Hybrid Helmet Cure Cycle Optimization 

by David M. Spagnuolo and Eugene Napadensky 

ARL-TR-4384 February 2008 

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Army Research Laboratory 

Aberdeen Proving Ground, MD 21005-5069 

ARL-TR-4384 February 2008 

Hybrid Helmet Cure Cycle Optimization 

David M. Spagnuolo and Eugene Napadensky 

Weapons and Materials Research Directorate, ARL 

Approved for public release; distribution is unlimited. 
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 Hybrid Helmet Cure Cycle Optimization 

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 DE25 

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6. AUTHOR(S) 

 David M. Spagnuolo and Eugene Napadensky (both of ARL) 

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 U.S. Army Research Laboratory 

 Weapons and Materials Research Directorate 

 Aberdeen Proving Ground, MD 21005-5069

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14. ABSTRACT 

 

Some of the recent work involving the use of thermoplastic materials for combat helmets has shown significant weight 

savings and improved protection. Unfortunately, the change to thermoplastic materials brings with it some important 

concerns. First, the stiffness is compromised with these materials so a hybrid type of helmet (a thermoplastic shell with 

thermoset inner or outer skins) is needed to reduce the deflection properties. This brings us to the second concern, 

processability. A typical combat helmet is made with a thermoset phenolic/polyvinylbutyral material, usually cured at 250°F 

with a 1-hour soaking time. Thermoplastics require higher temperatures for the fusion process to commence but require a 

much shorter soaking time. This work investigates potential cure cycles for a carbon fiber-epoxy prepreg1

, BT250-E, cured 

at higher temperatures, faster “ramp” rates, and shorter soaking times. A differential scanning calorimeter was used for 

measuring the degree of cure for the various cure cycles from which the most optimized cycle was selected, based on degree 

of cure and process time. 

1

pre-impregnated fibers; a reinforced plastics term for the reinforcing material that contains or is combined with the full complement of 

resin before the molding operation. 

15. SUBJECT TERMS

 BT250-E; cure cycle; degree of cure; DSC; epoxy

16. SECURITY CLASSIFICATION OF:

19a. NAME OF RESPONSIBLE PERSON

 David M. Spagnuolo

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Unclassified

b. ABSTRACT 

Unclassified

c. THIS PAGE 

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OF ABSTRACT 

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OF PAGES 

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 410-306-0770

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 Prescribed by ANSI Std. Z39.18
iii

Contents 

List of Figures iv

List of Tables iv

1. Introduction 1

2. Experimental 1

2.1 Theory ............................................................................................................................1 

2.2 Materials..........................................................................................................................2 

2.3 Equipment .......................................................................................................................3 

2.4 Experimental Procedure ..................................................................................................3 

2.4.1 Cure Cycles .........................................................................................................3 

2.4.2 Differential Scanning Calorimetry ......................................................................3 

3. Results and Discussion 4

3.1 Degree of Cure ................................................................................................................4 

3.2 Exotherm as an Indicator of Cure Level .........................................................................4 

3.3 Glass Transition Temperature as an Indicator of Cure Level .........................................7 

3.4 Apex Position as an Indicator of Cure Level ..................................................................8 

4. Conclusions 9

5. References 10 

Distribution List 11 
iv

List of Figures 

Figure 1. DSC scans of cured and uncured carbon fiber-epoxy prepreg....................................... 2 

Figure 2. Determining the degree of curing from the exothermic peak......................................... 4 

Figure 3. DSC scans for B-series of cure cycles (25 oC to 149 oC at 5 oC/min)............................ 6 

Figure 4. Degree of cure (for cycle B) as a function of holding time............................................ 6 

Figure 5. Examples of Tg shift related to cure levels..................................................................... 7 

Figure 6. The relationship between Tg and cure level as estimated by exothermic peak area....... 8 

Figure 7. Apex position as an indicator of cure level. ................................................................... 9 

List of Tables 

Table 1. List of evaluated cure cycles............................................................................................ 3 

Table 2. DSC results. ..................................................................................................................... 5 
1

1. Introduction 

In an effort to develop a lighter weight helmet that provides the same or better ballistic qualities 

as compared to currently fielded helmets, a new system composed of thermoplastic fabrics, 

molded with thermoset prepregs was designed at ARL. Proposed manufacturing of the helmet 

involved pressure molding a number of plies of aramid fabric with a thermoplastic film, and two 

plies of carbon fiber-epoxy prepreg, BT250-E (Bryte Technologies, Inc.) that would add 

structural strength. The manufacturer’s recommended cure cycle for BT250-E was to ramp 

(gradually increase) the part from 70 °F to 250 °F at rate of 2 to 5 °F per minute (while applying 

25 inches mercury vacuum minimum) and to hold for 1 hour; the part was then cooled to below 

160 °F, pressure was released, and the part removed (1). 

It was assessed that because of the slow ramp times and long holding time, mass production of 

these helmets will be impractical. Following the manufacturer’s recommended processing 

parameters for the carbon fiber-epoxy prepreg would result in a turn-over time of 78 to 96 minutes 

per helmet. In order to develop a shorter cure cycle, it was decided that a faster ramp time and a 

higher temperature should be investigated. Since the aramid-thermoplastic used in the helmet will 

have to be heated to 300 °F (149 °C) in order for the melting/solidification process to be complete, 

it was decided that a new cure cycle with a final temperature holding time at 300 °F should be 

designed for carbon fiber/epoxy prepreg. 

2. Experimental 

2.1 Theory 

The degree of cure for polymeric resins can be monitored by a number of different methods such 

as thermomechanical analysis (TMA), differential scanning calorimetry (DSC), rheology, etc. 

(2). In this case, it was monitored by DSC. As the instrument increases sample temperature at a 

controlled rate, the amount of energy required to raise the sample’s temperature changes when 

the material undergoes a physical (glass transition temperature [Tg], melting point, etc.) or 

chemical (any kind or reaction) changes. 

Evaluating these changes in an energy flow provides quantitative insight to what is happening to 

the sample. In this case, the exothermic peak (approximately 150 oC) related to the reaction of 

uncured resin was monitored (3). Since the peak area is proportional to the energy required for 

the reaction, it is related to the amount of uncured resin. Fully cured samples (with no unreacted 

resin) would have no peak at all, while “as received” prepreg would have the peak with the 

largest area (see figure 1). 
2

Glass transition temperature could also be monitored. Since Tg is related to the degree of cure 

(which is the same as the degree of cross-linking), the Tg of the resin will gradually shift to 

higher temperatures as the material is approaching the fully cured state. 

Attempting to monitor the degree of cure of prepregs is slightly more complicated as compared 

to a neat resin. Resin content in commercially available prepregs ranges from 30% to 45% by 

weight (4). Tg might be more difficult to observe since, for all intents and purposes, the sample 

size is dramatically decreased by the presence of fiber; thus, the signal intensity for the glass 

transition may be too low to monitor. On the other hand, the size of the exothermic peak (heat 

released during cure) is directly proportional to the amount of uncured resin, and since there is 

always some variation in prepreg resin-to-fiber ratios (resin-rich and resin-poor areas), it is 

expected that there will be some scatter in uncured and partially cured samples. These resin 

variations have minimal effect on the final properties of a manufactured part, but with DSC, this 

could be a major factor because of the small sample size (approximately 10 mg). 

-0.5

-0.3

-0.1

0.1

0.3

0.5

25 50 75 100 125 150 175 200 225 250

Temp (C)

Heat flow (W/g)

uncured 

cured

Figure 1. DSC scans of cured and uncured carbon fiber-epoxy prepreg. 

2.2 Materials 

Material chosen for this particular study was IM7-12K/BT250E-1, a Bryte Technology, Inc., 

prepreg. This prepreg, or unidirectional tape, was composed of IM7-12K graphite reinforcement 

with an epoxy resin, 37.8% resin content. The 12K represents the number of filaments per tow 

(untwisted bundle of filaments). The material was stored in a freezer at or below the manufacturer’s recommended storage temperature of 0 oF. The manufacturer-recommended cure cycle is 

2o to 5 oF temperature ramp to 250 oF, and 1 hour holding time. 
3

2.3 Equipment 

Equipment used in these experiments consisted of a 2920 DSC (TA Instruments), and an HP5890 

gas chromatograph (GC) oven (Hewlett Packard), chosen for its accurate temperature and rate 

controls to cure and partially cure prepreg samples. An analytical balance (precision- ±0.0001 g) 

was used to weigh the samples for the DSC. 

2.4 Experimental Procedure 

2.4.1 Cure Cycles 

The carbon fiber-epoxy prepreg samples (approximately 2x5 cm) were clamped in a small metal 

holder and cured inside the HP5890 GC oven. Three cure cycles (A, B, and C) were chosen for 

this experiment (see table 1) in addition to the “standard” cure cycle recommended by the 

manufacturer. In addition to variations in the holding temperature, holding time was also varied 

in order to optimize minimal time required for a complete cure. Immediately upon cooling, 

cured and partially cured samples were analyzed with the DSC. Unused portions of samples 

were retained in a freezer for repeated analysis. 

Table 1. List of evaluated cure cycles. 

Cure Cycle 

Initial 

Temperature 

(°C) 

Ramp Rate 

(°C/min) 

Final 

Temperature 

(°C) 

Holding 

Time (min) 

Cooling 

(min) 

Run Time 

(min) 

Standarda 25 3 121 60 3 95 

A-5 25 5 121 5 3 27 

A-15 25 5 121 15 3 37 

A-30 25 5 121 30 3 52 

B-0 25 5 149 0 3 28 

B-2.5 25 5 149 2.5 3 30 

B-5 25 5 149 5 3 33 

B-10 25 5 149 10 3 38 

C-5 25 10 149 5 3 20 a

Cure cycle recommended by manufacturer and converted to degrees Celsius

2.4.2 Differential Scanning Calorimetry 

DSC was performed on a 2920 DSC (TA Instruments). Samples were weighed (approximately 

10 mg each), placed into hermetically sealed aluminum pans, and run under a nitrogen purge. 

The DSC run conditions were to stabilize the temperature at 20 oC and then ramp at 10 oC/min to 

250 oC. Reference for the analysis was an empty aluminum pan of the same type as the ones used 

for the actual samples. 
4

3. Results and Discussion 

3.1 Degree of Cure 

The degree of cure was estimated from the area under the exothermic peak, normalized to the 

sample weight (5). An assumption had to be made that all samples have identical resin-to-fiber 

ratios. The degree of cure that resulted from various experimental cure cycles was estimated from 

the size of the exothermic peak relative to the “uncured” prepreg samples. Uncured samples were 

designated as 0% cured, and fully cured samples (showing no peak at all) as 100% cured. Technically, this is not correct, since prepreg by definition is already partially cured, but since prepreg 

is the starting point for these experiments, it is convenient to refer to that level of cure as 0%. The 

exothermic peaks in the DSC scans (at 150 oC) are getting smaller and smaller (see figure 2) as 

more and more of the available functional groups in the resin react with each other during the cure 

cycle, indicating an approach to a fully cured material. 

-0.3

-0.1

0.1

0.3

0.5

0.7

0.9

1.1

1.3

50 75 100 125 150 175 200 225 250

T ( oC)

W/g

0% Cured 

24% Cured (A-5)

76% Cured (A-15)

100% Cured (A-30)

100% Cured (Standard)

Figure 2. Determining the degree of curing from the exothermic peak. 

3.2 Exotherm as an Indicator of Cure Level 

The extent of cure/cross-linking reaction was estimated from the size of the exothermic peak, 

located in the vicinity of 150 oC on the DSC scans, using the following relationship: 
5

Hp

Hp Hs Cure

Δ

Δ − Δ % = 100 ∗

Where ΔHp is the partial heat of reaction for the original prepreg (128.25 joules per gram) and 

ΔHs is the partial heat of reaction for the specific partially cured sample being examined. In all 

cases, ΔH equals the area under the exothermic peak curve obtained by DSC and is measured in 

joules per gram. 

Pure resin was not available for these experiments, and fiber-to-resin ratios can fluctuate, 

depending on location, when such small samples are used (resin-rich and resin-poor areas). It is 

believed that these variations in resin content are responsible for the significant scatter in the 

joules-per-gram values (peak area) in the partially cured samples and this is especially true in the 

“uncured” samples. DSC results from different cure cycles are shown in table 2. The table also 

shows the area of the exothermic peak, the cure percentage based on the exothermic peak area, 

and the glass transition temperatures. 

Table 2. DSC results. 

Cure Cycle 

Weight 

(mg) 

Cure 

Temperature 

(°C) 

Ramp 

(°C/min)) 

Holding Time 

(min) 

Peak 

Area (J/g) 

Percent 

Cure 

Cure Cycle 

Time (min) 

Tg (°C) 

Uncured 7.2 NA NA NA 106 17.3 

Uncured 8.1 NA NA NA 144 -12.3 

Uncured 7.3 NA NA NA 111 13.5 

Uncured 10.9 NA NA NA 152 -18.5 

AV Uncured 128.25 0.0 

Standard 10.2 121 3 60 0 100.0 92 123 

A-5 13.6 121 5 5 97.5 24.0 24.2 35 

A-15 9.3 121 5 15 30.8 76.0 34.2 33 

A-30 9.9 121 5 30 0 100.0 49.2 121 

B-0 9.8 149 5 0 18.2 85.8 24.8 62 

B-0 11.5 149 5 0 19.2 85.0 24.8 65 

B-2.5 11.1 149 5 2.5 5.3 95.9 27.3 

B-5 10.6 149 5 5 0 100.0 29.8 127 

B-5 9.5 149 5 5 0.7 99.5 29.8 126 

B-10 10.6 149 5 10 0 100.0 34.8 127 

C-5 10.4 149 10 5 1.6 98.8 17.4 

The B series of cure cycles differs only in holding time at the final temperature. Figure 3 shows 

decreasing exothermic peaks as the holding time is increased from 0 to 10 minutes. The second 

peak (located at 220 oC) is believed to be related to the thermal decomposition of the polymer 

and is not considered as an indicator of the curing process. 

The data can also be represented to show the degree of cure as a function of holding time (see 

figure 4). 
6

-0.28

-0.26

-0.23

-0.21

-0.18

-0.16

-0.13

-0.11

-0.08

-0.06

-0.03

50 75 100 125 150 175 200 225 250

T ( oC)

Heat flow (W/g) 

85% Cure (B-0)

96% Cure (B-2.5)

100% Cure (B-5)

100% Cure (B-10)

Figure 3. DSC scans for B-series of cure cycles (25 oC to 149 oC at 5 oC/min). 

80

85

90

95

100

105

0 1 2 3 4 5 6 7 8 9 10 11

Holding Time (min) at 149C (300F)

Degree of cure (%)

Figure 4. Degree of cure (for cycle B) as a function of holding time. 

From this figure, it is clear that 99% of the curing process for cure cycle “B” is completed within 

the first 5 minutes. Of course, this pertains only to the experimental final temperature and 

heating rate (149 oC and 5 oC/min). Although it would be possible to make the claim that a 6- or 

7-minute holding time would be sufficient, unforeseen considerations in the manufacturing 

process could require slightly longer holding times. For instance, a thicker sample will require a 

longer time to reach the desired temperature. Thus, it would be wise to add a few minutes as a 

built-in safety factor. As it is, a 10-minute holding time will result in only a 38-minute run: 15 

minutes to ramp the temperature, a 10-minute holding time, and 3 minutes for cooling, unloading 

the finished part, and loading in a new pre-form (see table 1). That is a significant improvement 

from the original cure cycle of 95 minutes. Using this cure cycle will accelerate helmet 
7

production capacity by 250%, resulting in significant financial savings and an increased supply 

of essential, protective equipment for the U.S. military. 

These results can be further improved, provided that industrial manufacturing equipment can 

produce a controlled heating rate of 10 oC per minute (50 oF). The full scale of experiments using 

10 oC/min was not performed at this time, but with the use of the C-5 cure cycle (see table 2) as an 

initial indicator, required holding time can be estimated. A 5-minute holding time used for the 

C-5 cure cycle resulted in 98.8% cured resin. Assuming that the cure rate is similar to the B cycle 

shown in figure 4, it can be claimed that a cure cycle of 25 oC to 149 oC at 10 oC/min, with a 10-

minute holding time will result in a fully cured prepreg. 

Final run time for this variation would be 25 minutes, as compared to 38 minutes at 5 oC per 

minute ramp. With this cycle, the increase in production capacity would be 380%. However, 

industrial equipment of this type is more expensive and not readily available. 

3.3 Glass Transition Temperature as an Indicator of Cure Level 

Expected shift in the glass transition temperature (table 2) with increasing degree of cure to a 

higher temperature is well documented, even though different authors propose different equations 

describing the relationship between glass transition temperature and degree of cure (6, 7, 8). This 

technique sounded like a very promising path to verify a complete cure, but it did not give 

sufficiently reliable results in these experiments. Most likely, it is because of the combination of 

small amounts of actual resin in the sample and insufficient instrumental sensitivity. As a result, 

the Tg’s performed in the DSC scans were difficult to positively identify from the baseline noise, 

and in some runs, it was not possible at all. Figure 5 shows two of the stronger Tg’s, and one can 

see that even in these cases, exact value and or even the presence of a Tg can be argued for or 

against. 

0

0

50 60 70 80 90 100 110 120 130 140 150

T ( oC)

W/g

0

0

85% Cure (B-0)

100% Cure (B-10)

Tg

Tg

Figure 5. Examples of Tg shift related to cure levels. 
8

Even though they were not strong enough to be useful, the pattern observed follows welldocumented logarithmic relationships between the degree of cure (determined by area under the 

exothermic peak) and the glass transition temperature (see figure 6). The trend line shows a 

respectful (0.986) R2

 value1, and that indicates that given better instrumental sensitivity, it would 

be possible to better monitor the degree of cure via this technique. 

60

70

80

90

100

110

10 100 1000

Tg (log scale)

Degree of Cure (%)

 

y = 18.818Ln(x) + 8.7678

R2

 = 0.9857

60

70

80

90

100

110

20 30 40 50 60 70 80 90 100 110 120 130

Tg

Degree of Cure (%)

Figure 6. The relationship between Tg and cure level as estimated by exothermic peak area. 

3.4 Apex Position as an Indicator of Cure Level 

It was also noticed that the apex of the exothermic peak itself shifts positions, and this position 

may give some indication to the degree of cure (see figure 7). Here, the degree of cure is calculated from the area under the peak. Overall, the shift from 0% to 100% of cure is not very large 

(approximately 20 oC), but it does look like a real trend. Scatter of the Tg data points for uncured 

samples is very low (153 to 154.7 oC). This indicates that the position of the peak is independent 

of the quantity of unreacted resin—the issue that was the cause of large scatter in the data based 

on the peak area. However, as the cure rate progresses above 90%, scatter becomes a problem. 

This is mostly because of difficulties encountered with locating the apex on a peak that is rapidly 

disappearing as the degree of cure approaches 100%. Thus, this method favors accuracy in 

partially cured samples but becomes less useful as a tool to determine cure levels in highly cured 

samples. It still may be a very useful technique for determining the shelf life of prepreg or 

evaluating its condition after long periods of storage. 

 1R2

 value means the square of the correlation coefficient.
9

y = -6.4221x + 988.34

R2

 = 0.8718

-20

-10

0

10

20

30

40

50

60

70

80

90

100

110

120 125 130 135 140 145 150 155 160

Position of endotherm peak (oC)

% Cur

e

Peak Peak 

Area % Cure Apex

Cure cycle (J/g) ( C )

Uncured 106 17.3 154

Uncured 144 -12.3 154.7

Uncured 111 13.5 153.5

Uncured 152 -18.5 153

A-5 97.5 24.0 147.2

A-15 30.8 76.0 140.6

B-0 18.2 85.8 141.7

B-0 19.2 85.0 141.3

B-2.5 5.3 95.9 136

B-5 0.7 99.5 140.4

C-5 1.6 98.8 142.5

Figure 7. Apex position as an indicator of cure level. 

4. Conclusions 

Performed experiments show that it is possible to significantly shorten the cure cycle of IM7 

carbon fiber prepreg by increasing the cure temperature to 149 oC (300 oF) and boosting the 

heating rate. Depending on the capability of the heating press that will be used, manufacturing 

cycle times can be cut by 60% to 75%. This can be achieved if we increase the ramp rate to 5 to 

10 oC/min (9 to 18 oF/min) and shorten the holding time at the final temperature to 10 minutes. 

These numbers have about a 5-minute safety factor built in, since experiments with only 

5-minute holding times showed that the cure is 99% complete. Time required to produce each 

unit using this cure cycle would be 22 to 35 minutes as compared to 92 minutes with the 

manufacturer’s recommended cure cycle (5 oF/min temperature ramp to 250 oF and 1 hour hold). 

It is estimated that an additional 3 minutes would be required to cool the press, remove the 

finished product, and load the new pre-form. This would increase the production times to 25, 38, 

and 95 minutes, respectively. The overall potential benefit of this cure cycle (temperature ramp 

to 149 oC and 10 minutes holding time) would increase the production rate by 280% to 150%, 

depending on the maximum controlled temperature ramp capabilities of the press (5 oC or 10 oC), 

resulting in significant savings and flexibility of supply of essential military equipment. 
10

5. References 

1. Web site: http://www.brytetech.com/products_view.aspx?productid=7, May 2004. 

2. ASM International. Engineered Materials Handbook, Engineering Plastics, Volume 2, 

Materials Park, OH, 1988. 

3. Stevens, M.P. Polymer Chemistry, 3rd edition, Oxford University Press, 1999. 

4. Mallick, P. K. Fiber-Reinforced Composites Materials, Manufacturing, and Design, Second 

Edition, Marcel Dekker, Inc.: New York, 1993. 

5. Sun, L.; Pang, S.; Sterling, A.; Negulescu, I.; Stubblefield, M. Journal of Applied Polymer 

Science. 2002, 83, 1074-1083. 

6. Riccardi, C. C.; Adabbo,H. E.; Williams, R. J. J. Journal of Applied Scence. 1984, 29, 2481. 

7. Aronhime, M. T.; Gillham, J. K. Journal of Coatings Technology 1984, 56, 35. 

8. Hale, A.; Macosko, C. W.; Bair, H. E. Macromolecules 1991, 24, 2610. 
11

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