CN102746795B - Polishing solution for printed circuit microsections and preparation method thereof - Google Patents
Polishing solution for printed circuit microsections and preparation method thereof Download PDFInfo
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- CN102746795B CN102746795B CN 201210200306 CN201210200306A CN102746795B CN 102746795 B CN102746795 B CN 102746795B CN 201210200306 CN201210200306 CN 201210200306 CN 201210200306 A CN201210200306 A CN 201210200306A CN 102746795 B CN102746795 B CN 102746795B
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Abstract
The invention discloses a polishing solution for printed circuit microsections and a preparation method thereof, belonging to the technical field of printed circuit board manufacture. The polishing solution is used for polishing the printed circuit board microsections, and is suitable for observational studies of polishing copper, nickel and other coatings fixed by using crystal glue. The polishing solution comprises alumina powder, gallic acid(3,4,5-trihydroxybenzoic acid) and organic solvents. The polishing solution has the characteristics of simple preparation process, low price, and long time stable storage. The microsections polished by the polishing solution have smooth surface and are convenient for observation.
Description
Technical field
The invention belongs to the Manufacturing Technology for PCB field, particularly the polishing technology of printed electronic circuit microsection in making.
Background technology
The miniaturization of printed circuit board and densification demand for development realize the hole miniaturization of inter-level interconnects function and the universalness of the interior buried blind via technology of application plate.The hole metallization process need first passes through electroless plating or black hole shape pore-forming inner conducting layer, then electroplate thickening, but toward firmly being subject to the impact that electroplating solution composition, electroplating technological parameter and design aspect ratio are large, the quality of hole metallization can't qualitatively be controlled, therefore need by the metallized effect of microsection means spy hole, finally select suitable design and electroplating solution to guarantee the high quality of hole metallization.
Make the microsection process and should guarantee that the layer on surface of metal of epoxy resin polyester resin and circuit card section is smooth smooth in the situation that do not destroy the hole metallization original effect, thereby realize the reliable observation of hole metallization quality.After the sand papering of different meshes, microsection finally also needs to experience polishing process, and the quality of polishing effect will directly affect the efficiency of observation.Polishing process is to utilize polishing cloth and polishing medium to carry out the level and smooth processing of modifying to the microsection surface, and the quality of the particles used system of polishing is huge for the polishing effect impact.The polishing medium that possesses the excellent polishing effect, its granular system must possess following requirement: (1) micro mist epigranular is consistent; (2) purity is high; (3) dispersiveness and adsorptivity are good; (4) powder granule has certain lattice form, forms sharp keen wedge angle when broken, to improve polishing efficiency; (5) suitable hardness and density are arranged, and with the aqueous solution, good wetting property and suspension are arranged.Corundum type aluminum oxide hardness is high, when its trickle powder rotates with polishing cloth, can effectively to the surface of section, carry out the trace cutting, and the surface finish of section is high, meets the basic demand of polishing effect.
Polishing medium commonly used comprises polishing powder and polishing fluid.What in polishing process, the most generally use is polishing powder, mainly contain silicon carbide polishing powder, rare-earth type polishing powder and aluminum oxide polishing powder etc., this type of polishing powder belongs to the solid phase polishing material, can realize coarse polishing process, but the powder consumption can't accurately be controlled and cause the large waste of consumption many, storage period is long easily causes particle agglomeration, and polishing powder size distribution inequality causes the cut of microsection many, affects the polishing whole structure.Polishing fluid belongs to the liquid phase polishing material, thereby is that polishing powder is dispersed in organic or inorganic solution and forms certain density polishing powder dispersion liquid.With polishing powder, compare, polishing fluid has obvious advantage: due to the parcel of liquid continuous phase, make the not directly contact each other of polishing powder particle, reduced agglomeration; Polishing fluid viscosity is low, and even particle distribution is effectively controlled usage quantity.When but the minuteness particle coacervate in polishing fluid is separated into single particle or also evenly invades organic solution by the molecular small agglomerates of a small amount of grain, particle is because surface can greatly and easily produce and soak phenomenon, if particle makes its surface form organic membrane or with electrostatic double layer or form Polymer adsorption layer etc. because soaking, capital produces positive effect to the preliminary dispersion of particle, but the degree of depth of particle is disperseed should consider the balance of dispersion of particles and reunion.And prepare reliable and stable polishing fluid, be exactly in fact the polishing powder degree of depth to be dispersed in to the process of solution, therefore must carry out by particle the surface adsorption effect that the methods such as chemical modification or chemically modified weaken particle, strengthen interparticle repulsive interaction energy, finally reduce particle generation agglomeration.(the Chinese invention patents such as Nie's blessing people, number of patent application 200610001059.8) utilize ultrasonic dispersion to prepare the rare earth polishing for chemically machinery polished, (the Chinese invention patent such as Zhang He, number of patent application 201010591103.1) utilize mechanical mixing method to prepare the silicon carbide polishing fluid, Gao Lu etc. (Chinese invention patent, number of patent application 201010170416.X) utilize the high speed shear legal system for alumina polishing solution.It is all more valuable that these prepare the related plant and instrument of the method for polishing fluid, technical process complexity, widespread use during the PCB be not suitable at heavy industrialization produces.The method that Zhai Haijun etc. (Chinese invention patent, number of patent application 201110244241.7) have adopted ball milling, processing, separate, disperse has been prepared nano diamond polishing liquid, its production process complexity, length consuming time.The invention provides a kind of method that realizes the easy making polishing fluid by ball milling refinement and agitation and dilution.
Summary of the invention
The invention provides a kind of polishing fluid that is specifically designed to polishing printed circuit board microsection, be applicable to the observational study that polishing adopts the coating such as the fixing copper of polyester resin, nickel.This polishing fluid is comprised of alumina powder jointed, gallic acid (Gallic Acid) and organic solvent, this polishing fluid has that preparation process is simple, low price, polishing fluid can be stablized the characteristics of depositing for a long time, through the microsection surfacing of its polishing, is convenient to observe.
Detailed technology scheme of the present invention:
A kind of printed electronic circuit microsection polishing fluid, comprise alumina powder jointed, gallic acid and organic solvent, and each constituent mass degree is: alumina powder jointed 0.5%～3%, gallic acid 0.1%～1%, and all the other are organic solvent; Described organic solvent is ethanol or ethylene glycol.
The preparation method of polishing fluid for a kind of printed electronic circuit microsection, comprise the steps:
Step 1: preparation gallic acid organic solution.Gallic acid is dissolved in ethanol or ethylene glycol organic solvent, is mixed with the solution of 0.5% to 1% concentration.
Step 2: ball milling.After being mixed, the alumina powder jointed gallic acid organic solution of preparing with step 1 carries out the ball milling thinning processing.
Step 3: dilution.Mixed system interpolation gallic acid, ethanol or ethylene glycol organic solvent after step 2 ball milling thinning processing disperse dilution, are mixed with final polishing fluid; The mass percentage content of alumina powder jointed in described polishing fluid, gallic acid and organic solvent is: alumina powder jointed 0.5%～3%, gallic acid 0.1%～1%, and all the other are organic solvent; Described organic solvent is ethanol or ethylene glycol.
Gallic acid is a kind of additive of stable mixed system, when the mass percent concentration in polishing fluid is 0.1%～1%, can effectively improve polishing effect, keeps alumina powder jointed uniform and stable being dispersed in organic solution.The pre-dispersed liquid that in step 1, the organic solution of gallic acid is processed as the aluminum oxide ball milling, its effect is to serve as the alumina powder jointed lubricant of ball milling refinement.The particle diameter of the alumina powder jointed particle after ball-milling processing is controlled at 100 ± 5nm, and effectively excessive the and gravitate of inhibited oxidation aluminium powder body particle size is heavy gathers in the organic solvent bottom.Aluminum oxide pre-dispersed liquid after ball-milling processing directly adds organic solvent and gallic acid disperses dilution, during dilution, adopts mechanical stirring or magnetic agitation, to accelerate the alumina powder jointed rate of dispersion at organic solvent.
The invention has the beneficial effects as follows:
The invention provides polishing fluid of a kind of PCB of being specifically designed to microsection and preparation method thereof, when quality product reaches existing standard, reduced production cost, simple and easy to operate and can stablize and deposit for a long time after polishing fluid is mixed with, do not reunite, can transport for long-distance or preserve.
The accompanying drawing explanation
Fig. 1 is polishing fluid preparation method schematic flow sheet for printed electronic circuit microsection provided by the invention.
Fig. 2 is the scanning electron microscope diagram sheet of ball milling rear oxidation aluminium powder body.
Fig. 3 is the metaloscope picture of microsection.
Embodiment
Can realize the present invention by following example:
Example 1:
The preparation of solvent system: by gallic acid, ratio as required is dissolved in ethanol, is made into the solution that concentration is 0.5% to 1%.
The solvent that takes a morsel and prepare, as lubricant, carry out ball-milling processing 12 hours to alumina powder jointed.The solvent cut that aluminum oxide suspension after ball milling use is prepared is the ratio of above-mentioned requirement extremely, and stirs.
The polishing fluid prepared that takes a morsel is placed on wetting polishing cloth, carries out polishing, and it is smooth that the polyester resin surface just can reach surfacing through processing in about ten minutes, the obvious cut of nothing under opticmicroscope.
The polishing fluid prepared can be preserved for a long time under air-proof condition.
Example 2:
The preparation of solution system: by gallic acid, ratio as required is dissolved in ethylene glycol, is made into the solution that concentration is 0.1% to 0.5%.
According to the step of example 1, the solvent that takes a morsel and prepare, as lubricant, carry out ball-milling processing 12 hours to alumina powder jointed.The solvent cut that aluminum oxide suspension after ball milling use is prepared is the ratio of above-mentioned requirement extremely, and stirs.
The polishing fluid prepared that takes a morsel is placed on wetting polishing cloth, carries out polishing, and it is smooth that copper layer surface just can reach surfacing through processing in about ten minutes, the obvious cut of nothing under opticmicroscope.
Claims (4)
1. a printed electronic circuit microsection polishing fluid, comprise alumina powder jointed, gallic acid and organic solvent, and each constituent mass degree is: alumina powder jointed 0.5%～3%, gallic acid 0.1%～1%, and all the other are organic solvent; Described organic solvent is ethanol or ethylene glycol.
2. the preparation method of a printed electronic circuit microsection use polishing fluid, comprise the steps:
Step 1: preparation gallic acid organic solution; Gallic acid is dissolved in ethanol or ethylene glycol organic solvent, is mixed with the solution of 0.5% to 1% concentration;
Step 2: ball milling; After being mixed, the alumina powder jointed gallic acid organic solution of preparing with step 1 carries out the ball milling thinning processing;
Step 3: dilution; Mixed system interpolation gallic acid, ethanol or ethylene glycol organic solvent after step 2 ball milling thinning processing disperse dilution, are mixed with final polishing fluid; The mass percentage content of alumina powder jointed in described polishing fluid, gallic acid and organic solvent is: alumina powder jointed 0.5%～3%, gallic acid 0.1%～1%, and all the other are organic solvent; Described organic solvent is ethanol or ethylene glycol.
3. the preparation method of polishing fluid for printed electronic circuit microsection according to claim 2, is characterized in that, the particle diameter of the alumina powder jointed particle after step 2 ball-milling processing is controlled at 100 ± 5nm.
4. the preparation method of polishing fluid for printed electronic circuit microsection according to claim 2, it is characterized in that, when the mixed system after step 3 pair step 2 ball milling thinning processing is diluted, adopt mechanical stirring or magnetic agitation, to accelerate the alumina powder jointed rate of dispersion at organic solvent.
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| CN 201210200306 CN102746795B (en) | 2012-06-18 | 2012-06-18 | Polishing solution for printed circuit microsections and preparation method thereof |
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| CN 201210200306 CN102746795B (en) | 2012-06-18 | 2012-06-18 | Polishing solution for printed circuit microsections and preparation method thereof |
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| CN103728167B (en) * | 2013-12-23 | 2015-09-16 | 四川材料与工艺研究所 | A kind of method that light metal hydride metallographic specimen is preserved for a long time and observation procedure |
| CN106769169A (en) * | 2017-02-17 | 2017-05-31 | 安徽国家铜铅锌及制品质量监督检验中心 | A kind of preparation method of printed circuit board failed areas sample |
| CN107699138A (en) * | 2017-10-31 | 2018-02-16 | 诺土（上海）新材料技术有限公司 | A kind of preparation method of the alumina polishing solution of water-based controlled particle size |
| CN108336218B (en) * | 2018-01-29 | 2021-12-07 | 长安大学 | Piezoelectric composite material for road and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1576339A (en) * | 2003-07-03 | 2005-02-09 | 福吉米株式会社 | Polishing composition |
| CN1787895A (en) * | 2003-05-12 | 2006-06-14 | 高级技术材料公司 | Improved chemical mechanical polishing compositions for copper and associated materials and method of using same |
| CN101041769A (en) * | 2006-03-23 | 2007-09-26 | 富士胶片株式会社 | Metal polishing slurry |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1787895A (en) * | 2003-05-12 | 2006-06-14 | 高级技术材料公司 | Improved chemical mechanical polishing compositions for copper and associated materials and method of using same |
| CN1576339A (en) * | 2003-07-03 | 2005-02-09 | 福吉米株式会社 | Polishing composition |
| CN101041769A (en) * | 2006-03-23 | 2007-09-26 | 富士胶片株式会社 | Metal polishing slurry |
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