DATA BASE GENERATION FOR MODELLING OF POWDER

MATERIAL FORMING DURING HIP

The success in manufacturing of complex shape parts by HIPing from

different powder materials is dramatically dependent on the accuracy of the
prognosis for the geometry of the part after HIPing and appropriate capsule design.
The most advanced techniques of such modelling describing the behaviour of
PM materials at high pressures and temperatures (for instance, Ashby technique) are
based on the principles of mechanics for the media with irreversible compressibility
and require a great amount of the experimental parameters to be determined.
LNT has developed and tested the special technique for creating the
necessary data bases with the minimum set of powder material parameters involved,
optimized for the adequate modelling of the HIP process.
Shrinkage of powder material during HIP has the following main
mechanisms of deformation: plasticity, creep and diffusion. Strict account of
these mechanisms is an extremely complicated task as one should determine here a
lot of rheological characteristics of material. The investigations showed that an
adequate description of shrinkage for typical HIP cycles may be done on the basis of
plasticity theory applied to powder materials. It is connected with the fact that the
main distortion of the part takes place on the first stages of densification, during
plastic deformation of powder. Further densification takes place under constantly
growing pressure. At this moment the dwell stage on densification, after the main
densification is over, the mechanisms of high temperature creep and diffusion start
working.
So the task is reduced to solving of a system of plasticity theory
equations, including: equilibrium equations, cinematic equations for the
deformation rate components, discontinuity equation, determinative equations,
thermal conductivity equations and Green's plasticity criterion (as the most
appropriate one):
  
2 2

 (1)
2
2 + 0
2 =
f f
s

1 2

, where f 1 and f 2 - some functions accounting the effect of average stress

0 and stress intensity factor T on densification and function of yield strength s
versus density.
The main problem which determines the adequacy and effectiveness of
the model of HIP process - the problem of data base creation for powder materials.
For creating such data base, f 1 and f 2 functions from the main equations and
plasticity criterion (1) are required.

Description of the experimental technique

In order to create the data base it is first of all necessary to define the
two functions f 1 and f 2.
These functions determine the average stress and density relationship ( f 1 )
and sheer stress influence on the densification ( f 2 ). It is obvious however, that
temperature factor also means much and it should be included directly or
indirectly into the equations.
Experiments on densification and shear deformation in the whole area of the
parameters ( - density, P - pressure and T - temperature) are very labor-
consuming. In practice, however, there exist deliberately impossible combinations
of these parameters (see fig. 2 ). Therefore, the area in which the information is really
needed can be substantially narrowed.
 Experiments were made as follows: special capsules with powder were
HIPped at regimes imitating a real technological process. At definite values of T and
P the cycle was cut down and the capsules were quickly cooled down in order to
avoid densification on an "idle" part of cycle (fig. 3). After HIPping and removing
the capsule, the density of compact was defined and samples for further plasticity
tests were manufactured.
The second important item of the procedure is the definition of conditions of
plastic deformation tests of the densified material. As the material is always
in the limited stress-strained state during HIP, temperature conditions of the
shear tests should be the same as they were during HIPing. It means that if the
sample was HIPped at T1 , it should be tested at T1 too. Thus, samples were tested
by means of hot upsetting at corresponding temperatures.
Test results were processed in the following way:
Determination of f 1 :
For upsetting of samples Green's criterion is:
  
2 2

 (2)
2
2 + 0
2 =
f f
s

1 2

,where  =  3 - intensity of tangential stress;

3
1
 0
=
33
- average stress;

 3
- compression stress.
Then
 
 /  −  0i /
2
f 1i
=
2
i
2
si
2
f 2i 

,where i - point of the HIP trajectory.

Determination of f 2 :
Green's criterion for HIP conditions is:

 =
2
2
2 (3)
f
s

,where P - HIP pressure;

s - yield strength of the monolitic material at HIP temperature;

Then f =
 i
2i
 si

,where i - point of the HIP trajectory.

Test results made it possible to obtain regressive relationships of f 1 and
f 2 functions versus density.

Besides that, for more convenient calculation, temperature function of yield

strength s may be substituted by its density function as temperature and density
are synonymously interconnected in one and same HIP cycle. So, the function for s
can be presented as follows:
 s
=  exp(    ) (6)
 where  ,  - coefficients,
 - density.
The following experiments illustrate this data base generation technique for a Ni base
powder alloy of the proprietary composition

Special capsules from 1018 mild steel of 1,325”OD, 1,190” ID and 7,3”
long with powder were built, filled, hot out-gassed and HIPed in the interrupted
HIP cycles imitating a real technological process for a 2050F HIP cycle as well
as in the 2050F HIP cycle of Kittyhawk to produce full density samples needed
for the evaluation of the rheological properties.

Figure 1. HIPed cans after the interrupted (standing) and full dense (machined)
coupons

Actual HIP regimes used in the test procedure are presented in the Table 1
and the diagrams of the interrupted HIP cycles- below.
 Table 1.Experimental HIP Cycles

HIP Cycles Temperature HIP Pressure Soak Capsule Average

,°C ,°F Max, Psi Max, Mpa time # density, %
#1186 R1 727 1340 11565 79.7 0 A1 74.62
A2
#1186 R2 827 1520 12665 87.3 0 B1 76.54
B2
#1186 R3 882 1620 13280 91.6 0 C1 81.43
C2
#1186 R4 954 1750 14072 97.0 0 D1 93.38
D2
#1186 R5 999 1830 14567 100.4 0 E1 96.96
E2
#KH 1121 2050 15000 103.4 3-4 Hours KH1 100
KH2
KH3

Figure 2. Interrupted 1340F HIP cycle

Figure 3. Interrupted 1520F HIP cycle
Figure 4. Interrupted 1620F HIP cycle

Figure 5. Interrupted 1750F HIP cycle

 Figure 6. Interrupted 1830F HIP cycle

After HIP the cans were removed from the samples by machining or acid
leaching (the latter- for the brittle porous samples). Figure 7 shows the view of
the samples prepared for high temperature compression tests.

Figure 7. Porous and full dense samples for high temperature compression tests

The geometrical and physical description of porous samples and their initial
characteristics is presented in the Table 2.
Porous and full dense samples were then subjected to hot compression
tests at the creep strain rates at the same temperatures, when the corresponding
HIP cycles were interrupted so, that real yield properties of porous material in
the densification point were measured.
High temperature compression test were done at the Metals Technology
Inc using the 30,000lb testing machine equipped with a load cell and a furnace
(Figures 8, 9). Upsetting strain rate was kept at the level of 10-3/sec
corresponding to the actual strain rate during HIP. Figure 10 presents the view
of the porous sample (with a thermo-couple attached) after the compression
test.
 TH results of the tests were recorded electronically as well as on the paper
diagrams (Figure 11) enabling to interpret the deformation pattern and to extract
the values needed for calculation of the rheology functions f 1 and f 2 .

Figure 8. 30,000 lb compression testing machine with a furnace.

Figure 9. Electric furnace used for hot compression tests
Table 2 Porous test samples size and density

# HIP Temp # # Diam Height Volume Mass Dens Relative

Cycle ,°F Capsule Sample ,mm ,mm ,mm3 ,g g/sm3 Dens%
#1186R1 1340F A1,A2 1 29,04 47,00 31,13 195,80 6,29 75,06
726,7C 2 29,08 46,72 31,03 192,20 6,19 73,91
3 29,22 48,08 32,24 201,90 6,26 74,73
4 29,14 47,68 31,79 198,800 6,25 74,63
5 29,19 47,97 32,10 201,400 6,27 74,87
6 29,13 46,26 30,82 192,500 6,25 74,52
Average: 74,62
#1186R2 1520F B1,B2 1 28,69 47,50 30,71 196,20 6,39 76,23
826,7C 2 28,58 47,10 30,21 195,80 6,48 77,34
3 22,70 30,84 12,48 80,40 6,44 76,87
4 22,10 29,94 11,48 73,20 6,37 76,06
5 22,67 27,64 11,16 71,50 6,41 76,48
6 28,61 43,70 28,09 179,50 6,39 76,26
Average: 76,54
#1186R3 1620F C1,C2 1 19,60 25,00 7,54 52,20 6,92 82,58
882,2C 2 19,50 24,05 7,18 48,80 6,79 81,08
3 19,64 28,31 8,58 58,20 6,79 80,98
4 19,72 26,53 8,10 54,800 6,76 80,70
5 28,09 46,05 28,53 194,00 6,80 81,14
6 27,90 46,61 28,49 196,000 6,88 82,10
Average: 81,43
#1186R4 1750F D1,D2 1 16,67 28,70 6,26 48,80 7,79 92,97
954,2C 2 16,59 27,94 6,04 47,00 7,78 92,86
3 16,49 28,48 6,08 47,90 7,88 93,98
4 16,60 26,44 5,72 44,80 7,83 93,43
5 25,42 42,79 21,71 170,20 7,84 93,56
6 25,85 43,87 23,02 180,40 7,84 93,50
Average: 93,38
#1186R5 1830F E1,E2 1 16,51 28,70 6,14 49,70 8,09 96,53
998,9C 2 16,51 29,84 6,39 51,70 8,09 96,57
3 16,17 27,45 5,64 45,80 8,12 96,95
4 16,61 28,08 6,08 49,50 8,14 97,08
5 25,44 43,17 21,93 178,70 8,15 97,22
6 25,42 43,81 22,23 181,50 8,16 97,41
Average: 96,96
Table 2 (continued) Dense test samples size
and density, (100%, Dense samples)

# HIP Temp # Capsule # Sample Diam Height Volume Mass Dens Tap
Cycle ,°F ,mm ,mm ,mm3 ,g g/sm3 Dens%
#KH 2050F 1 AA 14,57 20,48 3,41 28,60 8,38 99,95
1121C AB 14,56 20,39 3,39 28,40 8,37 99,83
BA 14,82 21,17 3,65 30,60 8,38 99,99
BB 15,00 21,83 3,86 32,40 8,40 100,22
2 CA 14,89 24,00 4,18 35,100 8,40 100,22
CB 14,99 23,66 4,18 35,000 8,38 100,03
DA 14,96 22,63 3,98 33,400 8,40 100,20
DB 14,98 23,64 4,17 34,900 8,38 99,96
3 EA 14,96 24,79 4,36 34,500 7,92 94,48
EB 14,95 22,77 4,00 33,500 8,38 100,02
Y(extra) 14,94 24,34 4,27 35,800 8,39 100,12
Average: 8,39 100%

Figure 10. Porous sample B6 after compression test

Figure 11. Test diagram for the porous sample B6
 Table 3 presents the results of upsetting of the full dense Ni-base alloy at
the temperatures of the corresponding HIP cycles and the measured values of the
yield strength and Figure 12 illustrates the function of the yield strength versus
temperature.
Table 3. Yield strenght of the full dense Ni
base alloy

T Sample P0.2 * P0.2 * Diam Area 0.2 **

°F/°C # ,Lb ,H ,mm mm2 ,Mpa
1340/726,7 AA 27250 121214,05 14,57 166,73 727,02
AB 21000 93412,66 12,52 123,11 758,76
1520/826,7 BA 20250 90076,50 14,82 172,50 522,19
BB 18000 80068,00 15,00 176,71 453,09
1620/882,2 CA 7750 34473,72 14,89 174,13 197,97
CB 8750 38921,94 14,99 176,48 220,55
1750/954,2 DA 4000 17792,89 14,96 175,77 101,23
DB 4600 20461,82 14,98 176,24 116,10
1830/998,9 EA 2600 11565,38 14,96 175,77 65,80
EB 2700 12010,20 14,95 175,54 68,42
* conventional yield load (uniaxial upset tests)
** conventional yield strength

Figure 12. Yield strength of full dense ….Ni base alloy versus temperature
 Table 4 presents the results of high temperature compression tests of
porous Ni base alloy samples carried out at the temperatures of corresponding
HIP cycles and the measured values of the conventional yield strength.
Figures 13 shows the value of the yield strength for porous samples as a
function of temperature.
Table 4. Yield strength of porous samples

T Sample P0.2 * P0.2 * Diam Area 0.2 **

°F/°C # ,Lb ,H ,mm mm2 ,Mpa
1340/726,7 A1 19045 84716,39 29,04 662,34 127,90
A2 18710 83226,23 29,08 664,17 125,31
A3 13710 60985,12 29,22 670,58 90,94
A6 17840 79356,28 29,13 666,32 119,10
1520/826,7 B1 26250 116765,83 28,69 646,56 180,59
B3 19750 87852,38 22,70 404,71 217,08
B4 20250 90076,50 22,10 383,60 234,82
B5 20750 92300,61 22,67 403,64 228,67
1620/882,2 C1 11500 51154,55 19,60 301,72 169,54
C2 10750 47818,39 19,50 298,65 160,12
C3 10000 44482,22 19,64 302,95 146,83
C6 24500 108981,44 27,90 611,23 178,30
1750/954,2 D1 4250 18904,94 16,67 218,25 86,62
D2 4200 18682,53 16,59 216,16 86,43
D3 5400 24020,40 16,49 213,57 112,47
1830/998,9 E1 3200 14234,31 16,51 214,08 66,49
E2 3100 13789,49 16,51 214,08 64,41
E3 3000 13344,67 16,17 205,36 64,98
* conventional yield load (uniaxial upset tests)
** conventional yield strength
 Figure 13. Yield strength versus temperature for the porous Ni base alloy
samples obtained in the interrupted HIP cycles.

The interpretation of the data from the Tables 1,2,3, and 4 and charts presented
on the Figures 12 and 13 allows to derived the f 1 and f 2 functions

3. Determination of f 1 and f 2 functions

Determination of f 1 and f 2 functions was done in accordance with

Green's plasticity criterion:
 
2 2

2 + 0
2 = 
2 (2)
f f
s

1 2

,where  =  3 - intensity of tangential stress;

3
 1
 0
=
33
- average stress;

 3
- compression stress.

s - yield strength of the monolithic material at HIP temperature;

Basing on these equations and the results of the HIP tests and compression tests
the values of f 1 and f 2 functions can be derived.
The results of the analysis are presented in the Table 5.

Table 5 . f 1 and f 2 functions

HIP HIP
Temperature Density Pressure Yield strength, Mpa f1 f2
,°F ,% ,Mpa Dense Porous
1340 74,62 80,0 742,89 115,81 0,178 0,187
1520 76,54 87,8 487,64 199,92 0,630 0,312
1620 81,43 91,6 209,26 163,70 0,974 0,758
1750 93,38 97,4 108,66 95,17 0,926 1,553
1830 96,96 100,8 67,11 65,29 0,996 2,602
2050 100,00 1

Figure 14 and 15 illustrate the values of f 1 and f 2 functions versus

temperature and density correspondingly.
The values of f 1 and f 2 were embedded into the HIP modeling software
in the form of the Data Base.
 F1,F2 functions versus temperature

3,0

2,5 F1
F2

2,0
F1,F2

1,5

1,0

0,5

0,0
1200 1300 1400 1500 1600 1700 1800 1900 2000 2100
Temperature, °F

Figure 14 The values of f 1 and f 2 functions versus temperature

 F1,F2 functions versus density

3,0

F1
2,5
F2

2,0
F1,F2

1,5

1,0

0,5

0,0
65 70 75 80 85 90 95 100
Density, %

Figure 15 The values of f 1 and f 2 functions versus density