Effect of curing conditions on mechanical properties of benzoxazine resin-based unidirectional strip materials

doi:10.21203/rs.3.rs-3607756/v1

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Effect of curing conditions on mechanical properties of benzoxazine resin-based unidirectional strip materials

https://doi.org/10.21203/rs.3.rs-3607756/v1

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Because of the characteristics of high temperature resistance, high thermal stability, no component overflow after curing, Benzoxazine resin-based composite is widely used in the high temperature working area such as the rear section of the domestic C919 large passenger aircraft involved in the development process. In this paper, the influence of curing process conditions such as curing temperature, curing pressure and holding time on the mechanical properties of benzoxazine resin-based composites was evaluated by using the autoclave curing process, in order to select the optimal curing process conditions, and the hygrothermal aging property of the material at 71℃ was also evaluated. The results show that the curing temperature has little effect on the compressive strength and shear strength. With the decrease of curing pressure, the compressive and shear properties of the materials decreased slightly. With the increase of holding time, the compression strength increases slightly, the compression modulus decreases slightly, and the shear strength changes little. Under the condition of 71℃, the reduction of interlaminar shear strength is less than 10%, so the material has excellent performance in the aspect of resistance to damp and anti-aging property.

chemical process conditions

benzoxazine resin-matrix composites

mechanical properties

anti-aging property

In the field of civil aviation, the proportion of composite materials for fuselage structure is becoming increasingly important, among which resin matrix composite is greatly known for its light weight, high specific strength, high specific modulus, designability and some other characteristics. In this way, resin matrix composite can take place of metal material and is widely used in civil aviation. However, composite material is still in the beginning stage when it comes to domestic aircraft. In the domestic aircraft ARJ21, the use of composite material is account for less than 3% compared with the total weight of the ARJ21 aircraft, while in the domestic C919 large passenger aircraft, the composite material comes in about 15%. As is shown in the Picture 1, in the manufacturing process of the domestic C919 large passenger aircraft’s rear fuselage parts, the composite material around the auxiliary power unit (APU) is highly required to be stable under high temperature and damp & heat aging due to the need of installing auxiliary power unit (APU), gas emission system at high temperature and pressure, and liquid emission system under high temperature. That is the reason why the benzoxazine resin-matrix composite comes into being. Benzoxazine resin-matrix composite behaves well in high temperature resistance, high thermal stability, no component after curing and high DMA-Tg value and so on. As a result, benzoxazine resin-matrix composite is increasingly used in high-temperature structural region in aerospace components.

We are now aiming at the Benzoxazine resin-matrix which is designed for the domestic C919 large passenger aircraft’s rear fuselage parts. In order to explore an optimal curing process condition for composite parts, we study the effects of different curing temperatures, curing pressures and holding time on the mechanical properties of the composite materials and the effects of different curing conditions on the internal porosity of the composite parts at the same time.

In this paper, we compare the changes in the shear strength of benzoxazine resin-matrix composites under the same curing conditions, one is under dry conditions at room temperature and the other is at the temperature of 71°C under damp heat aging conditions, and we also study the resistance of benzoxazine resin-matrix composites in damp heat aging.

1.1 The Raw Material of Benzoxazine Resin-matrix Composites

In this experiment, we conducted the curing process with the use of autoclave. The raw materials we used were Henkel's Loctite BZ 9704/UD SM 130/35 unidirectional tape prepreg (Loctite unidirectional tape for short), and the adhesive film was Henkel's Loctite BZ 9691 grade.

1.2 Preparation

In order to verify the effects of different curing temperatures, curing pressures and holding time on the mechanical properties of the material. We utilized the autoclave curing process, the form of vacuum bag molding together with pressure curing, and selected the curing parameters shown in Table 1-Table 3, and completed the preparation and curing of three batches of Loctite unidirectional belt mechanical test plates under respective curing conditions.

Table 1

Different curing temperature conditions process parameters
Number	Curing Temperature/℃	Autoclave inner pressure/MPa	Warming rate/(℃/min)	Holding time/ min	Cooling rate (℃/min)
1	185	0.6	1–3	180	0–3
2	179	0.6	1–3	180	0–3
3	191	0.6	1–3	180	0–3

Table 2

Process parameters under different curing pressure conditions
Number	Curing temperature/℃	Autoclave inner pressure/MPa	Warming rate /(℃/min)	Holding time / min	Cooling rate/ (℃/min)
1	185	0.6	1–3	180	0–3
2	185	0.5	1–3	180	0–3

Table 3

Process parameters under different holding time conditions
Number	Curing temperature/℃	Autoclave inner pressure /MPa	Warming rate/(℃/min)	Holding time/ min	Cooling rate(℃/min)
1	185	0.6	1–3	180	0–3
2	185	0.6	1–3	240	0–3
3	185	0.6	1–3	480	0–3

1.3 Experimental Approaches

In order to verify the internal quality and mechanical properties of Loctite unidirectional mechanical test plates cured under different process conditions, the USL ultrasonic C-scanning equipment was used to detect the internal quality of the test plates, and LEICA DMI5000M metallographic optical microscope was used to detect the internal porosity of the Loctite unidirectional mechanical test plates, according to the GB3365 method, and the mechanical properties of the Loctite unidirectional mechanical test plates were tested according to the method shown in Table 4. We set the parameters as follows: the mechanical testing machine model was INSTRON 5565, the drop weight impact testing machine model was INSTRON 8803, and the impact energy was 30J.

The wet treatment conditions were as follows: immersion in water at the temperature of 71.0°C ± 5.0°C for 336 ± 6 hours before carrying out the tests.

Table 4

Test item details
Number	Tests	Size /mm	Plate layup	Number of samples/parts	Standard
1	Compressive strength and modulus	140×12	[45/0/-45/90]_2s	10	ASTM D6641
2	Shear strength(dry)	18×6	[0]₂₄	10	ASTM D2344
2	Shear strength(wet)	18×6	[0]₂₄	10	ASTM D2344
4	CAI	150×100	[+ 45/0/-45/90]_4s	10	ASTM D 7136/ ASTM D 7137

2.1 Non-destructive testing results of Loctite unidirectional belt force test plates

After ultrasonic C-scanning detection, the non-destructive testing of the test plate is qualified, and the C-scanning schematic diagram is shown in Fig. 2.

2.2Effect of curing temperature on the mechanical properties of Loctite unidirectional test plates

2.2.1 Compressive Strength Testing Results

In order to analyze the influence of different curing temperature conditions on the conventional compressive properties of Loctite unidirectional tape test plates, the compressive strength and compressive modulus properties of three batches of Loctite unidirectional tape materials were cured respectively at the temperature of 179°C, 185°C and 191°C, and the test results are shown in Table 5 and Table 6.

Table 5

Compression strength at different curing temperatures
Number	Curing temperature/℃	Compression strength /MPa
		Batch 1		Batch 2		Batch 3		Batch 1–3
		AVG	CV/%	AVG	CV/%	AVG	CV/%	AVG	CV/%
1	179	701	3.2	706	3.6	694	5.0	700	3.9
2	185	706	7.4	717	3.1	695	5.0	706	5.4
3	191	708	4.2	734	4.2	688	2.2	710	4.5

Table 6

Compression modulus at different curing temperatures
Number	Curing temperature/℃	Compression modulus /GPa
		Batch 1		Batch 2		Batch 3		Batch 1–3
		AVG	CV/%	AVG	CV/%	AVG	CV/%	AVG	CV/%
1	179	45.3	7.9	7.9	2.8	44.4	2.5	44.9	5.0
2	185	45.0	5.3	5.3	1.7	43.9	2.3	45.0	3.9
3	191	46.5	7.8	8.8	1.4	44.3	2.6	45.7	5.7

From the data above, it can be analyzed that there is no significant difference in the compressive strength and compressive modulus of Loctite unidirectional belt material under the conditions of 179°C, 185°C and 191°C at the curing temperature of the autoclave, that is, the change of curing temperature in this temperature range has little impact on the compressive properties of the material, and the compressive properties of the three batches of materials are basically unchanged, and the concentration of the test results is fair (CV value less than 8%).

2.2.2 Results of shear strength properties

In order to analyze the effects of different curing temperature conditions on three batches of Loctite unidirectional tape test plates, their shear strength were at different curing temperature, which were room temperature and low humidity, high temperature and humidity. They were separately cured at 179°C, 185°C and 191°C, and the testing results are shown in Table 7 and Table 8.

Table 7

Shear strength at different curing temperatures (room temperature and low humidity)
Number	Curing temperature/℃	Shear strength /MPa
		Batch1		Batch 2		Batch 3		Batch 1–3
		AVG	CV/%	AVG	CV/%	AVG	CV/%	AVG	CV/%
1	179	104.3	1.4	93.2	2.3	92.6	3.2	96.7	6.1
2	185	103.4	2.8	94.2	3.5	93.2	3.3	97.0	5.7
3	191	105.6	1.4	93.4	5.8	95.1	1.7	98.0	6.5

Table 8

Shear strength at different curing temperatures (high temperature and humidity)
Number	Curing temperature/℃	Shear strength/MPa
		Batch 1		Batch 2		Batch 3		Batch 1–3
		AVG	CV/%	AVG	CV/%	AVG	CV/%	AVG	CV/%
1	179	95.6	3.6	91.7	2.8	92.8	1.9	93.4	3.3
2	185	94.7	5.5	94.7	1.7	90.7	3.0	93.4	4.2
3	191	93.7	3.5	94.1	3.8	90.2	3.4	92.7	3.9

Through the data above, it can be analyzed that the mechanical testing plate made under the conditions of autoclave curing temperature of 179°C, 185°C and 191°C has no obvious difference in the interfacial shear strength of Loctite unidirectional belt material, that is, the curing temperature change has little effect on the interlaminar shear of the material in this temperature range, the shear performance of the three batches of materials is basically unchanged, and the concentration of the test results is fair (CV value is less than 8%).

By comparing the shear strength data of dry and wet testing plates at room temperature at the same degree of curing, it can be concluded that the shear strength of batch 1 is reduced by 9.3%, the high-temperature wet shear strength of batch 2 is reduced by 0.1%, and the high-temperature wet shear strength of batch 3 is reduced by 2.6%. The reason for this phenomenon is due to the extremely low water absorption of benzoxazine resins ^[21].

2.3 Effects of curing pressure on the mechanical properties of Loctite unidirectional tape materials

2.3.1 Compressive strength performance testing results

In order to analyze the influence of different curing pressure conditions on the conventional compressive properties of Loctite unidirectional belt test plates, we tested three batches of Loctite unidirectional belt materials which were cured under two different curing pressure conditions, one was under the condition of 0.6MPa and the other was 0.5MPa.We analyzed the compressive strength and compressive modulus properties, and the test results are shown in Table 9 and Table 10.

Table 9

Compressive strength under different curing pressure conditions
Number	Curing pressure/MPa	Compressive strength/MPa
		Batch 1		Batch 2		Batch 3		Batch 1–3
		AVG	CV/%	AVG	CV/%	AVG	CV/%	AVG	CV/%
1	0.6	706	7.4	717	3.1	695	5.0	706	5.4
2	0.5	671	4.8	708	3.3	674	3.9	684	4.6

Table 10

Compression modulus under different curing pressure conditions
Number	Curing pressure/MPa	Compressive modulus/GPa
		Batch 1		Batch 2		Batch 3		Batch 1–3
		AVG	CV/%	AVG	CV/%	AVG	CV/%	AVG	CV/%
1	0.6	45.0	5.3	46.0	1.7	43.9	2.3	45.0	3.9
2	0.5	44.3	1.9	46.1	2.4	43.9	2.8	44.8	3.2

Through the data above, it can be analyzed that under different curing pressure conditions, with the decrease of curing pressure, the compressive properties of Loctite unidirectional belt materials are slightly reduced, the compressive modulus of the three batches of material laminates basically remains unchanged, and the concentration of test results is fair (CV value is less than 8%).

2.3.2 Shear strength performance testing results

In order to analyze the effects of different curing pressure conditions on the performance of Loctite unidirectional belt testing plate in dry shear strength at room temperature and wet state at high temperature, we tested them separately, one was under dry shear strength at room temperature and the other was under wet shear strength at high temperature and wet state. They were all cured under the conditions of 0.6 MPa and 0.5 MPa in the autoclave, and the testing results are shown in Table 11 and Table 12.

Table 11

Shear strength under different curing pressures (room temperature and low humidity)
Number	Curing pressure/MPa	Shear strength/MPa
		Batch 1		Batch 2		Batch 3		Batch 1–3
		AVG	CV/%	AVG	CV/%	AVG	CV/%	AVG	CV/%
1	0.6	103.4	2.8	94.2	3.5	94.2	3.5	97.0	5.7
2	0.5	104.2	1.8	93.8	1.5	93.8	1.5	96.8	6.0

Table 12

Shear strength under different curing pressures (high temperature and wet condition)
Number	Curing pressure/MPa	Shear strength /MPa
		Batch 1		Batch 2		Batch 3		批次1–3
		AVG	CV/%	AVG	CV/%	AVG	CV/%	AVG	CV/%
1	0.6	94.7	5.5	94.7	1.7	90.7	3.0	93.4	4.2
2	0.5	93.2	3.8	92.0	6.9	93.1	1.0	92.8	4.4

Through the data above, it can be analyzed that there is no obvious difference in the interlaminar shear strength of Loctite unidirectional belt material, the mechanical testing plate of which were made under the conditions of 0.5MPa and 0.6MPa curing pressure of autoclave. That is, the change of curing pressure in this temperature range has little impact on the interlaminar shear of the material, and the shear performance of the three batches of materials is basically unchanged. The concentration of test results is fair(CV value is less than 8%).

By comparing the shear strength data of dry and wet at room temperature and the same curing pressure, it can be concluded that the shear strength of batch 1 is reduced by 9.5%, the high-temperature wet shear strength of batch 2 is reduced by 0.7%, and the high-temperature wet shear strength of batch 3 is reduced by 2.2%.

As a result, it can be found that benzoxazine resin matrix composites have excellent resistance to damp heat aging.

2.4 Effects of holding time on the mechanical properties of Loctite unidirectional bands

2.4.1 Compressive strength performance testing results

In order to analyze the influence of different holding time curing conditions on the conventional compressive properties of Loctite unidirectional belt testing plates, the compressive strength and compressive modulus properties of three batches of Loctite unidirectional belt materials were cured under the conditions of 180 min, 240 min and 480 min at autoclave pressure of 0.6Mpa, and the testing results are shown in Table 13 and Table 14.

Table 13

Compression strength under curing conditions with different holding time
Number	Holding time/min	Compressive strength/MPa
		Batch 1		Batch 2		Batch 3		Batch 1–3
		AVG	CV/%	AVG	CV/%	AVG	CV/%	AVG	CV/%
1	180	706	7.4	717	3.1	695	5.0	706	5.4
2	240	733	3.6	686	3.1	711	3.6	710	4.3
3	480	729	3.5	680	4.9	741	2.7	717	5.2

Table 14

Compression modulus under curing conditions with different holding time
Number	Holding time/min	Compressive modulus/GPa
		Batch 1		Batch 2		Batch 3		Batch 1–3
		AVG	CV/%	AVG	CV/%	AVG	CV/%	AVG	CV/%
1	180	45.0	5.3	46.0	1.7	43.9	2.3	45.0	3.9
2	240	43.9	1.5	43.2	2.3	43.6	2.8	43.6	2.3
3	480	43.3	4.9	43.2	1.6	44.8	3.2	43.8	3.8

From the above data, it can be analyzed that under the conditions of 180min, 240min and 480min, the compressive strength of the Loctite unidirectional belt test plate increases slightly (the added value is 3.68%), but its compressive modulus remains basically unchanged, mainly because with the extension of the curing time, the internal quality of the composite test plate tends to be stable, the residual stress decreases ^[22], and the interface properties between carbon fiber and resin are improved ^[23] .The concentration of test results was fair (CV values were all less than 8%).

2.4.2 Shear strength performance testing results

In order to analyze the effects of different holding time curing conditions on the performance of Loctite unidirectional belt testing plate in the dry state at room temperature and in the wet state at high temperature, we tested three batches of Loctite unidirectional belt materials with the pressure of 0.6MPa and cured under the holding time conditions of 180 min, 240 min and 480 min. The testing results are shown in Table 15 and Table 16.

Table 15

Shear strength under curing conditions with different holding time (room temperature and low humidity)
Number	Holding time/min	Shear strength/MPa
		Batch 1		Batch 2		Batch 3		Batch 1–3
		AVG	CV/%	AVG	CV/%	AVG	CV/%	AVG	CV/%
1	180	103.4	2.8	94.2	3.5	92.8	93.2	97.0	5.7
2	240	104.8	1.9	98.7	1.1	90.7	101.8	101.7	2.9
3	480	104.4	1.4	100.5	1.1	90.2	99.5	101.5	3.6

Table 16

Shear strength under different holding time curing conditions (high temperature and wet state)
Number	Holding time/min	Shear strength /MPa
		Batch 1		Batch 2		Batch 3		Batch 1–3
		AVG	CV/%	AVG	CV/%	AVG	CV/%	AVG	CV/%
1	180	94.7	5.5	94.7	1.7	90.7	3.0	93.4	4.2
2	240	98.5	2.3	94.9	2.2	96.9	0.5	96.7	2.4
3	480	95.6	2.1	93.2	2.7	95.7	1.6	94.8	2.4

Through the data above, it can be analyzed that there is no obvious difference in the interlaminar shear strength of Loctite unidirectional belt material, the mechanical testing plate of which were made under the conditions of 180min, 240min and 480min respectively, that is to say the change of curing and holding time have little impact on the interlaminar shear of the material during the holding time, the shear performance of the three batches of materials basically remains unchanged, and the concentration of testing results is fair(CV value is less than 8%).

By comparing the shear strength data of dry and wet state at room temperature for the same holding time, it can be concluded that the shear strength of batch 1 decreased by 7.6%, the high-temperature wet shear strength of batch 2 decreased by 0.4%, and the high-temperature wet shear strength of batch 3 did not decrease.

As a result, it can be found that benzoxazine resin matrix composites have excellent resistance to damp heat aging.

2.4.3 Compressive strength performance test results after impact

In order to analyze the effect of different holding time curing conditions on the compressive strength properties of Loctite unidirectional belt testing plates after impact, three batches of Loctite unidirectional belt materials were cured under the conditions of 180 min, 240 min and 480 min at a pressure of 0.6MPa, and the testing results are shown in Table 17.

Table 17

Compressive strength after impact under curing conditions with different holding time
Number	Holding time/min	Compressive strength after impact /MPa
		Batch 1		Batch 2		Batch 3		Batch 1–3
		AVG	CV/%	AVG	CV/%	AVG	CV/%	AVG	CV/%
1	180	233.6	2.9	246.4	4.7	235.5	3.7	238.5	4.4
2	240	240.9	3.2	235.4	6.3	240.7	3.1	238.9	4.4
3	480	238.4	4.0	259.4	7.2	240.6	3.4	246.1	6.4

Through the data above, it can be analyzed that there is no obvious difference in the compression performance of the laminate after impact under the conditions of 180min, 240min and 480min, and the compression performance after impact is slightly improved after holding time of 480min compared with the other two conditions. The main reason is that with the extension of curing time, the internal quality of the composite testing plate tends to be stable, the residual stress is reduced, the interface properties between carbon fiber and resin are improved, and the concentration of the testing results is fair (CV value is less than 8%).

2.4 Effects of different process conditions on the internal porosity content of Loctite unidirectional belt materials

In order to verify the effects of different curing temperatures, curing pressures and holding time on the internal porosity content of the material, this experiment used autoclave curing process to perform metallographic detection on three batches of Loctite unidirectional belt material testinng plates which were manufactured by different curing processes, the sample size was 10mm*20mm, and the porosity results of each batch of testing plates are shown in Table 18.

Table 18

Internal pore content under different curing conditions
Number	Curing temperature/℃	Internal pore content /%
		Batch 1		Batch 2		Batch 3		Batch 1–3
		AVG	CV/%	AVG	CV/%	AVG	CV/%	AVG	CV/%
1	179	0.006	1.6	0.001	3.5	0.002	1.5	0.003	2.2
2	185	0.003	1.4	0.003	1.4	0.005	1.2	0.004	1.3
3	191	0.007	1.6	0.007	1.1	0.01	2.5	0.008	2.1
	Curing pressure/MPa	AVG	CV/%	AVG	CV/%	AVG	CV/%	AVG	CV/%
4	0.6	0.003	1.4	0.003	1.4	0.005	1.2	0.004	1.3
5	0.5	0.001	3.2	0.026	0.8	0.006	1.4	0.011	1.6
	Holding time/min	AVG	CV/%	AVG	CV/%	AVG	CV/%	AVG	CV/%
6	180	0.003	0.003	1.4	4.7	0.005	1.2	0.004	1.3
7	240	0.008	0.005	1.5	6.3	0.003	2.6	0.005	2.1
8	480	0.008	0.009	1.2	7.2	0.004	1.1	0.007	1.3

From the data above, it can be analyzed that the internal porosity content of the composite testing plate is extremely low and there is no obvious difference in the above curing process parameter range, what indicates that the change within the above curing conditions has little effect on the internal porosity content of Loctite unidirectional belt material. Appropriately increasing the curing pressure, holding time and curing temperature is conducive to controlling the internal porosity content of the composite testing board.

(1)Under the conditions of 179°C, 185°C and 191°C, the compressive strength and modulus of Loctite unidirectional belt material change slightly, that is to say the curing temperature has little effect on the compressive properties of the material in this temperature range, the interlaminar shear strength of the dry and wet state of the material changes little, that is, the curing temperature has little effect on the in-plane shear of the material in this temperature range, and when the curing temperature is 179°C and 185°C, the porosity value of the laminate is the lowest. Take all the results above into account, it can be considered that 185°C is the most suitable curing temperature.

(2)Under the holding time conditions of 180 min, 240 min and 480 min, the compressive strength of Loctite unidirectional belt material increased slightly; the shear strength between dry and wet laminar changed very little, and the shear performance of laminate was slightly affected by extended curing time; the porosity of the laminate did not change significantly after extended curing time; the compressive performance of Loctite unidirectional belt material was slightly improved after 480 min of thermal insulation. Extended holding time has no obvious effect on the internal porosity of the composite testing plate, and 180min can be considered as a more suitable insulation time period based on the factors of molding efficiency and economy and so on.

(3)Under the conditions of 0.5MPa and 0.6MP, the change of curing pressure has little effect on the compressive properties of the composites, there is no obvious difference between the dry and wet shear properties of the materials, and the increase of curing pressure can reduce the porosity to a certain extent, so it can be considered that 0.6MPa is a more suitable curing pressure parameter.

(4)Under the same curing conditions, the difference between the dry shear strength and the high-temperature wet shear strength of Loctite unidirectional belt material is small, and the reduction of high-temperature wet shear strength is less than 10%, indicating that Loctite unidirectional belt material has excellent resistance to damp heat aging.

(5)Due to cost reasons, the effects of curing temperature and holding time on compression properties after impact were not evaluated in this test.

Author Contributions

Tian Yang: Investigation, Formal analysis, Writing-Original Draft. Sun Zhongwen: Conceptualization, Methodology, Translation, Writing-Review and Editing. Sun Jiehui: Conceptualization, Methodology, Review and Editing. Zhu Jinhai: Conceptualization, Methodology, Review and Editing , Formal analysis. Corresponding author Guo Yuan: Conceptualization, Methodology, Supervision, E-mail:[email protected].

Funding

This research was sponsored by Jiangsu Provincial Science and Technology Achievement Transformation Project. All funding resources are acknowledged.

Data Availability

The datasets generated during and/or analyzed during the current study are available from the corresponding author on reasonable request.

Consent for Publication

Submission of this article implies that the work described has not been published previously, that it is not under consideration for publication elsewhere.

Conflict of Interest

We declare no conflict of interest.

We don’t have any competing interests as defined by Springer, or other interests that might be perceived to influence the results or discussion reported in this paper.

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Effect of curing conditions on mechanical properties of benzoxazine resin-based unidirectional strip materials

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