CN103320820A - Acid bright copper-plating electroplating process - Google Patents

Acid bright copper-plating electroplating process Download PDF

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Publication number
CN103320820A
CN103320820A CN2013102410561A CN201310241056A CN103320820A CN 103320820 A CN103320820 A CN 103320820A CN 2013102410561 A CN2013102410561 A CN 2013102410561A CN 201310241056 A CN201310241056 A CN 201310241056A CN 103320820 A CN103320820 A CN 103320820A
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copper
copper plating
workpiece
brightening agent
acid
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CN2013102410561A
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CN103320820B (en
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蒋文中
杨利东
吴天东
张念利
闻国民
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河南江河机械有限责任公司
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Abstract

The invention relates to an acid bright copper-plating electroplating process. The process comprises the steps of preparation of a copper plating solution, workpiece pretreatment, acid bright copper plating and the like. The process can continuously plate multiple copper coatings which are some millimeters thick on the surface of a metal substrate without electroplating for several times; the process guarantees good binding force between electroplated cast copper and the substrate, and can bear external force from turning, milling, drawing, externally throwing and other machining; and a plating solution is good in stability and uniform in surface.

Description

The acid bright copper plating electroplating technology
Technical field
The invention belongs to the electroplating technology field, be specifically related to a kind of acid bright copper plating electroplating technology.
Background technology
Acid copper-plating has current efficiency high (near 100%), and composition is simple, can obtain the coating of full light, good toughness behind the adding brightening agent, is the at present the most superior plating of leveling property, bright property.Therefore the price of metallic copper, is widely used in China far below metallic nickel in addition.
Well-known is to contain the chlorion of finite concentration scope in the acid copper plating solution.But it is very delicate on the impact of sour copper.Prove according to theoretical investigation, when chloride ion content is on the low side, chlorion mainly exists with dsp2 hydridization form at the electronic configuration of cathodic area and copper formation surface complex, and complex ion stability is excessively strong, and causes the cathodic polarization value to increase, the required activation energy of bivalent cupric ion reduction raises, be unfavorable for cupric step-by-step reduction, cupric directly to the zerovalent copper reaction, leveling property occurs poor, coarse, the dendritic coating of coating, pin hole, even the phenomenon such as burn.When chlorine ion concentration was too high, the electronic configuration of cathodic area surface complex mainly existed with sp3d2 type form, and cathodic polarization is too small, caused the luminance brightness of copper coating to descend, the low current density district variation that walks.
At present, adopt common electroplating technology, plate the copper layer of several mm thick at metallic matrix, mainly have following problem:
When 1, coating surpassed certain thickness, the unit time, interior thickness of coating increase was too slow, and the time is longer, need to be divided into repeatedly carrying out;
2, copper layer and metallic matrix bonding force are poor, and work-ing life is short, and later process need to add man-hour, coating and Matrix separation;
3, plating bath is unstable, and the copper gold-plating can appear in coating surface, and outward appearance is very coarse, and processing causes difficulty to later process.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of acid bright copper plating electroplating technology, and this technique has overcome the coating surface unfairness, the defective of hot tearing is arranged, and the coating that this technique is electroplated is even, bright, and bonding force is good, and solidity to corrosion is stronger.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of acid bright copper plating electroplating technology comprises preparation, workpiece pre-treatment and the acid bright copper plating of copper plating solution, and these technique concrete steps are as follows:
(1) preparation of copper plating solution
The copper plating solution proportioning raw materials is with 2 m 3Deionized water be benchmark, copper sulfate is 360~440kg, sulfuric acid is 120~180kg, gac is 4~6kg, hydrochloric acid 100~180g, brightening agent A are that 12~16L and brightening agent B are 1.2~2L;
The specific configuration method is as follows:
A. under stirring, press the copper plating solution proportioning raw materials with 2 m 3Deionized water injects 3 m 3Pre-with in the groove;
B. stirring is lower, adds 120~180kg sulfuric acid in step a, and the pre-interior solution temperature of groove of using of control is between 33~37 ℃;
C. under stirring, in step b, add 360~440kg copper sulfate, be stirred to till the fully dissolving;
D. under stirring, in step c, be sprinkled into equably 4~6kg gac, stop behind stirring 1~2 h, with filtering after the solution clarification in the groove, change filtrate over to 6 m in advance 3Plating tank in;
E. stir down, add 100~180g hydrochloric acid in the filtrate in the steps d plating tank, regulate chloride ion content;
F. under stirring, add 12~16L brightening agent A and 1.2~2L brightening agent B in step e, stop behind stirring 2~3 h, the solution that obtains is copper plating solution; Described brightening agent A is hydrogen peroxide;
Described brightening agent B is mixed with by 2-mercaptobenzimidazole, sodium polydithio-dipropyl sulfonate, polyoxyethylene glycol, ethylene thiourea, sodium lauryl sulphate, hydrochloric acid and deionized water and forms, wherein, 2-mercaptobenzimidazole 0.0003~0.001g/L, sodium polydithio-dipropyl sulfonate 0.015~0.02 g/L, polyoxyethylene glycol 0.05~0.1 g/L, ethylene thiourea 0.0003~0.0008 g/L, sodium lauryl sulphate 0.05~0.1 g/L and hydrochloric acid 0.02~0.08 g/L;
(2) workpiece pre-treatment: adopt conventional alkaline copper plating technique that workpiece is carried out pre-copper facing;
(3) acid bright copper plating: put into the plating tank that contains copper plating solution at pre-copper-plated workpiece, carrying out acid bright copper plating at workpiece surface shunts workpiece simultaneously, the copper plating solution temperature is controlled between 31~37 ℃, and cathode current density is 1.5~6A/dm 2, anodic current density 0.5~2.5A/dm 2, electroplating time is 55~65 h.
The copper plating solution proportioning raw materials is with 2 m in the described step (1) 3Deionized water be benchmark, copper sulfate is 380~420kg, sulfuric acid is 140~170kg, gac is 5~6kg, hydrochloric acid 120~160g, brightening agent A are that 13~15L and brightening agent B are 1.5~1.8L.
The copper plating solution proportioning raw materials is with 2 m in the described step (1) 3Deionized water be benchmark, copper sulfate is 390~400kg, sulfuric acid is 150~160kg, gac is 5~5.5kg, hydrochloric acid 140~150g, brightening agent A are that 14~14.5L and brightening agent B are 1.6~1.7L.
To the workpiece wire that to shunt the part flow arrangement that adopts be closed circle in lower end of plating piece hanger one side mounting specifically, described closed circle is positioned at the workpiece lower end vertically over against workpiece in the described step (3).
Described wire is selected copper material.
The present invention has positive beneficial effect:
1. compare with common copper-plating technique, Technology Bright Acidic is electroplated cast copper can plate several mm thick continuously on metal base surface copper coating, does not need to electroplate several times; Electroplate cast copper and basal body binding force good, can bear car, mill, the machines such as stretching, outer throwing add external force; Bath stability is good, surface uniform.
2. the method is by adopting conventional alkaline copper plating technique that workpiece is carried out pre-treatment, and the steps such as acid bright copper plating can obtain the level and smooth copper layer of light.Wherein acidic copper-plating of bright liquid is take copper sulfate and sulfuric acid as main component, in plating bath, add brightening agent A and brightening agent B gained coating even, bright, bonding force is good, solidity to corrosion is stronger.
3. the present invention can make workpiece surface smooth by to shunting in the pretreated workpiece Technology Bright Acidic electroplating process, and coating is even.
Embodiment
The present invention is described in further detail below in conjunction with embodiment, but do not limit content of the present invention.
Embodiment 1: a kind of acid bright copper plating electroplating technology, comprise preparation, workpiece pre-treatment and the acid bright copper plating of copper plating solution, and these technique concrete steps are as follows:
(1) preparation of copper plating solution
The copper plating solution proportioning raw materials is with 2 m 3Deionized water be benchmark, copper sulfate is 400kg, sulfuric acid is 160kg, gac is 5kg, hydrochloric acid 150g, brightening agent A are that 15L and brightening agent B are 1.6L;
The specific configuration method is as follows:
A. under stirring, press the copper plating solution proportioning raw materials with 2 m 3Deionized water injects 3 m 3Pre-with in the groove;
B. under the stirring, add 160kg sulfuric acid in step a, the pre-interior solution temperature of groove of using of control is at 33 ℃;
C. under stirring, in step b, add 400kg copper sulfate, be stirred to till the fully dissolving;
D. stir down, in step c, be sprinkled into equably the 5kg gac, stop after stirring 2 h, filter after clarifying with solution in the groove in advance, change filtrate over to 6 m 3Plating tank in;
E. stir down, add 150g hydrochloric acid in the filtrate in the steps d plating tank, regulate chloride ion content;
F. stir down, add 15L brightening agent A and 1.6L brightening agent B in step e, stop after stirring 2.5 h, the solution that obtains is copper plating solution; Described brightening agent A is hydrogen peroxide;
Described brightening agent B is mixed with by 2-mercaptobenzimidazole, sodium polydithio-dipropyl sulfonate, polyoxyethylene glycol, ethylene thiourea, sodium lauryl sulphate, hydrochloric acid and deionized water and forms, wherein, 2-mercaptobenzimidazole 0.0006g/L, sodium polydithio-dipropyl sulfonate 0.02 g/L, polyoxyethylene glycol 0.05g/L, ethylene thiourea 0.0005 g/L, sodium lauryl sulphate 0.07 g/L and hydrochloric acid 0.06 g/L;
(2) workpiece pre-treatment: adopt conventional alkaline copper plating technique that workpiece is carried out pre-copper facing;
(3) acid bright copper plating: put into the plating tank that contains copper plating solution at pre-copper-plated workpiece, carrying out acid bright copper plating at workpiece surface shunts workpiece simultaneously, the copper conductor that it is closed circle in lower end of plating piece hanger one side mounting specifically that workpiece is shunted the part flow arrangement that adopts, described closed circle is positioned at the workpiece lower end vertically over against workpiece, the copper plating solution temperature is controlled at 33 ℃, and cathode current density is 1.5A/dm 2, anodic current density 0.5A/dm 2, electroplating time is 60 h.
With the copper coating workpiece that this technique obtains the copper coating of appearance is polished, without peeling; Then workpiece is carried out quick sawing, copper coating is followed between the workpiece without peeling; At last, workpiece is carried out quick cutter mill, the discovery copper coating is not peeled off yet with workpiece; Copper coating is good with the bonding force of workpiece.
Embodiment 2: a kind of acid bright copper plating electroplating technology, comprise preparation, workpiece pre-treatment and the acid bright copper plating of copper plating solution, and these technique concrete steps are as follows:
(1) preparation of copper plating solution
The copper plating solution proportioning raw materials is with 2 m 3Deionized water be benchmark, copper sulfate is 360kg, sulfuric acid is 180kg, gac is 6kg, hydrochloric acid 120g, brightening agent A are that 14L and brightening agent B are 1.5L;
The specific configuration method is as follows:
A. under stirring, press the copper plating solution proportioning raw materials with 2 m 3Deionized water injects 3 m 3Pre-with in the groove;
B. under the stirring, add 180kg sulfuric acid in step a, the pre-interior solution temperature of groove of using of control is at 35 ℃;
C. under stirring, in step b, add 360kg copper sulfate, be stirred to till the fully dissolving;
D. stir down, in step c, be sprinkled into equably the 6kg gac, stop after stirring 2 h, filter after clarifying with solution in the groove in advance, change filtrate over to 6 m 3Plating tank in;
E. stir down, add 120g hydrochloric acid in the filtrate in the steps d plating tank, regulate chloride ion content;
F. under stirring, add 14L brightening agent A and 1.5L brightening agent B in step e, stir, stop behind 3 h, the solution that obtains is copper plating solution; Described brightening agent A is hydrogen peroxide;
Described brightening agent B is mixed with by 2-mercaptobenzimidazole, sodium polydithio-dipropyl sulfonate, polyoxyethylene glycol, ethylene thiourea, sodium lauryl sulphate, hydrochloric acid and deionized water and forms, wherein, 2-mercaptobenzimidazole 0.0003g/L, sodium polydithio-dipropyl sulfonate 0.02 g/L, polyoxyethylene glycol 0.08 g/L, ethylene thiourea 0.0007g/L, sodium lauryl sulphate 0.06 g/L and hydrochloric acid 0.04g/L;
(2) workpiece pre-treatment: adopt conventional alkaline copper plating technique that workpiece is carried out pre-copper facing;
(3) acid bright copper plating: put into the plating tank that contains copper plating solution at pre-copper-plated workpiece, carrying out acid bright copper plating at workpiece surface shunts workpiece simultaneously, the copper conductor that it is closed circle in lower end of plating piece hanger one side mounting specifically that workpiece is shunted the part flow arrangement that adopts, described closed circle is positioned at the workpiece lower end vertically over against workpiece, the copper plating solution temperature is controlled at 35 ℃, and cathode current density is 3A/dm 2, anodic current density 1.5A/dm 2, electroplating time is 62 h.
With the copper coating workpiece that this technique obtains the copper coating of appearance is polished, without peeling; Then workpiece is carried out quick sawing, copper coating is followed between the workpiece without peeling; At last, workpiece is carried out quick cutter mill, the discovery copper coating is not peeled off yet with workpiece; Copper coating is good with the bonding force of workpiece.
Embodiment 3: a kind of acid bright copper plating electroplating technology, comprise preparation, workpiece pre-treatment and the acid bright copper plating of copper plating solution, and these technique concrete steps are as follows:
(1) preparation of copper plating solution
The copper plating solution proportioning raw materials is with 2 m 3Deionized water be benchmark, copper sulfate is 420kg, sulfuric acid is 160kg, gac is 5kg, hydrochloric acid 130g, brightening agent A are that 16L and brightening agent B are 1.8L;
The specific configuration method is as follows:
A. under stirring, press the copper plating solution proportioning raw materials with 2 m 3Deionized water injects 3 m 3Pre-with in the groove;
B. under the stirring, add 160kg sulfuric acid in step a, the pre-interior solution temperature of groove of using of control is at 36 ℃;
C. under stirring, in step b, add 420kg copper sulfate, be stirred to till the fully dissolving;
D. stir down, in step c, be sprinkled into equably the 5kg gac, stop after stirring 2 h, filter after clarifying with solution in the groove in advance, change filtrate over to 6 m 3Plating tank in;
E. stir down, add 130g hydrochloric acid in the filtrate in the steps d plating tank, regulate chloride ion content;
F. under stirring, add 16L brightening agent A and 1.8L brightening agent B in step e, stop behind stirring 2~3 h, the solution that obtains is copper plating solution; Described brightening agent A is hydrogen peroxide;
Described brightening agent B is mixed with by 2-mercaptobenzimidazole, sodium polydithio-dipropyl sulfonate, polyoxyethylene glycol, ethylene thiourea, sodium lauryl sulphate, hydrochloric acid and deionized water and forms, wherein, 2-mercaptobenzimidazole 0.001g/L, sodium polydithio-dipropyl sulfonate 0.015 g/L, polyoxyethylene glycol 0.08g/L, ethylene thiourea 0.0007g/L, sodium lauryl sulphate 0.08 g/L and hydrochloric acid 0.05g/L;
(2) workpiece pre-treatment: adopt conventional alkaline copper plating technique that workpiece is carried out pre-copper facing;
(3) acid bright copper plating: put into the plating tank that contains copper plating solution at pre-copper-plated workpiece, carrying out acid bright copper plating at workpiece surface shunts workpiece simultaneously, the copper conductor that it is closed circle in lower end of plating piece hanger one side mounting specifically that workpiece is shunted the part flow arrangement that adopts, described closed circle is positioned at the workpiece lower end vertically over against workpiece, the copper plating solution temperature is controlled at 36 ℃, and cathode current density is 5A/dm 2, anodic current density 2.5A/dm 2, electroplating time is 55h.
With the copper coating workpiece that this technique obtains the copper coating of appearance is polished, without peeling; Then workpiece is carried out quick sawing, copper coating is followed between the workpiece without peeling; At last, workpiece is carried out quick cutter mill, the discovery copper coating is not peeled off yet with workpiece; Copper coating is good with the bonding force of workpiece.
Embodiment 4: a kind of acid bright copper plating electroplating technology, comprise preparation, workpiece pre-treatment and the acid bright copper plating of copper plating solution, and these technique concrete steps are as follows:
(1) preparation of copper plating solution
The copper plating solution proportioning raw materials is with 2 m 3Deionized water be benchmark, copper sulfate is 360kg, sulfuric acid is 120kg, gac is 6kg, hydrochloric acid 120g, brightening agent A are that 12L and brightening agent B are 1.2L;
The specific configuration method is as follows:
A. under stirring, press the copper plating solution proportioning raw materials with 2 m 3Deionized water injects 3 m 3Pre-with in the groove;
B. under the stirring, add 120kg sulfuric acid in step a, the pre-interior solution temperature of groove of using of control is between 33 ℃;
C. under stirring, in step b, add 360kg copper sulfate, be stirred to till the fully dissolving;
D. under stirring, in step c, be sprinkled into equably the 6kg gac, stop behind the stirring 1.5h, with filtering after the solution clarification in the groove, change filtrate over to 6 m in advance 3Plating tank in;
E. stir down, add 120g hydrochloric acid in the filtrate in the steps d plating tank, regulate chloride ion content;
F. stir down, add 12 brightening agent A and 1.2 brightening agent B in step e, stop after stirring 2.5 h, the solution that obtains is copper plating solution; Described brightening agent A is hydrogen peroxide;
Described brightening agent B is mixed with by 2-mercaptobenzimidazole, sodium polydithio-dipropyl sulfonate, polyoxyethylene glycol, ethylene thiourea, sodium lauryl sulphate, hydrochloric acid and deionized water and forms, wherein, 2-mercaptobenzimidazole 0.001g/L, sodium polydithio-dipropyl sulfonate 0.015 g/L, polyoxyethylene glycol 0.09 g/L, ethylene thiourea 0.0005 g/L, sodium lauryl sulphate 0.05g/L and hydrochloric acid 0.04g/L;
(2) workpiece pre-treatment: adopt conventional alkaline copper plating technique that workpiece is carried out pre-copper facing;
(3) acid bright copper plating: put into the plating tank that contains copper plating solution at pre-copper-plated workpiece, carrying out acid bright copper plating at workpiece surface shunts workpiece simultaneously, the copper conductor that it is closed circle in lower end of plating piece hanger one side mounting specifically that workpiece is shunted the part flow arrangement that adopts, described closed circle is positioned at the workpiece lower end vertically over against workpiece, the copper plating solution temperature is controlled between 31~37 ℃, and cathode current density is 5A/dm 2, anodic current density 2.5A/dm 2, electroplating time is 63 h.
With the copper coating workpiece that this technique obtains the copper coating of appearance is polished, without peeling; Then workpiece is carried out quick sawing, copper coating is followed between the workpiece without peeling; At last, workpiece is carried out quick cutter mill, the discovery copper coating is not peeled off yet with workpiece; Copper coating is good with the bonding force of workpiece.

Claims (5)

1. acid bright copper plating electroplating technology comprises preparation, workpiece pre-treatment and the acid bright copper plating of copper plating solution, and it is characterized in that: these technique concrete steps are as follows:
(1) preparation of copper plating solution
The copper plating solution proportioning raw materials is with 2 m 3Deionized water be benchmark, copper sulfate is 360~440kg, sulfuric acid is 120~180kg, gac is 4~6kg, hydrochloric acid 100~180g, brightening agent A are that 12~16L and brightening agent B are 1.2~2L;
The specific configuration method is as follows:
A. under stirring, press the copper plating solution proportioning raw materials with 2 m 3Deionized water injects 3 m 3Pre-with in the groove;
B. stirring is lower, adds 120~180kg sulfuric acid in step a, and the pre-interior solution temperature of groove of using of control is between 33~37 ℃;
C. under stirring, in step b, add 360~440kg copper sulfate, be stirred to till the fully dissolving;
D. under stirring, in step c, be sprinkled into equably 4~6kg gac, stop behind stirring 1~2 h, with filtering after the solution clarification in the groove, change filtrate over to 6 m in advance 3Plating tank in;
E. stir down, add 100~180g hydrochloric acid in the filtrate in the steps d plating tank, regulate chloride ion content;
F. under stirring, add 12~16L brightening agent A and 1.2~2L brightening agent B in step e, stop behind stirring 2~3 h, the solution that obtains is copper plating solution; Described brightening agent A is hydrogen peroxide;
Described brightening agent B is mixed with by 2-mercaptobenzimidazole, sodium polydithio-dipropyl sulfonate, polyoxyethylene glycol, ethylene thiourea, sodium lauryl sulphate, hydrochloric acid and deionized water and forms, wherein, 2-mercaptobenzimidazole 0.0003~0.001g/L, sodium polydithio-dipropyl sulfonate 0.015~0.02 g/L, polyoxyethylene glycol 0.05~0.1 g/L, ethylene thiourea 0.0003~0.0008 g/L, sodium lauryl sulphate 0.05~0.1 g/L and hydrochloric acid 0.02~0.08 g/L;
(2) workpiece pre-treatment: adopt conventional alkaline copper plating technique that workpiece is carried out pre-copper facing;
(3) acid bright copper plating: put into the plating tank that contains copper plating solution at pre-copper-plated workpiece, carrying out acid bright copper plating at workpiece surface shunts workpiece simultaneously, the copper plating solution temperature is controlled between 31~37 ℃, and cathode current density is 1.5~6A/dm 2, anodic current density 0.5~2.5A/dm 2, electroplating time is 55~65 h.
2. acid bright copper plating electroplating technology according to claim 1 is characterized in that: the copper plating solution proportioning raw materials is with 2 m in the described step (1) 3Deionized water be benchmark, copper sulfate is 380~420kg, sulfuric acid is 140~170kg, gac is 5~6kg, hydrochloric acid 120~160g, brightening agent A are that 13~15L and brightening agent B are 1.5~1.8L.
3. acid bright copper plating electroplating technology according to claim 1 is characterized in that: the copper plating solution proportioning raw materials is with 2 m in the described step (1) 3Deionized water be benchmark, copper sulfate is 390~400kg, sulfuric acid is 150~160kg, gac is 5~5.5kg, hydrochloric acid 140~150g, brightening agent A are that 14~14.5L and brightening agent B are 1.6~1.7L.
4. acid bright copper plating electroplating technology according to claim 1, it is characterized in that: to the workpiece wire that to shunt the part flow arrangement that adopts be closed circle in lower end of plating piece hanger one side mounting specifically, described closed circle is positioned at the workpiece lower end vertically over against workpiece in the described step (3).
5. acid bright copper plating electroplating technology according to claim 1, it is characterized in that: described wire is selected copper material.
CN201310241056.1A 2013-06-18 2013-06-18 Acid bright copper plating electroplating technology CN103320820B (en)

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CN103469260A (en) * 2013-09-27 2013-12-25 昆山纯柏精密五金有限公司 Acid copper plating method of hardware
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CN105921706A (en) * 2016-05-19 2016-09-07 西峡龙成特种材料有限公司 On-line repair method for continuous casting crystallizer copper plate
CN106367782A (en) * 2016-08-26 2017-02-01 湖北吉和昌化工科技有限公司 Electroplating liquid of sub-acid system electroplated bright copper as well as preparation method and electroplating process of electroplating liquid
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CN111088509A (en) * 2020-01-17 2020-05-01 浙江金欣新材料科技股份有限公司 Acidic copper plating additive and preparation method thereof
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CN103469260A (en) * 2013-09-27 2013-12-25 昆山纯柏精密五金有限公司 Acid copper plating method of hardware
CN103911635B (en) * 2014-03-21 2016-02-24 复旦大学 A kind of copper electroplating solution
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