CN106398555B - A kind of solidification glue and preparation method thereof of printed circuit microsection sample preparation - Google Patents
A kind of solidification glue and preparation method thereof of printed circuit microsection sample preparation Download PDFInfo
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- CN106398555B CN106398555B CN201610370426.5A CN201610370426A CN106398555B CN 106398555 B CN106398555 B CN 106398555B CN 201610370426 A CN201610370426 A CN 201610370426A CN 106398555 B CN106398555 B CN 106398555B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
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Abstract
The invention belongs to printed circuit technical field of metallographic detection, and in particular to a kind of solidification glue and preparation method thereof of printed circuit microsection sample preparation.The solidification glue is made of component A and B component system, by mass component A include 98.5~99.5% acrylic polymer, 0.5~1.5% initiator and 0.1~0.5% surfactant；B component includes 50%~70% acrylate monomer, 0.45~1% promotor and 30~50% cosolvent.When use after mixing by component A and B component in mass ratio 1.5~2.5, it is placed in room temperature curing in embedding die, curing time is 0.5~1.5h.Solidification glue component provided by the invention is simple, and preparation method is easy to operate, molding is fast, and low in cost, heat release is gently, the transparency is good and is sliced adhesion strength height, is suitable for the preparation of printed circuit microsection sample and Metallographic Analysis of Semi.
Description
Technical field
The invention belongs to printed circuit technical field of metallographic detection, and in particular to a kind of printed circuit microsection sample preparation
Solidification glue and preparation method thereof.
Background technique
The production of printed circuit board is a kind of process that multi-process is mutually coordinated.The superiority and inferiority of preceding working procedure product quality, directly
The production for influencing next procedure is connect, or even is directly related to the quality of final products.Thus, critical process is exactly quality control
System.Printed circuit board technology till now, up to tens kinds of dedicated Quality Detection equipment, instrument.As detection means
One of microsection technology, irreplaceable great function is played in this field.
Microsection technology has many advantages, such as that equipment investment is relatively small, has a wide range of application, reliability and accuracy are high, In
In the production process of printed circuit board, effect is embodied in the following aspects: (1) in terms of the inspection of raw material, passing through metallographic
Microtomy can obtain following information: examine whether copper foil, substrate thickness meet the needs of printed circuit board production；Insulation is situated between
The arrangement mode of matter layer and prepreg；In insulating medium layer, glass fibre through broadwise arrangement mode and resin content；Lamination
Board defect fold, pin hole, scratch, pit, lamination cavity, day shift and bubble etc.；(2) in the control of production process quality, metallographic is cut
Chip technology is mainly used in the Hole Wall Roughness detection after drilling operating；Registration inspection after multilayer printed circuit board laminating process
It surveys；Hole wall desmearing effect detection；Hole metallization condition detection and throwing power evaluation；(3) in the test of product reliability,
The be embodied in thickness of coating measurement of microsection technology, Thermal Stress Experiment, thermal shock experiment and plated through-hole simulation repeat to weld
Experiment etc..
Currently, the solidification glue for making metallographic specimen can be roughly divided into epoxy resin and crylic acid resin.Generally
The solidification glue of epoxy resin is made of liquid-state epoxy resin, curing agent and catalyst, and epoxy resin is a kind of oligomer, and solid
Agent reaction generates tridimensional network and reaches final requirement after room temperature or heating.This solidification glue is transparent,
With excellent permeance property, cure shrinkage is small, solidifies 50 DEG C of maximum temperature, is suitable for hot special sensitivity or has micropore seam
Structure sample is inlayed.[2008,26 (1): PM technique 53~56] describes several vacuum using epoxy resin to document
Impregnation formulation, but this method curing time is longer, can just be fully cured within generally more than 8 hours.
Esters of acrylic acid solidification glue is generally bicomponent system, i.e. solid powder component A and liquid B component by a certain percentage
It reconciles uniformly, is placed in embedding die and solidifies, obtain microsection.In such esters of acrylic acid solidification glue solid component mainly at
Dividing is acrylic polymer, such acrylate cures glue uses oxidation-reduction system, solid using radical polymerization mechanism
Change.Document [plating and is covered with paint, lacquer, colour wash, etc., 2007,26 (12): 21~24] and Chinese patent CN104535393A, being described using self-solidifying
The method of type dental base acrylic resin powder and dental basse acrylic resin liquid production metallographic specimen, this method are easy production, and molding is rapid, but in dental base acrylic resin powder used
Mostly mixed with colorant, the cured product transparency is bad.Currently, esters of acrylic acid solidification glue is many kinds of on the market, but it is made
It is relative complex to make technique, be its cost is also relatively high.
Summary of the invention
In consideration of it, preparing that simple, rapid shaping, thermal discharge are small, low-cost can be used for printing the present invention provides a kind of
The solidification glue of circuit microsection sample preparation processed.
The present invention also provides a kind of preparation method of above-mentioned printed circuit microsection sample preparation solidification glue.
In order to solve the above technical problems, the present invention takes following technical scheme:
A kind of solidification glue of printed circuit microsection sample preparation, is made of component A and B component system, and when use is to pass through
Redox initiation system causes free radical polymerization and cured, by mass, wherein component A includes 98.5~99.5%
Acrylic polymer, 0.5~1.5% initiator and 0.1~0.5% surfactant；B component include 50%~
70% acrylate monomer, 0.45~1% promotor and 30~50% cosolvent.
Preferably, in the component A, acrylic polymer, molecular formula (R2CCH2COOR1)n, structural formula is such as
Under:
Wherein, R1Refer to methyl, ethyl, propyl, isopropyl, normal-butyl, tert-butyl, isobutyl group, iso-octyl or dodecane
Base；R2Refer to hydrogen, methyl or ethyl；Its average molecular weight is 1~60,000；
Wherein, in the component A, initiator is benzoyl peroxide, methyl ethyl ketone peroxide, cumyl peroxide, idol
Nitrogen bis-isobutyronitrile, isopropyl benzene hydroperoxide and/or tert-butyl hydroperoxide；
Wherein, in the component A, surfactant is neopelex or lauryl sodium sulfate；
Wherein, in the B component, acrylate monomer, molecular formula R4CCH2COOR3, structural formula is as follows:
R3Refer to methyl, ethyl, normal-butyl, 2,3- glycidyl, ethoxy, hydroxypropyl, hydroxyl butyl, isopropyl or tertiary fourth
Base；R4Refer to hydrogen, cyano, methyl or ethyl；
Wherein, in the B component, promotor is n,N-Dimethylaniline, N, N- dimethyl-p-toluidine, ethylenediamine, three
Ethamine, tetramethyl thiourea, vinylthiourea and/or cobalt naphthenate；
Wherein, in the B component, cosolvent is toluene, chloroform, acetone, butanone or ethyl acetate.
The preparation method of the solidification glue of above-mentioned printed circuit microsection sample preparation, includes the following steps:
Step 1: weigh acrylic polymer powder, thereto add 0.5~1.5% initiator and 0.1~
0.5% surfactant, ground and mixed is uniform, is prepared into component A；
Step 2: weighing acrylate monomer, add 0.45~1% promotor and 30~50% cosolvents, stirring thereto
It is uniformly mixed, is prepared into B component；
The solidification glue using when be by component A and B component in mass ratio 1.5~2.5 after mixing, be placed in embedding die
In solidified.Solidification temperature is room temperature, and curing time is 0.5~1.5h.
The beneficial effects of the present invention are: the solidification glue component of the printed circuit microsection sample preparation is simple, preparation method
It is easy to operate, molding is fast, low in cost, heat release is gentle, the transparency is good, high with slice adhesion strength, be suitable for printed circuit
The preparation of microsection sample and Metallographic Analysis of Semi.
Detailed description of the invention
Fig. 1 is the transparent effect figure that slice is inlayed after embodiment solidification glue is mixing cured；
Fig. 2 is the effect picture that embodiment solidification glue observes metallographic structure for microsection.
Specific embodiment
Embodiment 1
Component A
Polymethyl methacrylate 10g is weighed, adds 0.1g benzoyl peroxide and 0.05g dodecyl sulphate thereto
Sodium is uniformly mixed with mortar grinder；
B component
4g methyl methacrylate purity 99.0% and 2g acetone purity 99.5% are weighed, 0.01g N, N- are added dropwise thereto
Dimethyl-p-toluidine is uniformly mixed.
Above-mentioned prepared component A and B component 2:1 in mass ratio are placed in internal diameter 25mm, in the embedding die of high 22mm,
Solidification 30 minutes is carried out at room temperature.As shown in Figure 1, the transparent effect of slice is inlayed after mixing cured for the present embodiment solidification glue
Figure.
Embodiment 2
Component A
Weigh polymethyl methacrylate 20g；0.15g benzoyl peroxide and 0.05g detergent alkylate are added thereto
Sodium sulfonate is uniformly mixed.
B component
8g methyl methacrylate purity 99.0% and 4g ethyl acetate purity 99.5% are weighed, adds 0.03g thereto
N,N-Dimethylaniline is uniformly mixed.
Above-mentioned prepared component A and B component 2:1 in mass ratio are placed in internal diameter 25mm, in the embedding die of high 22mm,
Solidification 30 minutes is carried out at room temperature.As shown in Fig. 2, the effect of metallographic structure is observed for microsection for the present embodiment solidification glue
Fruit figure.
Claims (3)
1. a kind of solidification glue of printed circuit microsection sample preparation, is made of component A and B component system, it is characterised in that: press matter
Meter, component A include 98.5~99.5% acrylic polymer, 0.5~1.5% initiator and 0.1~0.5%
Surfactant；B component includes 50%~70% acrylate monomer, 0.45~1% promotor and 30~50% hydrotropy
Agent；
In the component A, acrylic polymer, molecular formula (R2CCH2COOR1)n, structural formula is as follows:
Wherein, R1Refer to methyl, ethyl, propyl, isopropyl, normal-butyl, tert-butyl, isobutyl group, iso-octyl or dodecyl；R2
Refer to hydrogen, methyl or ethyl；
The initiator are as follows: benzoyl peroxide, methyl ethyl ketone peroxide, cumyl peroxide, azodiisobutyronitrile, isopropylbenzene
Hydrogen peroxide and/or tert-butyl hydroperoxide；
The surfactant is neopelex or lauryl sodium sulfate；
In the B component, acrylate monomer, molecular formula R4CCH2COOR3, structural formula is as follows:
Wherein, R3Refer to methyl, ethyl, normal-butyl, 2,3- glycidyl, ethoxy, hydroxypropyl, hydroxyl butyl, isopropyl or tertiary fourth
Base；R4Refer to hydrogen, cyano, methyl or ethyl；
The promotor is N, accelerine, N, N- dimethyl-p-toluidine, ethylenediamine, triethylamine, tetramethyl thiourea, second
Alkenyl thiocarbamide and/or cobalt naphthenate；
The cosolvent is toluene, chloroform, acetone, butanone or ethyl acetate；
The average molecular weight of acrylic polymer is 1~60,000 in the component A.
2. the preparation method of the solidification glue of printed circuit microsection sample preparation as described in claim 1, includes the following steps:
Step 1: weigh acrylic polymer powder, by mass percentage thereto addition 0.5~1.5% initiator and
0.1~0.5% surfactant, ground and mixed is uniform, is prepared into component A；
Step 2: weighing acrylate monomer, add 0.45~1% promotor and 30~50% cosolvents thereto, be stirred
Uniformly, it is prepared into B component.
3. the solidification glue of printed circuit microsection sample preparation as described in claim 1, application method are as follows: by the A group of solidification glue
To divide with B component in mass ratio 1.5~2.5 after mixing, is placed in embedding die and is solidified, solidification temperature is room temperature, Gu
The change time is 0.5~1.5h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610370426.5A CN106398555B (en) | 2016-05-30 | 2016-05-30 | A kind of solidification glue and preparation method thereof of printed circuit microsection sample preparation |
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| CN201610370426.5A CN106398555B (en) | 2016-05-30 | 2016-05-30 | A kind of solidification glue and preparation method thereof of printed circuit microsection sample preparation |
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| CN106398555B true CN106398555B (en) | 2019-11-05 |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108168970A (en) * | 2017-12-18 | 2018-06-15 | 西安赛特思迈钛业有限公司 | A kind of cold working method for making sample of metallographic specimen |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1580170A (en) * | 2003-08-01 | 2005-02-16 | 沈阳黎明航空发动机(集团)有限责任公司 | Adhesive for making sticky brazing filler material |
| CN101343520A (en) * | 2007-07-09 | 2009-01-14 | 周建明 | Double-component cold curing adhesive, preparation and application thereof |
| CN103360553A (en) * | 2013-07-15 | 2013-10-23 | 肇庆富盛复合材料有限公司 | Normal-temperature bi-component or multi-component curing system and application thereof |
| CN103911079A (en) * | 2014-04-10 | 2014-07-09 | 临海市吉谷胶粘剂有限公司 | Transparent regular-temperature curing acrylate adhesive with high intensity |
| CN104231946A (en) * | 2014-10-08 | 2014-12-24 | 天津儒创新材料科技有限公司 | Adhesive special for normal-temperature quickly-cured organic glass |
-
2016
- 2016-05-30 CN CN201610370426.5A patent/CN106398555B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1580170A (en) * | 2003-08-01 | 2005-02-16 | 沈阳黎明航空发动机(集团)有限责任公司 | Adhesive for making sticky brazing filler material |
| CN101343520A (en) * | 2007-07-09 | 2009-01-14 | 周建明 | Double-component cold curing adhesive, preparation and application thereof |
| CN103360553A (en) * | 2013-07-15 | 2013-10-23 | 肇庆富盛复合材料有限公司 | Normal-temperature bi-component or multi-component curing system and application thereof |
| CN103911079A (en) * | 2014-04-10 | 2014-07-09 | 临海市吉谷胶粘剂有限公司 | Transparent regular-temperature curing acrylate adhesive with high intensity |
| CN104231946A (en) * | 2014-10-08 | 2014-12-24 | 天津儒创新材料科技有限公司 | Adhesive special for normal-temperature quickly-cured organic glass |
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