SU1645276A1 - Moulding composition - Google Patents

Description

(21) 4433992/05

(22) 04.19.88

(46) 04.30.91. Yul N 16 (72) T.V. Kashinska, T.N.Putilina, L.K.Lkoeva, M.L.R. Zantseva, N.I.Nesterov and S.A. Derevnko

(53) 678.643 (088.8)

(56) Japanese Application No. 61-95020,

cl. C 08 G 59/62, I 01 L 23/30, 1984.

(54) PRESS COMPOSITION

(57) The invention relates to the field of epoxy moldings and can be used to seal semiconductor devices and integrated circuits. EFFECT: enhanced mechanical strength.

hardened material while maintaining high electrical insulation properties due to its use in a press composition, including, in weight, hrs: epoxyresol formaldehyde oligomer SO; hardener - cresol-formaldehyde novolac oligomer 50-67; accelerator - 2-methylimidazole 3.4-3.8; filler - powdered quartz 345-363, anti-adhesive additive - wax 5.0-5.5, additionally flame retardant - antimony oxide 0.2-7.6 to modifier 6.7-17.1 selected from the group comprising diglycidyl ether tetrabrom - diphenylolpropane, tetrabromopyrocatechol, dibromobutenol, dibromoneopentylgnecol. 2 tab.

ABOUT)

The invention relates to epoxy molding materials and can be used for sealing semiconductor devices and integrated circuits.

The purpose of the invention is to increase the mechanical strength of the press composition while maintaining its high electrical insulating properties.

Tetrabromodiphenylolpropane (UP-631 grade) diglycidyl ether is obtained by reacting tetrabromodiphenylpropane with epichlorohydrin. The content of bound bromine is 50%.

Tetrabromopyrocatechol is obtained by pyrocatechol fermentation in various solvents, inorganic acids, in water at 25–3 ° C, followed by

washing the resulting compound with hydrobromic or hydrochloric acid, 1% sulphite-soda solution and water. The content of bound bromine is at least 72%.

Dibromoneopentyl glycol is produced by the interaction of pentaerythritol with hydrogen bromide in a solvent, water at 110 ° C.

Dibromobutenol is obtained by reacting butynediol with bromine (1:.: 1 mol) in a solvent at 20-30 C.

A solid epoxy-cresol-formaldehyde oligomer, obtained by epoxylation of cresol-formaldehyde novolac oligomer with epichlorohydrin in the presence of chlorine, is used as the basis of the press composition.

In addition, triethylbenzylammonium at C n for 2.5 h followed by dehydrochlorination with solid caustic soda and washing. Epox novolac oligomer has a number average mole. 1000-1200, the content of epoxy groups 20%, the total chlorine content of 0.3%. Epoxy equivalent wounded him 180-200, i.e. is within the range of epoxy equivalent values of an o-cresol-wave olnomer in a known press material. Cresolformalrgidpmi novolac oligomer, which is an intermediate in the synthesis of epoxinovolac oligomer and used as its otnerbitel, nonvMam- polycondensation of o-cresol with a form. Easily (ratio 1: 0.93 mol, respectively) in an acidic medium (hydrochloric acid) at 80 + 1 ° 0 for 4 h.

2-Methylimmidazole is synthesized from egylenediamine and acetic acid (according to 1: 1.17 mol, respectively) using an AP-64 forming aluminum alumina catalyst (granulation 1-2 mm, platinum content not less than 0.57) with a stream of hydrogen at 400 ° C for 3 hours. The anti-adhesive additive is beeswax, the filler is KP-P brand dust-like quartz, previously dried at 250 ° G for 8 hours.

Standard samples for testing were obtained by injection molding at 165i5 ° C,% pressure of 15.0 MPa, followed by heat treatment at 200 ° C for 8 hours.

Bending stress at fracture and flexural modulus of elasticity were determined on five bars of (80iO, 2) x (l040.2) x (4, r) fO, 2) mm.

The volume electrical resistance was determined at a constant voltage of 100-105 V on three disks with a diameter of 50 + 0.5 mm and a thickness of 0.8-1.0 mm.

Dielectric loss tangent

and the dielectric constant of op-Sn tilimidazole 3.6; beeswax 5.5;

-., n f

divided into three disks with a diameter of 4; 0t5 mm and a thickness of 0.8-1.0 mm, flammability - in five bars (120 ± 10) x (10 ± 0.5) x (3-5) mm.

The gelation time was determined on a heated metal plate.

Press compositions were prepared by the method including the following steps:

quartz powder 363; antimony oxide 7.6; the modifier of formula I is 17.3 (i.e. the bromine content in the binder is greater than 5 May.7).

The potted press composition is not ecological: it has a long gel formation time, the samples are removed from the mold flexible, easily damaged and

five

j

with.

about

. ; (

dg

.S

thirty

understanding of the filled base by melt combination of the following components, wt.h .: eioksikresolformal- dehydro oligomer 100; quartz powder 212-234; anti-adhesive additive of 3.2-3.5; modifier 6.7-17.1; temperature 160 + 10 ° C, time 3-6 min;

obtaining a filled hardener by combining in the melt (temperature I6oi.1i) 0g, time 3-4 min) of the following components, in weight: cresolformaldehyde oligomer 50.0-67.0; quartz powder 129-133; antimony oxide 0.2-7.6; curing accelerator 3.4-3.3; anti-adhesive additive 1.8-2.0;

grinding filled asnovy and hardened, sieving (sieve 063) and mixing them.

Examples 1 and 2. The compositions of the obtained press compositions are given in table. 1. As a modifier, tetrabromodiphenylolpropane (I) diglycidyl ether was used.

Press compositions are made by the method described above.

Example 3. According to the method described above, a press composition is prepared that includes, in weight, h: rpoxy-cresol — formaldehyde oligomer 100; cresol-- (formaldehyde oligomer 67.0; 2-megaplnimidazole 3.8; beeswax 5.2; quartz powder; 34 antimony oxide 1,2; modifier T b, 5 (i.e., the content of bromine P less than 2 May.).

The resulting composition has lower mechanical strengths and dielectric values. Similar results were obtained for compositions containing the same amount, 7,8-tetrabromopyrocatechol (II), dibromobutendpol (Hi), dibromoneopentine glpcol (LV).

II p and me. According to the method described above, a press composition is made, including mac.h .: epoxycresol-formaldehyde oligomer 100; cresol is a formaldeptic opigomer 57.0; 2-methylimidazole 3,6; beeswax 5.5;

 ., n f

quartz powder 363; antimony oxide 7.6; the modifier of formula I is 17.3 (i.e., the bromine content in the binder is greater than 5 May.7).

The potted press composition is non-technological: it has a long gel time, the samples are removed from the mold by flexible, easily damaged and

exfoliate. In appearance, they do not meet the standards.

Similar results were obtained for compositions with the same amount of additives II, III and IV.

II p and mep 5. According to the method described above, a press composition is made, which, in May, includes: epoxyresol formaldehyde oligomer 100; creole formaldehyde oligomer 67.0; 2-methylimidazole 3.8; beeswax 5,1; quartz powder 349; modifier I 10.3 and does not contain antimony oxide.

The resulting composition in terms of mechanical and electrical insulation properties is similar to the press composition of example 1, but differs from it.

a little less time gel-20 properties, it contains

vani and greater flammability.

Similar results were obtained for the remaining compositions with the addition of modifiers II, III and IV, but not containing antimony oxide III.

Example According to the method described above, a press composition is made, including, m.ch .: epoxycresol-formaldehyde oligomer 100; creole formaldehyde oligomer 57.0; 2-methylimidazole 3.8; beeswax 5.5; quartz powder 349; modifier I 10,3; antimony oxide 7,8.

The resulting press composition is non-technological: it has a large gel time, the samples are fragile, easily damaged when removed from the mold, the mechanical properties are reduced.

Similar results were obtained for press compositions with additives

clamps II, III and IV, and a given amount of antimony oxide.

In tab. 1 shows the compositions of the press compositions; in tab. 2 - their properties.

Claims (1)

Invention Formula A press composition for sealing semiconductors, including an epoxy-cresol-formaldehyde oligomer, a hardener — a cresol-formaldehyde novolac oligomer, a hardening accelerator — 2-methylimidazole, a sharpened quartz and anti-adhesion additive — a wax, which is made with a pattern, a shar- form quartz and an anti-adhesive additive — a raffus, a sharpening quartz and an anti-adhesion additive — a wax, a pattern, a shar- form quartz and an anti-adhesion additive — a pattern, a sharpening quartz and an anti-adhesion additive — a wax that has the same pattern as a sharpening quartz and an anti-adhesion additive — a pattern, a sharpened quartz and an adhesion additive — a pattern, a sharpening quartz and an anti-adhesive additive — maintaining high electrical insulation ka beeswax and additionally anti-pyrene — antimony and a modifier selected from the group including tetrabromodiphenyl-propane di-glycidyl ether, tetrabromo-pyrocatechin, di-bromobutendiol, dibromine-pentyl glycerol, in the following ratio. . components, ma.ch .: i i Epoxyresol formaldehyde oligomer 100 Kresol formaldehyde novolac oligomer50-67 2-Methylimidazole 3.4-3.8 Dusty quartz 345-363 Beeswax 5.0-5.5 Antimony oxide 0.2-7.6 Specified modifier 6.7-17 ,one ldr lno but- ck 100 3.8 5.2 349 1.8 100 100 100 100 3.4 5.4 351 5.1 3.8 5.2 348 1.2 3.6 5.5 3.8 5.1 363349 7,6 10.3 17.1 6.5 17.3 10.3 100 67.0 50.0 67.0 57.0 67.0 57.0 3.6 5.5 10.3 349 7,8 100 100 3.6 5.5 3.8 5.1 363349 7,6  17.3 10.3 100  57.0 67.0 57.0 3.6 5.5 10.3 100 67.0 3.8 5.2 6.7 100 3.3 5.4 349348358 7.81.83.1 11.1 00 67.0 67.0 3.3 5.9 7.7 100 67.0 3.8 5.3 100 3.5 5.3 12.8 100 3.3 5.5 345353352363 0,27,61,35,1 8.2 13.7 100 50.0 67.0 67.0 3.8 5.0 333 100 61 3.5 5.2 347 0.3 12.6 100 101} 5964 3.43,7 5,35,3 344343 3.57.3 17.0 11.1 w-ewi 1h; 3N 2427 784 9770 A 2 22 4-10 4.2 93.6 82.7 67.0 9542 22 14 46 22 g  3-10 10 8, 1,1-Ю 2 3,54,6 94, P 66.4 87.0 39.3 89.5 100.0 103.0 98.8 69.3 88.6 8740 6406 9314 9139 9884 9864 8710 9658 8506 10115 3722 2530222523 28 29 74.8 84, L 9550 9660 33 27 5644510-34173776132 2810172611251423192720 153 21 i; 4.1015 3-Ю15 6-10 (ЈГ 3-11№ 3-Ю 5 2-Ю15 4-1015 3 2-я 5 3-Ю15 4 - 2 Ю 5  MO-2 1-1) 8,2-10 ch. Z-Yu 3 1 G.G1 1. 1, 1 9-10 one , 2, 34,34,24,34,34,34,34,04,34,3 4,1