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RE-IR-71-60
TECHNICAL REPORT
Joseph Monk.
Septe~mber 1971
RESEARCH DIRECTORATE
Roproducod by
NATIONAL TECHNICAL
INFORMATION SERVICE
Sprngfiaod, Va. 221_,1
Approved for public release, distribution unlimited.
\ C,
REPRODUCED FROM
BEST AVAILABLE COPY
I
Unclassified
Secuntiy Classification
DOCUMENT CONTROL DATA R & D
($esurity classifiction of fIIl, body of *betraCt and lnd.img e. noteiion ru.i be .nf.,.d uh.n rh. ov. rail report
P"'1 I' M ,ed,
i OR0GIN&ING 4CTI wlTVy (COrvpO.r. .utho-) I.. APCN? SgCURIT, CLA IISI CATION
Joseph Menke
1 "900117 OATI 7A, TOTAL NO. OF PAAGES 17b, NO. OFP REPS
September 1971 21 2
14i. CONTRACT Of GRANT NO. 90. ORlGINATOR'l* REPOIRT NuU.JINE1lh
POR I C UT Is ILogol.
DISCLAIMER:
The find~ings of this report are not to be construed as
an official Department of the Army position unless so designated
by other authorized documents.
~Ifl~ ~')
* 2' *
l.w,. IL .
I I\ ....
I
UncIlassified
Security Classification
LINK A
2. Manganese Phosphating
5. Conversion Coatings
Unclassified
Mcurity Claesification
A'-
*t
9 1
S BLANK PAGE.
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1a
M..---.
ADD
RESEARCH DIRECTORATE
TECHNICAL REPORT
RE-TR-71-60
Joseph Menke
September 1971
i
ABSTRACT
n--k nirartnratp. Weai)ons
Work Was condu(.Le6 Y
Development and Engi-
Laboratory at Rock Island, Research,
Weapons Command to determine
ncering Directorate, U. S. Army associated with the
the composition of and the reactions
coatings. An improved phos-
formation of manganese-phosphate from a stock manganese
produced
phate coating was studied as
addition of manganese citrate,
phosphating bath to which an Processing was accomplished
tartrate, or gluconate was made. above 212OF with steam pres-
in an autoclave at temperatures and pressure
sure. The coatings produced by conventional
thermal analysis, X-ray
methods were examined by differential analysis. The chemical
diffraction, and atomic absorption was Fe3(PO4)2-2MnHP04'
structure of the conventional coating
that of the pressure phos-
4H20, a form of hureaullte, and phosphate heptahydrate,
phate coating was mainly manganese
Mn3(PO,)2-7H20,
CONTENTS
Page
Title Page
ii
Abstract
Table of Contents ii
Objective
Background
2
Approach
6
Results
9
Discussion
11
Conclusions
12
Recommendations
13
Literature Cited
14
Distribution
iii
OBJECTIVE
BACKGROUND
3MnHP04 - Mn
3 (PO4) 2 + H-PO 4 (2)
APPROACH
2
to whinh 10 grams per liter of manganese tartrate had been
added. Processing wds accomolished in an autoclave at <-
psig (214'F) of steam pressure for 30 minutes. A third
group of the :p) i.eLi wa .Pt Ut::d racvanti.na
Iae
manganese-phosphating bath to which 10 grams per liter of
manganese qluconate had been added. Processing was accom-
plished in an autoclave at ,l psig (213'F) of steaml pressure
for 30 mInutes.
3
CDOC O= D OD C) ODD CD
~
1~ ~ ) CCDC ) oID3
) C
a-
In
A
w
< 0
00
a.-
C7
02
V)0
S 3-
UQ)
CDc U iC
cli C,
-0 0D
0 C
0 - r- cr-
0' 0'
43
0~r
. D
024- 03J 234-
0 =- 3 CL,
J ~ ~ CL 0-
CL
- 0 0
V) CL 3/ la, 0 CL3
'A 0 S- 0
000
0 3tC' C'a :
.3- 0 .43 UCL
02 ~~~ S-44))
4-'
-C)
C~
C0
4 -
0
-04
02 ~~ ~ .0 ~L C4 UU C-0 >43
0 0- 0 0 0 4' 0.
C 01 0 01
IC C
0'C
~
m
V)~~~~ ~~nV)c
4'C
0"C
V) ca ' nc n Cc
00 0 clt 0 C\
0 0
CD
(n01iD C - C14 m~~
-~ ~'.C. ~
(C\ C c
CDC
LM (L.
RESULTS
6
I0
00
C)C) C))
0 0'
410
ol -
C000 C) C-
01 C>C)
0 L-
0- cu 0D
0~d
-- x
00LA 0u
000 * l--
ZL~ .- L 00 00
LUJ 0 IL.U.A.C
0 73
U-- CL
0 C*
UJ JL
0f a D ')
0 WU U E~
C)C)
2:
L(l/)
I- (D ('000CD0 00 CD m
000 000 4
(U-
) 000
S- w U() q
a w 4J U-)
LU e- r
)
w--~ w.L
~La w ui:
2!: - 4-'
E- 00 0000 00
000 000
V) w-4-
cu 0
> >
0~0 0
~~
a)V4C)4 ~ 4. ~ 1 - ~ C
to- r_ 4-)tO.4o
V) ~ ~ -4JU+L.4
C 4-)
4.~-) -~-
IA 41s L-
41 SI-
U4-30 U 4-30
U 4-) 04-)O0)
0
I
diffraction pattern are more intense when compared with the
diffraction pattern for conventional manganese-phosphate.
These two peaks correspond to the two major peaks present
in the X-ray diffraction pattern of manganese pyrophosphate.
!T date, the pr~otnre of ovroohosphate in the pressure
phosphate-coating has not been confirmed.
8
DISCUSSION
The reactions
associated with the formation of a pres-
sure , -p tc c'~tin" must t4 intn consideration
two major factors: (1) the addition of manganese citrate,
tartrate, or gluconate and (2) the inclusion of processing
parameters above 212'F by steam pressure. The reactions
which may occur when manganese citrate, tartrate, or glu-
conate are added to a phosphating solution can be summarized
by consideration of the fact that organic radicals can:
9
I
the pressure phosphate coating:
H2 0,' ,UH 2
I I
0 H H H H
0 /0
R - C + H2 - R - C + OH- (6a)
0 H
R C + 2H 2 - >R - C - OH + OH (6b)
""0 ~H
10
with the use of optical rotation techniques, reveals that
the organic constituent is decreased from 1.0 to approxi-
mately 0.5 per cent.
CONCLUSIONS
11
II
5. The chemical reactions in phosphating solutions
modified as indicated in this work are capable of producing
coatings with exceptional resistance to heat and corrosion.
kLCUMMENDATiONS I
12
LITERATURE CITED
13
DISTRIBUTION
Copies
A. Department of Defense
Commanding General
U. S. Army Materiel Command
ATTN: AMCRD-GF 1
AMCRD-TC 1
AMCRD-R, Mr. H. Cohen 1
Washington, 0. C. 20315
Commanding General
U. S, Army Tank-Automotive Command
Warren, Michigan 48090 2
Commanding General
U. S. Army Weapons Command
ATTN.: AMSWE-RD I
AMSWE-PP 1
AMSWE-SM 1
Rock Island, Illinois 61201
Commanding General
U. S. Army Missile Command
ATTN: Documentation & Technical Info. Br. 2
AMSMI-RRS, Mr. R. E. Ely 1
AMSMI-RSM, Mr. E. J. Wheelahan 1
Redstone Arsenal, Alabama 35809
14