Hoʻomākaukau a me ka loiloi hana o ke kiʻekiʻe wela ke kū'ē Prepreg Epoxy Resin

2023-02-02

1. Introduction


  As an important thermosetting resin, epoxy resin has good electrical properties, chemical stability, excellent mechanical properties and adhesive properties, and is widely used in many fields. In recent years, with the rapid growth of the consumption of epoxy resin in China, many new requirements have been put forward for the variety structure of epoxy resin. The demand for high-temperature resistant epoxy resin in some high-end products is increasing. Although some varieties of high-temperature resistant epoxy resin have been developed at home and abroad, and a certain output has been formed, it still cannot meet the current and future development needs. The main foreign manufacturers of this kind of special epoxy resin include Dow Chemical of the United States, Tokyo Chemical of Japan, Mitsubishi Gas Chemical, etc. Since its original purpose is mainly for military use, foreign countries have imposed a long-term technical blockade on the manufacturing technology of this kind of material and restricted its export. The output of products developed in China is limited and the price is expensive, which can not meet the current rapid growth demand of civil use [4]. In order to meet the domestic demand for high-temperature resistant epoxy resin, it is urgent to develop high-temperature resistant epoxy resin with suitable viscosity, good processing technology, good product storage stability and moderate cost.


  Ma keia pepa, multifunctional epoxy resin a epoxy resin E51 hoʻohui ʻia, a koho ʻia ka ʻōnaehana hoʻōla kūpono e hoʻomaikaʻi i ka pale wela o ka epoxy resin. I ka manawa like, hoʻoponopono ʻia ka viscosity a me nā waiwai piha o ka ʻōnaehana resin e ka ratio e hoʻokō i nā koi hana a hoʻololi i ka hana ʻana o ka prepreg wela wela. ʻO Prepeg kahi mea waiwai nui o ka hana ʻana FR4 pepa, 3240 pepa epoxy, pepa bakelite a me 3026 pepa pulupulu phenolic.


EPOXY RESIN E51


2. Hoʻokolohua


  a. Nā mea maka, nā mea hana a me nā mea hana


  I. Raw Materials: multifunctional epoxy resin (A), general epoxy resin E51 (B), kiʻekiʻe-mehana ho'ōla lāʻau (C), toughener (D), accelerator (E).


  II. Nā mea hana a me nā mea hana: ka mea hoʻomaʻamaʻa kikoʻī, KOREALABOTECH244 - 1544 gel time tester, TAAR2000 rheometer, TA50WS differential scanning calorimeter (DSC), INSTRON2382 universal material tester, gluing machine, prepreg machine.


  b. Hoʻomākaukau i ka laʻana hoʻāʻo


  I. Ka hoʻomākaukau ʻana i ka resin: wela a hoʻoheheʻe i ka resin epoxy a me ka mea hoʻopaʻapaʻa i kekahi ʻāpana, e hoʻoulu a hiki i ka hui ʻana ke ʻano like ʻole, maʻalili i lalo o 80 ℃, hoʻohui i ka mea hoʻōla a me ka accelerator, hoʻomaʻemaʻe a wehe i nā ʻōpū, a hui like.


  II. Ka hoʻomākaukau ʻana i ke kino hoʻolei resin: e ninini i ka ʻōnaehana resin i hoʻokuʻu ʻia i loko o ka mold preheated i ka wā wela, a hoʻopaʻa ʻia e like me kahi ʻōnaehana hoʻōla.


  III. Ka hoʻomākaukau ʻana i ke kiʻi ʻoniʻoni hoʻoheheʻe wela: e hoʻokomo i ka resin hehee i loko o ka pahu glue o ka applicator glue, e hoʻoneʻe i ka resin i ka pepa hoʻokuʻu e pili ana ma o ka roller, a laila hoʻomoʻa i ke kiʻi paʻa paʻa ma o ka mea hoʻoluʻu no ka uhi kiʻiʻoniʻoni.


  IV. ʻO ka hoʻomākaukau ʻana o ka carbon fiber prepreg: ʻo nā papa luna a me lalo i uhi ʻia o ke kiʻi resin a me ka fiber carbon i hui pū ʻia e kahi mīkini hana. ʻO nā papa ʻelua o ka resin film a me ka hoʻoikaika ʻana i ka fiber e hana i kahi ʻano "sandwich". Hoʻopiliʻia ka resin i loko o ka fiber ma o ka hoʻomehanaʻana i ka pā wela a me ka hoʻomehana a me ka hoʻokuʻuʻana o nā huila hoʻomehanaʻehā e hana i ka prepreg.


  V. Ka hoʻomākaukau ʻana i nā ʻāpana hoʻāʻo prepreg: ʻoki a uhi i ka prepreg e like me ka maʻamau hoʻāʻo, paʻa a hana ʻia e like me kekahi ʻōnaehana hoʻōla, a laila ʻoki ʻia i loko o nā ʻāpana hoʻāʻo maʻamau.


3. Nā hopena a me nā kūkākūkā


a. Ka hoʻomākaukau ʻana i ke ʻano resin


  Wahi a nā koi pale wela o ka resin, ua hoʻoholo ʻia ka mahana hoʻololi aniani TgDSC o ka ʻōnaehana resin e ≥ 190 ℃. I ka manawa like, pono ka resin no ka hana ʻana i nā prepregs wela wela. Pono ka resin i semi-paʻa i ka lumi wela, ʻaʻole pili i nā lima, ʻaʻole pili i ka pepa, a kūpono ka manawa gel resin. Wahi a ka ʻike hana, ua hoʻoholo ʻia ka wahi palupalu o ka resin he 35 ~ 45 ℃, a ʻo ka manawa gel ma 170 ℃ ua hoʻoholo ʻia he 20 ~ 30min.


  ʻO ka mea mua, ua hui pū ʻia ka multifunctional epoxy resin (A) a me ka toughener (D) i ka ratio o 100/10, a ua hoʻohui ʻia kekahi nui o ka mea hoʻōla wela kiʻekiʻe (C), me ka ʻole o ka hoʻohui ʻana i ka epoxy resin E51 (B) a. accelerator (E), a laila e noiʻi ʻia ka hana o ka ʻōnaehana resin. E like me ka nānā ʻana o ke kumu 1 #~4 # ma ka Papa 1, me ka piʻi mālie ʻana o ka nui o ka mea ho'ōla wela kiʻekiʻe (C), ke hōʻike nei ka Tg o ka ʻōnaehana resin i kahi ʻano piʻi, akā e emi mālie ka ikaika tensile; ʻO ka manawa gel, kahi palupalu a me Tg o ka formula 2 #~4 # hiki ke hoʻokō i nā koi.


Papa 1 Nā ʻāpana a me nā waiwai o nā resins like ʻole

haʻilula

Ka nui o ka nui

(A/B/C/D/E)

Wae hooluolu/℃

Ka manawa gel (170 ℃)/min

Tg DSC/℃

Ka ikaika uʻi/MPa

1

100/0/45/10/0

37.3

38

186

39

2

100/0/50/10/0

38.5

29

207

34

3

100/0/55/10/0

38.8

27

210

25

4

100/0/60/10/0

39.1

26

224

20

5

90/0/40/10/0.3

41.0

16

-

-

6

70/20/25/15/0.3

40.0

26

191

44

7

75/15/25/15/0.3

40.0

27

203

58


  I mea e hoʻoponopono ai i ka ikaika tensile o ka resin me ka ʻole o ka hōʻino ʻana i nā waiwai wela o ka resin, pono e hōʻemi i ka nui o ka mea hoʻōla wela kiʻekiʻe (C) a hoʻohui i kekahi hapa o ka accelerator (E). ʻO ka pili ʻana, ʻo ka nui o ka mea hoʻola i hoʻohui ʻia he nui a he liʻiliʻi ka nui o ka accelerator i hoʻohui ʻia. ʻO ka hui ʻole ʻana i ka hana maoli he maʻalahi ke kumu o ka pahū resin. No laila, pono e hoʻoponopono i ke kaʻina hui ʻana o ka resin. ʻO ka mua, e hoʻohana i ka epoxy resin E51 (B) maʻamau e wili i ka mea ho'ōla wela kiʻekiʻe (C) a me ka accelerator (E), a laila hoʻohui i ka hui ʻana i loko o ka resin ma hope o ka epoxy resin (A) a me ka paʻakikī (D). ) ua hui pū ʻia ma ke ʻano like.


  Hiki ke ʻike ʻia mai ka Formula 5 ma ka Papa 1, ʻoi aku ka pōkole o ka manawa gel ma mua o ka Formula 1 ke hoʻohui ʻia ka accelerator (E). Ke hiki aku ka resin i ka gel, e wikiwiki ana ka molecular network crosslinking, a e hoʻololi koke ka resin mai ke kūlana kahe viscous i ka moku aniani. Ma muli o ka hoʻohui ʻana o ka mea paʻakikī i loko o kēia resin, nui ka viscosity resin, ʻilihune ka wai resin, a paʻakikī ka ea e hoʻokuʻu. Inā wikiwiki loa ka manawa gel, a ʻaʻole i hoʻokuʻu ʻia ka resin bubbles, ua gel ka resin, kahi e hoʻopiʻi ai i nā hemahema e like me ka nāwaliwali o ka pilina ma waena o ka resin a me ka fiber, cavities, a me nā mea ʻē aʻe, ʻaʻole kūpono i ka hana ma hope o ka hana. ka huahana a me ka hoʻomaikaʻi ʻana i ka hana ʻana o nā mea hana. No laila, pono e hoʻemi ʻia ka nui o ka lāʻau lapaʻau. Papa 1 ʻOi aku ka kiʻekiʻe o ka ikaika tensile o ka formula 6 a me ka formula 7 ma mua o ka formula 4 ke hoʻohui ʻia ka ʻōnaehana hoʻōla wela (C) - accelerator (E) me ka epoxy resin E51 (B). Eia nō naʻe, ma muli o ka nui o ka epoxy resin E51 (B) ma ke ʻano 6, e pili ana i ka mahana hoʻololi aniani Tg o ka ʻōnaehana, ua koho hope ʻia ke kumu 7 ma ke ʻano he resin.


  b. Rheological waiwai o ka resin


  I mea e hoʻokō ai i nā koi o ke kaʻina hana hoʻoheheʻe wela prepreg, ua hoʻāʻo ʻia nā ʻano rheological o ka resin formula 7 i nā mahana like ʻole, a hōʻike ʻia nā hopena ma ka Papa 2. Hiki ke ʻike ʻia mai ka Papa 2 e hoʻololi ka viscosity resin me ka mahana. No laila, i ke kaʻina hana o ka hoʻomākaukau ʻana i ka resin film, hiki ke hoʻoponopono ʻia ka viscosity resin ma ke kāohi ʻana i ka mahana e hoʻokō i nā koi o ka hoʻomākaukau ʻana i ka resin film.


Papa 2 Resin viscosity ma na wela like ole

Ka wela/℃

Viscosity/Pa · s

60

312

70

86

80

33

90

14

100

7.6


  I ka wā o ka uhi ʻana, e hoʻopilikia ka viscosity a me ka mahana i ka mānoanoa a me ka maikaʻi o ke kiʻi paʻa. No ka laʻana, ke kiʻekiʻe loa ka viscosity, ʻilihune ka wai, ʻaʻole kūpono i ka hoʻokumu ʻana i kahi kiʻi resin maikaʻi. Ke haʻahaʻa loa ka viscosity, maʻalahi ke nalowale. ʻO ke kumu nui, ua hoʻohui ʻia ka lāʻau lapaʻau i ka ʻōnaehana resin epoxy, a ua wela ka resin no ka manawa lōʻihi i ka hoʻomākaukau ʻana o ke kiʻiʻoniʻoni. Ke kiʻekiʻe loa ka mahana, hiki i nā macromolecules a me nā ʻāpana kaula ke hele i ka neʻe wela, e pili ana i ke ola o nā huahana i hoʻopau ʻia. No laila, i ka wā e hoʻomākaukau ai i ke kiʻi paʻa, pono e haʻahaʻa ka mahana ma lalo o ke ʻano e hoʻokō ʻia ai nā koi kaʻina. Hiki ke ʻike ʻia mai ka Papa 2 i ka nui o ka resin viscosity ma 60 ℃, e pili ana i ka paʻa o ka hoʻomākaukau kiʻiʻoniʻoni, no laila ua koho ʻia ʻo 70 ℃ e like me ka mahana kiʻiʻoniʻoni.


 c. Ka hoʻoholo ʻana o ka ʻōnaehana hoʻōla


  Hiki i kahi ʻōnaehana ho'ōla maikaʻi ke hoʻomaikaʻi i ka hana o ka huahana, inā ʻaʻole ia e hoʻopilikia wale i ka hana o ka huahana akā lawe pū kekahi i nā pilikia kaʻina hana. Hiki ke hoʻoholo ʻia ka ʻōnaehana hoʻōla e ka hoʻokolohua DSC non-isothermal. Ma nā ʻano wela wela o 5 ~ 25 ℃/min, pili ka ʻōnaehana resin i ka wela o ka hopena mua (Ti), ka wela o ka hopena kiʻekiʻe (Tp) a me ka wela hopena hopena (Tf) (Pakaukau 3). Hiki ke loa'a ka wela wela o ka hopena (Ti), ka wela wela o ka hopena (Tp) a me ka wela wela o ka hopena (Tf) ma ka laiki 0 e like me ka hoohalike laina o na mea ekolu.


Papa 3 Ti, Tp a me Tf ma na uku wela okoa

Laki wela/℃/min

Ti/℃

Tp/℃

Tf/℃

5

163

193

217

10

165

198

237

15

173

209

249

20

182

225

270

25

187

234

296


d. Ka loiloi pale wela


  ʻO ke kūpaʻa wela o ka ʻōnaehana resin e loiloi ʻia e ka wela deformation wela, ka mahana hoʻololi aniani a me ka wela wela decomposition decomposition o ka mea. ʻO ka mahana hoʻololi aniani ʻo Tg ka wela o ka mea mai ka moku aniani a i ke kūlana elastic kiʻekiʻe, ʻo ia ka ʻikepili koʻikoʻi e hoʻoholo ai i ka mahana lawelawe mea. ʻO ka mahana hoʻololi aniani i ka pihi DSC he 203 ℃.


e. ʻO ka loiloi o nā waiwai mechanical o nā resins a me nā composites


  Hōʻike ka Papa 4 i ka ʻikepili o nā waiwai tensile a me ka piko o ka resin i ho'ōla ʻia. Papa 5 hoike i ka mechanical waiwai ikepili o carbon fiber prepreg unidirectional laminates. E like me ka ʻikepili ma ka Papa 4, hiki i nā ʻano mechanical o ka ʻōnaehana resin a me ka carbon fiber prepreg ke hoʻokō i nā koi waiwai.


fr4 pepa

Papa 4 Nā waiwai mīkini o ke kino hoolei resin

Auana

Waiwai Pahuhopu

Waiwai ʻiʻo

Waiwai Tensile

Ikaika U'i/MPa

≥55

58.6

ʻO ka modulus tensile/GPa

≥3

3.48

Hana Kulou

Ka ikaika piko/MPa

≥85

117

Modulus piko/GPa

≥3

3.52


Papa 5 Mechanical waiwai o carbon fiber prepreg unidirectional laminate

Auana

Waiwai Pahuhopu

Waiwai ʻiʻo

Waiwai Tensile

Ka ikaika uʻi longitudinal/MPa

≥20000

2500

Lohitudinal tensile modulus/GPa

≥120

128

ʻO ka ikaika tensile transverse/MPa

≥28

34.2

Modulus tensile transverse/GPa

≥7

7.18

Hana Kulou

Ka ikaika piʻo lōʻihi/MPa

≥1400

1440

Modulus kulou lōʻihi/GPa

≥130

132

Hana Hoʻopiʻi

Ka ikaika compressive longitudinal/MPa

≥800

1195

Ka ikaika compressive transverse/MPa

≥120

131

Hana ʻAhi

Ka ikaika shear interlayer/MPa

≥75

86.2

3240 pepa epoxy

4. Panina

  

  Ma kēia pepa, ka multifunctional epoxy resin a me ka laulā epoxy resin E51 ua hui pū ʻia, a ua koho ʻia ka ʻōnaehana hoʻōla kūpono-accelerator no ka hoʻomohala ʻana i ka resin prepreg epoxy resin prepreg kiʻekiʻe, a ua hoʻāʻo ʻia nā waiwai o ka resin a me ka composite.


  a. ʻO ka resin epoxy multi-functional he mea pono i ka hoʻomaikaʻi ʻana i ka pale wela o ka ʻōnaehana. Ke 75/15/25/15/0.3 ka lākiō nui o ka ʻōnaehana (A / B / C / D / E) i ka wela wela a hiki ke hoʻokō i nā koi o ka hana prepreg wela wela.


  b. Ua hoʻāʻo ʻia nā ʻōkuhi DSC o ka ʻōnaehana resin ma nā ʻano wela wela e nā hoʻokolohua DSC. ʻO ka ʻōnaehana hoʻōla maikaʻi loa o ka ʻōnaehana resin ʻo 160 ℃/1h+180 ℃/3h ma ka laina laina.


  c. ʻO ka ʻōnaehana resin he pale wela maikaʻi loa, a ʻo ka Tg i ana ʻia e DSC he 203 ℃.


  d. ʻO nā waiwai mechanical o ka ʻōnaehana resin a me ka carbon fiber prepreg e hoʻokō i nā koina waiwai.


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