CHAPTER - 7

CHEMICAL ETCHING OF lnBi:Te SINGLE CRYSTALS

 CHAPTER - 7

CHEMICAL ETCHING OF lnBi:Te SINGLE CRYSTALS

The work carried out and reported by the present author in this
chapter, deals with the results from the chemical etching study of the
cleavage plane of Te doped InBi single crystals. No systematic study on
chemical etching of these single crystals has so far been reported. The
present author has developed three chemical etchants, The results
obtained with these new dislocation etchants are discussed and compared

for the best dislocation etchant among them. The author has used these
etchants to assess the perfection of crystals and in the study of
deformation of these crystals.

Chemical etching is the simplest method for revealing dislocations.

The selective nature of the etching phenomenon is influenced by a
number of factors like, the nature of the individual crystals, crystalline
perfection, crystallographic orientation, type and concentration of impurities
in the crystals as well as in the etchant, the temperature and the
hydrodynamics of the solid-liquid interface. Chemical etching has a wide
range of applications and it is used :

1. for revealing defects in the crystalline materials, to study the

behaviour and mode of formation of dislocations.

2. for orientation determination in conjunction with optical goniometry.

3. for preparation of clean surfaces.

4. to obtain reproducible electrical properties of semiconductors.

96
5. to determine the content of impurity distributions and

6. for controlled removal of materials.

The discussion which follows is confined to the use of chemical

etching for studying crystalline defects (dislocations in particular) only.

For the formation of etch pits at dislocation sites, the etching rate
along the dislocation line is very essential to be greater than that on the

rest of the surface. It has been proposed that increase in the etching
rate along a dislocation line is due to the strain field associated with the

dislocation. Therefore it is an accepted fact that chemical etching is a

simple, rapid and valid method revealing dislocations which makes it a

valuable tool for studying perfection and plasticity of crystalline materials.

Etching methods have been successfully developed for various single
crystals namely Germanium, Silicon^2 Silicon- Iron, Zinc, Lithium
flouride, Silicon carbide, Copper-aluminium alloys, Bi Sb(2-y) Tex
Se(3-x)(9) and Bismuth telluride^ etc. to mention only a few. Typically

etching has been used on (511) and (511) planes to evidence the polar
structure of CdTe crystals (Iwanaga et al)(. Dislocation etching can be

very fruitfully used to test the crystal perfection and slip deformation
under the effect of as low an impurity concentration as 0.05 at.%
(Imashimizu et al^).

Various methods have been employed to establish a relation

between etch pits and dislocations :

1. perfect matching of etch pits on matched cleaved surfaces.

97
2. repetition of the pattern on successive etching or polishing and
etching which allows the tracing of dislocations to some depth within
the crystal.

3. introducing various types of plastic deformation and looking for

corresponding increased etch pit density.

There is no report whatsoever, on lnBi:Te single crystals, found in

literature. However, a brief review of dislocation etching studies on InBi
single crystals reported by previous workers, is given below.

InBi is a lll-V intermetallic compound. The etchant known as CP-4

and first developed for germanium by Vogel et al^13\ has been widely

used, with modifications, to reveal dislocations in almost all other lll-V

compounds and other intermetallic compounds. But these etchants have
not been found successful on InBi because InBi behaves quite differently
in chemical reactions. Though the cleavage surface of InBi has a high
optical reflectivity and an exceptionally low tendency to oxidize in air, it
has an equally high tendency to corrode under chemical reactions. Roy
et al^ and Walter^ have reported various dislocation etchants and

shown that the results were quite difficult to be reproduced and frequently
the etch pits were of irregular shape. The dislocation etchants reported
by Roy et al^ are composed as follows :

1. 6 parts 80% tartaric acid,

10 parts 3% H2O2 and

2 parts HNO3

2. 6 parts 80% tartaric acid,

10 parts 3% H202,

2 parts HNO3 and

4 parts 0.5 M KMn04

98
 3. 6 parts 80% tartaric acid,

10 parts 3% H2O2,

2 parts HNO3 and

30 parts glycerine

These etchants were used by Desai^ on cleavage surface of

InBi single crystals. He obtained etch pits of highly irregular shape and

the surface in general corroded after using the first etchant. Frequently, it

was further observed that the surface contour was spoiled to such an

extent that the etch pits, if at all developed, become indistinguishable

from the general surface. For the second etchant, again corrosion of the

surface was seen and the etch pits were rounded. The third etchant was

found better than the former etchants in the sense that the surface

corrosion was less and the etch pit shape was better defined.

Walter^ has also reported some dislocation etchants which are

as follows :

(1) CP-4A ; H2O : CH3COOH - 1:1:1

CP-4A = HNOs : HF : CH3COOH - 5:3:3

(2) HNO3 : H2O2 : 40% tartaric acid - 1:1:6

(3) I2 (Concentrated methanol solution) : Methanol

(4) Br2 : Methanol - 1:12.5

However, among these etchants, the etchant no.3, consisting of

iodine was found to give satisfactory and easily reproducible results as

per the studies reported by Desai^16^ Although, this etchant has a

preferrential attack without oxidizing the general surface, it does not give

pits of any specific shape.

99
 Bhatt et al^ have also developed a dislocation etchant consisting

of 1 part "A" and 10 parts CH3COOH (glacial), where "A" is 10 parts

0.05M Cr03 and 1 part HNO3 (70%). They obtained well defined point

bottomed square pits, exhibiting the four-fold symmetry of the (001)

cleavage plane and further observed that this etchant was capable of

revealing dislocations intersecting the cleavage plane. They have also

used this etchant to measure the average dislocation density of InBi

single crystals.

A systematic study of the development of new etchants was

undertaken and the results are compared. In attributing the etch pits to

dislocations, the following criteria are adopted :

(1) Matching of etch pits on cleavage counter parts should be

reasonably good.

(2) Etch pit density (i.e., dislocation density) should remain constant and

it should not increase after repeated etching.

(3) If the crystal is deformed, e.g., by an indentation or a scratch, there

should appear an increased density of pits around the deformation

site and preferably the pits should delineate the slip rosettes.

Single crystals of lnBi:Te grown by the horizontal zone melting

technique were cleaved at 0C temperature with a sharp blade along

(001) plane. Freshly cleaved faces were etched in the dislocation etchant

for a few seconds. They were then cleaned in distilled water and finally

air-dried. The etch patterns were studied under Vickers Projection

Microscope. It should be noted at the outset that practically no change

in the etch pattern was observed in the crystals having impurity

concentrations of Te ranging from 0.1 at.% to 2.0 at.%.

100
Development of an etchant :

The inhomogeneities in the grown crystals are revealed by etching

because of reactions at inherently different rates at the inhomogeneity
sites. The structural defects like point defects, line defects, inclusions,
segregated area etc., are selectively attacked by the etching reagent and
as a consequence their precise locations are manifested finally by some

visible etching characteristics, such as cavities, striations, local

decolouration etc. Before etching, many of the inhomogeneities and
defects associated with the section of interest may be small in size and
even entirely invisible. But during etching, the area occupied originally by
certain of these inhomogeneities will increase in size beyond their original
dimensions and eventually reach a size which will be visible and

amenable to detailed study under a variety of optical techniques.

The successful application of etching depends upon several

factors. Among them, some important factors are as follows :

(1) The condition of the crystal surface that is to be etched.

(2) Chemical composition of the etching reagent selected.

(3) Temperature of the etching reagent selected.

(4) The length of time the specimen is etched.

As far as the etching reagent is concerned, it should possess the

following characteristics :

(1) The reagent should be of such composition that it will give good all
round results and reveal the greatest number and variety of

101
 structural characteristics, defects and irregularities present. At the

same time, it should be able to distinguish its effect from those

produced by any of the etchants which can attack on only definite

type of defects. Thus, the selective etching should enable one to

study only specific defects.

(2) The reagent should be simple in composition and stable so that its

concentration will not change appreciably upon standing or during

use at room temperature and also if possible, at moderately higher

temperatures.

(3) The reagent should have constant characteristics at a particular

temperature so that the conditions of etching can be easily

reproduced. The temperature and time of etching are also important

factors to be decided in the etching process.

(a) Temperature of etching : The rate at which the etching

reagent attacks the specimen, depends upon the temperature at

which etching takes place. The precise influence of temperature,

however, varies according to the composition and previous history

of the specimen. It is, therefore, desirable for reproducible results

to carry out etching experiments only at definite temperatures.

(b) Time of etching : The time of etching is perhaps one of the

most important factors contributing to successful etching and

attendant appearance of the structure enabling their detailed study

possible with the help of optical techniques. For example, for short

time of etching as compared to that appropriate for a particular

material, the etched structure will not be completely developed nor

will be sufficient details revealed to permit accurate interpretation of

the etched area. However, too long a time of etching is just as

102
 unsatisfactory as one too short, owing to details of the surface
structure being thereby obscured to varying degrees and frequently
some parts of the structure being completely obliterated. The time
of etching depends upon the conditions of the specimen (i.e.,

normalized, hardened, etc.) and the temperature of the reagent.

(4) The reagent, while acting on the specimen should not form products
which will precipitate on the surface of the specimen considered, but
must have such a composition that reaction products are
immediately dissolved chemically or physically in the solution. They
must possess closer affinity with the etchant than with the specimen.

(5) The reagent should be non-injurious and non-toxic to the person

conducting the work.

(6) For orientation determination, the etchant should develop etch pits or
facets with plane faces accurately parallel to crystallographic planes

of low indices.

Looking to the above requirements of the etchant and the surface

to receive it (i.e., in the present case, cleavage plane (001) of lnBi:Te

single crystals), it was found after several trials that the etchants
developed by the present author possessed most of the properties

discussed above and was well suited for revealing dislocations.

It is well known that for metals, the necessary ingredients of an

etchant are generally an oxidant and a complexant which may,
respectively, react with the specimen surface and dissolve the products
formed. Nitric acid is a well known oxidant for etching of metals and in

the present case also, it was found to be a well suited oxidizing agent

103
for etching of the cleavage plane (001) of lnBi:Te single crystals. It was

also observed that the crystal surface in question has a high tendency to

corrode and frequently to capture the reaction products, as also evident

from the earlier reported results on etching. This fact poses a severe

difficulty in developing a successful etchant. However, after several trials

with a large number of chemicals in combination with HNO3, a few

successful etchants were developed. Some important developments

obtained during various trials with these chemicals are discussed below.

All the etching trials were carried out at room temperature on freshly

cleaved (001) surfaces. All chemicals used were of A.R. grade and the

aqueous solutions were prepared in double distilled water. The

water-soluble ingredients of the etchant, wherever mentioned in the

discussion below, should be understood as saturated solutions in double

distilled water at room temperature.

Etchant-A :

For the initial trials, nitric acid (70%) was tried in various dilutions

ranging from 10 to 1 percent in water. Even at the lowest dilution, there

was general corrosion of the surface observed. To suppress this, Acetic

acid (glacial) and then Methanol/Acetone were tried in different proportions

with nitric acid. In the case of acetic acid, the reaction of nitric acid was

suppressed to some extent but at the same time its presence always

resulted in formation of reddish film on the surface. With addition of

methanol/acetone, the formation of film was nearly eliminated but a

general corrosion of the surface prevailed. However, tiny nucleations of

etch pits were observed in the back ground. Quite many trials with these

three were done without any significant improvement. Therefore a fourth

ingredient, namely K2Cr207 in aqueous solution was added. This

composition of the etchant led to a systematic sequence of trials for the

development of the dislocation etchant. Some of the significant trials

104
together with their etching characteristics are outlined in table 1. It can

be seen that among these trials the first significant result was obtained

with (1 part 10% K2Cr207) + (10 parts CH3COOH) + (0.1 part HNO3).

A typical etch pattern obtained with 20 seconds of etching time is

shown in figure 1. Here the etch pit shape is ill-defined. Increasing nitric

acid to 0.3 parts produced an effect of imparting a little shape,

approximate square, to the pits, as can be seen in figure 2. There is

little or no corrosion of the general surface but at the same time the

etch pits do not have uniform size. The final satisfactory result obtained

was with nitric acid further increased to 0.5 part. Figure 3 illustrates a

typical etched surface showing clear point bottomed scattered etch pits.

The shape of the etch pits is also regular and nearly well defined

square. Further they have the same orientation. As can be seen in the

table above, any further increase of nitric acid spoils the result.

From the results obtained with the above trials, it seem that nitric

acid may be the main oxidizing agent, whereas K2 Cr2 O7 and acetic

acid are likely to be complexing agents, dissolving the reaction products

removing them from the surface into the solution. This is because K2 Cr2

O7 by itself was not found to produce any reaction with the crystal

surface; but still however, its presence only has resulted in the final

desirable etching characteristics.

Although the etch pattern produced by the etchant bears a

general character of dislocation etch-pits, namely, the point bottomed

nature, uniform size and orientation and the symmetry of the working

plane, it is essential to establish its reliability as a dislocation etchant.

Therefore a few standard tests were carried out.

105
 n
Fig.3 x 500
 TABLE -1

EFFECT OF ETCHANT COMPOSITION ON ETCHING CHARACTERISTICS :

(FOR ETCHANT-A)

Sr. Etchant Etching Etching characteristics

No. time sec.

1. 1 Part 10% K2Cr207 10 irregular shape of pits &

5 parts Methanol no observable corrosion.
10 parts CH3COOH
0.5 part HNO3 20 approximate circular pits,
corrosion.

2. 1 part 10% K2Cr207 10 increased corrosion, no

5 parts Methanol effect on the etch-pit shape
10 parts CH3COOH
1 part HNO3

3. 1 part 10% K2Cr207 10 few square & circular shape

10 parts Acetone pits without observable
10 parts CH3COOH corrosion.
0.1 part HNO3 20 as above but little corrosion
observed.

4. 1 part 10% K2Cr207 10 corrosion increased.

10 parts Acetone
10 parts CH3COOH
0.2 part HNO3

5. 1 part 10% K2Cr207 10 nearly square shaped pits

10 parts Acetone with more observable corro
10 parts CH3COOH sion.
0.5 part HNO3

106
Sr. Etchant Etching Etching characteristics
No. time sec.

6. 1 part 10% K2Cr207 10 irregular shape of pits with

5 parts Acetone little surface corrosion
10 parts CH3COOH
1 part HNO3 20 increased surface corrosion.

7. 1 part 10% K2Cr2C>7 10 no reaction

10 parts CH3COOH 20 irregular shape of pits with
0.1 part HNO3 little surface corrosion (Fig.1).

8. 1 part 10% K2Cr207 10 The edges of pits are not

10 parts CH3COOH rectilinear and the pits are
0.3 part HNO3 of various sizes (Fig.2).
20 as above but little corrosion
observed.

9. 1 part 10% K2Cr207 10 few square shaped pits of

10 parts CH3COOH small size.
0.4 part HNO3 20 size of pits increased with
the same number of pits.
30 as above with little observable
corrosion.

10. 1 part 10% K2Cr207 10 square shape point bottomed

10 parts CH3COOH pits, nearly of same size
0.5 part HNO3 (Fig-3).
(Etchant-A) 20 size of pits increased.
30 pits with increased size & no
surface corrosion observed.

11. 1 part 10% K2Gr207 10 square shape point bottomed

10 parts CH3COOH pits with little observable
0.6 part HNO3 corrosion.
' 20 corrosion increased.

107
 One of the most important tests applicable for the cleavage
surfaces is to establish one to one correspondence between the etch pits
produced on the cleavage counterparts. Also this test itself is generally
considered a quite adequate proof that the etch pits mark the sites

where the dislocations intersect the surface.

Figures 4(a) and 4(b) are the photographs of etch patterns

produced on the oppositely matched cleavage counterparts. It can be
seen that both the position and the number of etch pits are in exact one
to one correspondence. It may be noted that one of the surfaces,

namely, the one shown in figure 4(b) was etched for a longer time to
distinguish it from its counterpart. Such tests were carried out on many
samples. While in most of the cases, such one to one correspondence
was observed, some of the patterns showed deviations to a tolerable
extent. For example in figures 5(a) and 5(b), some mismatch is observed.
(Note that due to overfocus the pit boundaries have lost their optical
contrast). This may be due to branching and bending of dislocations at
the cleavage plane (Sagar et al and Bhatt et al)^18,19^, which may be

quite possible due to severe dislocation interaction in a region containing

large number of dislocations as indicated by etch grooves seen in the

photograph.

The test of successive etching is based on the fact that a

dislocation line cannot terminate within the crystal. Figures 6(a) and 6(b)
show the etch patterns obtained on the same region on the same
cleavage surface etched for 10 and 15 seconds, respectively. It can be
seen that the pits have to some extent increased in size with the etching
time, whereas their number has remained the same, indicating thereby
that the pits are at the sites of emergence of dislocation.

108
 x 450 Fig.4(b) x 450
Fig. 4(a)

Fig. 5(a) x 425 Fig. 5(b) x 42 5

Fig. 6(a) X 4-25

Fig.6(b) x 4-25

Fig. 7 x U25
 In addition to the randomly distributed .etch pits found on the

cleaved surfaces, distinct rows of closely spaced pits and branching of

the rows were also observed as shown in figure 7. These rows

resemble the low angle boundaries commonly observed in metallic and

intermetallic crystals (Sagar et al^18,22^, Bhatt et al^19\ Amelinckx^,

Brown et al*2^ and Yim et al^). A model based on minimum free

energy (Wernick)^ for dislocation tilt boundary gives the relation :

na = nb + nc

where na, nb and nc are average density of pits along A,B and C

boundaries, respectively. In the above figure, this relation is satisfied with

A,B and C designations indicated on the photograph.

To test the capability of the etchant to reveal fresh dislocations,

the specimen was indented (with Vickers hardness indenter) and etched.

The resulting etch pattern near the indentation mark consists of well

defined rows of etch pits as seen in figure 8. The rows are in two

distinct mutually perpendicular directions implying delineation of slip traces

produced by the deformation. The slip system {110} - <001 > (Bhatt et
al^) would give traces along < 110 > directions on the cleavage plane

(001). Therefore the rows of etch pits observed above must be along
[110] and [1T0]. Since the edge of the etch pit is also parallel to the

etch pit rows, it must be along a < 110 > direction. Thus the etchant is

capable of revealing freshly introduced dislocations.

There is also a secondary slip system reported in this crystal.

This is {100} <001 >. This was observable in the present case also.

When a specimen surface is indented by a sharp pin and etched in the

dislocation etchant, the secondary slip trace together with the primary slip

trace was observed as can be seen in figure 9. The etch pit row parallel

109
SZV X
to the etch pit diagonal is in the [100] direction which is the intersection
of the (100) plane with the cleavage plane (001) and thus corresponds to
the secondary slip. The rows parallel to the etch pit edge are due to the
primary slip.

Figure 10 is an interesting photograph of the etch pattern

produced on an as-cleaved surface. The two sets of rows of etch pits
observed here are inclined at about 45 to each other and one of them

is parallel to the etch pit edge while the other is parallel to the diagonal.
Therefore it is possible that these rows delineate dislocations produced by
primary and secondary slip which might have occurred during the
process of cleavage or due to mechanical handling. Another typical
example is given in figure 11. The large number of slip traces indicate
the specimen to be highly deformed.

Thus the etchant "A" is a dislocation etchant as can be concluded

from the results of various tests and the etch patterns observed in the
above two cases. Specifically, it is capable of revealing grown-in, aged
and fresh dislocations intersecting the cleavage plane.

Etchant - B :

in this etchant, nitric acid was retained and organic solvents like
methanol, acetone and tartaric acid were used to replace K2 Cr2 O7 of
etchant "A". The best composition obtained was as under :

(10 parts tartaric acid) + (8 parts acetone) + (10 parts glacial acetic
acid) + (1 part HNO3).

110
Fig.11 x UOO
Few of the significant trials and their results are enlisted in table 2. A
study of the table implies that nitric acid plays an important role in

developing shape of the etch pits which is controlled by the proportion of

the nitric acid in the etchant. It should be noted that the etchant has two
important reaction features,

(1) Evolution of bubbles at the specimen surface is associated with

starting of the reaction.

(2) With the progressive etching of the specimen, the surface is not
tarnished and does not become too coarse to be unsuitable for
study in depth and extension.

For testing this etchant as a dislocation etchant, the tests like

matching of etched cleavage counterparts, successive etching etc., were
conducted. Figures 12(a) and 12(b) show the etch patterns on oppositely
matched cleavage surfaces. It can be seen that there is a good general
matching of the pits. However, few mismatches are also observed. This
may be due to reasons like uneven stresses developed at the time of
cleaving the specimen, branching and bending of dislocations at cleavage
plane, etc.

Figures 13(a) and 13(b) show the etch patterns obtained after
successive etching for 20 and 25 seconds, respectively. While the number
of pits is the same in (a) and (b), the pit size in (b) is larger indicating
continuation of the dislocation lines into the depth of the specimen.

111
 TABLE - 2

EFFECT OF ETCHANT COMPOSITION ON ETCHING CHARACTERISTICS :

(FOR ETCHANT B)

Sr. Etchant Etching Etching characteristics

No. time sec.

1. 10 parts tartaric acid 20 square shape pits with

7 parts Methanol corrosion.
2 parts Acetone
3 parts CH3COOH
0.1 part HNO3

2. 10 parts tartaric acid 20 few square shape point

7 parts Methanol bottomed pits with little
4 parts Acetone observable corrosion.
3 parts CH3COOH
0.1 part HNO3

3. 10 parts tartaric acid 20 irregular shape of pits.

8 parts Acetone
10 parts CH3COOH
0.5 part HNO3

4. 10 parts tartaric acid 20 very few square shape pits

8 parts Acetone and some circular in shape
10 parts CH3COOH but the rest irregular in
0.8 part HNO3 shape.

5. 10 parts tartaric acid 15 square shape point bottomed

8 parts Acetone pits in small size without
10 parts CH3COOH observable corrosion.
1 part HNO3
(Etchant-B) 20 number of pits remains same
but the size increased and
no surface corrosion
observed.
30 many clear square shape
point bottomed pits of
larger size without observable
corrosion.

6. 10 parts tartaric acid 20 irregular shape of pits

8 parts Acetone with surface corrosion.
10 parts CH3COOH
1.2 part HNO3

112
Fig.12(a) x UQO Fig. 12(b) x 400


> yM ' ' ' %

'i* u 8
*/ 1
X
m *o(
-xj
V.Q

Fig. 13(a) x500

.
o n
v o
Jr-*
us;
Fig. 13(b) x 500

Fig. 14 x 450
 Figure 14 is the etch pattern obtained around a scratch produced
on the surface. Very large number of etch pits indicate severe
deformation produced by the scratch. Thus the etchant is capable of
revealing fresh dislocations.

Figure 15 is a typical etch pattern obtained by this etchant

showing rows of etch pits as well as randomly scattered etch pits. The
rows of etch pits may be associated with low angle boundaries.

Figure 16 shows a good example of intersecting low angle

boundaries revealed by the etchant. As in the previous case, relation
na = nb + nc is satisfied.

From the results obtained with this etchant, it can be concluded

that the etchant is capable of revealing fresh and grown-in dislocations
intersecting the cleavage plane.

Etehant-C :

In the course of trials for the development of etchant B, following

composition was also found to work as a dislocation etchant :

(10 parts tartaric acid) + (7 parts methanol) + (3 parts glacial acetic

acid) + (0.1 part HNO3 (70%)).

Matching of efcch pattern obtained on the cleavage counter parts

is shown in figures 17(a) and 17(b). A fairly good correspondence of
etch pits is observed. But, an important feature is also to be noted

namely, the pits do not all have well defined square shape.

113
Fig. 15 x 350

Fig.16 x 4-50
Fig. 17(a) x ^50 Fig. 17(b) x ^50
 The result of successive etching test is shown in figures 18(a)

and 18(b), which are the etch patterns obtained after etchings of 40 and
60 seconds, respectively. Increase in etch pit size with etching time is

evident.

Figure 19 shows intersecting low angle boundaries which satisfy

the relation na = nb + nc.

Figure 20 shows well scattered etch pits produced by the etchant.

It provides good example of non-uniformity of the etch pit shape as well

as deviations from the square shape. Also there can be observed a few
cases of non-uniform size.

When a crystal ingot was deformed by bending and then cleaved

at different places, followed by etching a cleaved surface, a general high
etch pit density was observed in almost all the cases. A typical pattern
of clusters and rows of etch pits obtained is shown in figure 21. Thus

the etchant is capable of revealing fresh dislocations. The etching test of

scratched and indented surfaces also confirmed this.

From the above observations, it can be concluded that the

etchant "C" can be used as a dislocation etchant.

The main features of etchants A,B and C are given in table 3.

From the discussions above and table 3, it can be said that the etchant

"A" is the best of the three.

114
 JKtferfr*

Fig.18(a) x UOO

dbfttl If

Fig.18(b) x 400

Fig.19 x 400
Fig..20 x 400

R'g-21 X 400
 TABLE - 3

Etchant Composition Minimum Shape of order of Remark

etching etch pit dislocation
time in density
second revealed
in cm'2

A 1 part 10% K2Cr207 10 Well defined 104 - Etching time can

+ 10 parts GhaCOOH point bottomed be increased upto
+ 0.5 part HNO3 square 30 seconds without
surface corrosion.

- Exact one to one

correspondence of
etch pits on the
matched cleavage
faces.

B 10 parts tartaric acid 15 point bottom 104 - Etching time can

+ 8 parts acetone ed square be increased upto
+ 10 parts CH3COOH 40 seconds without
+ 1 part HNO3 causing surface
corrosion.

- Fairly good general

correspondence of
etch pits on the
matched cleavage
faces.

C 10 parts tartaric acid 25 point bottom 104 - Etching time can

+ 7 parts methanol ed ill-defined be increased upto
+ 3 parts CH3COOH square pits 60 seconds without
+ 0.1 part HNO3 corrosion.

- Hence the etchant

may be suitable to
study dislocation
motion.

- Frequently non
uniform shape and
size of etch pits.

115
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