JPH0494891A - Flux for soldering and solder containing resin - Google Patents

Abstract

PURPOSE:To enable soldering to a metal difficult-to-soldering by using a perfect hydrogenized rosin as a basis agent and adding the specific rates of piperidine hydrobromide and monoethanol amin hydrofluoride. CONSTITUTION:The completely hydrogenized rosin is used as the basis agent. As the additive to this basis, at least piperidine hydrobromide and monoethanol amin hydrofluride are added. These added quantities are made to in the range of 1wt. part-100wt. parts to 1000wt. parts of the basis. Further, the basis is composed of the completely hydrogenized rosin and hydrogen-added rosin with incompletely hydrogenized rosin. By this method, flux for soldering having a little scattering and good workability can be provided.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to soldering flux and flux-cored solder using the flux as a core (note that those skilled in the art refer to flux-cored solder as flux-cored solder). There is.

) regarding.

[Prior art] Soldering flux is used as the core of cored solder, and when joining metals by soldering, it chemically promotes interalloy compounds, and also removes oxides on the metal surface to increase activity. It is something to give.

Conventionally, natural rosin, which is easy to produce, has generally been used as a base for soldering flux. Furthermore, halogen compounds are commonly used as additives for the base, and among these, chlorine compounds are often used.

[Problems to be Solved by the Invention] However, when natural rosin is used as a base, the color of the residue after soldering becomes brownish-brown, which poses a problem in terms of appearance. on the other hand,
When a chlorine compound, which is a halogen compound, is used as an additive for the base material, the amount of scattering during soldering increases in proportion to the chlorine content, which poses a problem. Further, soldering flux using only a chlorine compound as an additive can only be used for metals that are relatively easy to solder, and it is difficult to solder metals such as stainless steel or iron.

Therefore, the object of the present invention is to achieve a finish with a thinner residue after soldering and an excellent appearance, and to reduce the amount of scattering during soldering work, and to be able to solder difficult-to-solder metals such as stainless steel or iron. To provide soldering flux and flux cored solder which enable soldering and have excellent workability.

[Means for Solving the Problems] In order to solve the above problems, the first invention uses fully hydrogenated rosin as a base, and contains at least piperidine hydrobromide and monoethanolamine as additives for the base. A hydrofluoride salt is added, and the amount added is equal to that of base 1 in both cases.
The flux for soldering is characterized by being in a range of 1 part by weight or more and 100 parts by weight or less per 1,000 parts by weight.

A second invention for solving the above-mentioned problems mainly consists of a fully hydrogenated rosin and a hydrogenated rosin obtained by incompletely hydrogenating the rosin, and the proportion of the fully hydrogenated rosin is 25% by weight or more based on the total weight of the rosin. Using a base in which the remainder is hydrogenated rosin, at least piperidine hydrobromide and monoethanolamine hydrofluoride are added as additives to the base, and the amounts of both are as follows. The flux for soldering is characterized in that the amount is in the range of 1 part by weight or more and 100 parts by weight or less based on 1000 parts by weight of the base.

The fully hydrogenated rosin described above is a product obtained by completely hydrogenating rosin (hard pine resin, main component being niabinitic acid). The general properties of this completely hydrogenated rosin are shown in Table 1.

It is compatible with Table 1 (ethylene/vinyl acetate rubber), etc.

The hydrogenated rosin refers to rosin that has been incompletely hydrogenated. The general properties of this hydrogenated rosin are shown in Table 2.

Table 2 shows the solubility of fully hydrogenated rosin in ethanol, IP
It is soluble in A (isopropyl alcohol), esters, ketones, and aromatic solvents, and insoluble in water and methanol. Regarding the compatibility of KR-611, NR (natural rubber), 5BR (styrene-butadiene rubber), 5I
The solubility of S (styrene-isoprene-styrene), 5BS (styrene-butadiene-styrene), CR (chloroprene rubber), acrylic resin, polyamide resin, and EVA hydrogenated rosin is good for NR, 5BR1 wax, ethyl cellulose, and EVA. dissolve. As for the compatibility of Hyperel, it is soluble in alcohol, esters and hydrocarbon solvents, but insoluble in water.

In the second invention, the percentage of fully hydrogenated rosin is set to be 25% by weight or more because if the content is less than this, problems will arise in terms of compatibility and segregation between the additive and the base material, and a flux with uniform quality will not be obtained. This is so that you will not be affected.

More preferably, the proportion of fully hydrogenated rosin is 50% by weight or more, and most preferably 90% by weight of fully hydrogenated rosin and the remaining 10% by weight of hydrogenated rosin.

The hydrobromide of piperidine is synthesized from piperidine and hydrobromic acid by a conventional method, and the weight ratio used in the synthesis is preferably 15 parts of hydrobromic acid to 15 parts of piperidine IO. In addition, the hydrofluoric acid salt of monoethanolamine is synthesized from monoethanolamine and ammonium hydrogen fluoride by a conventional method, and the weight ratio used for the synthesis is 30 parts of monoethanolamine to ammonium hydrogen fluoride. It is preferable to set it to 10.

The reason for using at least both piperidine hydrobromide and monoethanolamine hydrofluoride as additives is to enable soldering to various difficult-to-solder metals. That is, the former additive enables soldering to iron and nickel, and the latter enables soldering to stainless steel.

The amount of piperidine hydrobromide to be added is 1 part by weight or more and 100 parts by weight or less per 1000 parts by weight of the base, and the amount of hydrofluoride of monoethanolamine is also limited to 1,000 parts by weight. The amount may be 1 part by weight or more and 100 parts by weight or less based on 1000 parts by weight of the base. The amount of both added varies depending on the type of base material, and is set to an appropriate amount that provides a flux of uniform quality. The amount of each additive added is 1
The reason why the amount is set at 1 part by weight or more per 1,000 parts by weight is because if the amount added is less than this, it will not be possible to solder to difficult-to-solder materials such as stainless steel or iron. This is because if the amount added is greater than this, the residue after soldering may cause corrosion of the base material and a decrease in electrical insulation.

The preferred amount of piperidine hydrobromide is base material 1.
The amount is preferably 17 to 43 parts by weight, more preferably 20 to 30 parts by weight per 1,000 parts by weight, and for the hydrofluoric acid salt of monoethanolamine, the preferable addition amount is 1 part by weight of the base.
The amount is 8 to 24 parts by weight, more preferably 14 to 18 parts by weight per 1,000 parts by weight. The best addition amount is 15 parts by weight of piperidine hydrobromide and 4 parts by weight of ethanolamine hydrobutorate per 1000 parts by weight of the base. The above additives may be added to the base by heating the base to about 150° C. and then adding piperidine hydrobromide and monoethanolamine hydrofluoride.

A third invention for solving the above problem is a core of a cored solder as claimed in claim 1 (first invention) or claim 2 (second invention).
It is said to be a flux-cored solder characterized by being the soldering flux described above.

The above-mentioned flux-cored solder is a common solder alloy, such as Sn(
An alloy of tin) and Pb (lead) or the alloy or Sn or p
b, Ag (silver), Bi (bismuth), CD (cadmium), In (indium), Sb (antimony), Cu (
Manufactured using a conventional method using a solder alloy containing one or more metals such as copper.

[Function] When the soldering fluxes of the first and second inventions are used for soldering, they lighten the color of the residue after soldering. The fully hydrogenated rosin of the base material contributes to the color of the residue, and soldering lightly colors the residue.

Hydrobromide of piperidine and hydrofluoride of monomethanolamine enable soldering to metals such as stainless steel or iron, and reduce scattering during soldering.

Since the third invention is a solder using the soldering flux of the first or second invention as a core, it can be soldered as is, and has the same effect as the first and second inventions described above.

[Example] Next, the present invention will be explained in detail.

Example 1 The degree of coloring caused by heating when natural rosin, hydrogenated rosin, and fully hydrogenated rosin were used in various blending ratios as a base material for soldering flux was investigated as follows.

That is, 1000 g of base material with various compounding ratios shown in Table 3.
Additives piperidine hydrobromide and monoethanolamine hydrobutorate were added while heating the mixture to 150°C to complete a flux. The above piperidine hydrobromide is prepared by combining piperidine (10g) and hydrobromic acid (
15g), and the above monoethanolamine hydrobutatate is obtained by reacting monoethanolamine (15g).
2g) was reacted with ammonium hydrogen fluoride (4g) while stirring the alcohol.

130℃ for the various fluxes obtained as above.
Heating at 150°C, 170°C or 200°C for 24 hours,
The degree of coloration in each case was observed with the naked eye. The results are shown in Table 3.

(Continued on next page) Table 3 In Table 3, the blending ratio of the base is shown in weight %. In addition, regarding the marks that indicate the degree of coloration due to heating conditions, ◎ indicates that the color does not change much even after heating and is light yellow. ○ indicates that the color changes slightly after heating and becomes light brown. △ The mark indicates that the color changes after heating and becomes brown, and the X mark indicates that the part that comes into contact with air changes to black after heating.

Table 3 shows that the base containing natural rosin (lots 1 and 2) turned brown when heated at 150°C for 124 hours, whereas the base containing 100% by weight fully hydrogenated rosin (lot 3) Even when heated under the same conditions, it only turned light brown. and fully hydrogenated rosin (10-90% by weight) and hydrogenated rosin (100-90% by weight)
10% by weight) (Lots 4 to 9) exhibit only a light brown or pale yellow color even when heated at 200° C. for 24 hours, and are excellent in appearance. In particular, as the blending ratio of hydrogenated rosin increased, coloring due to heating decreased.

Example 2 In this example, in order to investigate the uniformity of the quality of solder flux, the compatibility of additives with the base material and the presence or absence of segregation of additives due to heating time were investigated.

1000g of the base containing natural rosin, hydrogenated rosin, and fully hydrogenated rosin at various blending ratios shown in Table 4.
Piperidine hydrobromide and monoethanolamine hydrobutorate, which were produced in the same manner as in the example using the same amount of raw materials, were added to various bases as additives in the same manner as in the first example,
Completed Flux. The compatibility of each flux was visually determined by determining whether the additive was in an opaque dispersion state with respect to the base. If they are completely compatible, they are in a transparent state. On the other hand, regarding segregation, three samples were taken from the top, middle and bottom after heating and a halogen content test was conducted according to JIS Z 3197 (Testing method for resin flux for soldering). The results of this example are shown in Table 4.

Table 4 The symbols in Table 4 are as follows: ◎ indicates that the material remains transparent even after heating, indicating good compatibility and no segregation; ○ indicates that the transparency slightly decreases after heating; Regarding segregation, there is a slight difference in the halogen content between the top and bottom of the sample, but there is no significant difference. △ indicates that the sample becomes cloudy after heating and the halogen content between the top and bottom of the sample is 0. .1% to 0.15% difference, and the X mark indicates that a deposit is formed after heating and that there is a 0.16% to 0.2% difference in halogen content between the top and bottom of the sample. It shows that there is.

As shown in Table 4, the compatibility and segregation results showed the same tendency, and fluxes using bases consisting of 100% by weight of natural rosin or finished hydrogenated rosin (lots 1 or 3) and 10% by weight of hydrogenated rosin. % and fully hydrogenated rosin (Lot 4) has the best compatibility and segregation, but as the proportion of hydrogenated rosin in the base increases, the compatibility and segregation decrease. It was understood that both conditions worsened.

Example 3 100 g of hydrogenated rosin and 90 g of fully hydrogenated rosin
Piperidine hydrobromide (the amount of hydrobromic acid used in its production is 5-25 g) and monoethanolamine hydrobutorate (the amount of ammonium hydrogen fluoride used in its production) is added to 1000 g of a base consisting of 0 g. A flux was prepared in the same manner as in Example 1 using various weights of 0.05 to 8 g) as an additive.

The above piperidine hydrobromide was synthesized using 15 parts by weight of hydrobromic acid to 10 parts of piperidine, and the above monoethanolamine hydrofluoride was synthesized by using 15 parts by weight of hydrobromic acid to 10 parts of piperidine. It was synthesized using ammonium hydrogen hydride IO.

The properties of the various fluxes completed as described above were investigated in terms of spreading, corrosive properties, electrical insulation properties, and voltage application resistance. The characteristic values of flux in Table 5 are JIS Z 3283 (Flux cored solder)
According to JIS Z3197, the flux test method is
(Test method for resin-based flux for soldering). However, the electrical insulation test was conducted at a temperature of 38±2℃ and a relative temperature of 9.
0±5%, 9('I""ayt, 1." of 100v voltage)
°°°″″44”′”°”041 “1-! - Closed.
Figure 1 shows the results.

In Figure 1, the vertical axis is the number of grams of ammonium hydrogen fluoride used in the production of monoethanolamine hydrofluoric acid added to 1000 g of the base, and the horizontal axis is the production of piperidine hydrobromide added to 1000 g of the base. g of hydrobromic acid used for
The meanings of the symbols in FIG. 1 are as shown in Table 5.

(continued on next page) In Table 5, the spread is the result of investigating stainless steel and iron.

That is, the results obtained when the additives were used in the amounts indicated by the values on the vertical and horizontal axes at the locations marked with symbols in FIG. 1 are shown by various symbols in Table 5.

Curves 1 and 2 in FIG. 1 show preferred ranges of the amounts of ammonium hydrogen fluoride and hydrobromic acid used in the production of additives based on flux characteristics, and in the region below curve 1, the amount of additives is Since there is little, the spreading characteristics are poor.
In the region above curve 2, although the spread is good, the amount of additive is too large, which deteriorates properties such as corrosion resistance and electrical insulation, making it unsuitable. i.e. curves 1 and 2
Addition amounts in the region between the two provide good flux properties.

As shown in Figure 1 and Table 5, judging from the various characteristics of the flux, the preferred amount of monoethanolamine hydrofluoride to be added is 8 g for 1000 g of base material consisting of 100 g of hydrogenated rosin and 900 g of fully hydrogenated rosin.
~24g, and a more preferable addition amount is 14~18g
It is. On the other hand, for piperidine hydrobromide, the preferable addition amount for the above base is 17 to 43 g1, and the more preferable addition amount is 20 to 30 g. The most preferable addition amounts for the above base are 4 g of ammonium hydrogen fluoride used in the production of monoethanolamine hydrobutyrate and 15 g of hydrobromic acid used in the production of piperidine hydrobromide. This is the case.

Example 4 100g of hydrogenated rosin and 900g of fully hydrogenated rosin
The scattering of flux was investigated using the following method when hydrobromic acid of various amines was used as an additive to a base consisting of.

Hydrobromide salts of various amines synthesized using 10 g of various amines and 15 g of hydrobromic acid were added to the above base while heating it to about 150° C. to complete a flux. Each sample was made by processing this flux into solder using a conventional method and was tested.

The test method was to fix the soldering iron at a height of 50 mm above the test paper and conduct the soldering iron at a light temperature of 300±20°C and a speed of 20 mm/sec.The results were judged by comparing the scattering distance and amount of scattering. . The results of this example are shown in Table 6.

Table 6 The symbols in Table 6 are: ◎ indicates that the amount of scattering is 50% or more within 50 mm, ○ indicates that the amount of scattering is 50% or more within a radius of 100 mm, △ indicates that the amount of scattering is 50% or more within a radius of 100 mm. This indicates that the amount is 50% or more within a radius of 150 mm, and that the X mark indicates that it will scatter throughout the area.

As shown in Table 6, when aniline is used as the amine, there is little scattering and the results are good, but in this case the color changes when heated. In addition, cyclohexylamine and diethylamine have a strong pungent odor, resulting in poor workability and furthermore, diethylamine is unsatisfactory due to its large amount of scattering. Hydrazine is also defective due to large amount of scattering. For monoethanolamine and piperidine, scattering is almost good, and there is no discoloration due to heating (there is no irritating odor, so they are suitable for actual use.

[Effects of the Invention] According to the inventions of claims 1 to 3, there are provided a flux for solder material and a flux-cored solder that has a light residue after soldering and provides an excellent finish in terms of appearance.

Furthermore, the present invention provides a flux for soldering materials and a cored solder that can be used to solder metals such as iron or nickel that are difficult to solder to, and have good workability with little scattering.

[Brief explanation of the drawing]

FIG. 1 is a graph showing the effect of the amount of additives on soldering flux characteristics in Example 4.

Claims (1)

[Claims] 1. Completely hydrogenated rosin is used as a base, and at least piperidine hydrobromide and monoethanolamine hydrofluoride are added as additives to the base, and the amount of addition is A soldering flux characterized in that both amounts are in a range of 1 part by weight or more and 100 parts by weight or less based on 1000 parts by weight of the base. 2. Mainly composed of fully hydrogenated rosin and hydrogenated rosin obtained by incompletely hydrogenating rosin, the proportion of the fully hydrogenated rosin is 25% by weight or more based on the total weight of the rosin, and the remainder is hydrogenated rosin. A certain base is used, and at least piperidine hydrobromide and monoethanolamine hydrofluoride are added as additives to the base, and the amounts of both are based on 1000 parts by weight of the base. A soldering flux characterized by being in a range of 1 part by weight or more and 100 parts by weight or less. 3. A flux-cored solder in which flux is embedded in the core portion of the solder, wherein the flux is the one according to claim 1 or claim 2.