CN105606416A - Preparation method of glass sample for testing glass solid defects - Google Patents
Preparation method of glass sample for testing glass solid defects Download PDFInfo
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- CN105606416A CN105606416A CN201510981373.6A CN201510981373A CN105606416A CN 105606416 A CN105606416 A CN 105606416A CN 201510981373 A CN201510981373 A CN 201510981373A CN 105606416 A CN105606416 A CN 105606416A
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- sample
- glass
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- sample strip
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/02—Non-SPM analysing devices, e.g. SEM [Scanning Electron Microscope], spectrometer or optical microscope
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
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- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Radiology & Medical Imaging (AREA)
- Sampling And Sample Adjustment (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention discloses a preparation method of a glass sample for testing glass solid defects. The method comprises the following steps: cutting glass to be tested into a sample piece which contains solid defects; fixing the sample piece: fixing the sample piece on a fixing device; polishing: laying the fixed sample piece on a polishing pad, enabling the sample piece to be closely adhered to the polishing pad, driving the polishing pad to move, polishing the sample piece, and taking down and cleaning the sample piece, so as to obtain the glass sample; the polishing time is 10 to 20min. The preparation method has the advantages of high safety in operation and high efficiency.
Description
Technical field
The present invention relates to glass processing field, be specifically related to a kind of for measuring the solid-state defect of glassThe preparation method of glass sample.
Background technology
In Improving Glass Manufacturing Processes, because raw material introducing is molten, melt-forming drips, crystalThe solid phase inclusion defect (solid-state defect) that the reasons such as growth cause, as particle, calculus, crystallization etc.Glass defect is having a strong impact on glass yields. The microstructure of solid-state defect is observed andComposition detection can be judged defect source fast, targetedly solid-state defect is carried out to countermeasure minimizingSolid-state defect is bad.
Because solid-state defect itself varies in size, different, position is different, need through grindingMill, polishing could correctly effectively be observed detection to glass sample defect.
Less and the out-of-shape of the common area of sample detecting for microstructure, large-scale polishingMachine is not suitable for, and generally adopts manual polishing, with the polished glass of fingerhold by being pressed in throwingOn light pad, carry out polishing, the hand-held sample of constant polishing of exerting oneself is generally wanted more than 2 hours,Efficiency is very low, and reason is that hand-held sample is difficult to exert oneself in vertical direction, and some are not advisedBlock glass sample is sharply sharp, carries out milled processed with fingerhold sample, to operationPersonnel's incised wound is stabbed also and is often occurred, and staff dare not go firmly to press.
Summary of the invention
The object of this invention is to provide a kind of for measuring the system of glass sample of the solid-state defect of glassPreparation Method, can improve the preparation efficiency of glass sample greatly, and it is right effectively to reduce in polishing processThe injury of finger, has ensured staff's safety.
The object of the invention is to be achieved through the following technical solutions:
The invention provides a kind of for measuring the preparation side of glass sample of the solid-state defect of glassMethod, comprises the steps:
Glass-cutting to be measured is become to sample strip, and described sample strip contains solid-state defect;
Fixing described sample strip: described sample strip is fixed in fixture;
Polishing: the described sample strip fixing is placed on polishing pad, make described sample strip withPolishing pad fits tightly, and drives polishing pad to move, and described sample strip is carried out to polishing,Take off described sample strip and clean and obtain described glass sample; The time of described polishing is10-20min。
Further, described being fixed as is bonded to described sample strip described with binding agentIn fixture.
Further, described binding agent is paraffin.
Further, described fixing described sample strip specifically comprises the steps:
The paraffin of getting described in 2-5g is placed in described fixture, and heating makes described paraffinMelting, is placed on described sample strip on the paraffin of melting, cooling can be by described sampleSheet is fixed.
Further, the described described sample strip of taking off is that heating makes described binding agent melting,Then take off described sample strip.
Further, described polishing is the oxidation that drips 20-40wt% on described polishing padUnder the condition of cerium polishing fluid, carry out.
Further, described heating-up temperature is 50-120 DEG C.
Further, described fixture comprises fixed head and the sidewall being connected with its edge,Described fixed head material is corundum, zirconia or graphite, described in described sample strip is bonded inFixed head on.
Further, the Area Ratio of described fixed head and described sample strip is 2-5:1.
Further, described fixed head is circular, and the vertical section of described sidewall is arc,Described fixture one end is openend, and described openend with the diameter of fixed head ratio is1-3:1。
Compared with prior art, technical solution of the present invention at least has following beneficial effect:
To carry out polishing different from existing finger prosthesis clamping glass sheet, in the present invention, adoptFixture is fixed sample strip, has avoided contacting of staff and sheet glass and polishing pad, therebyEnsure operating personnel's safety.
In the present invention, choose cleverly suitable fixture material and binding agent and cooperatively interacted,Both realize the fixing of sample, ensured again that binding agent easily removed, and can not affect sheet glassMeasure.
Brief description of the drawings
To be the present invention throw for the preparation method of the glass sample of measuring the solid-state defect of glass Fig. 1Electro-optical device structural representation;
It is solid for measuring the preparation method of glass sample of the solid-state defect of glass that Fig. 2 is the present inventionSurely there is the fixture schematic diagram of sample strip.
Detailed description of the invention
For clearer elaboration content of the present invention and technical scheme, below in conjunction with better enforcementScheme gives detailed explanation, is noted that preferred embodiment is just for originally convenient hereThose skilled in the art are easier to understand technical scheme of the present invention, not as the present invention program'sLimit.
The present patent application adopts fixture that sample is fixed, the finger that has prevented operating personnel withThe contact of glass and polishing pad, has improved security; Say with fixed form preferably belowBright the present invention program.
The technical scheme that the embodiment of the present invention provides adopt suitable binding agent and fixed head material skilfulWonderful combination, and on fixed head, be provided with sidewall, reach following effect: the first, can realizeFixing of glass sample can not be dropped it in polishing; The second, staff's hand is notContact with polishing pad with glass sample, ensured staff's safety; Three, realize polishingAfter easily glass sample is taken off, and remove binding agent, do not damage glass sample; Four,Sidewall and fixed head close fit, realize fixed head stressed evenly, and then ensured sample withThe combination of polishing pad is tight, and the sample that can not cause because of unbalance stress comes off.
Fig. 1 is burnishing device structural representation, and as shown in Figure 1, burnishing device comprises and being fixed withFixture 1, polishing pad 2 and the leakage fluid dram 3 of sample strip; Fig. 2 is fixed with consolidating of sample stripDetermine the structural representation of device; As shown in Figure 2, the fixture that is fixed with sample strip comprises solidDetermine plate 101, sidewall 102 and sample strip 103, sample strip 103 is bonded on fixed head;
Here it should be noted that:
For making sample strip be difficult for dropping when the polishing, should ensure that fixed head 101 has certain roughness,Fixed head 101 also should have certain hardness, prevent in the process of pressing cracked, generally select corundum,Zirconia, graphite etc.;
Binding agent should be selected paraffin, because its sample strip 103 difficult drop-offs can ensure polishing time,Can ensure again polishing complete after the removing ratio of binding agent be easier to, only need after heating fixed head 101Take off the rear cleaning of sample strip 103, can not cause binding agent not clean up or clean timeSample strip 103 is caused to damage and wait impact mensuration below;
Sidewall 102 and fixed head 101 close fit, staff only needs hand-held sidewall 102The marginal portion of openend, presses downwards, can ensure that fixed head 101 is stressed evenly, therebyEnsure that sample strip can not drop because of unbalance stress in polishing process; For furtherConvenient heating fixed head 101, the longitudinal section of sidewall 102 is circular arc, its openend area ratioFixed head 101 areas are large, solid will be difficult to heating and melting binding agent, as opening if be changed toEnd is unfavorable for heating compared with young pathbreaker, during as heating fixed heads 101 such as use alcolhol burners, and the firstth, fireThe not accessible fixed head 101, two of flame, easily makes side wall temperatures too high, is unfavorable for staff's handHold operation.
Fixed head 101 is 2-5:1 with the Area Ratio of sample strip 103, and ratio is too little will cause sampleProduct sheet 103 easily comes off, and ratio will increase too greatly the friction of polishing pad 2 and fixed head 101,Thereby affect polishing;
In polishing process, can on polishing pad, drip polishing fluid, in polishing process, polishing fluid is from throwingAfter flowing out on light pad 2, flow out through leakage fluid dram 3, add polishing fluid and be conducive to polishing.
In glass sample, an assay method for solid-state defect, comprises the steps:
(1) glass sample that contains solid-state defect is cut into proximity test sample size and treat sample preparationProduct sheet: area is: 5mm × 5mm-30mm × 30mm, thickness is: 0.1-1.5mm;
(2) by the corundum crucible back-off of 500ml, 3g paraffin is placed on to its centre position, bottom,Pick up corundum crucible and tip upside down on alcolhol burner, to crucible bottom heating, make paraffin melting, by sampleProduct sheet is placed on the paraffin of melting; Use blade applying light, extinguish the cooling crucible bottom of alcolhol burner;The environment temperature of cooling down operation is lower than 30 DEG C, and excess Temperature approaches the softening temperature of paraffin, is difficult forSolidify;
(3) by upright the crucible of bonding sample hand-held on polishing grinder, be manually polished to scarceFall into fully exposure and do not disappear, using thin blade that sample is taken off and clean up;
Here it should be noted that: when polishing, can on polishing machine polishing pad, add cerium oxide polishingIn liquid process of lapping, evenly add polishing fluid, concentration is 20-40wt%; Cerium oxide solution can makePolishing effect is better, and efficiency is higher;
(7) prepared sample has good electron microscope observation, detects effect. Preferably,Use scanning electron-microscopic observation solid defects table looks, or electron spectrometer combines, pointAnalyse elemental analysis.
Embodiment 1
(1) the irregular glass of 12 hours glass surface devitrification defects of 1000 DEG C of constant temperature will be observed in advancePiece sample, is cut into glass blocks and the sample that accounts for crucible bottom 1/5 size, sample strip with cutting machineRetain surface on glass, thickness is 1.5mm.
(2) will get approximately 3 grams, paraffin with wallpaper cutter is placed on and is more than or equal to 200ml circular arc corundum crucibleBottom;
(3) crucible of back-off is heated on alcolhol burner to 50 DEG C and makes the even melting of paraffin, crucibleSidewall can not heat;
(4) sample upper surface is buckled in to cooled and solidified on paraffin downwards, with a small amount of paraffin powderBe placed on sample surrounding, by the heating of wallpaper cutter, by powder smelting, sample envelope cemented solid, coolingSolidify; Surrounding scribbles paraffin, can reduce the edge of polishing pad and sample strip in polishing processFrictional force;
(5) by upright the crucible of the sample that bondd hand-held manually polishing on polishing grinder, throwPhotoreduction process evenly drips the cerium oxide polishing slurry of concentration 40wt%, polishing 15 minutes, heating crucibleBottom, to 80 DEG C, makes paraffin melting, takes off sample strip, and cleaning can obtain glass sample;
(6) sample of preparation is used to scanning electron-microscopic observation solid defects table looks, orElectron spectrometer combines, amalyzing substances constituent analysis; Result is as shown in table 1.
Comparative example:
(1) the irregular glass of 12 hours glass surface devitrification defects of 1000 DEG C of constant temperature will be observed in advancePiece sample, cuts into pieces.
(2) by the upwards hand-held manually polishing on polishing grinder of sample upper surface, polishing processDrip polishing fluid, 150min, cleans up sample to dry maintenance cleaning;
(3) use scanning electron-microscopic observation to detect in the sample of preparation, amalyzing substances becomesAnalyze; The results are shown in Table 1.
Embodiment 2
(1) sample that the LTPS-LCD glass of production line thickness 0.7mm is contained to platinum particleProduct, are cut into 15 times of big or small sample strip of defect by glass blocks with cutting machine.
(2) will get approximately 2 grams, paraffin with wallpaper cutter is placed on and is more than or equal to 200ml graphite crucible bottom;
(3) make paraffin even to 120 DEG C the crucible of back-off heating crucible bottom on alcolhol burnerMelting;
(4) sample is placed in the paraffin liquid of melting and presses down gently with cutter rib, wait paraffin cooling,Sample envelope cements solid;
(5) by upright the crucible of bonding sample hand-held manually polishing on polishing grinder, throwPhotoreduction process evenly drips the cerium oxide polishing slurry of concentration 20wt%, and polishing 5 minutes is used wallpaperCutter takes off sample to clean up to dry and keeps clean;
(6) sample of preparation is used to electron microscope observation solid defects table looks and analyzes solid-stateDefect composition; Result is as shown in table 1.
Comparative example:
(1) sample that the LTPS-LCD glass of production line thickness 0.7mm is contained to platinum particleProduct, cut into pieces.
(2) by the upwards hand-held manually polishing on polishing grinder of sample upper surface, polishing processDrip polishing fluid, 100min, cleans up sample to dry maintenance cleaning;
(3) use scanning electron-microscopic observation to detect in the sample of preparation, amalyzing substances becomesAnalyze; The results are shown in Table 1.
In the sample strip polishing process of above embodiment and comparative example, staff can be right in real timeSample strip is observed, and meets mensuration requirement to it, can according to staff's real-time judgeEnsure that polishing can make defect expose completely, can not cause because polishing time is long and cause againDefect disappears.
Embodiment prepares sample and manual sample Electronic Speculum test result and the following table 1 of time prepared:
Table 1 embodiment and comparative example measurement result contrast table
As can be seen from Table 1, the sample preparation efficiency of the inventive method is apparently higher than existing manual systemThe sample preparation time of sample: embodiment 1 is 20min, and its comparative example sample preparation time is 150min; RealExecuting the 2 sample preparation times of example is 10min; Its comparative example sample preparation time is 100min;
The measurement result of solid-state defect from sample, its testing result and existing manual systemSample is compared, and result is consistent, visible, and method for making sample of the present invention is ensureing the base of sample qualityOn plinth, greatly shorten the sample preparation time, improved detection efficiency; On the other hand, can also be greatlyReduce the security of staff in sample making course.
In the present patent application, do not use up part, those skilled in the art can select according to prior artBecome.
The above be only the specific embodiment of the present invention, but protection scope of the present invention alsoBe not limited to this, any be familiar with those skilled in the art the present invention disclose technology modelIn enclosing, can expect easily changing or replacing, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of described claim.
Claims (10)
1. for measuring the preparation method of glass sample for the solid-state defect of glass, its feature existsIn, comprise the steps:
Glass-cutting to be measured is become to sample strip, and described sample strip contains solid-state defect;
Fixing described sample strip: described sample strip is fixed in fixture;
Polishing: the described sample strip fixing is placed on polishing pad, make described sample strip withPolishing pad fits tightly, and drives polishing pad to move, and described sample strip is carried out to polishing,Take off described sample strip and clean and obtain described glass sample; The time of described polishing is10-20min。
2. according to claim 1 for measuring the system of glass sample of the solid-state defect of glassPreparation Method, is characterized in that, described being fixed as is bonded to described sample strip with binding agentIn described fixture.
3. according to claim 2 for measuring the system of glass sample of the solid-state defect of glassPreparation Method, is characterized in that, described binding agent is paraffin.
4. according to claim 3 for measuring the system of glass sample of the solid-state defect of glassPreparation Method, is characterized in that, described fixing described sample strip specifically comprises the steps:
The paraffin of getting described in 2-5g is placed in described fixture, and heating makes described paraffinMelting, is placed on described sample strip on the paraffin of melting, cooling can be by described sampleSheet is fixed.
5. according to claim 2 for measuring the system of glass sample of the solid-state defect of glassPreparation Method, is characterized in that, the described described sample strip of taking off is that heating makes described bondingAgent melting, then takes off described sample strip.
6. according to claim 1 for measuring the system of glass sample of the solid-state defect of glassPreparation Method, is characterized in that, described polishing is to drip 20-40wt% on described polishing padThe condition of cerium oxide polishing slurry under carry out.
According to described in claim 4 or 5 for measuring the glass sample of the solid-state defect of glassPreparation method, it is characterized in that, described heating-up temperature is 50-120 DEG C.
8. according to claim 2 for measuring the system of glass sample of the solid-state defect of glassPreparation Method, is characterized in that, described fixture comprises fixed head and is connected with its edgeSidewall, described fixed head material is corundum, zirconia or graphite, described sample strip bondingOn described fixed head.
9. according to claim 8 for measuring the system of glass sample of the solid-state defect of glassPreparation Method, is characterized in that, the Area Ratio of described fixed head and described sample strip is 2-5:1.
10. according to claim 8 for measuring the glass sample of glass solid-state defectPreparation method, is characterized in that, described fixed head is circular, the vertical section of described sidewallFor arc, described fixture one end is openend, described openend and fixed head straightFootpath is than being 1-3:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510981373.6A CN105606416A (en) | 2015-12-23 | 2015-12-23 | Preparation method of glass sample for testing glass solid defects |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510981373.6A CN105606416A (en) | 2015-12-23 | 2015-12-23 | Preparation method of glass sample for testing glass solid defects |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107219163A (en) * | 2017-05-10 | 2017-09-29 | 东旭科技集团有限公司 | It is a kind of to measure the apparatus and method that speed is thinned in glass chemistry |
| CN108982182A (en) * | 2018-07-27 | 2018-12-11 | 彩虹显示器件股份有限公司 | A kind of method for making sample and detection method for finely ground particles composition detection in electronic glass |
| RU2807677C1 (en) * | 2023-09-14 | 2023-11-21 | Акционерное общество "Концерн "Центральный научно-исследовательский институт "Электроприбор" | Method for preparing glassy samples for electron probe microanalysis of chemical composition |
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| JPH09166526A (en) * | 1995-12-14 | 1997-06-24 | Nec Corp | Preparation od sample for transmission type electron microscope |
| JP2004340851A (en) * | 2003-05-19 | 2004-12-02 | Sumitomo Metal Mining Co Ltd | Sample polishing method |
| JP2008229734A (en) * | 2007-03-16 | 2008-10-02 | Fujitsu Ltd | Grinding apparatus and method |
| KR20080102877A (en) * | 2007-05-22 | 2008-11-26 | 정태승 | Method for manufacturing a test sample for transmission electron microscope |
| CN101894900A (en) * | 2010-06-25 | 2010-11-24 | 北京工业大学 | Method for manufacturing white light LED by single crystals |
| CN103792127A (en) * | 2014-01-24 | 2014-05-14 | 西安空间无线电技术研究所 | Preparation method of LTCC (Low Temperature Co-fired Ceramic) section sample |
| CN103868922A (en) * | 2014-03-13 | 2014-06-18 | 攀钢集团攀枝花钢铁研究院有限公司 | Phase identification method for vanadium slag rich in various impurity elements |
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| JPH09166526A (en) * | 1995-12-14 | 1997-06-24 | Nec Corp | Preparation od sample for transmission type electron microscope |
| JP2004340851A (en) * | 2003-05-19 | 2004-12-02 | Sumitomo Metal Mining Co Ltd | Sample polishing method |
| JP2008229734A (en) * | 2007-03-16 | 2008-10-02 | Fujitsu Ltd | Grinding apparatus and method |
| KR20080102877A (en) * | 2007-05-22 | 2008-11-26 | 정태승 | Method for manufacturing a test sample for transmission electron microscope |
| CN101894900A (en) * | 2010-06-25 | 2010-11-24 | 北京工业大学 | Method for manufacturing white light LED by single crystals |
| CN103792127A (en) * | 2014-01-24 | 2014-05-14 | 西安空间无线电技术研究所 | Preparation method of LTCC (Low Temperature Co-fired Ceramic) section sample |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107219163A (en) * | 2017-05-10 | 2017-09-29 | 东旭科技集团有限公司 | It is a kind of to measure the apparatus and method that speed is thinned in glass chemistry |
| CN108982182A (en) * | 2018-07-27 | 2018-12-11 | 彩虹显示器件股份有限公司 | A kind of method for making sample and detection method for finely ground particles composition detection in electronic glass |
| RU2807677C1 (en) * | 2023-09-14 | 2023-11-21 | Акционерное общество "Концерн "Центральный научно-исследовательский институт "Электроприбор" | Method for preparing glassy samples for electron probe microanalysis of chemical composition |
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Application publication date: 20160525 |