CN115594171A - Carbon pore process nano graphite dispersion liquid and preparation method thereof - Google Patents
Carbon pore process nano graphite dispersion liquid and preparation method thereof Download PDFInfo
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Abstract
The invention provides a carbon pore process nano graphite dispersion liquid and a preparation method thereof. The invention adopts nano graphite/reduced nano graphite oxide/conductive carbon black as a conductive substrate, ensures that the carbon hole dispersion liquid has good dispersion effect, can be stored for a long time without generating sedimentation, and can obtain uniform adsorption and a good conductive film after acting on a PCB (printed circuit board) through hole. The nano graphite dispersion liquid has good dispersion effect, can keep the problem of sedimentation for 1 year, has uniform distribution of carbon films formed on the hole walls, low resistivity and good conductive effect, and has excellent electroplating quality.
Description
Technical Field
The invention relates to the technical field of circuit board hole metallization, in particular to a carbon hole process nano graphite dispersion liquid and a preparation method thereof.
Background
The carbon hole process is a process for metallizing the holes, and the main process flow of the process is glue removal → neutralization → whole holes → carbon holes → acid cleaning → drying → whole holes → carbon holes → micro-etching → drying, the time of the whole process is short, toxic volatile chemicals such as formaldehyde and the like do not exist, noble metal palladium is not needed to be used as a copper deposition catalyst, and the process has the excellent characteristics of environmental friendliness, short process flow and low cost, and is a new process for replacing the traditional chemical copper deposition. The nano graphite/conductive carbon black is used to prepare dispersion liquid which is adsorbed on glass fibers and base materials on the hole wall of the printed circuit board to form a uniform and fine conductive layer.
Most of the conventional carbon pore process dispersions use graphite particles/carbon black as a conductive matrix, for example, patent US 5389270a discloses a composition and a method for preparing a non-conductive substrate for electroplating, which has good conductivity but poor dispersion performance, and since the graphite particles are in a sheet structure, an adsorption layer is easily too thick when being adsorbed on the pore wall of a circuit board, and the conductivity is inferior to that of a mixture of nano-graphite and conductive carbon black.
The invention adopts nano graphite/reduced nano graphite oxide/conductive carbon black as a conductive substrate, ensures that the carbon hole dispersion liquid has good dispersion effect, can be stored for a long time without generating sedimentation, and can obtain uniform adsorption and a good conductive film after acting on a PCB (printed circuit board) through hole.
Disclosure of Invention
The invention provides a carbon pore process nano graphite dispersion liquid and a preparation method thereof, aiming at the defects of the prior art, the invention adopts nano graphite/reduced oxidized nano graphite/conductive carbon black as a conductive substrate, ensures that the carbon pore dispersion liquid has good dispersion effect, can be kept for a long time without generating sedimentation, and can obtain uniform adsorption and a good conductive film after acting on a PCB (printed Circuit Board) through hole.
The technical scheme of the invention is as follows: a carbon pore process nano graphite dispersion liquid comprises a conductive matrix, an alkaline agent, a dispersing agent, a surfactant, a binder and a solvent.
Preferably, the dispersion comprises the following components in percentage by weight:
0.02-5% of conductive substrate;
0.05-5 parts of alkaline agent;
0.02-5% of dispersant;
0.05 to 1.5 percent of surfactant;
0.01 to 3 percent of binder
The balance of solvent.
Preferably, the dispersion comprises the following components in percentage by weight:
0.1-3% of conductive substrate;
0.5-2 parts of alkaline agent;
0.1 to 2 percent of dispersant;
0.1 to 1 percent of surfactant;
0.05 to 1.5 percent of binder
The balance of solvent.
Preferably, the conductive matrix is a composition of reduced-oxidized nano graphite, nano graphite and conductive carbon black, and the ratio of the reduced-oxidized nano graphite to the conductive carbon black is as follows: (0.1-3): 1: (0.05-1).
Preferably, the layer thickness of the reduced nano graphite oxide is 60-450nm; the sheet diameter is 200-500nm; the layer thickness of the nano graphite is 60-150nm; the sheet diameter is 200-500nm;
the particle size of the conductive carbon black is 80-500nm.
Preferably, the alkaline agent is KOH and K 2 CO 3 In a ratio of (0.5-3): (7-9.5) maintaining the dispersion at pH =10.5-11.5.
Preferably, the dispersant is one or a mixture of more of a dispersing agent NNO, a dispersing agent MF, alkyl polyether (PO-EO copolymer), nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, dodecyl polyoxyethylene ether, dinonylphenol polyoxyethylene ether, diethanolamide stearic acid monoglyceride and acrylic emulsion.
Preferably, the surfactant is one or a mixture of polyethylene glycol, polyethylene oxide propylene oxide block polymer, isooctanol polyoxyethylene ether phosphate, fatty acid methyl ester ethoxylate, polyvinyl alcohol, polypropylene alcohol, polyether amine and polyvinylpyrrolidone.
Preferably, the binder is at least one selected from the group consisting of a para-diethylene glycol fatty acid ester, glycerol monostearate, polyoxyethylene sorbitan monostearate, polyoxypropylene mannitol dioleate, tetraethylene glycol monostearate, polyoxypropylene stearate, polyoxyethylene lanolin alcohol, polyoxyethylene acrylate, polyoxyethylene alkylphenol, polyoxyethylene alkyl ether, polyacrylic acid, and polyoxyethylene monolaurate.
Preferably, the invention also provides a preparation method of the carbon pore process nano graphite dispersion liquid, which comprises the following steps:
s1), firstly, dissolving a part of nano graphite and sodium nitrate in concentrated sulfuric acid, then slowly adding potassium permanganate, and maintaining for 5 hours at 100 ℃;
s2), filtering the solution, reducing the filter residue by using hydrazine hydrate, and adding the reduced-oxidized nano-graphite filter residue into the solution after filtering to obtain a reduced-oxidized nano-graphite solution;
s3) adding another part of nano graphite into the reduced and oxidized nano graphite solution, wherein the part of nano graphite is used as one part of the conductive matrix;
s4) adding conductive carbon black accounting for a certain proportion of the nano graphite into the solution obtained in the step S3);
and S5), then adding a certain amount of alkaline agent, dispersant, surfactant, adhesive and solvent, stirring for 2 hours by using a high-speed cutting machine, and putting into ultrasonic equipment for ultrasonic treatment for 2 hours to obtain the nano graphite dispersion liquid.
Preferably, step S1), the nano-graphite: the mass ratio of sodium nitrate is not 1:1, (the mass ratio of the nano graphite to the potassium permanganate is 1:3.
Preferably, in step S2), the molar ratio of the nano-graphite to the hydrazine hydrate is 1:3.
preferably, the mass ratio of the reduced graphite oxide, the nano graphite and the conductive carbon black is as follows: (0.1-3): 1: (0.05-1).
The invention has the beneficial effects that:
1. the nano-graphite dispersion liquid has good dispersion effect, can keep the problem of sedimentation for 1 year, and has the advantages of uniform distribution of carbon films formed on the hole walls, low resistivity, good conductive effect and excellent electroplating quality.
Drawings
FIG. 1 is a graph showing the particle size distribution of a dispersion prepared in example 2 of the present invention;
FIG. 2 is a graph showing a particle size distribution of a dispersion prepared in comparative example 1 of the present invention;
FIG. 3 is a graph showing DTV carbon pore results for dispersions prepared in example 2 of the present invention;
FIG. 4 is a graph showing the DTV plating effect of the dispersion prepared in example 2 of the present invention;
Detailed Description
The following further describes embodiments of the present invention in conjunction with the attached figures:
example 1
Preparation of reduced-oxidized nano graphite
S101) under the ice bath condition, dissolving 5g of nano graphite and 5g of sodium nitrate in 200ml of concentrated sulfuric acid, slowly adding 15g of potassium permanganate, continuously stirring, maintaining at 0 ℃ for 2 hours, heating to 80 ℃, stirring for 2 hours, cooling, filtering out the solution, cleaning a filter cake with 3% hydrogen peroxide, removing residual potassium permanganate and manganese dioxide to obtain brown oxidized nano graphite, and performing vacuum drying;
s102), then adding 5g of oxidized nano graphite into 1L of deionized water, then adding 5ml of hydrazine hydrate, stirring and heating the system to 98 ℃ for 4 hours, cooling and filtering to obtain black redox nano graphite.
Example 2
Preparation of nano-graphite dispersion liquid
The weight fractions of the components are as follows: 4.1% of conductive matrix, 9% of alkaline agent, 2% of dispersing agent, 1% of surfactant, 1% of binder and 82.9% of deionized water.
Wherein, the conductive substrate is: reducing and oxidizing the nano graphite: nano graphite: conductive carbon black =1:1:0.05 percent of the total weight of the mixture,
the alkaline agent is: KOH: k 2 CO 3 ＝1：7；
The dispersing agent is: dispersing agent NNO: dispersing agent MF: nonylphenol polyoxyethylene ether =2:1:0.5;
the surface active agent is: polyethylene glycol: polyethylene oxide propylene oxide block polymer: polyetheramine =1:2: 2;
the adhesive is as follows: diethylene glycol fatty acid ester: tetraethylene glycol monostearate: polyoxypropylene stearate =1:1:3;
82.9g of deionized water;
stirring, stirring in a high-speed cutting machine for 2h, and ultrasonic treating in an ultrasonic instrument for 2h to obtain the nano graphite dispersion.
Example 3
Preparation of nano-graphite dispersion liquid
The weight fractions of the components are as follows: 3.6% of conductive matrix, 7% of alkaline agent, 1% of dispersing agent, 0.6% of surfactant, 0.3% of binder and 87.5% of deionized water.
Wherein the conductive matrix is: reducing and oxidizing the nano graphite: nano graphite: conductive carbon black =3:1:0.05%, and the alkaline agent is: KOH: k is 2 CO 3 ＝1：6；
The dispersing agent is: dispersing agent NNO: dinonyl phenol polyoxyethylene ether: dinonylphenol polyoxyethylene ether =2:1:0.5;
the surface active agent is: isooctanol polyoxyethylene ether phosphate: fatty acid methyl ester ethoxylate: polyvinyl alcohol: polypropylene glycol =1:2:2:1;
the adhesive is as follows: polyoxypropylene mannitol dioleate: tetraethylene glycol monostearate: polyoxypropylene stearate =1:1:3;
87.5g of deionized water, stirring uniformly, putting into a high-speed cutting machine, stirring for 2h, and then putting into an ultrasonic instrument for ultrasonic treatment for 2h to obtain the nano-graphite dispersion liquid.
Example 4
Preparation of nano-graphite dispersion liquid
The weight fractions of the components are as follows: 4.4% of conductive matrix, 6% of alkaline agent, 0.8% of dispersing agent, 0.3% of surfactant, 0.6% of binder and 88.0% of deionized water.
Wherein the conductive matrix is: reducing and oxidizing the nano graphite: nano graphite: conductive carbon black =0.5:1:0.05 percent of the total weight of the mixture,
the alkaline agent is: KOH: k 2 CO 3 ＝1：9；
The dispersing agent is: dispersing agent MF: dinonyl phenol polyoxyethylene ether: diethanolamide stearic acid monoglyceride =2:0.8:0.8;
the surface active agent is: polyether amine: polyvinylpyrrolidone: isooctyl alcohol polyoxyethylene ether phosphate =1:2: 2;
the adhesive is as follows: polyoxypropylene stearate: polyoxyethylene lanonol ethers: polyoxyethylene acrylate =1:1:3;
and 82.9g of deionized water, stirring uniformly, putting into a high-speed cutting machine, stirring for 2 hours, and then putting into an ultrasonic instrument for ultrasonic treatment for 2 hours to obtain the nano-graphite dispersion liquid.
Example 5
Preparation of nano-graphite dispersion liquid
The weight fractions of the components are as follows: 4.0% of conductive matrix, 8% of alkaline agent, 0.8% of dispersing agent, 0.3% of surfactant, 0.6% of binder and 86.3% of deionized water.
Wherein the conductive matrix is: reduction and oxidation of nano-graphite: nano graphite: conductive carbon black =1:1:0.05 percent of the total weight of the mixture,
the alkaline agent is: KOH: k 2 CO 3 ＝1：9；
The dispersing agent is: dispersing agent NNO: dinonyl phenol polyoxyethylene ether: diethanolamide stearic acid monoglyceride =2:1:1;
the surface active agent is: polyether amine: polyvinylpyrrolidone: isooctyl alcohol polyoxyethylene ether phosphate =1:2: 2;
the adhesive is as follows: polyoxypropylene stearate: polyoxyethylene lanonol ethers: polyoxyethylene acrylate =1:1:3;
86.3g of deionized water, stirring uniformly, putting into a high-speed cutting machine, stirring for 2 hours, and then putting into an ultrasonic instrument for ultrasonic treatment for 2 hours to obtain the nano-graphite dispersion liquid.
Example 6
Preparation of nano-graphite dispersion liquid
The weight fractions of the components are as follows: 4.2% of conductive matrix, 8% of alkaline agent, 0.5% of dispersing agent, 0.3% of surfactant, 0.4% of binder and 88.0% of deionized water.
Wherein the conductive matrix is: reducing and oxidizing the nano graphite: nano graphite: conductive carbon black =1.5:1:0.05 percent;
the alkaline agent is: KOH: k 2 CO 3 ＝1：9；
The dispersing agent is: dispersing agent MF: polyoxyethylene nonyl phenyl ether: diethanolamide stearic acid monoglyceride =1.5:1: 1;
the surface active agent is: polyether amine: polyvinylpyrrolidone: isooctyl alcohol polyoxyethylene ether phosphate =1:1: 1;
the adhesive is as follows: polyoxypropylene stearate: polyoxyethylene lanonol ethers: polyoxyethylene acrylate =1:1: 1;
and 82.9g of deionized water, stirring uniformly, putting into a high-speed cutting machine, stirring for 2 hours, and then putting into an ultrasonic instrument for ultrasonic treatment for 2 hours to obtain the nano-graphite dispersion liquid.
Example 7
Performance testing
1. After the dispersion was prepared, the following procedure was followed for testing
Cleaning → whole hole → nano graphite carbon hole → acid cleaning → drying → micro etching.
The nano-graphite carbon pore treatment was performed using the nano-graphite dispersion prepared in examples 2 to 6 at a temperature of 25 ± 5 ℃ for 60s.
The acid wash used a 5% sulfuric acid solution for 20s.
Microetching used a sodium persulfate/sulfuric acid system with 80g of sodium persulfate dissolved in 5% sulfuric acid.
Clean use of 5% SCC-66 product from Guangdong Shuichong Ltd in aqueous solution for 30s;
the whole wells were prepared by dissolving 5% of SCC-67 from Guangdong Shuichi GmbH in water at 50 + -5 deg.C for 60s.
2. Particle size measurement of nano-graphite dispersion
0.05ml of the nano-graphite dispersion was diluted 2000 times with deionized water, and the particle size was measured with a Malvern particle size Analyzer manufactured by UK corporation.
3. DTV testing
Based on the conductivity measurement of DTV-Chain/Hull panel: 25ASF area is not less than 6 holes, and 10ASF area is not less than 5 holes, wherein 0.3mm plate thickness is 1.2mm; the inspection method is electroplating under the following conditions: current 1A, time 10min; the standard high area is more than 5 holes, and the low area is more than 3 holes; the test tool was a hull cell.
4. Cracking test
Percent cracking in thermal shock test: 288 ℃ C., 10s,6 times, as determined according to the industry Standard procedure IPC-TM-650-2.6.8 (Thermal Stress, plated-Through Holes).
5. Sink test
The dispersion was sealed in a graduated cylinder and the height of sedimentation was observed at intervals, and the time when stratification occurred was recorded as the time of sedimentation. The time for the occurrence of sedimentation is required to be more than or equal to 12 months, and the test results are shown in Table 1:
TABLE 1 test results
Peak 1&1 'is the same profile, and peak 2&2' is also the same profile.
The particle size distribution of the dispersion prepared in example 2 is shown in fig. 1, the DTV carbon pore result is shown in fig. 3, and the DTV plating effect is shown in fig. 4.
Comparative example 1
In this embodiment, reduced graphite oxide nanoparticles are used as the conductive matrix, and the weight fractions of the components are as follows: 4.1% of conductive matrix (reduced and oxidized nano graphite), 9% of alkaline agent, 2% of dispersing agent, 1% of surfactant, 1% of binder and 82.9% of deionized water. The dispersion C1 was obtained by following the preparation method of example 2 of the present invention.
The particle size distribution of the dispersion of this example is shown in FIG. 2.
Comparative example 2
In the embodiment, nano graphite is solely used as a conductive matrix, and the weight fractions of the components are as follows: 4.1% of conductive matrix (nano graphite), 9% of alkaline agent, 2% of dispersing agent, 1% of surfactant, 1% of binder and 82.9% of deionized water. The dispersion C2 was prepared by referring to the preparation method of example 2 of the present invention.
Comparative example 3
In this embodiment, conductive carbon black is used as a conductive matrix, and the weight fractions of the components are as follows: 4.1% of conductive matrix (conductive carbon black), 9% of alkaline agent, 2% of dispersant, 1% of surfactant, 1% of binder and 82.9% of deionized water. The dispersion C3 was obtained by carrying out the preparation in accordance with the preparation method of example two of the present invention.
Comparative example 4
In this embodiment, nano graphite + conductive carbon black is used as a conductive matrix, and the weight fractions of the components are as follows: 4.1% of conductive matrix (nano graphite and conductive carbon black), 9% of alkaline agent, 2% of dispersing agent, 1% of surfactant, 1% of binder and 82.9% of deionized water. The dispersion C4 was obtained by carrying out the preparation in accordance with the preparation method of example two of the present invention.
Comparative example 5
In this embodiment, the weight fractions of the components are: 4.1% of conductive matrix, 9% of alkaline agent, 1% of surfactant, 1% of binder and 84.9% of deionized water. The dispersion C5 was obtained by conducting the preparation according to the second preparation method of the present invention.
The dispersions of comparative examples 1-5 were tested using the test method described in example 7 and the results are shown in Table 2:
TABLE 2 test results
The peaks 1&1 'are the same distribution curve, and the peak 2&2' is also the same distribution curve.
The foregoing embodiments and description have been presented only to illustrate the principles and preferred embodiments of the invention, and various changes and modifications may be made therein without departing from the spirit and scope of the invention as hereinafter claimed.
Claims (10)
1. A carbon pore process nano graphite dispersion liquid is characterized in that: the dispersion comprises the following components in percentage by weight:
0.02-5% of conductive substrate;
0.05-5 parts of alkaline agent;
0.02-5% of dispersant;
0.05 to 1.5 percent of surfactant;
0.01 to 3 percent of binder
The balance of solvent.
2. The carbon pore process nano graphite dispersion liquid according to claim 1, characterized in that: the dispersion comprises the following components in percentage by weight:
0.1-3% of conductive substrate;
0.5-2 parts of alkaline agent;
0.1 to 2 percent of dispersant;
0.1 to 1 percent of surfactant;
0.05 to 1.5 percent of binder
The balance of solvent.
3. The carbon pore process nano graphite dispersion liquid according to claim 1 or 2, characterized in that: the conductive substrate is a composition of reduced-oxidized nano graphite, nano graphite and conductive carbon black, and the mass ratio of the reduced-oxidized nano graphite to the conductive carbon black is as follows: (0.1-3): 1: (0.05-1).
4. The carbon pore process nano graphite dispersion liquid according to claim 1 or 2, characterized in that: the thickness of the layer of the reduced and oxidized nano graphite is 60-450nm; the sheet diameter is 200-500nm; the layer thickness of the nano graphite is 60-150nm; the sheet diameter is 200-500nm;
the particle size of the conductive carbon black is 80-500nm.
5. The carbon pore process nano graphite dispersion liquid according to claim 1 or 2, characterized in that: the alkaline agent is KOH and K 2 CO 3 In a ratio of (0.5-3): (7-9.5) maintaining the dispersion at pH =10.5-11.5.
6. The carbon pore process nano graphite dispersion liquid according to claim 1 or 2, characterized in that: the dispersing agent is one or a mixture of more of a dispersing agent NNO, a dispersing agent MF, alkyl polyether (PO-EO copolymer), nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, dodecyl polyoxyethylene ether, dinonylphenol polyoxyethylene ether, diethanol amide stearic acid monoglyceride and acrylic emulsion.
7. The carbon pore process nano graphite dispersion liquid according to claim 1 or 2, characterized in that: the surfactant is one or a mixture of polyethylene glycol, polyethylene oxide propylene oxide block polymer, isooctanol polyoxyethylene ether phosphate, fatty acid methyl ester ethoxylate, polyvinyl alcohol, polypropylene alcohol, polyether amine and polyvinylpyrrolidone.
8. The carbon pore process nano graphite dispersion liquid according to claim 1 or 2, characterized in that: the binder is at least one of diethylene glycol fatty acid ester, glyceryl monostearate, polyoxyethylene sorbitan monostearate, polyoxypropylene mannitol dioleate, tetraethylene glycol monostearate, polyoxypropylene stearate, polyoxyethylene lanolin alcohol ether, polyoxyethylene acrylate, polyoxyethylene alkylphenol, polyoxyethylene alkyl formula ether, polyacrylic acid and polyoxyethylene monolaurate.
9. A method for preparing the carbon pore process nanographite dispersion of any one of claims 1 to 8, comprising the steps of:
s1), firstly, dissolving a part of nano graphite and sodium nitrate in concentrated sulfuric acid, then slowly adding potassium permanganate, and maintaining for 5 hours at 100 ℃;
s2), filtering the solution, reducing the filter residue by using hydrazine hydrate, and adding the reduced-oxidized nano-graphite filter residue into the solution after filtering to obtain a reduced-oxidized nano-graphite solution;
s3) adding another part of nano-graphite into the reduction-oxidation nano-graphite solution, wherein the part of nano-graphite is used as one part of the conductive matrix;
s4) adding conductive carbon black accounting for a certain proportion of the nano graphite into the solution obtained in the step S3);
and S5), then adding a certain amount of alkaline agent, dispersant, surfactant, adhesive and solvent, stirring for 2 hours by using a high-speed cutting machine, and putting into ultrasonic equipment for ultrasonic treatment for 2 hours to obtain the nano graphite dispersion liquid.
10. The method for preparing the carbon pore process nano-graphite dispersion liquid according to the claim 9, wherein in the step S1), the nano-graphite: the mass ratio of sodium nitrate is not 1:1, (the mass ratio of the nano graphite to the potassium permanganate is 1:3;
step S2), the molar ratio of the nano graphite to the hydrazine hydrate is 1:3.
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