CN109444195A - A kind of preparation method of the scanning electron microscope sample of nanoscale barium titanate powder - Google Patents
A kind of preparation method of the scanning electron microscope sample of nanoscale barium titanate powder Download PDFInfo
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- CN109444195A CN109444195A CN201811611262.6A CN201811611262A CN109444195A CN 109444195 A CN109444195 A CN 109444195A CN 201811611262 A CN201811611262 A CN 201811611262A CN 109444195 A CN109444195 A CN 109444195A
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- barium titanate
- titanate powder
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- electron microscope
- scanning electron
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/30—Accessories, mechanical or electrical features
- G01N2223/312—Accessories, mechanical or electrical features powder preparation
Abstract
The present invention discloses a kind of preparation method of the scanning electron microscope sample of nanoscale barium titanate powder, the following steps are included: S1, dispersion, nanoscale barium titanate powder and dispersing agent are taken according to the proportion of mass ratio 1:5, nanoscale barium titanate powder is poured into dispersing agent and ultrasound, the suspension of barium titanate is obtained；Rectangular silicon glue frame is placed in the sample stage with conducting resinl, and the suspension that a dropping step S1 is obtained into rectangular silicon glue frame by S2, sampling；It is then placed in baking oven and dries, obtain barium titanate powder primary sample；S3, tabletting sample preparation, S4, metal spraying obtain the nanoscale barium titanate powder sample for being able to carry out scanning electron microscope test；This method can guarantee being uniformly dispersed for barium titanate powder particle, and surface particles overall leveling avoids scanning electron microscope vacuum chamber from being contaminated, and improve picture quality.
Description
Technical field
The present invention relates to the preparation technical field of scanning electron microscope sample, specifically a kind of nanoscale barium titanate powder
Scanning electron microscope sample preparation method.
Background technique
As a kind of new function ceramic material to grow up in recent decades, barium titanate is due to its unique electronics knot
Structure has multiple functions, and purposes is relatively broad.Wherein, electric property is its most important performance, as a kind of electronic ceramics material
Material, the index for influencing its performance is more, such as titanium barium molar ratio, pattern, granular size, purity.The wherein pattern of particle and big
Small measurement often by scanning electron microscope, scanning electron microscope can quickly, it is intuitive, accurately observe barium titanate powder
The case where body.
Currently, being often scanned electron microscopyc sample preparation there are two types of method: first is that powder is directly smeared for barium titanate powder
In on conducting resinl, second is that suspension is made in powder and dispersing agent, drip on silicon wafer or conducting resinl.For first method,
Although time-consuming short, for nanoscale powder, due to surface energy with higher, particle is easy to reunite, dispersibility
Not high, the pattern taken does not conform to the actual conditions, and influences the aesthetics of picture, and adhesion strength is not between the powder and conducting resinl having
It is high, it is possible to pollute vacuum chamber.For second method, if hanging drop on conducting resinl, conducting resinl conduct after drying
Substrate, surface uneven have certain influence to sample topography and picture overall aesthetics, if hanging drop is in silicon wafer
On, during drying, with the evaporation of moisture, particle is also easy to reunite.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation sides of the scanning electron microscope sample of nanoscale barium titanate powder
Method, this method can guarantee being uniformly dispersed for barium titanate powder particle, and surface particles overall leveling avoids scanning electron microscope vacuum chamber
Room is contaminated, and improves picture quality.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of preparation method of the scanning electron microscope sample of nanoscale barium titanate powder, comprising the following steps:
S1, dispersion,
Nanoscale barium titanate powder and dispersing agent are taken according to the proportion of mass ratio 1:5, nanoscale barium titanate powder is poured into dispersion
It is in agent and ultrasonic, obtain the suspension of barium titanate；
S2, sampling,
Rectangular silicon glue frame is placed in the sample stage with conducting resinl, and the suspension that a dropping step S1 is obtained into rectangular silicon glue frame；
It is then placed in baking oven and dries, obtain barium titanate powder primary sample；
S3, tabletting sample preparation,
Rectangular silicon glue frame is removed, is flattened barium titanate powder primary sample surface with sheet glass, and blow away barium titanate powder primary
Extra dust around sample；
S4, metal spraying,
Metal spraying processing is carried out to barium titanate powder primary sample, obtains the nano grade titanium for being able to carry out scanning electron microscope test
Sour barium dust sample.
Further, dispersing agent described in step S1 is the ethyl alcohol of 95% or more concentration.
Further, the temperature of step S2 baking oven is 80~90 DEG C.
Further, the sheet glass of step S3 is glass slide.
Further, it is 6*10 that the vacuum degree in vacuum chamber is sputtered when step S4 metal spraying-2Pa, electric current 5mA, sputtering time
For 30s.
The invention has the advantages that
One, it is improved on the basis of liquid sample preparation method, the ratio of nanoscale barium titanate powder and dispersing agent is increased, is made
The higher suspension of concentration is conducive to available multiple layer powder accumulation sample after drying.
Two, silica gel rectangle frame is fixed on conducting resinl, hanging drop in silica gel rectangle frame, can guaranteeing to suspend in this way
Liquid will not be spread during drying to surrounding, if not using silica gel rectangle frame, hanging drop is more on conducting resinl
Remaining suspension can be spread to surrounding at once, and the uniform powder sample of multilayer is seldom arrived after drying.
Three, tabletting is carried out with glass slide to the sample after drying, the powder sample of surfacing can be obtained, the figure taken
The clear quality of piece is high.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples:
Fig. 1 is the scanning electron microscope (SEM) photograph for the nanoscale barium titanate powder sample that the method for the present invention obtains；
Fig. 2 is the partial enlargement diagram of Fig. 1.
Specific embodiment
The present invention provides a kind of preparation method of the scanning electron microscope sample of nanoscale barium titanate powder, including following
Step:
S1, dispersion,
Nanoscale barium titanate powder and dispersing agent are taken according to the proportion of mass ratio 1:5, nanoscale barium titanate powder is poured into dispersion
It is in agent and ultrasonic, obtain the suspension of barium titanate；The dispersing agent is the ethyl alcohol using 95% or more concentration；
S2, sampling,
Rectangular silicon glue frame is placed in the sample stage with conducting resinl, and the suspension that a dropping step S1 is obtained into rectangular silicon glue frame；
It is then placed in baking oven and dries, the temperature of baking oven is 80~90 DEG C, obtains barium titanate powder primary sample after dispersion liquid volatilization；It is outstanding
The dripping quantity of supernatant liquid is determined without particular/special requirement according to actual service condition；
S3, tabletting sample preparation,
Rectangular silicon glue frame is removed, is flattened barium titanate powder primary sample surface with clean sheet glass, and blown away with ear washing bulb
Extra dust around barium titanate powder primary sample；Sheet glass uses glass slide；
S4, metal spraying,
Metal spraying processing is carried out to barium titanate powder primary sample, vacuum degree when metal spraying in sputtering vacuum chamber is 6*10-2Pa, electricity
Flowing is 5mA, sputtering time 30s, obtains the nanoscale barium titanate powder for being able to carry out scanning electron microscope test after metal spraying
Sample.
In conjunction with shown in Fig. 1 and Fig. 2, testing electronic microscope is scanned to obtained nanoscale barium titanate powder sample,
By picture it can be seen that nanoscale barium titanate powder sample particle is uniformly dispersed, surface particles overall leveling avoids scanning electricity
Mirror vacuum chamber is contaminated, and picture quality is high.
The above described is only a preferred embodiment of the present invention, being not intended to limit the present invention in any form；Appoint
What those skilled in the art, without departing from the scope of the technical proposal of the invention, all using the side of the disclosure above
Method and technology contents make many possible changes and modifications to technical solution of the present invention, or are revised as the equivalent reality of equivalent variations
Apply example.Therefore, anything that does not depart from the technical scheme of the invention according to the technical essence of the invention do above embodiments
Any simple modification, equivalent replacement, equivalence changes and modification, all of which are still within the scope of protection of the technical scheme of the invention.
Claims (5)
1. a kind of preparation method of the scanning electron microscope sample of nanoscale barium titanate powder, which is characterized in that including following
Step:
S1, dispersion,
Nanoscale barium titanate powder and dispersing agent are taken according to the proportion of mass ratio 1:5, nanoscale barium titanate powder is poured into dispersion
It is in agent and ultrasonic, obtain the suspension of barium titanate；
S2, sampling,
Rectangular silicon glue frame is placed in the sample stage with conducting resinl, and the suspension that a dropping step S1 is obtained into rectangular silicon glue frame；
It is then placed in baking oven and dries, obtain barium titanate powder primary sample；
S3, tabletting sample preparation,
Rectangular silicon glue frame is removed, is flattened barium titanate powder primary sample surface with sheet glass, and blow away barium titanate powder primary
Extra dust around sample；
S4, metal spraying,
Metal spraying processing is carried out to barium titanate powder primary sample, obtains the nano grade titanium for being able to carry out scanning electron microscope test
Sour barium dust sample.
2. a kind of preparation method of the scanning electron microscope sample of nanoscale barium titanate powder according to claim 1,
It is characterized in that, dispersing agent described in step S1 is the ethyl alcohol of 95% or more concentration.
3. a kind of preparation method of the scanning electron microscope sample of nanoscale barium titanate powder according to claim 1,
It is characterized in that, the temperature of step S2 baking oven is 80~90 DEG C.
4. a kind of preparation method of the scanning electron microscope sample of nanoscale barium titanate powder according to claim 1,
It is characterized in that, the sheet glass of step S3 is glass slide.
5. a kind of preparation method of the scanning electron microscope sample of nanoscale barium titanate powder according to claim 1,
It is characterized in that, sputtering the vacuum degree in vacuum chamber when step S4 metal spraying is 6*10-2Pa, electric current 5mA, sputtering time 30s.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811611262.6A CN109444195A (en) | 2018-12-27 | 2018-12-27 | A kind of preparation method of the scanning electron microscope sample of nanoscale barium titanate powder |
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| CN201811611262.6A CN109444195A (en) | 2018-12-27 | 2018-12-27 | A kind of preparation method of the scanning electron microscope sample of nanoscale barium titanate powder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110987549A (en) * | 2019-10-23 | 2020-04-10 | 包头钢铁（集团）有限责任公司 | Sample preparation method for detecting particle size of blast furnace slag particles |
| CN113008923A (en) * | 2021-03-04 | 2021-06-22 | 西北工业大学 | Method for preparing soil sample by scanning electron microscope energy spectrum |
| CN113063717A (en) * | 2021-03-17 | 2021-07-02 | 包头钢铁（集团）有限责任公司 | Method for guiding ore blending by measuring shape of iron ore particles |
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| EP2273528A1 (en) * | 2008-04-28 | 2011-01-12 | Hitachi High-Technologies Corporation | Transmission electron microscope, and method of observing specimen |
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| KR20170050250A (en) * | 2015-10-30 | 2017-05-11 | 한국기초과학지원연구원 | Specimen Multi-loading Device for Grid of TEM |
| CN206627539U (en) * | 2017-04-13 | 2017-11-10 | 皖西学院 | A kind of ESEM cryptogam sample preparation sample stage |
| CN108760785A (en) * | 2018-06-05 | 2018-11-06 | 安徽中创电子信息材料有限公司 | A kind of method of scanning electron microscope observation barium titanate superfine powder |
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- 2018-12-27 CN CN201811611262.6A patent/CN109444195A/en not_active Withdrawn
Patent Citations (7)
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| CN1290348A (en) * | 1998-02-10 | 2001-04-04 | 李·H·安格罗斯 | Analytic plate and method |
| CN101511481A (en) * | 2005-07-08 | 2009-08-19 | 艾可尼西斯公司 | Slide deposition chamber |
| EP2273528A1 (en) * | 2008-04-28 | 2011-01-12 | Hitachi High-Technologies Corporation | Transmission electron microscope, and method of observing specimen |
| CN204008244U (en) * | 2014-07-07 | 2014-12-10 | 山西出入境检验检疫局检验检疫技术中心 | Small insects slide sample is made vessel |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110987549A (en) * | 2019-10-23 | 2020-04-10 | 包头钢铁（集团）有限责任公司 | Sample preparation method for detecting particle size of blast furnace slag particles |
| CN113008923A (en) * | 2021-03-04 | 2021-06-22 | 西北工业大学 | Method for preparing soil sample by scanning electron microscope energy spectrum |
| CN113063717A (en) * | 2021-03-17 | 2021-07-02 | 包头钢铁（集团）有限责任公司 | Method for guiding ore blending by measuring shape of iron ore particles |
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Application publication date: 20190308 |
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