CN103757669B - Electroplate tin liquor - Google Patents
Electroplate tin liquor Download PDFInfo
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- CN103757669B CN103757669B CN201410028502.5A CN201410028502A CN103757669B CN 103757669 B CN103757669 B CN 103757669B CN 201410028502 A CN201410028502 A CN 201410028502A CN 103757669 B CN103757669 B CN 103757669B
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Abstract
The invention discloses a kind of tin liquor of electroplating, comprise following raw material components: (A) tin salt, the concentration of stannous ion is 1-100g/L; (B) acid: the total concentration of acid is 10-200g/L; (C) surfactant: structural formula is R1COO(C2H4O)nH、R2S(C2H4O)mOne or more in the non-ionic surface active agent of H, the total concentration of surfactant is 1-20g/L; (D) electric current dispersant: containing dicarboxylic acids analog derivative or its salt of unsaturated bond, 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. Plating tin liquor of the present invention can be optimized steel ball in electrotinning cylinder, electronic component to the CURRENT DISTRIBUTION between conducting sphere, stops steel ball, the plating of electronic component bonding on conducting sphere, improves the quality of electrotinning product.
Description
Technical field
The present invention relates to electrotinning technical field, particularly relate to a kind of electricity that can improve electrotinning CURRENT DISTRIBUTIONTin plating electrolyte.
Background technology
Along with the development of electronic equipment, size is little, multi-functional, high-performance, the electronic component that becomes easy to operateDevelopment trend. For being welded on equipment that electronic devices and components are more prone to, need to be enterprising at electronic componentRow is zinc-plated to improve solderability. Because the size of electronic component is less, more sticky than being easier to that two components and parts occurProblem together, is called for short " duplex ", below replaces with " duplex ". The generation of duplex has significantly reduced productThe qualification rate of product, the duplex rate (amount of duplex product is than product population) that adopts traditionally stannous sulfate to electroplateVery high. Have document to disclose under the sub-tin system of sulfamic acid for this reason, adopt citric acid, gluconic acid, pyrophosphoric acid,The salt of enanthic acid, malic acid and the one of gluconolactone be as complexing agent, and a kind of HLB table of being greater than 10Surface-active agent is for improving the duplex rate of electronic component.
There is document to disclose employing inorganic acid and organic acid and salt thereof, and add tungsten salt, molybdenum salt and manganese saltTo reduce the growth of tin palpus. Also do not use complexing agent by the plating tin liquor of bibliographical information, in pH value lower than 1In solution, adopt acid, N, N bis-polyoxyalkylenes-N-alkylamine, amine oxide or mixture, 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, in electrotinning process, especiallyThe distribution that is electric current in barrel plating process is very inhomogeneous, and 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 relativeLittle. Therefore cause near the steel ball of conducting sphere and electronic component electrotinning speed, be easily deposited in together alsoBe bonded on conducting sphere, form " caking ", and the inner electronic component that lumps fails all to cover tin. Conducting sphereWith the caking of steel ball, electronic component, cause the decline of yield rate, and the product that may occur empty plating flows into and closesIn lattice product, the possibility that empty plated product is chosen is almost nil, causes serious product hidden danger. And electric currentInhomogeneity caused the thickness of product to have fluctuation to a certain extent, reduced the uniformity of product.
Pile up the problem of adhesion for improving steel ball and electronic component near conducting sphere, electronic component in increasing batchThe uniformity of thickness of coating, thus the appearance without zinc-plated defective products stopped, and the present invention has carried out a large amount of surfacesActivating agent, additive test, optimize CURRENT DISTRIBUTION, reduces 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 electrotinning CURRENT DISTRIBUTION.
Concrete technical scheme is as follows:
A kind of tin liquor of electroplating, comprises following raw material components:
(A) tin salt, the concentration of stannous ion is 1-100g/L;
(B) acid: one or more in organic acid, inorganic acid, the total concentration of acid is 10-200g/L;
(C) surfactant: structural formula is R1COO(C2H4O)nH、R2S(C2H4O)mThe nonionic of HOne or more in surfactant, the total concentration of surfactant is 1-20g/L, wherein R1、R2ForC4-C20Alkyl, the integer that n, m are 4-12;
(D) electric current dispersant: containing dicarboxylic acids analog derivative or its salt of unsaturated bond, concentration is0.01-2g/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 raw material components therein:
(A) tin salt, the concentration of stannous ion is 5-20g/L;
(B) acid: one or more in organic acid, inorganic acid, the total concentration of acid is 10-100g/L;
(C) surfactant: structural formula is R1COO(C2H4O)nH、R2S(C2H4O)mThe nonionic of HOne or more in surfactant, the total concentration of surfactant is 1-10g/L, wherein R1、R2ForC4-C20Alkyl, the integer that n, m are 4-12;
(D) electric current dispersant: containing dicarboxylic acids analog derivative or its salt of unsaturated bond, concentration is0.01-0.5g/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 dicarboxylic acids analog derivative containing unsaturated bond is thereinWherein R3For CH2=or H (CH2)xCH=，R4For (CH2)y，xFor the integer of 1-8, the integer that y is 1-4.
In an embodiment, the described dicarboxylic acids analog derivative containing unsaturated bond is 2-ethylene penta 2 thereinAcid, 2-trimethylene glutaric acid or 2-trimethylene succinic acid.
In an embodiment, described surfactant is sad polyoxyethylene ester, valeric acid polyoxyethylene thereinEster, laurate polyoxyethylene ester, octane polyoxyethylene thioalcohol, lauryl mercaptan APEO or 18 sulphurOne or more in alcohol APEO.
In an embodiment, described tin salt is for replacing or unsubstituted alkyl or silane alcohol base sulfonic acid Asia thereinTin.
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 inorganic acid is sulfuric acid or hydrochloric acid.
In an embodiment, described organic acid is pyrovinic acid or ethylsulfonic acid therein.
In an embodiment, described conducting salt is novalgin, pyrovinic acid potassium, ethylsulfonic acid thereinSodium, ethylsulfonic acid potassium, sodium phenolsulfonate or naphtholsulfonic acid sodium; Described pH value conditioning agent is highly basic.
Principle of the present invention and advantage are as follows:
The dicarboxylic acids analog derivative that plating tin liquor of the present invention contains unsaturated bond by employing disperses as electric currentAgent and be different from the surfactant of prior art, can optimize steel ball, electronic component in electrotinning cylinderTo the CURRENT DISTRIBUTION between conducting sphere, stop steel ball, the plating of electronic component bonding on conducting sphere, improve electricityThe quality of tin-plated product.
The action principle that the present invention electroplates the each component of tin liquor is described below:
(A) stannous ion: stannous ion provides tin ion at Tin plating electrolyte, preferably adopts the sub-tin of organic acidSalt, comprises that stannous methanesulfonate, the sub-tin of ethylsulfonic acid etc. replace or unsubstituted alkyl or silane alcohol base sulphurThe sub-tin of acid, particularly preferably stannous methanesulfonate, content is (with Sn2+Content meter, g/L) be 1-100g/L, preferably1-20g/L, particularly preferably 13g/L.
(B) acid: the effect of acid is to regulate pH, adjusts the dissolution velocity of anode metal block tin. Suitable acid comprisesInorganic acid and organic acid, inorganic acid comprises sulfuric acid, hydrochloric acid; Organic acid comprises pyrovinic acid, ethylsulfonic acid etc.Replace or unsubstituted alkyl or silane alcohol base sulfonic acid. Particularly preferably pyrovinic acid, the content of pyrovinic acidFor 10-200g/L, be particularly preferably 10-100g/L.
(C) surfactant: selected fatty acid polyoxyethylene ester or senior polyoxyethylene thioalcohol, fatty acid polyglycolVinyl acetate or senior polyoxyethylene thioalcohol polarize for increasing as surfactant Main Function in solution,The wellability that strengthens electronic component, content is 1-20g/L, is preferably 1-10g/L, the content mistake of surfactantHeight can cause solution viscosity to increase, and increases the duplex probability of product electronic component, the too low polarization effect that increasesFruit is not obvious. Senior polyoxyethylene thioalcohol ratio is easier to same metallic tin and Sn2+Produce conjugation, strengthenElectrode polarization, plays increase nucleus formation speed, controls electrotinning layer crystal orientation. Aliphatic acid polyethenoxyBeing used in conjunction with of ester and senior polyoxyethylene thioalcohol can make high current density region and low current density district simultaneouslyObtain uniform coating.
Polyoxyethylene carboxylate (the C that can select1，R1COO(C2H4O)nH，R1Fatty acid carbons atomicityFor 4-20,20 >=n >=4), for example sad polyoxyethylene ester, valeric acid polyoxyethylene ester etc.
Senior polyoxyethylene thioalcohol (C2，R2S(C2H4O)mH,12≥m≥4,R2Carbon number be 4-20),Such as octane polyoxyethylene thioalcohol etc.
(D) electric current dispersant: the dicarboxylic acids analog derivative that contains unsaturated bond or its salt, its structural formula is as followsShown inWherein R3For CH2=or H (CH2)xCH=(integer that x is 1-8),R4For (CH2)y(integer that y is 1-4).
The effect of electric current dispersant in electroplate liquid is very obvious, contained unsaturated bond and two in its resultUnit's carboxylic acid can produce conjugation in electroplating process, reduces the voltage drop of electroplating element, can optimize and rollIn cylinder, steel ball, electronic component, to the CURRENT DISTRIBUTION between conducting sphere, are stopped steel ball, the plating of electronic component bondingOn conducting sphere. Its content is 0.01-2g/L, is preferably 0.01-0.5g/L. The content of electric current dispersant needsWithin being controlled at suitable scope, the conjugation of electric current dispersant is conducive to the nucleation in electroplating process, andHigher electric current dispersant can cause the bonding rate of product slightly to raise.
(E) conducting salt: be mainly novalgin, pyrovinic acid potassium, ethylsulfonic acid sodium, ethylsulfonic acid potassium,,Sodium phenolsulfonate, naphtholsulfonic acid sodium etc.
(F) pH value conditioning agent, is mainly highly basic, and pH value is controlled at 2.0-4.0, particularly preferably 3.0-3.5,This pH value is lower can be ensured the quality of coating and prevent Sn2+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 filter, ceramic filter, delay line, SAW filter,And other functional element, relay fuse, optics and other contact elements.
Plating mode: the applicable plating scope of this electroplate liquid is that the zinc-plated class of tin barrel plating, low speed has and can weld coatingProperty require dumb light zinc-plated.
Brief description of the drawings
Fig. 1 is the position of the schematic diagram of patch capacitor and C1, C2, C3;
Fig. 2 is the ESEM picture of embodiment 1 product;
Fig. 3 is the ESEM picture of comparative example 7 products;
Fig. 4 be HullCell plating sheet schematic diagram (is bright district,For scorch region).
Detailed description of the invention
By the following examples the application is further elaborated.
Embodiment 1
A kind of tin liquor of electroplating of the present embodiment, comprises following raw material components:
(A) tin salt: stannous methanesulfonate, the concentration of stannous ion is 13g/L;
(B) acid: pyrovinic acid, concentration is 50g/L;
(C) surfactant: laurate polyoxyethylene ((C2H4O)10) ester, concentration is 10g/L;
(D) electric current dispersant: 2-ethylene glutaric acid, concentration is 0.01g/L;
(E) conducting salt: sodium phenolsulfonate, 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 be 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 to producingProduct are 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 when voltage stabilization;
3, thickness of coating (X-ray test)
Adopt X-ray calibrator, get 30pcs sample test termination electrode C1, C2, the thickness of C3 face, as figureShown in 1, and average;
4, solderability test
Get at random 30pcs, first 85 DEG C 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, with cmRepresent, as shown in Figure 4;
The product plating out has been carried out to sem test (as shown in Figure 2), and coating is dense, and particle existsBetween 3-4 μ m.
Embodiment 2-11
The raw material composition of the plating tin liquor of embodiment 2-11 is as shown in table 1, plating condition and test event and realityExecute example 1 identical, 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,Light 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,C1, C2, that C3 thickness approaches expression covering power is better; Voltage is qualified lower than 1/2 of current value, electricityPress lower expression energy consumption less (voltage is lower than 6V).
Contrast by embodiment 1-11 can find, embodiment 3 and 4 has lower voltage, conducting sphereThere is no the phenomenon of generation and electronic component and steel ball caking, thickness homogeneous, there is good solderability, bondingRate is lower, HullCell has good covering performance in testing. Embodiment 7 is because electric current dispersant containsMeasure slightly highly, have increased slightly with respect to embodiment 4 product bonding rates, and embodiment 10 contains except electric current dispersantMeasure slightly high compared with embodiment 4 outside, surface-active contents is also slightly high, causes product bonding rate slightly high. Coating is twoConnection (bonding rate) is larger with the relation with contents of surfactant, and surface-active contents is too high or too low all canCause duplex rate to improve. The surface-active contents of embodiment 2,3 is higher, the surface-active of embodiment 11Agent content is on the low side, and therefore duplex is all higher, but still within acceptability limit. Solderability is mainly subject to coating shapeLooks impact is larger, and surface topography and surfactant, electric current dispersant and conductive agent have relation, wherein implementsExample 11 causes solderability variation because surface-active contents is on the low side. HullCell result mainly reflects current windowMouth size, is affected by surfactant, acid and conductive agent content mainly, wherein, and surface-active contents mistakeHeight, causes current range to narrow, and conducting salt and sour too high levels also can cause current range to narrow.
Voltage is mainly subject to concentration affects, conducting salt and the acid concentration of surfactant, conducting salt and the acid of solutionMeeting 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 composition of the plating tin liquor of comparative example 1-11 is as shown in table 2, plating condition and test event and realityExecute example 1 identical, result is as following table:
Table 2
Comparative example adopts benzylideneacetone, industrial gelatine, acrylic acid and 2-methylglutaric acid as electric current dispersant,Naphthols polyoxyethylene ((EO)n, n is 9-15) and ether, laruyl alcohol polyoxypropylene ((PO)n, n is 9-15) and ether and fatAlcohol APEO (AEO-9) is as surfactant, comparative example 1-11 anti-conducting sphere adhesion steel ball and paster electricityThe poor-performing of resistance, current range is narrower, and scorch region is excessive, and wherein the duplex of comparative example 4,5 is too high, thisHigher relevant with the concentration of surfactant. The solderability of comparative example 7 is bad, and ESEM picture is (as Fig. 3Shown in) can find that particle size is larger, greatly about 4-6 μ m, and there is more space, similar simple heapLong-pending form, easily causes solderability bad, and this is lower relevant with the concentration of surfactant. Comparative example 10 makesAs additive, find that by contrast it can not play reduction conducting sphere adhesion steel ball and paster electricity with acrylic acidThe effect of resistance, and its scope of application be sour environment pH lower than 1, and under this scope, comparative example 10In add after acrylic acid in HullCell test light and sub-bright district less, show to use current range comparisonNarrow. In comparative example 11, adopt 2-methylglutaric acid as electric current dispersant, test result can be found, 2-firstBase glutaric 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 this areaThose of ordinary skill, without departing from the inventive concept of the premise, can also make some distortion andImprove, these all belong to protection scope of the present invention. Therefore, the protection domain of patent of the present invention should be with appendedClaim is as the criterion.
Claims (6)
1. electroplate a tin liquor, it is characterized in that, comprise following raw material components:
(A) tin salt, the concentration of stannous ion is 1-100g/L;
(B) acid: one or more in organic acid, inorganic acid, the total concentration of acid is 10-200g/L;
(C) surfactant: structural formula is R1COO(C2H4O)nH、R2S(C2H4O)mThe nonionic of HOne or more in surfactant, the total concentration of surfactant is 1-20g/L, wherein R1、R2ForC4-C20Alkyl, the integer that n, m are 4-12;
(D) electric current dispersant: containing dicarboxylic acids analog derivative or its salt of unsaturated bond, concentration is0.01-2g/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;
The structural formula of the described dicarboxylic acids analog derivative containing unsaturated bond isWherein R3For CH2＝、H(CH2)xCH＝，R4For (CH2)y，xFor the integer of 1-8, the integer that y is 1-4;
Described tin salt is for replacing or unsubstituted alkyl or the sub-tin of silane alcohol base sulfonic acid;
Described organic acid is for replacing or unsubstituted alkyl or silane alcohol base sulfonic acid; Described inorganic acid is sulfuric acid or saltAcid;
Described conducting salt is novalgin, pyrovinic acid potassium, ethylsulfonic acid sodium, ethylsulfonic acid potassium, phenolSodium sulfonate or naphtholsulfonic acid sodium; Described pH value conditioning agent is highly basic.
2. plating tin liquor according to claim 1, is characterized in that, comprises following raw material components:
(A) tin salt, the concentration of stannous ion is 5-20g/L;
(B) acid: one or more in organic acid, inorganic acid, the total concentration of acid is 10-100g/L;
(C) surfactant: structural formula is R1COO(C2H4O)nH、R2S(C2H4O)mThe nonionic of HOne or more in surfactant, the total concentration of surfactant is 1-10g/L, wherein R1、R2For C4-C20Alkyl, the integer that n, m are 4-12;
(D) electric current dispersant: containing dicarboxylic acids analog derivative or its salt of unsaturated bond, concentration is0.01-0.5g/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. according to the plating tin liquor of claim 1 or 2, it is characterized in that the described binary containing unsaturated bondCarboxylic acid derivative is 2-ethylene glutaric acid, 2-trimethylene glutaric acid or 2-trimethylene succinic acid.
4. plating tin liquor according to claim 1 and 2, is characterized in that, described surfactant isSad polyoxyethylene ester, valeric acid polyoxyethylene ester, laurate polyoxyethylene ester, octane polyoxyethylene thioalcohol,One or more in lauryl mercaptan APEO or stearylmercaptan APEO.
5. plating tin liquor according to claim 1 and 2, is characterized in that, described tin salt is methylThe sub-tin of sulfonic acid or the sub-tin of ethylsulfonic acid.
6. plating tin liquor according to claim 1 and 2, is characterized in that, described organic acid is methylSulfonic acid or ethylsulfonic acid.
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| CN109518233B (en) * | 2018-11-27 | 2020-07-14 | 东莞美坚化工原料有限公司 | Conductive solution for preventing miniature electronic component from being stuck on chip and preparation method thereof |
| CN109537013B (en) * | 2018-12-03 | 2020-12-04 | 上海雷迪埃电子有限公司 | Insulator electroplating method |
| CN109338408A (en) * | 2018-12-04 | 2019-02-15 | 中华全国供销合作总社天津再生资源研究所 | A kind of electrolyte and a kind of electrorefining method of useless electronic solder |
| CN109554730B (en) * | 2018-12-29 | 2020-11-13 | 广东光华科技股份有限公司 | Tin plating solution and preparation method and application thereof |
| CN111041534A (en) * | 2019-12-25 | 2020-04-21 | 戚英奎 | Tin plating solution |
| CN111139462B (en) * | 2020-01-16 | 2021-12-28 | 常熟市普华电工材料有限公司 | Electrotinning treatment process |
| CN111321435B (en) * | 2020-04-17 | 2022-03-01 | 广州鑫睿表面技术有限公司 | Acidic tin electroplating solution and preparation method and application thereof |
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