CN114752974A - Formula and preparation method of cyanide-free electrogilding liquid medicine for wafer - Google Patents

Formula and preparation method of cyanide-free electrogilding liquid medicine for wafer Download PDF

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Publication number
CN114752974A
CN114752974A CN202210405689.0A CN202210405689A CN114752974A CN 114752974 A CN114752974 A CN 114752974A CN 202210405689 A CN202210405689 A CN 202210405689A CN 114752974 A CN114752974 A CN 114752974A
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vessel
parts
cyanide
free
electrogilding
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陈跃
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Shenzhen Tianyue New Material Technology Co ltd
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Shenzhen Tianyue New Material Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/48—Electroplating: Baths therefor from solutions of gold
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/12—Semiconductors

Abstract

The invention provides a wafer cyanide-free electrogilding liquid medicine formula and a preparation method thereof, and relates to the technical field of electrogilding, wherein the wafer cyanide-free electrogilding liquid medicine formula comprises a first layer film, a second layer film and a third layer film, wherein the first layer film comprises the following components in percentage by weight: 70-90 parts of polyethylene terephthalate, 10-18 parts of glass fiber, 1-3 parts of a toughening agent and 5-7 parts of an antioxidant; the second layer of film comprises the following components in percentage by weight: 50-60 parts of polyethylene terephthalate, 20-25 parts of a flame retardant, 5-8 parts of a stabilizer and 3-6 parts of an opening agent; the third layer of film comprises the following components in percentage by weight: 80-85 parts of polyethylene terephthalate. The invention prepares the formula of the cyanide-free electrogilding liquid medicine for the wafer by compounding the first layer film, the second layer film and the third layer film, wherein the glass fiber is added into the first layer film to improve the strength, the second layer film has the characteristic of high fire resistance, and the third layer film can effectively inhibit static electricity and has remarkable progress.

Description

Formula and preparation method of cyanide-free electrogilding liquid medicine for wafer
Technical Field
The invention relates to the technical field of electrogilding, in particular to a formula of a wafer cyanide-free electrogilding liquid medicine and a preparation method thereof.
Background
Gold is widely applied to the industrial fields of electronics, instruments, aviation, aerospace and the like due to good conductivity, good weldability, low contact resistance, high temperature resistance and wear resistance, and has high chemical stability, good corrosion resistance and discoloration resistance, and an electrogilding coating is needed for electroplating semiconductor wafers.
However, when the existing cyanide-free electrogilding liquid medicine for wafers is actually used, particularly in the preparation process, the cyanide-free electrogilding liquid medicine for wafers is only stirred and mixed by a stirrer, and part of organic additives and inorganic additives are not completely dissolved, so that the using effect of the cyanide-free electrogilding liquid medicine for wafers is influenced, the practicability is poor, and improvement is needed.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a formula of a wafer cyanide-free electrogilding liquid and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme: the formula of the cyanide-free electrogilding liquid medicine for the wafer comprises a first layer of film, a second layer of film and a third layer of film, wherein the first layer of film comprises the following components in percentage by weight: 70-90 parts of polyethylene terephthalate, 10-18 parts of glass fiber, 1-3 parts of a toughening agent and 5-7 parts of an antioxidant; the second layer of film comprises the following components in percentage by weight: 50-60 parts of polyethylene glycol terephthalate, 20-25 parts of a flame retardant, 5-8 parts of a stabilizer and 3-6 parts of an opening agent; the third layer of film comprises the following components in percentage by weight: 80-85 parts of polyethylene terephthalate, 5-8 parts of antistatic agent, 10-12 parts of light stabilizer and 2-4 parts of antibacterial agent.
In order to improve the structural strength of the film, the invention improves that the toughening agent is any one of acrylonitrile-butadiene-styrene copolymer, chlorinated polyethylene and ethylene-vinyl acetate copolymer.
In order to reduce the oxidation speed of the film, the invention improves that the antioxidant is any one of antioxidant 168, antioxidant TNP, antioxidant MB, antioxidant CA, antioxidant 1010 and antioxidant 164.
In order to improve the fireproof effect, the invention improves that the fire retardant is any one of tributyl phosphate, Pyrol99, tricresyl phosphate, triphenyl phosphate and chlordane anhydride.
In order to maintain the chemical balance, the invention improves that the stabilizer is any one of dibutyltin dilaurate and polycarbodiimide, and the opening agent is any one of silicon dioxide opening agent and oleic acid amide.
In order to improve the antistatic effect, the invention improves that the antistatic agent is any one of antistatic agent SN and ECH antistatic agent, the light stabilizer is any one of benzophenone and benzotriazole, and the antibacterial agent is ethyl vanillin or vanillin.
A preparation method of a wafer cyanide-free electrogilding liquid formula comprises the following steps:
S1, preparing raw materials, weighing polyethylene terephthalate, glass fiber, a toughening agent, an antioxidant, a flame retardant, a stabilizer, an opening agent, an antistatic agent, a light stabilizer and an antibacterial agent, and placing the raw materials in a container for storage;
s2, crushing, namely putting the polyethylene terephthalate into a crusher, crushing the polyethylene terephthalate, and then grinding the crushed polyethylene terephthalate by using a grinder to obtain powder;
s3, stirring, namely respectively putting raw materials required by the first layer of film, the second layer of film and the third layer of film into a stirrer to be uniformly stirred, and then obtaining a first layer of film mixed raw material, a second layer of film mixed raw material and a third layer of film mixed raw material;
s4, drying, namely putting the first layer film mixed raw material, the second layer film mixed raw material and the third layer film mixed raw material into a dryer for drying for 50-60min to obtain dried first layer film mixed raw material, second layer film mixed raw material and third layer film mixed raw material;
s5, extruding, and then respectively extruding the first layer film mixed raw material, the second layer film mixed raw material and the third layer film mixed raw material through melt extrusion equipment;
S6, cooling, namely cooling the first layer of film mixed raw material, the second layer of film mixed raw material and the third layer of film mixed raw material in a room temperature environment;
s7, stretching, namely respectively carrying out longitudinal stretching, transverse stretching and shaping on the first layer film mixed raw material, the second layer film mixed raw material and the third layer film mixed raw material to obtain a first layer film, a second layer film and a third layer film;
s8, hot melting, splicing the first layer of film, the second layer of film and the third layer of film together through a hot melting machine, wherein the first layer of film is used as the topmost layer, the second layer of film is used as the middle layer, the third layer of film is used as the bottommost layer, and obtaining the finished product of the wafer cyanide-free electrogilding liquid formula after hot melting.
In order to mix the raw materials more uniformly, the invention improves that in the step S3, the rotating speed of the stirrer is 30-60 r/S.
In order to improve the service life of the film, the invention improves that in the step S6, the cooling speed is 20-45 ℃/min optimally.
In order to improve the stretching effect, the invention improves that in the step S7, the temperature of the longitudinal stretching is 90-110 ℃, and the temperature of the transverse stretching is 95-115 ℃.
Compared with the prior art, the method has the advantages that the ultrapure water is used as a solvent, and the method is purer compared with the traditional deionized water, so that the effective dissolution of each component can be effectively ensured, meanwhile, in the preparation method, the dissolution is carried out in a stirring and water bath mixing mode, the water temperature can be improved in a water bath heating mode, and further, the organic additive and the inorganic additive can be fully dissolved.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a process diagram of the preparation method of a cyanide-free electrogilding liquid for wafers according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
Referring to fig. 1, a formula of a cyanide-free electrogilding solution for a wafer comprises the following components in parts by weight:
78 parts of N, N-dimethylethanolamine, 12 parts of a main coordination agent, 6 parts of an auxiliary coordination agent, 2 parts of gold potassium chloride, 23 parts of ultrapure water, 25 parts of potassium carbonate, 9 parts of an additional additive, 5 parts of potassium tartrate and 1 part of phenylalanine.
In the embodiment, the resistivity of the ultrapure water is 18.25M omega/cm, and the pH value of the cyanide-free electrogilding liquid medicine is 8-11, so that the quality of the ultrapure water is ensured.
In this embodiment, the primary complexing agent includes any one or two of a hydantoin derivative, sodium pyrophosphite, and 5, 5-dimethylhydantoin.
In this embodiment, the auxiliary coordination agent is one or two of potassium oxalate, polyacrylamide, aminopyridine, S-methylisothiourea sulfate, and sodium n-dodecyl diphenyl ether disulfonate.
In this embodiment, the additional additives include organic additives and inorganic additives.
In this embodiment, the organic additive is one or more of butyl hydroxy anisole, tert-butyl hydroquinone, dibutyl hydroxy toluene and thymine, and the inorganic additive is one of sodium phenolate and sodium stearate.
Referring to fig. 1, a method for preparing a recipe of a cyanide-free electrogilding solution for a wafer includes the following steps:
s1, a preparation step, namely weighing N, N-dimethylethanolamine, a main coordination agent, an auxiliary coordination agent, gold potassium chloride, ultrapure water, potassium carbonate, an additional additive, potassium tartrate and phenylalanine in corresponding parts, and placing the weighed materials in a container for storage;
s2, dissolving, namely adding the ultrapure water into a vessel, then adding N, N-dimethylethanolamine, a main coordination agent and an auxiliary coordination agent into the vessel for dissolving for 15min, and standing for 10min after dissolving;
s3, stirring, then introducing the mixed solution in the vessel into an ultrasonic stirrer for stirring for 40min, then obtaining the stirred mixed solution, and then pouring the stirred mixed solution into the vessel;
s4, performing primary water bath, namely putting the vessel into a water bath heating tank to be heated to 72 ℃, then sequentially pouring the potassium chloride, the potassium carbonate, the potassium tartrate and the phenylalanine into the vessel to be fully dissolved, and taking the vessel out of the water bath heating tank after the potassium chloride, the potassium carbonate, the potassium tartrate and the phenylalanine are dissolved;
s5, cooling, then pouring the organic additive in the additional additive into the vessel, and then standing the vessel until the vessel is cooled to room temperature;
S6, performing water bath twice, then putting the vessel into a water bath heating tank again, heating to 85 ℃, after heating for 20min, putting the inorganic additive into the vessel, then continuously heating for 30min again, then stirring the vessel for 2min, and then taking the vessel out of the water bath heating tank;
and S7, adding the remaining ultrapure water into the vessel, and stirring for 19min by using a stirrer to obtain the cyanide-free electrogilding liquid medicine for the wafer.
In this embodiment, in step S7, the rotation speed of the stirrer is 20r/S, and the solution in the vessel can be stirred well at the rotation speed of 20 r.
In this embodiment, in the step S5, the speed of cooling the vessel to room temperature is 5 ℃/min, and the slow cooling mode can ensure the dissolution effect.
In this embodiment, in the step S7, the volume of the vessel is 2000ml, so that the stirring effect can be ensured, and the influence on the stirring effect and the preparation cost due to too large or too small volume can be avoided.
Example two
Referring to fig. 1, a formula of a cyanide-free electrogilding solution for a wafer comprises the following components in parts by weight:
80 parts of N, N-dimethylethanolamine, 15 parts of a main coordination agent, 6 parts of an auxiliary coordination agent, 2 parts of gold potassium chloride, 23 parts of ultrapure water, 30 parts of potassium carbonate, 15 parts of an additional additive, 5 parts of potassium tartrate and 1 part of phenylalanine.
In the embodiment, the resistivity of the ultrapure water is 18.25 MOmega/cm, and the pH value of the cyanide-free gold electroplating liquid is 8-11, so that the quality of the ultrapure water is ensured.
In this embodiment, the primary complexing agent includes any one or two of a hydantoin derivative, sodium pyrophosphite, and 5, 5-dimethylhydantoin.
In this embodiment, the auxiliary coordination agent is one or two of potassium oxalate, polyacrylamide, aminopyridine, S-methylisothiourea sulfate, and sodium n-dodecyl diphenyl ether disulfonate.
In this embodiment, the additional additives include organic additives and inorganic additives.
In this embodiment, the organic additive is one or more of butylated hydroxyanisole, tert-butylhydroquinone, dibutylhydroxytoluene, and thymine, and the inorganic additive is one of sodium phenolate and sodium stearate.
Referring to fig. 1, a method for preparing a recipe of a cyanide-free electrogilding solution for a wafer includes the following steps:
s1, a preparation step, namely weighing N, N-dimethylethanolamine, a main coordination agent, an auxiliary coordination agent, gold potassium chloride, ultrapure water, potassium carbonate, an additional additive, potassium tartrate and phenylalanine in corresponding parts, and placing the weighed materials in a container for storage;
S2, dissolving, namely adding the ultrapure water into a vessel, then adding N, N-dimethylethanolamine, a main coordination agent and an auxiliary coordination agent into the vessel for dissolving for 15min, and standing for 10min after dissolving;
s3, stirring, then introducing the mixed solution in the vessel into an ultrasonic stirrer for stirring for 45min, then obtaining the stirred mixed solution, and then pouring the stirred mixed solution into the vessel;
s4, performing primary water bath, namely putting the vessel into a water bath heating tank to be heated to 75 ℃, then sequentially pouring the potassium chloride, the potassium carbonate, the potassium tartrate and the phenylalanine into the vessel to be fully dissolved, and taking the vessel out of the water bath heating tank after the potassium chloride, the potassium carbonate, the potassium tartrate and the phenylalanine are dissolved;
s5, cooling, then pouring the organic additive in the additional additive into the vessel, and then standing the vessel until the vessel is cooled to room temperature;
s6, performing water bath twice, then putting the utensil into a water bath heating tank again, heating to 90 ℃, after heating for 30min, putting the inorganic additive into the utensil, then continuously heating for 30min again, then stirring the utensil for 2min, and then taking the utensil out of the water bath heating tank;
And S7, adding the rest ultrapure water into the vessel, and stirring for 20min by using a stirrer to obtain the cyanide-free gold electroplating liquid medicine for the wafer.
In this embodiment, in step S7, the rotation speed of the stirrer is 30r/S, and the solution in the vessel can be stirred well at the rotation speed of 30 r.
In this embodiment, in the step S5, the cooling speed of the vessel to room temperature is 5 ℃/min, and the slow cooling mode can ensure the dissolution effect.
In this embodiment, in the step S7, the volume of the vessel is 3000ml, so that the stirring effect can be ensured, and the influence of too large or too small volume on the stirring effect and the preparation cost can be avoided.
Electroplating was performed using the cyanide-free electrogilding solutions of the wafers obtained in examples one and two, and then XRF testing was performed using electrogilding wafers, the results of which are shown in table 1.
TABLE 1 gold plating thickness of electrogilding on Hertz coupon
Figure BDA0003602073720000081
The results in table 1 show that the electroplated gold wafer prepared by the invention has excellent control of the electroplating thickness uniformity and remarkable advancement.
It can be seen from the above embodiments that the invention prepares the recipe of the cyanide-free electrogilding solution for wafers by compounding the first layer film, the second layer film and the third layer film, in the first layer film, the glass fiber is added, the glass fiber has the characteristic of high mechanical strength, which also improves the mechanical strength of the first layer film, and at the same time, the added toughening agent can reduce the brittleness of the glass fiber and increase the toughness, thereby improving the bearing strength and prolonging the service life of the first layer film, in the second layer film, the flame retardant and the opening agent are added, wherein the flame retardant can make the invention more flame retardant and improve the flame resistance, and the added opening agent can improve the opening performance of the film, so that the high optical property of the film is more excellent, in the third layer film, the added antistatic agent can effectively inhibit static electricity, thereby avoiding the static electricity from affecting the normal use of electronic products, the general use of the invention is improved, and the added antibacterial agent can inhibit the breeding of bacteria, thereby improving the cleanliness, and having higher practicability and remarkable progress.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.

Claims (10)

1. The formula of the cyanide-free electrogilding liquid medicine for the wafer is characterized by comprising the following components in parts by weight:
50-80 parts of N, N-dimethylethanolamine, 10-20 parts of a main complexing agent, 5-8 parts of an auxiliary complexing agent, 1-3 parts of gold potassium chloride, 20-30 parts of ultrapure water, 20-35 parts of potassium carbonate, 5-15 parts of an additional additive, 3-5 parts of potassium tartrate and 1-2 parts of phenylalanine.
2. The formulation of the cyanide-free electrogilding solution for wafers as claimed in claim 1, wherein: the resistivity of the ultrapure water is 18.25 MOmega/cm, and the pH value of the cyanide-free gold electroplating liquid is 8-11.
3. The formulation of the cyanide-free electrogilding solution for wafers as claimed in claim 1, wherein: the main coordination agent comprises any one or two of hydantoin derivatives, sodium pyrophosphite and 5, 5-dimethyl hydantoin.
4. The formulation of the cyanide-free electrogilding solution for wafers as claimed in claim 1, wherein: the auxiliary coordination agent is one or two of potassium oxalate, polyacrylamide, aminopyridine, S-methylisothiourea sulfate and sodium n-dodecyl diphenyl ether disulfonate.
5. The formulation of the cyanide-free electrogilding solution for wafers as claimed in claim 1, wherein: the additional additives include organic additives and inorganic additives.
6. The formulation of the cyanide-free electrogilding solution for wafers as claimed in claim 5, wherein: the organic additive is any one or more of butyl hydroxy anisole, tert-butyl hydroquinone, dibutyl hydroxy toluene and thymine, and the inorganic additive is any one of sodium phenolate and sodium stearate.
7. A preparation method of a wafer cyanide-free gold electroplating liquid formula is characterized by comprising the following steps:
s1, preparing, namely weighing N, N-dimethylethanolamine, a main coordination agent, an auxiliary coordination agent, gold potassium chloride, ultrapure water, potassium carbonate, an additional additive, potassium tartrate and phenylalanine in corresponding parts, and placing the weighed materials in a container for storage;
s2, dissolving, namely adding the ultrapure water into a vessel, then adding N, N-dimethylethanolamine, a main coordination agent and an auxiliary coordination agent into the vessel to dissolve for 10-20min, and standing for 10min after the dissolution is finished;
s3, stirring, then introducing the mixed solution in the vessel into an ultrasonic stirrer for stirring for 30-40min, then obtaining a stirred mixed solution, and then pouring the stirred mixed solution into the vessel;
S4, performing primary water bath, namely putting the vessel into a water bath heating tank, heating to 70-80 ℃, then sequentially pouring the potassium chloride, the potassium carbonate, the potassium tartrate and the phenylalanine into the vessel to be fully dissolved, and taking the vessel out of the water bath heating tank after the potassium chloride, the potassium carbonate, the potassium tartrate and the phenylalanine are dissolved;
s5, cooling, then pouring the organic additive in the additional additive into the vessel, and then standing the vessel until the vessel is cooled to room temperature;
s6, performing water bath twice, then putting the vessel into the water bath heating tank again, heating to 85-90 ℃, after heating for 20-30min, putting the inorganic additive into the vessel, then continuously heating for 20-30min again, then stirring the vessel for 2min, and then taking the vessel out of the water bath heating tank;
and S7, adding the remaining ultrapure water into the vessel, and stirring for 10-20min by using a stirrer to obtain the cyanide-free electrogilding liquid medicine for the wafer.
8. The method for preparing the chemical formula of the cyanide-free electrogilding solution for wafers according to claim 7, wherein the chemical formula comprises the following steps: in step S7, the rotation speed of the stirrer is 20-30 r/S.
9. The method for preparing the wafer cyanide-free gold electroplating solution formula according to claim 7, wherein the method comprises the following steps: in step S5, the vessel is cooled to room temperature at a rate of 5 deg.C/min.
10. The method for preparing the wafer cyanide-free gold electroplating solution formula according to claim 7, wherein the method comprises the following steps: in step S7, the capacity of the vessel is 500-3000 ml.
CN202210405689.0A 2022-04-18 2022-04-18 Formula and preparation method of cyanide-free electrogilding liquid medicine for wafer Pending CN114752974A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103741181A (en) * 2014-01-10 2014-04-23 哈尔滨工业大学 Multi-coordination-agent cyanide-free electrogilding liquid and electrogilding process
CN103741180A (en) * 2014-01-10 2014-04-23 哈尔滨工业大学 Cyanide-free bright electrogilding additive and application thereof
CN104233384A (en) * 2014-09-17 2014-12-24 朱忠良 Cyanide-free gold electroplating solution and electroplating process using same
CN105350035A (en) * 2015-11-25 2016-02-24 广东致卓精密金属科技有限公司 Organic amine system non-cyanide electroplating gold plating bath and method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103741181A (en) * 2014-01-10 2014-04-23 哈尔滨工业大学 Multi-coordination-agent cyanide-free electrogilding liquid and electrogilding process
CN103741180A (en) * 2014-01-10 2014-04-23 哈尔滨工业大学 Cyanide-free bright electrogilding additive and application thereof
CN104233384A (en) * 2014-09-17 2014-12-24 朱忠良 Cyanide-free gold electroplating solution and electroplating process using same
CN105350035A (en) * 2015-11-25 2016-02-24 广东致卓精密金属科技有限公司 Organic amine system non-cyanide electroplating gold plating bath and method

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