CN108982819A - A method of examining electron level filler glue settleability - Google Patents
A method of examining electron level filler glue settleability Download PDFInfo
- Publication number
- CN108982819A CN108982819A CN201811031162.6A CN201811031162A CN108982819A CN 108982819 A CN108982819 A CN 108982819A CN 201811031162 A CN201811031162 A CN 201811031162A CN 108982819 A CN108982819 A CN 108982819A
- Authority
- CN
- China
- Prior art keywords
- sedimentation
- glue
- electron level
- settleability
- level filler
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/26—Oils; viscous liquids; paints; inks
Abstract
The present invention relates to a kind of methods for examining electron level filler glue settleability, and electron level filler glue to be measured is poured into container and is sealed, and record glue weight W1 and liquid level h0；Sealing container is horizontally arranged under the conditions of constant temperature and humidity；Using illumination and sedimentation scale h1 is recorded, when data are unchanged, the powder deposited in container is rolled into a ball into washing and drying, weighs weight W2；Sedimentation rate (%)=W2/W1*100%；Settling data is done into following arrangement: H1 (%)=(h0-h1)/h0, to sedimentation ratio H1 (%) and number of days (x) progress regression analysis is stood, obtains the sedimentation fitting function H1=f (x) of the powder；It differentiates to sedimentation fitting function and calculates rate of settling u1.Compared with prior art, the present invention realizes the effectively evaluating of electron level filling settlement, manages the quality of raw material, fills up the blank of filler inspection.
Description
Technical field
The present invention relates to copper-clad plate filler fields, more particularly, to a kind of side for examining electron level filler glue settleability
Method.
Background technique
With the development of copper-clad plate, adds inorganic filler and be widely used, inorganic filler particle size difference, glue work
The difference of skill design will cause in glue powder sedimentation and agglomeration speed is different, impacts to CCL industry, how to evaluate and fill out
Expect that settleability and glue settleability, current method are as follows:
Patent CN202126382 provides a kind of verifying attachment and method, which is mainly stirred by one group of dispersion
Device, beaker and graduated cylinder composition, can quickly detect the requirement that can filler fineness degree be satisfied with technique, although cannot be specifically anti-
The particle size of filler is mirrored, but can typically reflect very much the sedimentation degree of filler in actual use, is had
There is the advantages of at low cost, practical convenient, but this method exists as following drawbacks:
1, due to the volatilization of solvent in glue, the viscosity of glue can be got higher, and sinking speed and glue viscosity strong correlation cause
Test inaccuracy.
2, with the development of copper-clad plate, glue settleability is become better and better, if glue stands 10 days sinking speed < 10%, this
Method cannot intuitively test out the sinking speed of glue.
3, directly powder is added in alcohol and water for this method, the too low quick-fried reunion that will lead to powder of the viscosity of dispersed phase,
The sinking speed inaccuracy of actual test.
4, the visual sedimentation location of this method, there are the large errors of visual test data.
5, this method can only distinguish the biggish powder of D50, cannot effectively react copper-clad plate electron level filler
Requirement, test the good filler of settleability in this manner and be not necessarily applicable in being produced and used with copper-clad plate.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of inspection electron levels to fill out
Expect the method for glue settleability.
The purpose of the present invention can be achieved through the following technical solutions:
A method of electron level filler glue settleability is examined, using following steps:
(1) electron level filler glue to be measured is poured into container and is sealed, record glue weight W1 and liquid level h0；
(2) sealing container is horizontally arranged under the conditions of constant temperature and humidity；
(3) start to demarcate using glare light electric torch irradiation glue with Tyndall effect confirmation interface every 24 hours for 15 days
Point is recorded as sedimentation scale h1, is confirmed using glare light electric torch irradiation glue with Tyndall effect after 15 days every 48 hours
Separation record in interface is sedimentation scale h1 down from liquid level；
(4) when data are unchanged, the powder deposited in container is rolled into a ball into washing and drying, weighs weight W2；Sedimentation rate
(%)=W2/W1*100%；
(5) settling data is done into following arrangement: H1 (%)=(h0-h1)/h0.
(6) regression analysis is carried out to sedimentation ratio H1 (%) and standing number of days (d), obtains the sedimentation fitting function of the powder
H1=f (d)；
(7) it differentiates to sedimentation fitting function and calculates rate of settling u1.
Constant temperature and humidity condition in step (2) is 25 ± 5 DEG C, 45 ± 10%RH.
The powder group that 50 μm of strainer filtering agglomerate is used in step (3), then carries out washing and drying.
Step (6) input statistics processing procedure software minitab do various conditions (powder producer or production in different processing procedures because
The sub parameter such as glue viscosity, homogenizing time, coupling agent ratio) sedimentation ratio H1 (%) and stand number of days (X), recurrence
Analytic function.
Rate of settling calculation formula in step (7) are as follows:
Wherein x indicates to stand number of days,Indicate that sedimentation ratio is to the derivative for standing number of days
The rate of settling.
Compared with prior art, the invention has the following advantages that
(1) effectively evaluating for realizing electron level filling settlement manages the quality of raw material, fills up filler inspection
Blank.
(2) this method effectively carries out simple surfaces processing to electron level filler, solves the factors such as glue viscosity and causes
Reunion cause sinking speed to judge incorrectly.
(3) this method is by being put into glue using vial and sealed horizontal stewing process with scale, effectively
It has managed the volatilization of glue solvent, has reduced that glue viscosity is inconsistent to lead to practical sinking speed deviation.
(4) this method application Tyndall effect is effectively accurately surveyed using glare light electric torch observation sedimentation liquid level separation
The data for measuring sedimentation, reduce the error of visual observation
(5) this method carries out mathematics model analysis to data using statistical software, fits settling height and stands number of days
Functional relation, and give the calculation formula of sinking speed with the method for derivative derivation, settleability is judged in intuitive comparison.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
Embodiment 1-4
A kind of preparation method for examining electron level filling settlement, each component and ingredient are as shown in table 1.Wherein epoxy resin
For bisphenol A epoxide resin, phenolic resin is linear phenolic resin, and electron level filler slurry is that (A/B/C/D is aluminium hydroxide slurry
Slurry made by the different company of the aluminium hydroxide produced respectively), curing agent is dicyandiamide, and catalyst agent is -4 first of 2 ethyl
Base imidazoles, coupling agent are amino silicane coupling agent, solvent is ethylene glycol monomethyl ether.
Table 1
| Title material | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Epoxy resin (g) | 205 | 255 | 255 | 255 |
| Phenolic resin (g) | 85 | 85 | 85 | 85 |
| Electron level filler slurry (g) | 200(A) | 200(B) | 200(C) | 200(D) |
| Curing agent (g) | 6.5 | 6.5 | 6.5 | 6.5 |
| Catalyst (g) | 1.0 | 1.0 | 1.0 | 1.0 |
| Coupling agent (g) | 0.2 | 0.2 | 0.2 | 0.2 |
| Solvent (g) | 6.0 | 6.0 | 6.0 | 6.0 |
Epoxy resin, phenolic resin are added in solvent, coupling agent is injected in resin solution using sprayer, is opened
It opens normal agitation (800~1000RPM of revolving speed) and surface treatment 2h is carried out to resin solution；
It is gradually added electron level filler slurry into resin, solvent, coupling agent mixed resin solution, is opened after addition common
(800~1000RPM of revolving speed) is stirred to stir 1 hour,
It is stirred 1 hour using ultrasonic stirrer,
It opens high shear homogeneous emulsifying machine (7000-30000RPM) and stirs 0.5~1 hour to system progress homogenize process
Until 25 μm of < of fineness test (being tested using Hegman grind gage)；
Curing agent, the dissolution of catalyst solvent are finished in advance, be added to filler, solvent, coupling agent, in resin system；
It opens normal agitation (800~1000RPM of revolving speed) and 1~2h of mixed processing is carried out to system；
The viscosities il 1 of testing glue
By electron level filler to be measured prepare glue (or same copper-clad plate manufacturer pass through different process conditions modulation glue
Water) (maximum scale 165mm) sealing is poured into the vial with graduated scale, record glue weight W1:1000g and liquid level
H0:158mm
By glue sealing in the vial of sealing, bottleneck coats vaseline, is placed on constant temperature constant humidity baking oven (25 DEG C, 45%RH)
Interior marble platform is horizontal positioned.
Start to irradiate glue using glare light electric torch every 24 hours in 15 days, confirms interface separation with Tyndall effect
It is recorded as sedimentation scale h1；It is sedimentation scale h1 after 15 days down from liquid level every 48 hour records
When data are unchanged；Using the powder washing and drying of 50 μm of strainer filtering agglomerates, by what is deposited in PE bottle
Powder group's washing and drying weighs weight W2；50 μm of sedimentation rate (%)=W2/W1*100%.
Settling data is done into following arrangement: H1 (%)=(h0-h1)/h0.
Input statistics processing procedure software minitab does various conditions, and (the different processing procedure factors in powder producer or production are for example
The parameters such as glue viscosity, homogenizing time, coupling agent ratio) sedimentation ratio H1 (%) and stand number of days (X), regression analysis,
Obtain the sedimentation fitting function H1=f (d) of the powder；
It differentiates to function and calculates rate of settling u1
The results are shown in Table 2.
Table 2
The settleability of embodiment 3 is best in terms of data.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (5)
1. a kind of method for examining electron level filler glue settleability, which is characterized in that this method uses following steps:
(1) electron level filler glue to be measured is poured into container and is sealed, record glue weight W1 and liquid level h0；
(2) sealing container is horizontally arranged under the conditions of constant temperature and humidity；
(3) sedimentation scale h1 is recorded as with Tyndall effect confirmation interface separation；
(4) when data are unchanged, the powder deposited in container is rolled into a ball into washing and drying, weighs weight W2；Sedimentation rate (%)=
W2/W1*100%；
(5) settling data is done into following arrangement: H1 (%)=(h0-h1)/h0；
(6) regression analysis is carried out to sedimentation ratio H1 (%) and standing number of days (d), obtains the sedimentation fitting function H1=of the powder
f(d)；
(7) it differentiates to sedimentation fitting function and calculates rate of settling u1.
2. a kind of method for examining electron level filler glue settleability according to claim 1, which is characterized in that step
(2) the constant temperature and humidity condition in is 25 ± 5 DEG C, 45 ± 10%RH.
3. a kind of method for examining electron level filler glue settleability according to claim 1, which is characterized in that step
(3) sedimentation location is recorded using illumination in.
4. a kind of method for examining electron level filler glue settleability according to claim 1, which is characterized in that step
(4) the powder group that 50 μm of strainer filtering agglomerate is used in, then carries out washing and drying.
5. a kind of method for examining electron level filler glue settleability according to claim 1, which is characterized in that step
(7) in, rate of settling calculation formula are as follows:
Wherein x indicates to stand number of days,Indicate that sedimentation ratio is to settle to the derivative for standing number of days
Rate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811031162.6A CN108982819A (en) | 2018-09-05 | 2018-09-05 | A method of examining electron level filler glue settleability |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811031162.6A CN108982819A (en) | 2018-09-05 | 2018-09-05 | A method of examining electron level filler glue settleability |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108982819A true CN108982819A (en) | 2018-12-11 |
Family
ID=64544834
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811031162.6A Pending CN108982819A (en) | 2018-09-05 | 2018-09-05 | A method of examining electron level filler glue settleability |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108982819A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101281113A (en) * | 2007-04-03 | 2008-10-08 | 王飞 | Fuel suspended substance sedimentation detecting system |
| CN202126382U (en) * | 2011-06-02 | 2012-01-25 | 金安国纪科技（珠海）有限公司 | Detecting device for filler setteability |
| CN103717669A (en) * | 2011-08-04 | 2014-04-09 | 株式会社日立制作所 | Epoxy resin composition for cast molding and electrical device using same |
| CN107238553A (en) * | 2017-07-21 | 2017-10-10 | 华北理工大学 | The method that filling slurry critical flow velocity is detected with rate of settling detection means and with it |
| CN107603149A (en) * | 2017-08-28 | 2018-01-19 | 南亚新材料科技股份有限公司 | One kind examines electron level filler fish purpose method |
| CN107827593A (en) * | 2017-11-30 | 2018-03-23 | 贵阳开磷化肥有限公司 | One kind is without flocculation humic acid Water soluble fertilizer and preparation method thereof |
-
2018
- 2018-09-05 CN CN201811031162.6A patent/CN108982819A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101281113A (en) * | 2007-04-03 | 2008-10-08 | 王飞 | Fuel suspended substance sedimentation detecting system |
| CN202126382U (en) * | 2011-06-02 | 2012-01-25 | 金安国纪科技（珠海）有限公司 | Detecting device for filler setteability |
| CN103717669A (en) * | 2011-08-04 | 2014-04-09 | 株式会社日立制作所 | Epoxy resin composition for cast molding and electrical device using same |
| CN107238553A (en) * | 2017-07-21 | 2017-10-10 | 华北理工大学 | The method that filling slurry critical flow velocity is detected with rate of settling detection means and with it |
| CN107603149A (en) * | 2017-08-28 | 2018-01-19 | 南亚新材料科技股份有限公司 | One kind examines electron level filler fish purpose method |
| CN107827593A (en) * | 2017-11-30 | 2018-03-23 | 贵阳开磷化肥有限公司 | One kind is without flocculation humic acid Water soluble fertilizer and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| 周西顺等: "《溶液》", 30 November 1980, 河南人民出版社 * |
| 安佳丽: "聚氨酯导热灌封胶的制备及性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 张建伟等: "壳聚糖对中药甘草水提液的絮凝效果及沉降模型", 《过程工程学报》 * |
| 张浩: "电子灌封胶的制备及性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6484446B2 (en) | Curing agent for epoxy resin, epoxy resin composition and material containing the same | |
| CN109443864B (en) | Sample preparation method for detecting weather resistance of titanium dioxide | |
| CN107108226A (en) | The method for preparing graphene with high pressure homogenizing is pre-processed using high speed homogenisation | |
| EP1930359A1 (en) | High-stability microencapsulated hardener for epoxy resin and epoxy resin composition | |
| CN106833478A (en) | A kind of high-performance refractory type double-component silane modified polyether seal glue and preparation method | |
| CN108047766A (en) | A kind of method that nano-calcium carbonate surface is modified | |
| CN104119547B (en) | Application of microcrystalline wax in pre-dispersed masterbatch formula, pre-dispersed masterbatch formula and preparation method of formula | |
| CN105008071B (en) | Silver powder | |
| CN101583648A (en) | Latent curing agent | |
| CN112986060A (en) | Method for detecting dispersibility of titanium dioxide in oil paint | |
| CN108982819A (en) | A method of examining electron level filler glue settleability | |
| CN106318056A (en) | Anti-irradiation easy-decontamination paint and preparation method thereof | |
| CN103242705A (en) | ITO (Indium Tin Oxide) conductive glass temporary protection printing ink and preparation method thereof | |
| CN112858120A (en) | Method for testing ink fineness by adopting laser particle size analyzer | |
| CN110144186B (en) | Filler-free underfill adhesive and preparation method thereof | |
| CN109912932A (en) | A kind of halogen-free adhesive of high CTI value and its preparation method and application | |
| CN104502566A (en) | Method for testing water content of crude oil | |
| CN202126382U (en) | Detecting device for filler setteability | |
| CN107603149B (en) | Method for detecting electronic grade filler fish eyes | |
| CN109589632B (en) | Recovery method of stripping liquid | |
| CN105911190A (en) | Method for extracting nuciferine in folium nelumbinis by aid of ultrasonic processes | |
| CN105838036A (en) | Dielectric slurry, and preparation and application thereof | |
| CN110577788A (en) | Powder coating for food contact and preparation method thereof | |
| CN206536692U (en) | Silicone adhesive twin-screw production line base-material quality testing control system | |
| CN109777104A (en) | Aqueous polyether sulfone dispersion liquid and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181211 |