CN103018264A - Method for detecting dispersity of nickel powder - Google Patents
Method for detecting dispersity of nickel powder Download PDFInfo
- Publication number
- CN103018264A CN103018264A CN2012103726196A CN201210372619A CN103018264A CN 103018264 A CN103018264 A CN 103018264A CN 2012103726196 A CN2012103726196 A CN 2012103726196A CN 201210372619 A CN201210372619 A CN 201210372619A CN 103018264 A CN103018264 A CN 103018264A
- Authority
- CN
- China
- Prior art keywords
- nickel powder
- slurry
- slide
- dispersiveness
- electron microscope
- 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.)
- Granted
Links
Images
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention provides a method for detecting dispersity of nickel powder. The method comprises the following steps of: taking 3-5g of nickel powder into a beaker, adding 170-190ml of absolute ethyl alcohol, and stirring and performing ultrasonic treatment in ultrasonic waves for 5-15 minutes at the same time; performing static settlement for layering after the ultrasonic treatment is finished, wherein the upper layer is clear alcohol, and the lower layer is nickel powder slurry; taking the nickel powder slurry at the lower layer to a slide, coating the nickel powder slurry into a slurry tape with the length of 1-5cm through pulping tape equipment, and drying the slurry tape and the slide together; putting the dried slurry tape and the slide into a sample chamber of a scanning electron microscope, adjusting the parameters of the scanning electron microscope, and scanning and photographing; and analyzing the scanned and photographed photos. According to the method, the dispersity of nickel powder is rapidly and accurately detected, and the dispersing conditions of the nickel powder can be intuitively and clearly observed.
Description
Technical field
The present invention relates to powder detection technique field, be specifically related to a kind of method that detects the nickel powder dispersiveness.
Background technology
Nickel powder, as the nickel powder that adopts the PVD method to make, be mainly used in the electrocondution slurry field, can replace silver powder to be applied to wiring, encapsulation, connection in large scale integrated circuit plate, printed circuit board (PCB), the microelectronics industry etc., the miniaturization of microelectronic component is played an important role.
Along with the development of science and technology, more and more higher to the quality requirements of product, shape requirement is more and smaller and more exquisite.The requirement of microelectronic component is more and more less, and capacity requirement is increasing.Like this mean grain size of the material nickel powder made is required more and more littlely, the dispersed requirement become better and better.This dispersiveness to nickel powder is investigated and all there is very big challenge in dispersed accuracy, convenience, the efficiency that detects.
At present the dispersiveness of nickel powder detects the main indirectly method such as demonstrations of data that microscope visual inspection or roughness tester measure that adopts, and makes the dispersiveness detection of nickel powder have that proving time is long, accuracy in detection is low and can not go intuitively to observe the problems such as key point that affect the nickel powder dispersiveness.
Summary of the invention
Technical matters to be solved by this invention provide a kind of fast, accurately and can observe the method for the detection nickel powder dispersiveness of the dispersed situation of nickel powder visual and clearly.
The technical solution adopted in the present invention is:
A kind of method that detects the nickel powder dispersiveness, the method has following operation steps:
(1) gets 3～5g nickel powder to beaker, add 170～190ml absolute ethyl alcohol, ultrasonic 5～15min while stirring in ultrasound wave;
(2) staticly settle after ultrasonic the finishing, make layering to occur, it is clarification alcohol at the middle and upper levels, and lower floor is the nickel powder slurry;
(3) the nickel powder slurry that takes out lower floor spreads to the long slurry band of 1～5cm with slurrying strip equipment with the nickel powder slurry to slide, then the slurry band is dried together with slide;
(4) the slurry band after will drying is put into the sample chamber of scanning electron microscope together with slide, adjusts the scanning electron microscope parameter, carries out scanning shoot;
(5) photo of scanning shoot is analyzed.
Ultrasound wave adopts 20～60 ℃ constant-temperature ultrasonic in the described step (1).
Slurrying strip equipment is stainless steel in the described step (3), and limit for height is that 0.001mm, limit for width are 4cm, and the height of the slurry band that namely becomes with this slurrying strip equipment making is 0.001mm, the wide 4cm of being.
After the photo of scanning shoot analyzed contrast, the crucial form of expression of finding affect the nickel powder dispersiveness was powder ball, and what and size of powder ball directly affect the whole dispersiveness of sample.To this, for we have carried out classification and process for the dispersiveness of nickel powder, better show the dispersed data of nickel powder.The dispersiveness classification of nickel powder is as shown in table 1.
Table 1
| The nickel powder type | Characteristics |
| The A type | Surfacing, place, the visual field is without powder ball or a small amount of little powder ball (powder ball diameter≤5 μ m), 0.3mm are arranged 2Interior powder ball quantity is less than or equal to 10 places |
| Type B | The surface is substantially neat, powder ball little (powder ball diameter≤5 μ m), 0.3mm 2Interior powder ball quantity is between place, 10 place to 30 |
| The C type | The surface is substantially neat, and powder ball is large (powder ball diameter＞5 μ m), 0.3mm 2Interior powder ball quantity is less than or equal to 20 places |
| The D type | Surface irregularity, 0.3mm 2Interior powder ball quantity is greater than 30 places |
Compared with prior art, the present invention has following remarkable advantage and beneficial effect:
1, scanning electron microscope of the present invention directly is presented at the dispersed index of nickel powder on the photo of scanning shoot, both fast, directly perceived, embodied exactly again dispersed quality and the relevant surfaces characteristic of nickel powder.Adopt the dispersed detection method of nickel powder of scanning electron microscope simple to operate, shooting clear, powder phenomenon be obvious, and can observe intuitively the crucial form of expression that affect the nickel powder dispersiveness, draws accurately nickel powder dispersiveness data.
2, the present invention can judge the whole dispersed of powder quickly and intuitively, and can observe out intuitively affect the nickel powder dispersiveness key factor where or where be embodied in, seek out and cause dispersed bad reason, thereby can instruct production, be convenient to carry out targetedly production technology and improve.
Description of drawings
The electron scanning micrograph of A type nickel powder in the dispersiveness classification of shown in Figure 1 is nickel powder of the present invention;
The electron scanning micrograph of Type B nickel powder in the dispersiveness classification of shown in Figure 2 is nickel powder of the present invention;
The electron scanning micrograph of C type nickel powder in the dispersiveness classification of shown in Figure 3 is nickel powder of the present invention;
The electron scanning micrograph of D type nickel powder in the dispersiveness classification of shown in Figure 4 is nickel powder of the present invention.
Embodiment
Below in conjunction with embodiment the present invention is further described in detail, but is not limited to this.
A kind of method that detects the nickel powder dispersiveness, the method has following operation steps:
(1) gets the 4g nickel powder to the 250ml beaker, add 180ml absolute ethyl alcohol (top grade absolute alcohol, purity 〉=99.98%), the setting steady temperature is 25 ℃ in ultrasound wave (BRANSON-2510 type ultrasound wave, the U.S. must letter company produce), while stirring ultrasonic 6min;
(2) staticly settle after ultrasonic the finishing, make layering (about general 5min) to occur, it is clarification alcohol at the middle and upper levels, and lower floor is the nickel powder slurry, outwells upper strata clarification alcohol;
(3) take off layer nickel powder slurry to slide with sample spoon, the nickel powder slurry is hung the slurry band of making 3cm length with slurrying strip equipment (stainless steel, limit for height 0.001mm, limit for width 4cm), then put the slurry band into vacuum drying chamber (DZF-6050 type vacuum drying chamber, PVG Rong Feng scientific instrument company limited produce) together with slide, the lower 50 ℃ of oven dry 10min of vacuum state take out;
(4) the slurry band after will drying is put into the sample chamber of scanning electron microscope (JSM-6060 type scanning electron microscope, Jeol Ltd. produce) together with slide, adjust scanning electron microscope parameter (high vacuum resolution 3.5nm, low vacuum resolution 4.0nm, accelerating potential 25kV, operating distance 15mm, enlargement factor X200), carry out scanning shoot;
(5) photo of scanning shoot is analyzed, observed dispersed quality and the relevant surfaces characteristic of nickel powder, classify according to the dispersiveness of nickel powder, draw the accurately dispersed data of nickel powder.
The above embodiment of the present invention is can not be used for restriction the present invention to explanation of the present invention, and the implication suitable with claims of the present invention and any change in the scope all should be thought to be included in the scope of claims.
Claims (3)
1. method that detects the nickel powder dispersiveness is characterized in that having following operation steps:
(1) gets 3～5g nickel powder to beaker, add 170～190ml absolute ethyl alcohol, ultrasonic 5～15min while stirring in ultrasound wave;
(2) staticly settle after ultrasonic the finishing, make layering to occur, it is clarification alcohol at the middle and upper levels, and lower floor is the nickel powder slurry;
(3) the nickel powder slurry that takes out lower floor is hung the nickel powder slurry on the slurry band of making 1～5cm length with slurrying strip equipment to slide, then the slurry band is dried together with slide;
(4) the slurry band after will drying is put into the sample chamber of scanning electron microscope together with slide, adjusts the scanning electron microscope parameter, carries out scanning shoot;
(5) photo of scanning shoot is analyzed.
2. a kind of method that detects the nickel powder dispersiveness according to claim 1: ultrasound wave adopts 20～60 ℃ constant-temperature ultrasonic in the described step (1).
3. a kind of method that detects the nickel powder dispersiveness according to claim 1: slurrying strip equipment is stainless steel in the described step (3), and limit for height is that 0.001mm, limit for width are 4cm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210372619.6A CN103018264B (en) | 2012-09-29 | 2012-09-29 | Method for detecting dispersity of nickel powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210372619.6A CN103018264B (en) | 2012-09-29 | 2012-09-29 | Method for detecting dispersity of nickel powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103018264A true CN103018264A (en) | 2013-04-03 |
| CN103018264B CN103018264B (en) | 2015-03-04 |
Family
ID=47967110
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210372619.6A Active CN103018264B (en) | 2012-09-29 | 2012-09-29 | Method for detecting dispersity of nickel powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103018264B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103792121A (en) * | 2014-02-10 | 2014-05-14 | 河北钢铁股份有限公司邯郸分公司 | Preparation method for metallurgical powdered test sample |
| CN111024564A (en) * | 2019-12-30 | 2020-04-17 | 国联汽车动力电池研究院有限责任公司 | Rapid analysis method for dispersion uniformity of solid matter in lithium ion battery slurry |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10318892A (en) * | 1997-05-21 | 1998-12-04 | Sony Corp | Method for preparing observation sample for tem and sem |
| JP2008122104A (en) * | 2006-11-08 | 2008-05-29 | Hitachi Maxell Ltd | Method of preparing sample for powder observation |
| CN101832890A (en) * | 2010-04-16 | 2010-09-15 | 西安石油大学 | Technology for preparing micro-powder sample |
| CN102200497A (en) * | 2010-03-24 | 2011-09-28 | 国家纳米技术与工程研究院 | Method for preparing powdered test sample for transmission electron microscope |
-
2012
- 2012-09-29 CN CN201210372619.6A patent/CN103018264B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10318892A (en) * | 1997-05-21 | 1998-12-04 | Sony Corp | Method for preparing observation sample for tem and sem |
| JP2008122104A (en) * | 2006-11-08 | 2008-05-29 | Hitachi Maxell Ltd | Method of preparing sample for powder observation |
| CN102200497A (en) * | 2010-03-24 | 2011-09-28 | 国家纳米技术与工程研究院 | Method for preparing powdered test sample for transmission electron microscope |
| CN101832890A (en) * | 2010-04-16 | 2010-09-15 | 西安石油大学 | Technology for preparing micro-powder sample |
Non-Patent Citations (4)
| Title |
|---|
| 许天旱 等: "SEM粉末样品的超声波制备方法研究", 《电子显微学报》, vol. 29, no. 4, 31 August 2010 (2010-08-31), pages 403 - 406 * |
| 路承杰 等: "不同分散剂对纳米镍粉在乙醇溶液中分散性能的影像", 《材料导报》, vol. 21, 31 May 2007 (2007-05-31), pages 165 - 167 * |
| 马原辉 等: "扫描电镜粉末样品的制备方法", 《实验室科学》, vol. 14, no. 1, 28 February 2011 (2011-02-28), pages 148 - 150 * |
| 黄国勇 等: "单分散球形镍粉的制备与表征", 《过程工程学报》, vol. 7, no. 6, 31 December 2007 (2007-12-31), pages 1126 - 1130 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103792121A (en) * | 2014-02-10 | 2014-05-14 | 河北钢铁股份有限公司邯郸分公司 | Preparation method for metallurgical powdered test sample |
| CN111024564A (en) * | 2019-12-30 | 2020-04-17 | 国联汽车动力电池研究院有限责任公司 | Rapid analysis method for dispersion uniformity of solid matter in lithium ion battery slurry |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103018264B (en) | 2015-03-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Xu et al. | How rheological properties affect fine-line screen printing of pastes: a combined rheological and high-speed video imaging study | |
| CN104597324B (en) | A kind of determination method of via parameters and through hole impedance value on circuit board | |
| CN103018264B (en) | Method for detecting dispersity of nickel powder | |
| EP1818950A1 (en) | Composite magnetic sheet and production method thereof | |
| Jian et al. | High performance 3D printed electronics using electroless plated copper | |
| CN103578748A (en) | Laminated ceramic electronic component and method of fabricating the same | |
| Gupta et al. | Morphology and porosity of nanoporous Au thin films formed by dealloying of AuxSi1− x | |
| TW201602272A (en) | Conductive composition | |
| Carrijo et al. | Fabrication of Ti3SiC2-based pastes for screen printing on paper-derived Al2O3 substrates | |
| Zhang et al. | A strategy to detect the effect of electrode defects on the electrical reliability in multilayer ceramic capacitors | |
| Yong et al. | A cross-sectional profile based model for stripline conductor surface roughness | |
| Barone et al. | Electrical conduction and noise spectroscopy of sodium-alginate gold-covered ultrathin films for flexible green electronics | |
| Chen et al. | 3D printing of customizable and lightweight multilayer MXene/nanocellulose architectures for tunable electromagnetic interference shielding via direct ink writing | |
| Zhang et al. | 2D conductive MOF modified MXene nanosheets for poly (vinylidene fluoride) nanocomposite with high permittivity | |
| Iyer et al. | Fabrication and characterization of cellulose-based materials for biodegradable soil moisture sensors | |
| Cheng et al. | Boosting Zinc Storage Performance of Li3VO4 Cathode Material for Aqueous Zinc Ion Batteries via Carbon‐Incorporation: A Study Combining Theory and Experiment | |
| TW201537586A (en) | A conductive paste composition for forming conductive thin film on a flexible substrate and a method for producing the same | |
| CN106247920A (en) | A kind of surface strain based on the sandwich interdigital capacitor of elastic substrates detection device | |
| Cahn et al. | Trace width effects on electrical performance of screen-printed silver inks on elastomeric substrates under uniaxial stretch | |
| CN207780119U (en) | A kind of device for dielectric constant test | |
| CN206863170U (en) | A kind of circuit board four line test machine of rigid curved probe | |
| Bodenstein et al. | Influence of printing parameters in fully pad-printed electroluminescence panels on curved surfaces | |
| US8341587B2 (en) | Method of managing process factors that influence electrical properties of printed circuit boards | |
| Kim et al. | High frequency characteristics of printed Cu conductive circuit | |
| CN104048858A (en) | Method for plating copper on rock sample for scanning electron microscope |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20161028 Address after: 223801 Suqian province high tech Development Zone, Jiangshan Road, No. 23, No. Patentee after: Jiangsu Bo move new materials Limited by Share Ltd Address before: Yinzhou District Shiqi car 315153 Zhejiang city in Ningbo province where extensive science and Technology Park Patentee before: Ningbo Guangbo New Nanomaterials Stock Co.,Ltd. |