t i c a l advantage i s a s a v i n g i n growth time and m a t e r i a l s , as w e l l as the possible attainment of h i g h l y - s u p e r i o r interfacial properties. Growth o f a t y p i c a l l a s e r s t r u c t u r e p r e s e n t l y t a k e s about 2 hours and i n v o l v e s f o u r p r e h e a t c y c l e s , i n c l u d i n g one a t each o f the two c a v i t y interfaces. InP i s p a r t i c u l a r l y s u s c e p t i b l e t o d e c o m p o s i t i o n e f f e c t s at e l e v a t e d t e m p e r a t u r e s . W i t h the new system, the t o t a l growth time i s reduced t o 30 min, and a l l p r e h e a t c y c l e s a r e e l i m i n a t e d ( e x c e p t f o r the o r i g i n a l one, which can be p o s i t i o n e d 1-10 pm below the l a s e r cavity). The reduced growth time would enable 15 o r more l a s e r wafers t o be grown i n a s i n g l e day. The e l i m i n a t i o n o f the p r e h e a t c y c l e s i s e x p e c t e d t o y i e l d c l e a n e r i n t e r f a c e s , which s h o u l d p r o v i d e l a s e r s w i t h lower t h r e s h o l d c u r r e n t d e n s i t i e s , h i g h e r e f f i c i e n c i e s , and b e t t e r r e l i a b i l i t y . Improved i n t e r f a c e s s h o u l d s i m i l a r l y enhance the performance o f a v a l a n c h e p h o t o d i o d e s , as d i s c u s s e d i n the p r e v i o u s s e c t i o n . These advantages are h i g h l i g h t e d i n T a b l e I I .


12.

OLSEN

Group III-V


Table I I .

Compound

Optoelectronic

Devices

233

Advantages o f D o u b l e - B a r r e l VPE R e a c t o r

•

Cleaner I n t e r f a c e s : C r y s t a l growth i s n o t i n t e r r u p t e d when growing m u l t i p l e ( h e t e r o e p i t a x i a l ) l a y e r s .

•

R a p i d D e v i c e Growth: A complete f o u r - l a y e r InGaAsP/InP/ InGaAsP/InP 1.3 fJm cw l a s e r s t r u c t u r e can be grown i n about 30 minutes. F i f t e e n o r more wafers o f t h i s type c o u l d be grown i n one day.

•

V e r y - t h i n L a y e r Growth: M u l t i p l e l a y e r s ( 1.4 pm i s d i f f i c u l t because o f d i s s o l u t i o n o f the a l l o y by the &P m e l t . A l t h o u g h t h i s problem can be c i r c u m v e n t e d by s p e c i a l growth t e c h n i q u e s , i t does l i m i t the f l e x i b i l i t y o f the LPE t e c h n i q u e s i n c e the u s u a l growth t e c h n i q u e s cannot be used h e r e . No such problems e x i s t f o r VPE, and m u l t i l a y e r h e t e r o s t r u c t u r e s w i t h bandgap wavelengths i n excess o f 2.0 |Jm can be f a b r i c a t e d u s i n g the same t e c h n i q u e s as f o r 1.3 |Jm d e v i c e s . This would i n c l u d e e m i t t e r s and d e t e c t o r s i n the 2-3.5 |Jm range ( u s i n g InGaAs/InAsP) and the 3-6 urn range ( u s i n g InGaSb/InAsSb). As l o n g wavelength GalnAsP l a s e r s , LEDs, and p h o t o d e t e c t o r s b e g i n t o r e p l a c e GaAs e m i t t e r s and S i d e t e c t o r s f o r l o w - l o s s f i b e r a p p l i c a t i o n s and as new a p p l i c a t i o n s a r i s e i n the 1.0-1.7 |Jm regime, l o o k f o r the VPE p r o c e s s t o p l a y an i n c r e a s i n g l y i m p o r t a n t r o l e i n the t e c h n o l o g y o f electronic devices.


12.

OLSEN

Group

III-V

Compound

Optoelectronic

Devices

239


Another i m p o r t a n t a p p l i c a t i o n concerns v i s i b l e l a s e r s . VPE can be used t o grow InGaP/GaAsP and InGaP/InGaAsP h e t e r o s t r u c t u r e s f o r l a s e r s which emit l i g h t near 7000 &. CW o p e r a t i o n a t 10°C was r e p o r t e d f o r 7050 8 InGaP/GaAsP l a s e r s by K r e s s e l (42) e t a l . U s u i e t a l (43) have r e p o r t e d cw room temperature o p e r a t i o n near 7600 & w i t h VPE InGaAsP/InGaP. (They a l s o r e p o r t e d reduced w a l l d e p o s i t s w i t h t h e a d d i t i o n o f s m a l l oxygen c o n c e n t r a t i o n s ) . As i n t e r e s t i n v i s i b l e l a s e r s i n c r e a s e s , d r i v e n by o p t i c a l r e c o r d i n g / p l a y b a c k and audio d i s c a p p l i c a t i o n s , VPE t e c h n o l o g y w i l l u n d o u b t e d l y become more w i d e s p r e a d i n o p t o e l e c t r o n i c a p p l i c a t i o n s . Acknowledgments T h i s paper was o r i g i n a l l y p r e s e n t e d a t t h e S p r i n g 1983 M e e t i n g o f The E l e c t r o c h e m i c a l S o c i e t y , I n c . h e l d i n San F r a n c i s c o , C a l i f . C o p y r i g h t 1983, The E l e c t r o c h e m i c a l S o c i e t y . Literature Cited 1. 2. 3.

4. 5. 6.

7.

8. 9.

10. 11.

12. 13. 14. 15.

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