CN103757669A - Electrolytic tinning liquid - Google Patents
Electrolytic tinning liquid Download PDFInfo
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- CN103757669A CN103757669A CN201410028502.5A CN201410028502A CN103757669A CN 103757669 A CN103757669 A CN 103757669A CN 201410028502 A CN201410028502 A CN 201410028502A CN 103757669 A CN103757669 A CN 103757669A
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Abstract
The invention discloses electrolytic tinning liquid, which comprises the following raw material components: (A) stannous salt of which the stannous tin ion concentration is 1-100g/L, (B) acid of which the total concentration is 10-200g/L, (C) a surfactant selected from one or more of nonionic surfactants of which the structural formula are as follows: R1COO(C2H4O)nH and R2S(C2H4O)mH, being 1-20g/L in the total concentration, (D) a current dispersing agent which is selected from an unsaturated bond-containing dicarboxylic acid derivative or a salt thereof and is 0.01-2g/L in concentration, (E) conducting salt of which the concentration is 2-10g/L, and (F) a pH regulating agent for regulating the pH value of the electrolytic tinning liquid to 2.0-4.0. By adopting the electrolytic tinning liquid, the current distribution among steel balls, electronic elements and conducting balls in an electrolytic tinning drum can be optimized, the steel balls and the electronic elements are prevented from being bonded on the conducting balls by means of electroplating, and the quality of electrolytic tinning products is improved.
Description
Technical field
The present invention relates to eleetrotinplate technical field, particularly relate to a kind of plating tin liquor that can improve eleetrotinplate distribution of current.
Background technology
Along with the development of electronics, size is little, multi-functional, high-performance, the development trend that becomes electronic component easy to operate.For being welded on equipment that electronic devices and components are more prone to, need on electronic component, carry out zinc-plated to improve weldability.Because the size of electronic component is less, than being easier to occur two coherent problems of components and parts, be called for short " duplex ", below with " duplex ", replace.The generation of duplex has significantly reduced the qualification rate of product, and the duplex rate (amount of duplex product is than product population) that adopts traditionally stannous sulfate to electroplate is very high.There is document to disclose under the sub-tin system of thionamic acid for this reason, adopt a kind of as complexing agent of the salt of citric acid, glyconic acid, tetra-sodium, enanthic acid, oxysuccinic acid and glucono-lactone, and a kind of HLB is greater than 10 tensio-active agent for improving the duplex rate of electronic component.
There is document to disclose employing mineral acid and organic acid and salt thereof, and add tungsten salt, molybdenum salt and manganese salt to reduce the growth of tin palpus.Also by the plating tin liquor of bibliographical information, do not use complexing agent, in pH value, adopt acid, N, N bis-polyoxyalkylenes-N-alkylamine, amine oxide or mixture in lower than 1 solution, and antioxidant, prevent that stannous ion is oxidized.But the too low meeting of pH value of this plating mode causes corrosion to equipment component.
Although above-mentioned prior art has solved the duplex problem of electronic component, but in eleetrotinplate process, especially in barrel plating process, the distribution of electric current is very inhomogeneous, cathode terminal (being generally conducting sphere) electric current is around large, apart from conducting sphere steel ball far away and electronic component because resistance and barrel plating staving are long-pending, electric current is relatively little.Therefore cause steel ball and electronic component eleetrotinplate speed near conducting sphere, be easily deposited in together and be bonded on conducting sphere, form " caking ", and the inner electronic component that lumps fails all to cover tin.The caking of conducting sphere and steel ball, electronic component, causes the decline of yield rate, and may occur that the product of empty plating flows in salable product, and the possibility that empty plated product is chosen is almost nil, causes serious product hidden danger.And the unhomogeneity of electric current has caused the thickness of product to have fluctuation to a certain extent, has reduced the consistence of product.
For improving steel ball and electronic component near conducting sphere, pile up the problem of adhesion, the homogeneity of electronic component thickness of coating in increasing batch, thus the appearance without zinc-plated defective products stopped, and the present invention has carried out a large amount of tensio-active agents, additive is tested, optimize distribution of current, reduce the gradient of electric current.
Summary of the invention
Based on this, the object of this invention is to provide a kind of plating tin liquor that can improve eleetrotinplate distribution of current.
Concrete technical scheme is as follows:
A plating tin liquor, comprises following feed composition:
(A) tin salt, the concentration of stannous ion is 1-100g/L;
(B) acid: one or more in organic acid, mineral acid, the total concn of acid is 10-200g/L;
(C) tensio-active agent: structural formula is R
1cOO (C
2h
4o)
nh, R
2s(C
2h
4o)
mone or more in the nonionogenic tenside of H, the total concn of tensio-active agent is 1-20g/L, wherein R
1, R
2for C
4-C
20alkyl, the integer that n, m are 4-12;
(D) electric current dispersion agent: containing di-carboxylic acid analog derivative or its salt of unsaturated link(age), concentration is 0.01-2g/L;
(E) conducting salt, concentration is 2-10g/L;
(F) pH adjusting agent, regulating the pH value of plating tin liquor is 2.0-4.0.
In an embodiment, comprise following feed composition therein:
(A) tin salt, the concentration of stannous ion is 5-20g/L;
(B) acid: one or more in organic acid, mineral acid, the total concn of acid is 10-100g/L;
(C) tensio-active agent: structural formula is R
1cOO (C
2h
4o)
nh, R
2s(C
2h
4o)
mone or more in the nonionogenic tenside of H, the total concn of tensio-active agent is 1-10g/L, wherein R
1, R
2for C
4-C
20alkyl, the integer that n, m are 4-12;
(D) electric current dispersion agent: containing di-carboxylic acid analog derivative or its salt of unsaturated link(age), concentration is 0.01-0.5g/L;
(E) conducting salt, concentration is 10g/L;
(F) pH adjusting agent, regulating the pH value of plating tin liquor is 3.0-3.5.
In an embodiment, the structural formula of the described di-carboxylic acid analog derivative containing unsaturated link(age) is therein
r wherein
3for CH
2=or H (CH
2)
xcH=, R
4for (CH
2)
y, the integer that x is 1-8, the integer that y is 1-4.
In an embodiment, the described di-carboxylic acid analog derivative containing unsaturated link(age) is 2-ethylene pentanedioic acid, 2-trimethylene pentanedioic acid or 2-trimethylene succinic acid therein.
In an embodiment, described tensio-active agent is sad polyoxyethylene ester therein, one or more in valeric acid polyoxyethylene ester, lauric acid polyoxyethylene ester, octane polyoxyethylene thioalcohol, lauryl mercaptan Soxylat A 25-7 or stearylmercaptan Soxylat A 25-7.
In an embodiment, described tin salt is for replacing or unsubstituted alkyl or the sub-tin of silane alcohol base sulfonic acid therein.
In an embodiment, described tin salt is the sub-tin of stannous methanesulfonate or ethylsulfonic acid therein.
In an embodiment, described organic acid is for replacing or unsubstituted alkyl or silane alcohol base sulfonic acid therein; Described mineral acid is sulfuric acid or hydrochloric acid.
In an embodiment, described organic acid is methylsulphonic acid or ethylsulfonic acid therein.
In an embodiment, described conducting salt is novalgin, methylsulphonic acid potassium, ethylsulfonic acid sodium, ethylsulfonic acid potassium, sodium sulfocarbolate or sulfonaphthol sodium therein; Described pH value conditioning agent is highly basic.
Principle of the present invention and advantage are as follows:
Plating tin liquor of the present invention contains unsaturated link(age) di-carboxylic acid analog derivative by employing is as electric current dispersion agent and the tensio-active agent that is different from prior art, can optimize steel ball in eleetrotinplate cylinder, electronic component to the distribution of current between conducting sphere, stop steel ball, the plating of electronic component bonding on conducting sphere, improve the quality of eleetrotinplate product.
The action principle that the present invention electroplates each component of tin liquor is described below:
(A) stannous ion: stannous ion provides tin ion at Tin plating electrolyte, preferably adopt organic acid tin salt, comprise that the sub-tin of stannous methanesulfonate, ethylsulfonic acid etc. replaces or unsubstituted alkyl or the sub-tin of silane alcohol base sulfonic acid, stannous methanesulfonate particularly preferably, content is (with Sn
2+content meter, g/L) is 1-100g/L, preferably 1-20g/L, particularly preferably 13g/L.
(B) acid: the effect of acid is to regulate pH, adjusts the dissolution rate of anode metal block tin.Suitable acid comprises mineral acid and organic acid, and mineral acid comprises sulfuric acid, hydrochloric acid; Organic acid comprises methylsulphonic acid, ethylsulfonic acid etc. and replaces or unsubstituted alkyl or silane alcohol base sulfonic acid.Methylsulphonic acid particularly preferably, the content of methylsulphonic acid is 10-200g/L, is particularly preferably 10-100g/L.
(C) tensio-active agent: selected fatty acid polyoxyethylene ester or senior polyoxyethylene thioalcohol, fatty acid polyethylene ester or senior polyoxyethylene thioalcohol polarize for increasing as tensio-active agent Main Function in solution, strengthen the wetting property of electronic component, content is 1-20g/L, be preferably 1-10g/L, the too high levels of tensio-active agent can cause soltion viscosity to increase, and increases the duplex probability of product electronic component, and too low to increase polarization effect not obvious.Senior polyoxyethylene thioalcohol ratio is easier to same metallic tin and Sn
2+produce conjugative effect, intensifier electrode polarization, plays increase nucleus formation speed, controls eleetrotinplate layer crystalline orientation.Being used in conjunction with of polyoxyethylene carboxylate and senior polyoxyethylene thioalcohol can make high current density region and low current density district obtain uniform coating simultaneously.
Polyoxyethylene carboxylate (the C that can select
1, R
1cOO (C
2h
4o)
nh, R
1fatty acid carbons atomicity is 4-20,20>=n>=4), sad polyoxyethylene ester for example, valeric acid polyoxyethylene ester etc.
Senior polyoxyethylene thioalcohol (C
2, R
2s(C
2h
4o)
mh, 12>=m>=4, R
2carbonatoms be 4-20), such as octane polyoxyethylene thioalcohol etc.
(D) electric current dispersion agent: the di-carboxylic acid analog derivative that contains unsaturated link(age) or its salt, its structural formula is as follows
r wherein
3for CH
2=or H (CH
2)
xcH=(integer that x is 1-8), R
4for (CH
2)
y(integer that y is 1-4).
The effect of electric current dispersion agent in electroplate liquid is very obvious, unsaturated link(age) and di-carboxylic acid contained in its result can produce conjugative effect in electroplating process, reduce the volts lost of electroplating element, steel ball in cylinder, electronic component be can optimize to the distribution of current between conducting sphere, steel ball, the plating of electronic component bonding stopped on conducting sphere.Its content is 0.01-2g/L, is preferably 0.01-0.5g/L.Within the content of electric current dispersion agent need to be controlled at suitable scope, the conjugation of electric current dispersion agent is conducive to the nucleation in electroplating process, and higher electric current dispersion agent can cause the bonding rate of product slightly to raise.
(E) conducting salt: be mainly novalgin, methylsulphonic acid potassium, ethylsulfonic acid sodium, ethylsulfonic acid potassium,, sodium sulfocarbolate, sulfonaphthol sodium etc.
(F) pH value conditioning agent, is mainly highly basic, and pH value is controlled at 2.0-4.0, and particularly preferably 3.0-3.5 can guarantee the quality of coating and prevent Sn under this pH value
2+be oxidized, can also reduce the corrosion to equipment; Electroplating temperature is controlled between 24-26.
Can use the electronic component of plating solution of the present invention to comprise, patch capacitor, Chip-R, chip inductor, paster fuse, quartz (controlled) oscillator, LC strainer, porcelain filter, retarding line, SAW strainer and other functional element, rly. safety fuse, optics and other contact members.
Plating mode: the applicable plating scope of this electroplate liquid is that the zinc-plated class of tin barrel plating, low speed has the dumb light of weldability requirement zinc-plated to coating.
Accompanying drawing explanation
Fig. 1 is the position of the schematic diagram of patch capacitor and C1, C2, C3;
Fig. 2 is the scanning electron microscope picture of embodiment 1 product;
Fig. 3 is the scanning electron microscope picture of comparative example 7 products;
Fig. 4 be HullCell plating sheet schematic diagram (is bright district,
for scorch region).
Embodiment
By the following examples the application is further elaborated.
Embodiment 1
A kind of plating tin liquor of the present embodiment, comprises following feed composition:
(A) tin salt: stannous methanesulfonate, the concentration of stannous ion is 13g/L;
(B) acid: methylsulphonic acid, concentration is 50g/L;
(C) tensio-active agent: lauric acid polyoxyethylene ((C
2h
4o)
10) ester, concentration is 10g/L;
(D) electric current dispersion agent: 2-ethylene pentanedioic acid, concentration is 0.01g/L;
(E) conducting salt: sodium sulfocarbolate, concentration is 10g/L;
(F) pH adjusting agent: KOH adjusts pH value to 3.2.
Electroplating process is as follows:
1, press the preparation of above-mentioned raw materials proportioning and electroplate tin liquor;
2, adopt filter (filter core is no more than 5 μ m) and refrigerator to plating solution filter, circulation, freezing;
3, control the ratio of steel ball and plating piece;
4, rack plating, barrel plating metal nickel dam;
5, rack plating, barrel plating metallic tin layer.
On the Chip-R of nickel plating, in 150L solution, carry out under the following conditions tin barrel plating, and product is evaluated.
Electroplate object: Chip-R; Cylinder: 4.5L
Rotating speed: 60 turn/min
Nickel plating: 31A; 120min
Zinc-plated: 12A; 90min
Chip-R: 0603 type; 2.8K Ω; 1.5Kg
Steel ball: diameter 0.5-0.7mm; 2.0Kg
Assessment item:
1, whether steel ball exists and piles up adhesion Chip-R and steel ball;
2, magnitude of voltage;
Be recorded in the situation of 12A electric current plating registration during voltage stabilization;
3, thickness of coating (X-ray test)
Adopt X-ray thickness tester, get 30pcs sample test end electrode C1, C2, the thickness of C3 face, as shown in Figure 1, and averages;
4, weldability test
Get at random 30pcs, first 85 ℃ are steamed 8h, then carry out reflow(Reflow Soldering) test
5, HullCell test
Adopt 0.5A electric current, 250mL solution testing, records the scope in bright district and sub-bright district, represents, as shown in Figure 4 with cm;
The product plating out has been carried out to sem test (as shown in Figure 2), and coating is dense, and particle is between 3-4 μ m.
Embodiment 2-11
The raw material of the plating tin liquor of embodiment 2-11 forms as shown in table 1, and plating condition and test event are identical with embodiment 1, and result is as following table:
Table 1
Δ represents that test result is good; X represents that test result is bad; Bonding rate is less represents that yield rate is higher, generally require to be no more than 10%; HullCell test result represents the length in light and sub-bright district, and bright district and the sub-bright district larger expression current window of scope are wider; Thickness of coating scope is qualified at 4-10 μ m, and C1, C2, that C3 thickness approaches expression covering power is better; Voltage is qualified lower than 1/2 of current value, the lower expression energy consumption of voltage less (voltage is lower than 6V).
Contrast by embodiment 1-11 can be found, embodiment 3 and 4 has the phenomenon that lower voltage, conducting sphere do not have generation and electronic component and steel ball caking, thickness homogeneous, have good weldability, bonding rate is lower, have good covering performance in HullCell test.Embodiment 7, because electric current dispersant is slightly high, has increased slightly with respect to embodiment 4 product bonding rates, and embodiment 10 is except electric current dispersant is slightly high compared with embodiment 4, and surfactant content is also slightly high, causes product bonding rate slightly high.Coating duplex (bonding rate) is larger with the relation with contents of tensio-active agent, and the too high or too low duplex rate that all can cause of surfactant content improves.The surfactant content surfactant content higher, embodiment 11 of embodiment 2,3 is on the low side, so duplex is all higher, but still within acceptability limit.It is larger that weldability is affected by coating morphology mainly, and surface topography and tensio-active agent, electric current dispersion agent and conductive agent have relation, and wherein embodiment 11 causes weldability variation because surfactant content is on the low side.HullCell result mainly reflects current window size, affected by tensio-active agent, acid and conductive agent content, and wherein, surfactant content is too high, causes range of current to narrow down, and conducting salt and sour too high levels also can cause range of current to narrow down.
Voltage is mainly subject to the concentration affects of tensio-active agent, conducting salt and the acid of solution, and meeting that conducting salt and acid concentration are on the low side causes voltage to raise, and surfactant concentration is too high, easily causes voltage higher.
Comparative example 1-11
The raw material of the plating tin liquor of comparative example 1-11 forms as shown in table 2, and plating condition and test event are identical with embodiment 1, and result is as following table:
Table 2
Comparative example adopts benzylideneacetone, technical gelatine, vinylformic acid and 2-methylglutaric acid as electric current dispersion agent, naphthols polyoxyethylene ((EO)
n, n is 9-15) and ether, lauryl alcohol polyoxypropylene ((PO)
nn is 9-15) ether and fatty alcohol-polyoxyethylene ether (AEO-9) be as tensio-active agent, the poor-performing of comparative example 1-11 anti-conducting sphere adhesion steel ball and Chip-R, range of current is narrower, scorch region is excessive, wherein the duplex of comparative example 4,5 is too high, and this is higher relevant with the concentration of tensio-active agent.The weldability of comparative example 7 is bad, and scanning electron microscope picture (as shown in Figure 3) can find that particle size is larger, greatly about 4-6 μ m, and there is more space, similar simple stacked form, easily causes weldability bad, and this is lower relevant with the concentration of tensio-active agent.Comparative example 10 is used vinylformic acid as additive, by contrast, find that it can not play the effect that reduces conducting sphere adhesion steel ball and Chip-R, and its use range is that sour environment pH is lower than 1, and under this scope, in comparative example 10, add after vinylformic acid in HullCell test light and sub-bright district less, show to use range of current narrow.In comparative example 11, adopt 2-methylglutaric acid as electric current dispersion agent, test result can find, 2-methylglutaric acid can not play the effect that prevents conducting sphere adhesion steel ball and Chip-R.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. electroplate a tin liquor, it is characterized in that, comprise following feed composition:
(A) tin salt, the concentration of stannous ion is 1-100g/L;
(B) acid: one or more in organic acid, mineral acid, the total concn of acid is 10-200g/L;
(C) tensio-active agent: structural formula is R
1cOO (C
2h
4o)
nh, R
2s(C
2h
4o)
mone or more in the nonionogenic tenside of H, the total concn of tensio-active agent is 1-20g/L, wherein R
1, R
2for C
4-C
20alkyl, the integer that n, m are 4-12;
(D) electric current dispersion agent: containing di-carboxylic acid analog derivative or its salt of unsaturated link(age), concentration is 0.01-2g/L;
(E) conducting salt, concentration is 2-10g/L;
(F) pH adjusting agent, regulating the pH value of plating tin liquor is 2.0-4.0.
2. plating tin liquor according to claim 1, is characterized in that, comprises following feed composition:
(A) tin salt, the concentration of stannous ion is 5-20g/L;
(B) acid: one or more in organic acid, mineral acid, the total concn of acid is 10-100g/L;
(C) tensio-active agent: structural formula is R
1cOO (C
2h
4o)
nh, R
2s(C
2h
4o)
mone or more in the nonionogenic tenside of H, the total concn of tensio-active agent is 1-10g/L, wherein R
1, R
2for C
4-C
20alkyl, the integer that n, m are 4-12;
(D) electric current dispersion agent: containing di-carboxylic acid analog derivative or its salt of unsaturated link(age), concentration is 0.01-0.5g/L;
(E) conducting salt, concentration is 10g/L;
(F) pH adjusting agent, regulating the pH value of plating tin liquor is 3.0-3.5.
3. plating tin liquor according to claim 1 and 2, is characterized in that, the structural formula of the described di-carboxylic acid analog derivative containing unsaturated link(age) is
r wherein
3for CH
2=, H (CH
2)
xcH=, R
4for (CH
2)
y, the integer that x is 1-8, the integer that y is 1-4.
4. according to the plating tin liquor of claim 3, it is characterized in that, the described di-carboxylic acid analog derivative containing unsaturated link(age) is 2-ethylene pentanedioic acid, 2-trimethylene pentanedioic acid or 2-trimethylene succinic acid.
5. plating tin liquor according to claim 1 and 2, it is characterized in that, described tensio-active agent is sad polyoxyethylene ester, one or more in valeric acid polyoxyethylene ester, lauric acid polyoxyethylene ester, octane polyoxyethylene thioalcohol, lauryl mercaptan Soxylat A 25-7 or stearylmercaptan Soxylat A 25-7.
6. plating tin liquor according to claim 1 and 2, is characterized in that, described tin salt is for replacing or unsubstituted alkyl or the sub-tin of silane alcohol base sulfonic acid.
7. plating tin liquor according to claim 6, is characterized in that, described tin salt is the sub-tin of stannous methanesulfonate or ethylsulfonic acid.
8. plating tin liquor according to claim 1 and 2, is characterized in that, described organic acid is for replacing or unsubstituted alkyl or silane alcohol base sulfonic acid; Described mineral acid is sulfuric acid or hydrochloric acid.
9. plating tin liquor according to claim 8, is characterized in that, described organic acid is methylsulphonic acid or ethylsulfonic acid.
10. plating tin liquor according to claim 1 and 2, is characterized in that, described conducting salt is novalgin, methylsulphonic acid potassium, ethylsulfonic acid sodium, ethylsulfonic acid potassium, sodium sulfocarbolate or sulfonaphthol sodium; Described pH value conditioning agent is highly basic.
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