SU1639921A1 - Compound for protection of melted solder surface against oxidation - Google Patents

Abstract

The invention relates to soldering, in particular, compositions for protecting a mirror of molten solder from oxidation, mainly during wave soldering, and can be used in the electrical, electronic, radio, instrument-making industries. The purpose of the invention is to increase the service life of the composition, reduce the consumption of solder and improve the quality of soldering. The composition contains the components in the following ratio, wt.%: Phenothiazine 0.3 - 3.0; ethoxylated condensation product of monoizononylphenol and tetramethyl dipropylene triamine 0.05-3.0; hydroxylated isoalkylphenols else. The durability of the composition is 40-45 h. The solder consumption decreases by 1.5-2 times. The composition allows the use of a closed flushing system, simplifying the washing operation and eliminating the use of flammable and explosive materials. 1 tab. § (L

Description

The invention relates to the field of soldering, in particular, to compositions for protecting a mirror of molten solder from oxidation, mainly during wave soldering, and can be used in the electrical, electronic, radio, instrument-making industry and other folk industries.

The aim of the invention is to increase the service life of the composition, reduce the consumption of solder and improve the quality of soldering. .

The composition contains the following components, wt%:

Phenothiazine 0.3-3.0

Hydroxyethylated monoizononylphenol condensation product

and tetramethyldipropylene triamine 0.05-3.0

Ethoxylated monoisoalkylphenols Else

When using this composition of a water-soluble protective fluid (HPA) to melt, the working capacity of the drug is maintained for 80 hours, and when used in soldering baths with a protective liquid of 0.5-1 cm at 260-275 ° C, the performance of the HPLC preparation is preserved. within 35.0 - 40 hours.

When using the composition, the consumption of solder is reduced by about 2 times, there is practically no slag

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with so

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education, the quality of paired compounds and labor productivity increase.

In addition, the product is completely washed after soldering with water at high speed and without the use of organic solvents.

The condensation product of monoizononylphenol and tetramethyldipropylentriamine, ethoxylated, for example, at 12 moles of ethylene oxide, acts as a stabilizer for thermal stability and a lifetime of the proposed PLC.

The use of oligononylphenol ether oligoethers ethoxylated with 3–30 mol of ethylene oxide (OE) as the basis of the preparation, where isononylphenol of the same nature as isononylphenol in a stabilizing additive improves the technological properties of the preparation.

. The components included in the composition have the following characteristics and purpose.

As a liquid organic base, simple oligoesters are used - a product of condensation of ethylene oxide and monoizononylphenols (monoisoalkylphenols) based on propylene trimers, having number average mol.m. 570-1540.

Simple oligoesters perform simultaneously the function of a carrier (base) and a surfactant, being an insulating medium for protecting the solder from oxidation.

The technology of preparing the composition from the starting components is simple and does not require expensive equipment and reagents. The preparation for protection of solder against oxidation is prepared by mixing in a certain sequence of components, taken in a calculated proportion.

Weigh and place in a temperature-controlled glass with a capacity of 2 liters of 99.65% by weight of monoizononylphenol-based oligoesters, for example Neonol AF9-12 (powder 996.5 g with oxyethylation degree 12 and mol.m. 748) with constant stirring, powdered phenothiazine is fed into the amount of Zg (0.3 wt.% 1). The mixture is stirred for 5-10 minutes until a homogeneous mass is obtained. The temperature in the beaker is maintained at a level of 70-30 ° C during the whole preparation operation. the mixture is charged with 0.5 g (0.05 wt.%) of a stabilizing additive (product monoizononil- condensation of phenol and tetrametildipropilentriami- to, ethoxylated to 12 moles ethylene oxide). During the stirring, the finished product was cooled gradually to 30-40 C and passed the test.

The prepared composition is a liquid from light brown dZ brown, not containing mechanical impurities.

In the obtained preparation, the following performance indicators are determined: flash point in an open crucible, kinematic viscosity, smoke (determined visually by the absence of emission of colored volatile products when heated to the working temperature), service life (thermal stability of the preparation, OST is determined in laboratory conditions in a special installation consisting of a thermostatted glass, filled with solder, with a capacity of 1.5 liters, an agitator for mixing solder, an electric cooker, a contact thermometer, an electronic switch soldering system; POS-61 solder is placed in a glass and poured on top with a layer of a VZZH preparation 0.5–1.5 cm thick; include the device and the system;

Every 8 hours of operation, the performance indicators of the PERS as well as the state of the surface of the protected solder are determined (visually); slag formation is determined by the presence of oxidation products in the system visually or by weighing; the quality and time of washing the steam products is determined visually.

To do this, in a thermostated glass with solder and HZZH at a temperature of soldering, lower samples of printed circuit boards in the amount of 2-3 pieces at 3-4 s. The remains of the VZH wash with the distilled water, time of washing is noted on a stop watch.

The corrosion resistance of the solder joints after washing off the protective liquid is determined by the absence of a corrosive effect on the solder joints.

The service life (life time) of a VZH in production conditions is determined on the installation of a mechanized wave soldering in the following order.

A thoroughly cleaned mechanized soldering bath, equipped with a wave former, with POS-61 solder, is poured in a quantity in order to create a protective layer over the solder of 0.5-1 cm, and heated to 250 ° C. When the required temperature is reached, the wave former is turned on and the wave soldering process is carried out. At the end of the working day, the engine is turned off, the solder is cooled. Subsequently, the process is repeated until the slag, the products of the destruction of the PERSA, etc., appear on the surface of the solder and in the HPA layer. During the lifetime of a VIAZ drug of this composition, the total operating time of the system (with the engine on) is taken before slag formation begins.

Solder quality is determined every 5-6 hours of engine running. Wave

5-6

solder, lost i-b pcs. test boards (double-sided printed circuit boards with 120 metallized holes) using a water-soluble flux (the flux is the same for all formulations). After soldering and washing the test boards, disposable soldering defects (non-solder, jumpers, icicles, pores, shells, etc.) are determined visually and under the microscope of the MBS. Solder consumption is determined after 18-20 hours of operation of the wave soldering unit with a protective liquid of the studied composition, soldering the test board in the amount of 8-10 pieces. using a water-soluble flux and washing the test board from the flux residuals and the HPLC with distilled water. Before the soldering and after washing, the test boards are dried at 80 ° C for 3 hours. The average difference is taken for the consumption of solder. The mass of the missing test boards and the original ones.

In connection with the short lifetime of the liquid obtained by the prototype, the consumption of solder using this protective composition was determined after 2-3 hours of operation of the installation.

For the criterion of consumption of solder (N), the ratio t rOT / tVsz (|; N, where t PROT is the consumption of solder on all solder joints of the test board when the mirror is protected by a sol

39921 °

totype; wz - The corresponding average solder consumption in the protection of one of the proposed composition of the PERS; N - reducing the consumption of solder, the number of times.

Examples of the composition and its properties are presented in the table.

From the analysis of the above formulations, it follows that oligoesters, which represent the monoisonylphenols ethoxy ethoxy (12 moles) ethylene oxide (12), have a service life of 10–10.5 hours in laboratory conditions and 3 hours in production conditions.

15 The average percentage of defects in soldering in comparison with the prototype is 1-2% higher, and the average consumption of solder on all solder joints of the test board is higher by 0.3 g. Solder consumption increased

20 1.05 times. The flash point of the composition is higher than that of the prototype, at 73 ° C. Introduction to the composition of one antioxidant supplement phenothiazine (example 13) increases the service life

25 of the composition in the laboratory for 3 hours, and in the production for 2 hours,

BEFORE

rises about.

flash point is about.

263 C (an increase of 3 ° C) compared with example 12. The rest

performance indicators the introduction of antioxidant has not had a significant impact.

The introduction of one stabilizing additive (Example 14) compared with Example 12 increased the flash point of the composition to 275 ° C, the other operational indicators did not change significantly.

The data of examples 12-14 clearly show that the proposed composition is characterized both by an increase in the service life and a decrease in the consumption of solder. In addition, the data from these examples confirm the need for the presence of all these components in the composition.

Compared with the prototype, all the compositions shown in the table have a significantly higher flash point and performance (service life). The compositions according to examples 1-11 have a smaller value of the average percentage of soldering defects and the average solder consumption of all solder joints of test boards, and are also characterized by a decrease in solder consumption.

A quantitative increase in antioxidant and stabilizing additives above 0.5 wt.% (Example 4) in the composition of the preparation does not improve the technological properties of the product, but is not economically feasible, since it leads to an increase in the cost of the preparation. The optimal ratio (examples 5 and 8-11) is the quantitative ratio of antioxidant and stabilizing additive by 0.5 wt.% And oligoethers 99 wt.%.

The increase in the number of ethylene oxide in monoisononylphenols does not impair the performance properties of the drug of the PERS in the compositions according to examples 9 and 10.

Due to the fact that simple oligo-ethers based on monoizononylphenols with the degree of hydroxyethylation of 7 and mol.m. 528 (Neonol AF9-7) are water-soluble products and are poorly washed from the surface of printed circuit boards. Therefore, the use of Neonol AF9-7 in the composition of the drug PERSON is impractical.

The use of oligononylphenol-based oligoesters with the degree of m 35 and mol.m. 1760 (Neonol AF9-35) in the composition of the preparation with a HPA preparation slightly worsens the quality of washing and lengthens the washing time.

Due to the proposed combination of the used raw materials, the technological properties of the composition are improved: the life of the preparation increases, the slag formation process slows down in time, the quality of solder protection from oxidation is improved, the temperature range of its application is extended. The flash point in an open crucible of the proposed composition is 306 ° C. The use of a composition with such a flash point eliminates fires and explosion hazards of production, improves working conditions, reduces emissions of harmful substances into the environment by eliminating smoking.

Thus, the composition to protect the solder from oxidation has a long service life (40-45 hours), ensuring

ten

15

20

25

35

3 (

40

The cost saving of the expensive POS-61 solder in technological soldering processes with the use of water-soluble fluxes and their compatibility with them, reduction of soldering defects and increase in labor productivity.

In addition, increased anti-corrosion properties of the composition. The proposed composition allows the use of a closed flushing system, simplify the washing operation and eliminate the use of flammable and explosive materials.

The mechanized soldering technology using the proposed oxidation protection composition is waste-free, which meets the current requirements of environmental protection.

Formula of the invention

An agent for protecting molten solder mirrors from oxidation, containing oligoesters based on ethylene oxide, phenothiazine, characterized in that, in order to increase the service life of the composition, reduce solder consumption and improve the quality of soldering, it additionally contains ethoxylated monoisononylphenol condensation product and tetramethyldipropylene triamine; ethoxylated at 12 mol of ethylene oxide, and as oligoethers, oxyethylated monoisoalkylphenols of the general formula SpNgp + 1SbN40 (CgN40) HG) H, where n 9, m 8-30 mol of ethylene oxide (at mol. m 570- 1540), in the following ratio, wt.%:

Phenothiazine Oxyethylated condensation product of monoizononylphenol and tetramethyldipropylenetriamine

Oxyethylamine n-monoisoalkylphenols of the indicated general formula

0.3-3.0

0.05-3.00

Rest

1 99.65 0.3

0.05

5.18

1.2

Good

40

In practice, there is no trace of oxides

Practical-Practically absent

Virtually unchanged

Also

Also

Same same same

79.0 1, 0

Triethanolamine

As the oligoethers, monoisonylphenols are ethoxy ethoxylated: in examples 1-7, 12-14 and 17 per 12 moles of ethylene oxide; in example 8 to 8 mol of ethylene oxide; in example 9 per 25 mol of ethylene oxide; in example 10, 30 moles of ethylene oxide; in example 11 per 10 mol of ethylene oxide; in example 16 to 35 mol of ethylene oxide.

In the numerator, the results of tests in laboratory conditions, T ™ 275+ 1 C; in the denominator, the results of tests under industrial conditions, T 250 ± 10 ° С.

192

1-8

3-4

5-7

6.3

Good 60 Practices - Presence of 1 - Strong oxidative formation - smoke

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Claims (1)

Claim Sos.tav to protect the mirror of the molten solder from oxidation, containing ethylene oxide-based oligoesters, phenothiazine, characterized in that, in order to increase the service life of the composition, reduce the consumption of solder and improve the quality of soldering, it additionally contains an ethoxylated condensation product of monoisononylphenol and tetramethyldipropylene triamine; oxyethylated to 12 mol of ethylene oxide, and ethoxylated monoisoalkylphenols of the general formula C _n H _{2n +} , C ₆ H ₄ 0 (C2H ₄ 0) _m H, where η = 9, w = 8-30 mol of ethylene oxide (at mol.m. 570-1540), in the following ratio of components, wt.%: Phenothiazine Oxyethylated ‘condensation product of monoisononylphenol and tetramethyldipropylenetriamine Oxyethylated monoisoalkylphenols of the indicated general formula 0.3-3.0 0.05-3.00 Rest CM Joint venture 1 ABOUT about With f X <0 5 then cx a £ 1O TO from' ABOUT I 1 1 About s about to about about M 1m to about in and then about about e- X σ » 2 to about f about. 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In the numerator are the results of tests in laboratory conditions, T = 275 + 1 C; in the denominator - the test results in an industrial environment, T = 250 ± 10 ° C.