CN105316663B - One kind prepares semi-conductor silicon chip nickel-plating liquid - Google Patents
One kind prepares semi-conductor silicon chip nickel-plating liquid Download PDFInfo
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Abstract
The invention discloses one kind to prepare semi-conductor silicon chip nickel-plating liquid, and its component includes：PH value regulator, compound complex agent and the deionized water that soluble nickel salt, reducing agent, hydrochloric acid and ammoniacal liquor form, compound complex agent is at least two in citric acid and its soluble-salt, tartaric acid and its soluble-salt, lactic acid and its soluble-salt, malic acid and its soluble-salt, succinic acid and its soluble-salt, ethylenediamine tetra-acetic acid and its soluble-salt, Hedta and its soluble-salt, and the pH value of nickel-plating liquid is 7.5~9.5.The nickel-plating liquid of the present invention adds the pH value regulator of hydrochloric acid and ammoniacal liquor composition, helps to maintain the pH stable in Ni-Speed；The weak acid and soluble-salt used as complexing agent can combine to form buffer system with pH value regulator, and further pH value is adjusted；Being used cooperatively at least two complexing agents can make nickel-plating liquid stability good, and nickel plating speed is moderate.
Description
Technical field
The present invention relates to nickel-plating liquid technical field of compositions, and in particular to one kind prepares semi-conductor silicon chip nickel-plating liquid.
Background technology
Nickel chemical plating technology is used for semiconductor components and devices, and covers one layer of contact material in component surface, this be from
The technology for the solution Ohmic contact that chemical field is introduced.It is in the nature that soluble nickel salt occurs with the reducing agent component in nickel-plating liquid
Redox reaction, the electronics that nickel ion acquisition reducing agent provides are reduced into metallic nickel and deposit to semiconductor components and devices surface.
Conventional chemical nickel-plating liquid of the prior art is alkaline nickel-plating liquid.CN102168258A discloses a kind of alkaline nothing
Electronickelling liquid, the composition of the nickel-plating liquid include nickel ion, reducing agent, the first chelating agent, the second chelating agent, stabilizer and water, the
The group that one chelating agent is made up of citric acid, ammonium citrate, sodium citrate, potassium citrate and its mixture, the second chelating agent
The group being made up of hydramine, ethylenediamine, diethylenetriamine, triethylene tetramine and its mixing, the pH of the alkaline electroless nickel plating liquid
It is worth for 7.0 to 10.0, in further preferred technical scheme, not from pH value regulator.Found in actual use, pH value
Influence to plating speed and nickel plating liquid system is very big, is embodied in：PH value raises, and plates speed and accelerates, but ascensional range be not it is very big,
But pH value is too high, the hydroxide ion of high concentration can weaken complexing of the complex system to nickel ion, cause to form hydrogen in the plating solution
Nickel oxide precipitates, and declines bath stability, the lost of life, can also influence the quality of nickel coating, and coating hole increases, nickel coating
Adhesion between silicon face is poor, and contact resistance between the two is larger.
The content of the invention
It is an object of the invention to overcome defect present in prior art, there is provided a kind of pH value control is stable, coating matter
Measure and high prepare semi-conductor silicon chip nickel-plating liquid.
To realize above-mentioned technique effect, the technical scheme is that：One kind prepares semi-conductor silicon chip nickel-plating liquid, and it is special
Sign is that its component includes：Soluble nickel salt, reducing agent, hydrochloric acid and ammoniacal liquor composition pH value regulator, compound complex agent and go
Ionized water, compound complex agent are selected from citric acid and its soluble-salt, tartaric acid and its soluble-salt, lactic acid and its solubility
Salt, malic acid and its soluble-salt, succinic acid and its soluble-salt, ethylenediamine tetra-acetic acid and its soluble-salt, hydroxyethyl vinyl
At least two in ethylenediamine triacetic acid and its soluble-salt, the pH value of nickel-plating liquid is 7.5~9.5.
Hydrochloric acid and ammoniacal liquor composition pH value regulator addition, can by the pH stable of nickel-plating liquid 7.5~9.5 it
Between, OH-Activated centre can be formed in silicon face, attract nickel ion and and then form uniform metal nickel dam, and in coating
Grain is smaller, and surface compact is smooth；In addition, the carboxyl, hydroxyl and amino in compound complex agent are ligands, in carboxyl and hydroxyl
Nitrogen-atoms in oxygen atom and amino has lone pair electrons to can take up Ni2+Space orbit, formed complex compound, increase Ni2+'s
Difficulty is hydrolyzed, contains at least two ligands in the material molecular structure of the optional scope of above-mentioned complexing agent, nickel ion can be same
When with two parts form coordinate bonds, the complex compound of formation has more stable cyclic structure, and compound use can form complexing
The more preferable bath system of energy, and then adjust nickel plating speed.The acid-base property of complexing agent differs, and the organic acid such as citric acid complexing agent is in weak
Acidity, the pH value of buffer system, further stable plating solution can be formed with pH value regulator.
Complexing agent citric acid, tartaric acid, lactic acid, malic acid, succinic acid, ethylenediamine tetra-acetic acid, hydroxyethyl vinyl diamines three
Water soluble salt corresponding to acetic acid is sodium salt, sylvite and ammonium salt；Soluble nickel salt is specially：Nickel acetate, nickel sulfate, nickel chloride；Also
The optional scope of former agent is hypophosphorous acid and salt, boride, borine, hydrazine etc..
In order to form stable nickel plating liquid system, optimize nickel plating effect, preferable technical scheme is that its component is by weight
Number meter includes：The pH value that 3~9 parts of soluble nickel salt, 8~13 parts of reducing agent, 14~30 parts of hydrochloric acid and ammoniacal liquor form is adjusted
Save agent, 5~11 parts of compound complex agent, 40~60 parts of deionized water.Nickel ion can excessively reduce the steady of nickel-plating liquid in solution
It is qualitative, coarse coating is easily formed, in addition, reducing agent excessively can also make plating speed too fast unmanageable.
Preferable technical scheme is that soluble nickel salt is selected from least one of nickel sulfate and nickel chloride.
Preferable technical scheme is that reducing agent is selected from least one of hypophosphorous acid and its soluble-salt.In general, it is secondary
The soluble-salt of phosphoric acid is sodium salt, sylvite or ammonium salt, in order to avoid introducing strong base ion, and ammonium ion mistake into nickel-plating liquid
More, ammonium ion and hydroxide ion, which combine to decompose, during nickel-plating liquid applied at elevated temperature produces ammonia, therefore more has going back for choosing
Former agent is hypophosphorous acid.
Compound complex agent includes the first complexing agent and the second complexing agent；First complexing agent be selected from citric acid and its ammonium salt,
Tartaric acid and its ammonium salt, lactic acid and its ammonium salt, malic acid and its ammonium salt kind；Second complexing agent be selected from ethylenediamine tetra-acetic acid and
At least one of its ammonium salt, Hedta.First complexing agent is to contain hydroxyl and carboxyl simultaneously in molecule
Complexing agent, the second complexing agent is the complexing agent containing amino and carboxyl simultaneously in molecule, and two kinds of complexing agents are used in combination can be with
Have the function that Synergistic, in addition, the addition of ethylenediamine tetra-acetic acid can promote hydrogen in hypophosphorous acid molecule and phosphorus atoms it
Between key die down, activate hypophosphite ion, hydrogen is easier mobile and absorption on by catalytic surface, improve the heavy of metallic nickel
Product speed, play a part of accelerating nickel plating.
In order that nickel-plating liquid possesses preferable complex performance, and nickel plating speed is moderate, and preferable technical scheme is the first network
The weight ratio of mixture and the second complexing agent is（3~6）:1.
Preferable technical scheme is that nickel-plating liquid also contains 0.001~1 part of stabilizer, and the stabilizer is to spread out selected from thiocarbamide
At least one of biology, unsaturated organic acid, the soluble organic salts of cerium and inorganic salts.Thiourea derivative, unsaturation are organic
Acid and cerium ion reactivity are higher, can occupy the active site of base material, form competition simultaneously with nickel ion and then suppress the analysis of nickel
Go out, prevent the Auto-decomposition of nickel-plating liquid, be favorably improved the stability of nickel-plating liquid.
Preferable technical scheme is, unsaturated organic acid be in maleic acid, aconitic acid, fumaric acid and itaconic acid extremely
Few one kind.
In order to ensure the feature of environmental protection of nickel-plating liquid stabilizer, further optimize the stability of nickel-plating liquid, preferable technical scheme
For the stabilizer is mixed by the soluble organic salts of fumaric acid and cerium, and the percentage by weight of fumaric acid is in stabilizer
25~45%.
Preferable technical scheme is, the nickel-plating liquid also contain 0.001~1 part of anion surfactant, described the moon from
Sub- surfactant is alcohol ether carboxylate analog anion surfactants.The addition of alcohol ether carboxylate analog anion surfactants
The adhesion between coating and silicon face can be increased, reduce contact resistance between the two.
The advantages of the present invention are：
The pH value regulator that the nickel-plating liquid of the present invention is formed by adding hydrochloric acid and ammoniacal liquor, helps to maintain in Ni-Speed
PH stable；The weak acid and soluble-salt used as complexing agent can combine to form buffer system with pH value regulator, enter one
PH value is adjusted step；In addition, being used cooperatively at least two complexing agents can make nickel-plating liquid stability good, for semiconductor silicon
Speed is moderate during piece nickel plating.
Embodiment
With reference to embodiment, the embodiment of the present invention is further described.Following examples are only used for more
Add and clearly demonstrate technical scheme, and can not be limited the scope of the invention with this.
Embodiment 1：
The semi-conductor silicon chip for preparing of embodiment 1 is with the composition of nickel-plating liquid：11 parts of soluble nickel salt, 5 parts of reducing agent,
PH value regulator, 4 parts of compound complex agent, 60 parts of the deionized water of 30 parts of hydrochloric acid and ammoniacal liquor composition, the pH value of nickel-plating liquid
For 7.5.Compound complex agent is lactic acid and sodium tartrate 1:1 mixes.Soluble nickel salt selects nickel acetate, and reducing agent is diformazan
Amine borine.
Hydrochloric acid is the hydrochloric acid that hydrogen cloride concentration is 37%, NH in ammoniacal liquor3Concentration be 29%.
Embodiment 2
The difference of embodiment 2 and embodiment 1 is that the composition of the nickel-plating liquid of embodiment 2 is：3 parts of soluble nickel salt, 13 parts
Reducing agent, 14 parts of hydrochloric acid and ammoniacal liquor composition pH value regulator, 11 parts of compound complex agent, 40 parts of deionized water, plating
The pH value of nickel liquid is 7.5.Complexing agent is selected from sodium citrate and Hedta, the weight ratio of two kinds of complexing agents
For 3:1, soluble nickel salt is nickel sulfate, and reducing agent is sodium hypophosphite.
Embodiment 3
The difference of embodiment 3 and embodiment 2 is that the composition of the nickel-plating liquid of embodiment 3 is：8 parts of soluble nickel salt, 8 parts
Reducing agent, 30 parts of hydrochloric acid and ammoniacal liquor composition pH value regulator, 5 parts of compound complex agent, 60 parts of deionized water, nickel plating
The pH value of liquid is 9.5.Complexing agent is malic acid ammonium and ethylenediamine tetra-acetic acid ammonium, and the weight ratio of two kinds of complexing agents is 6:1, it is soluble
Nickel salt is nickel chloride.
Embodiment 4
The difference of embodiment 4 and embodiment 2 is that the composition of the nickel-plating liquid of embodiment 4 is：5 parts of soluble nickel salt, 11
PH value regulator, 8 parts of compound complex agent, 50 parts of the deionized water that the reducing agent, 22 parts of hydrochloric acid and ammoniacal liquor of part form.Network
Mixture is ammonium citrate and ethylenediamine tetra-acetic acid, and the weight ratio of two kinds of complexing agents is 9:2, reducing agent is hypophosphorous acid.
Embodiment 5
The difference of embodiment 5 and embodiment 4 is, also containing 0.001 part of thiourea derivative in the nickel-plating liquid of embodiment 5.
Embodiment 6
The difference of embodiment 6 and embodiment 5 is, cerous sulfate and the crow that contained stabilizer is 1 part in the nickel-plating liquid of embodiment 6
Head acid, weight ratio are 1:1.
Embodiment 7
The difference of embodiment 7 and embodiment 6 is, contained stabilizer is maleic acid and itaconic acid in the nickel-plating liquid of embodiment 7,
Weight ratio is 1:1, weight fraction is 0.5 part.
Embodiment 8
The difference of embodiment 8 and embodiment 6 is that contained stabilizer is fumaric acid and citric acid in the nickel-plating liquid of embodiment 8
Cerium, the percentage by weight of fumaric acid is 25% in stabilizer.
Embodiment 9
The difference of embodiment 9 and embodiment 8 is, the weight hundred of fumaric acid in the compound stabilizer of the nickel-plating liquid of embodiment 9
Divide than being 45%.
Embodiment 10
The difference of embodiment 10 and embodiment 8 is, the weight of fumaric acid in the compound stabilizer of the nickel-plating liquid of embodiment 10
Percentage is 35%.
Embodiment 11-13
Embodiment 11-13 is distinguished as with embodiment 10：Analog anion surfactants containing alcohol ether carboxylate in nickel-plating liquid,
Contained parts by weight are respectively 0.001 part, 1 part and 0.5 part.
Comparative example
Comparative example is same as Example 4 as complexing agent, nickel-plating liquid component only with ammonium citrate.
The configuration of nickel-plating liquid：By complexing agent, water and partial ammonia water dissolving be placed in container, then add hydrochloric acid, ammoniacal liquor and
Part water, the aqueous solution of nickel salt is added, be eventually adding the aqueous solution of reducing agent, stir.
Nickel plating operates：
Silicon substrate after pre-treatment is placed in 80 DEG C of nickel-plating liquid and is coated with 10 minutes.
Coating surface morphology is observed：Gained sample is placed in the surface and section of coating obtained by electron scanning electricity Microscopic observation
Pattern；
Bath stability is tested：Chemical nickel-plating liquid 50mL is taken, is contained in 250mL beaker, the water-bath of immersion (80 ± l) DEG C
In, it is constant to bath temperature.Under agitation, palladium chloride solution 1mL that concentration is 100mg/L is measured in beaker with pipette.
Record in self seeding palladium chloride solution to beaker, chemical plating fluid starts the time that turbidity and precipitation is undergone occur, with second (s) table
Show.
Binding force of cladding material is tested：Carried out by GB/T5270-2005 standards.Line and cross cut test method：Existed with hard steel knife
Draw whether two tilt or peel off at a distance of 2mm parallel lines or 1mm square lattice, observation coating on coating.
For coating surface morphology compared with embodiment 2-13, surface is slightly coarse in embodiment 1；Under identical plating time, implement
The thickness of coating of example 1, embodiment 2 and embodiment 4-13 is thicker, about 3 μm, and the thickness of coating of embodiment 3 is about 2 μm, comparative example 4
Coating be about 1 μm, in addition, add surfactant embodiment 11-13 coating it is finer and close.
Bath stability test result shows that the nickel-plating liquid stability for adding the embodiment 5-13 of stabilizer is substantially better than reality
A 1-4 is applied, embodiment 8-13 nickel-plating liquid stability is best, and the clarification of nickel plating fluid samples is without precipitation, embodiment in stability test
Nickel plating fluid samples show slightly muddy in 1-4 sample stability test, but amount of precipitation is more than embodiment 5-7 sample.
Binding force of cladding material is tested：1-13 sample experiment result is that coating tilts without peeling and substantially, by contrast, real
The tilting degree for applying a 11-13 is less than embodiment 1-10, and embodiment 1-10 sample binding force of cladding material is slightly worse than embodiment 11-
13。
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, some improvements and modifications can also be made, these improvements and modifications
Also it should be regarded as protection scope of the present invention.
Claims (5)
1. one kind prepares semi-conductor silicon chip nickel-plating liquid, it is characterised in that its component includes：Soluble nickel salt, reducing agent, hydrochloric acid
With pH value regulator, compound complex agent and the deionized water of ammoniacal liquor composition, compound complex agent is selected from citric acid and its solubility
Salt, tartaric acid and its soluble-salt, lactic acid and its soluble-salt, malic acid and its soluble-salt, succinic acid and its soluble-salt,
At least two in ethylenediamine tetra-acetic acid and its soluble-salt, Hedta and its soluble-salt, nickel-plating liquid
PH value be 7.5~9.5；Its component count in parts by weight including：3~8 parts of soluble nickel salt, 8~13 parts of reducing agent, 14
PH value regulator, 5~11 parts of compound complex agent, 40~60 parts of the deionized water of~30 parts of hydrochloric acid and ammoniacal liquor composition；Plating
Nickel liquid also contains 0.001~1 part of stabilizer, and the stabilizer is mixed by the soluble organic salts of fumaric acid and cerium, stable
The percentage by weight of fumaric acid is 25~45% in agent, and the nickel-plating liquid also contains 0.001~1 part of anion surfactant, institute
It is alcohol ether carboxylate analog anion surfactants to state anion surfactant.
2. according to claim 1 prepare semi-conductor silicon chip nickel-plating liquid, it is characterised in that soluble nickel salt is selected from sulphur
At least one of sour nickel and nickel chloride.
3. according to claim 1 prepare semi-conductor silicon chip nickel-plating liquid, it is characterised in that reducing agent is selected from hypophosphorous acid
And its at least one of soluble-salt.
4. according to claim 1 prepare semi-conductor silicon chip nickel-plating liquid, it is characterised in that compound complex agent includes first
Complexing agent and the second complexing agent；First complexing agent be selected from citric acid and its ammonium salt, tartaric acid and its ammonium salt, lactic acid and its ammonium salt,
Malic acid and its ammonium salt；Second complexing agent in ethylenediamine tetra-acetic acid and its ammonium salt, Hedta extremely
Few one kind.
5. according to claim 4 prepare semi-conductor silicon chip nickel-plating liquid, it is characterised in that the first complexing agent and the second network
The weight ratio of mixture is（3~6）:1.
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| CN109516575A (en) * | 2017-09-18 | 2019-03-26 | 中国石油化工股份有限公司 | A kind of processing method of high iron circulation cooling water |
| CN109516577A (en) * | 2017-09-18 | 2019-03-26 | 中国石油化工股份有限公司 | A kind of processing method of high iron circulation cooling water |
| CN111349917A (en) * | 2018-12-24 | 2020-06-30 | 天津环鑫科技发展有限公司 | Gold plating solution for semiconductor chip, gold plating method and nickel and gold plating method |
| CN110308171A (en) * | 2019-06-04 | 2019-10-08 | 甘肃酒钢集团宏兴钢铁股份有限公司 | A kind of method of stainless-steel cold-rolling anneal oxidation skin microcosmic observation |
| CN112680757B (en) * | 2020-12-11 | 2021-10-19 | 浙江华晶整流器有限公司 | Electroplating nickel plating process of electrode |
| CN113061878A (en) * | 2021-03-19 | 2021-07-02 | 德星化工(苏州)有限公司 | High-adaptability chemical nickel plating solution and preparation method thereof |
| CN114751529A (en) * | 2022-01-13 | 2022-07-15 | 宜城成雄织造有限公司 | Environment-friendly phosphorus-free chelating agent and preparation method thereof |
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|---|---|---|---|---|
| CN102168258A (en) * | 2010-02-05 | 2011-08-31 | 芝普企业股份有限公司 | Electroless nickel plating solution for solar cell electrode |
| CN102212804A (en) * | 2011-05-27 | 2011-10-12 | 长春工业大学 | Alkali chemical plating solution and solution plating method thereof on silicon chip |
| KR101487890B1 (en) * | 2013-07-16 | 2015-02-03 | 한국생산기술연구원 | Electroless plating solution, method of electroless nickel plating using the same, and flexible nickel plating layer using the same |
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| JP3561240B2 (en) * | 2001-05-25 | 2004-09-02 | 京セラ株式会社 | Manufacturing method of wiring board |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102168258A (en) * | 2010-02-05 | 2011-08-31 | 芝普企业股份有限公司 | Electroless nickel plating solution for solar cell electrode |
| CN102212804A (en) * | 2011-05-27 | 2011-10-12 | 长春工业大学 | Alkali chemical plating solution and solution plating method thereof on silicon chip |
| KR101487890B1 (en) * | 2013-07-16 | 2015-02-03 | 한국생산기술연구원 | Electroless plating solution, method of electroless nickel plating using the same, and flexible nickel plating layer using the same |
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