CN109342476A - A kind of test method that glass is carried out using high aluminosilicate glass standard specimen - Google Patents
A kind of test method that glass is carried out using high aluminosilicate glass standard specimen Download PDFInfo
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- CN109342476A CN109342476A CN201811300198.XA CN201811300198A CN109342476A CN 109342476 A CN109342476 A CN 109342476A CN 201811300198 A CN201811300198 A CN 201811300198A CN 109342476 A CN109342476 A CN 109342476A
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- glass
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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
- G01N23/223—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 by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
-
- 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
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
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Abstract
The invention belongs to glass the field of test technology, specifically propose a kind of high aluminosilicate glass standard specimen and test method.A kind of test method that glass is carried out using high aluminosilicate glass standard specimen proposed, it is first determined the glass ingredient of high aluminosilicate glass standard specimen selects molten sample raw material according to glass ingredient and mass percent；Mixture is put into platinum-rhodium crucible, high temperature furnace is put into and is warming up to 1600 DEG C~1630 DEG C, keep the temperature 3 hours, the glass metal of melting is poured into mold, 600 DEG C of annealing furnace annealing is subsequently placed into and obtains the high aluminosilicate glass standard specimen of muti-piece；Standard sample establishes standard curve using X-fluorescence tester.The features such as the invention avoids sample preparations again, have test speed fast, and analysis result is accurate, convenient and efficient.
Description
Technical field
The invention belongs to glass the field of test technology, specifically propose a kind of high aluminosilicate glass standard specimen and test method, mainly
Quick test applied to high aluminosilicate glass sample.
Background technique
High aluminosilicate glass belongs to special industrial glass, and the content of aluminium silicon is very high in glass, have preferable chemical stability,
Mechanical strength and the lower coefficient of expansion.With the fast development in Chinese exports market and liquid crystal display market, high aluminosilicate glass
Demand appearance rapidly increase, more and more enterprises are all in the research and development and production for carrying out high aluminosilicate glass, it is necessary to high alumina silicon
Glass ingredient is accurately tested.X- Fluorescence Spectrometer can be used for the test to glass chemistry.
The method that traditional XRF establishes standard curve is that melted preparation mark is mixed with reagent by weighing various primary standard substances
Quasi- sample, because sample making amount is few, it is big that there are weighing errors, and exact value could be obtained by needing to compare by standard sample, and be protected
It is short to deposit the time, when XRF curves shift, can not periodically be corrected to standard curve, it is often necessary to series standard be melted again
Sample, this method is cumbersome, and melted sample stability is poor, can not reuse.
Summary of the invention
In order to solve the above technical problems, the purpose of the present invention is to provide a kind of high aluminosilicate glass standard specimen and test methods.
The present invention adopts the following technical solutions to accomplish the above objectives:
A kind of test method carried out using high aluminosilicate glass standard specimen to glass, the test method include following technique step
It is rapid:
1) glass ingredient of high aluminosilicate glass standard specimen is determined: the glass ingredient and mass percent of high aluminosilicate glass standard specimen are as follows:
SiO2 46%~64%, Al2O312%~30%, CaO 0~0.2%, MgO2%~8%, K2O0~7%, Na2O12%~19%；
2) molten sample raw material is selected according to the glass ingredient of step 1) and mass percent, the granularity control of raw material is 30 mesh~140
Mesh；SiO2Raw material provided by silica sand；The raw material of CaO is provided by calcium carbonate；K2The raw material of O is provided by potassium carbonate；Na2The raw material of O
It is provided by soda ash；Al2O3And the raw material of MgO is provided by alumina powder or aluminium hydroxide and magnesia powder；
3) in melting process, soda ash easily disperses, soda ash disperse calibration be 0.1%~0.3%；
3) uniformly by compound clarifier sodium chloride and antimony oxide premix, sodium chloride and antimony oxide account for the weight percent of mixture
Then mixed compound clarifier is mixed with other raw materials and is uniformly mixed by 0.4%~0.8%；
4) suitable quantity of water is added in raw material that will be uniformly mixed, continuess to mix uniformly, make mixture moisture be maintained at 1.5%~2.5% it
Between；When moisture is lower than 1.5%, raw material disperses seriously, and design ingredient is caused not to be consistent with actual constituent, when moisture is higher than 2.5%
When, hygroscopic raw material generates caking phenomenon；
5) mixture is put into platinum-rhodium crucible, is put into high temperature furnace and is warming up to 1600 DEG C~1630 DEG C, keeps the temperature 3 hours, will melt
The glass metal melted pours into mold, is subsequently placed into 600 DEG C of annealing furnace annealing and obtains high aluminosilicate glass standard specimen；
6) step 1) -5 is repeated) the high aluminosilicate glass standard specimen of muti-piece different glass constituent content is made；
7) obtained high aluminosilicate glass standard specimen polished, polished, it is glimmering using X as standard sample according to Glass Design ingredient
Optical tester establishes standard curve；
8) high alumina sample to be measured is tested according to the standard curve that step 6) is established；When high alumina sample surfaces to be measured are smooth
Mirror surface can be tested directly, if rough can be by being tested again after polishing.
A kind of high aluminosilicate glass standard specimen proposed by the present invention and test method by adopting the above technical scheme can be quickly right
High alumina glass sample is tested, and the standard sample of photo of production can not be changed with long-term preservation, property；When X- Fluorescence Spectrometer
When standard curve drifts about, the standard sample of photo of production can be used to calibration standard curve, avoid sample preparation again, there is test speed
The advantages that degree is fast, and analysis result is accurate, convenient and efficient.
Specific embodiment
The present invention is illustrated in conjunction with specific embodiments: (component content in embodiment is by percentage to the quality):
Embodiment:
(1) raw material preparation: prepare to contain SiO respectively2、Al2O3、CaO、MgO、K2O、Na2Raw material silica sand, aluminium powder, the magnesium of O component
The glass raw material of 30 mesh ~ 140 mesh is made in powder, soda ash, potassium carbonate, clarifying agent after being sieved.
(2) ingredient: according to Glass Design ingredient, calculating and weigh the quality of each glass raw material required for melted glass,
Middle silica sand 112.8g, aluminium powder 37.9g, magnesium powder 4.6g, soda ash 41g, potassium carbonate 2.6g, sodium chloride and the total 1.5g of antimony oxide, to mend
It disperses caused by repaying during charging, the soda ash calibration that disperses is 0.1% ~ 0.3%, total 200 grams of mixture, compound clarifier is pre-
It is mixed even, mixed clarifying agent is mixed with other raw materials then and is uniformly mixed.
(3) plus water mixes: raw material being added to suitable moisture after mixing, is continuesd to mix, batch, batch are obtained
Water tariff collection is between 1.5% ~ 2.5%.
(4) it is melted: platinum-rhodium crucible being put into high temperature furnace and is preheated, high temperature furnace heating curve is set, when temperature rises to 1350
DEG C when, uniformly mixed batch is poured into platinum-rhodium crucible, is melted in high temperature furnace, fusion temperature is 1630 DEG C, heat preservation three
A hour.
(5) it forms: the glass metal melted is poured into die for molding.
(6) it anneals: glass after molding being annealed in 600 DEG C of annealing furnace, cools to room temperature with the furnace.
(7) sample preparation: will form glass after cooling and polish, polishing, as 1# standard sample.
(8) according to the design ingredient of table 1, the quality of each glass raw material required for melted glass is calculated and weighed, repeats to walk
Suddenly other 9 standard samples are melted, wherein 3#, 6#, 7# sample in (3)-(7), and control fusion temperature is 1600 DEG C；2#, 5# sample
Product, control fusion temperature are 1610 DEG C；4#, 8#, 9#, 10# sample, control fusion temperature are 1630 DEG C of
(9) polish after standard sample be cut into 35mm*35mm, with dehydrated alcohol clean sample surfaces, by 1#, 2#, 3#, 4#,
5#, 6#, 7#, 8#, 9#, 10# sample, are sequentially placed into sample box, input each component percentage composition, sample corresponding to each sample
The chemical composition and mass fraction of product are as shown in table 1, each element fluorescence intensity tested according to X fluorescence spectrometer and known
Percentage composition establishes standard working curve.The linear coefficient of standard working curve wants 0.99 or more, can just meet the requirements measurement to
Glass specimen is surveyed, otherwise needs to correct again, establish standard working curve.
(10) high alumina glass sample to be measured is cut into 35mm*35mm, cleans sample with dehydrated alcohol, is put into sample box
In, the standard curve built up is called, i.e., available X fluorescence spectrometer is detected automatically to SiO in test sample2、Al2O3、CaO、MgO、
K2O、Na2O content.
Specific implementation formula is as shown in table 1.
Table 1: the design ingredient and mass fraction of high lead glass
Claims (1)
1. a kind of test method carried out using high aluminosilicate glass standard specimen to glass, it is characterised in that: the test method packet
Include following processing step:
1) glass ingredient of high aluminosilicate glass standard specimen is determined: the glass ingredient and mass percent of high aluminosilicate glass standard specimen are as follows:
SiO2 46%~64%, Al2O312%~30%, CaO 0~0.2%, MgO2%~8%, K2O0~7%, Na2O12%~19%；
2) molten sample raw material is selected according to the glass ingredient of step 1) and mass percent, the granularity control of raw material is 30 mesh~140
Mesh；SiO2Raw material provided by silica sand；The raw material of CaO is provided by calcium carbonate；K2The raw material of O is provided by potassium carbonate；Na2The raw material of O
It is provided by soda ash；Al2O3And the raw material of MgO is provided by alumina powder or aluminium hydroxide and magnesia powder；
3) in melting process, soda ash easily disperses, soda ash disperse calibration be 0.1%~0.3%；
3) uniformly by compound clarifier sodium chloride and antimony oxide premix, sodium chloride and antimony oxide account for the weight percent of mixture
0.4%~0.8%, mixed compound clarifier is mixed with other raw materials then and is uniformly mixed；
4) suitable quantity of water is added in raw material that will be uniformly mixed, continuess to mix uniformly, make mixture moisture be maintained at 1.5%~2.5% it
Between；
5) mixture is put into platinum-rhodium crucible, is put into high temperature furnace and is warming up to 1600 DEG C~1630 DEG C, keeps the temperature 3 hours, will melt
The glass metal melted pours into mold, is subsequently placed into 600 DEG C of annealing furnace annealing and obtains high aluminosilicate glass standard specimen；
6) step 1) -5 is repeated) the high aluminosilicate glass standard specimen of muti-piece different glass constituent content is made；
7) obtained high aluminosilicate glass standard specimen polished, polished, it is glimmering using X as standard sample according to Glass Design ingredient
Optical tester establishes standard curve；
8) high alumina sample to be measured is tested according to the standard curve that step 6) is established；When high alumina sample surfaces to be measured are smooth
Mirror surface can be tested directly, if rough can be by being tested again after polishing.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811300198.XA CN109342476A (en) | 2018-11-02 | 2018-11-02 | A kind of test method that glass is carried out using high aluminosilicate glass standard specimen |
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| CN201811300198.XA CN109342476A (en) | 2018-11-02 | 2018-11-02 | A kind of test method that glass is carried out using high aluminosilicate glass standard specimen |
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| CN109342476A true CN109342476A (en) | 2019-02-15 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114031292A (en) * | 2021-12-07 | 2022-02-11 | 中氢国储(杭州)精密制造有限公司 | Formula of high-alumina-silica glass tube and manufacturing method of high-alumina-silica glass tube |
| CN114295663A (en) * | 2021-12-28 | 2022-04-08 | 自然资源部第二海洋研究所 | Magnesium-based electron probe microbeam component analysis standard sample and preparation method thereof |
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| CN103323479A (en) * | 2013-06-18 | 2013-09-25 | 芜湖东旭光电科技有限公司 | Glass mixed batch uniformity determination method |
| CN104280415A (en) * | 2013-10-31 | 2015-01-14 | 东旭集团有限公司 | Method for accurately detecting components of raw glass sheets |
| CN106470951A (en) * | 2014-07-04 | 2017-03-01 | 旭硝子株式会社 | Chemical enhanced use glass and chemically reinforced glass |
| CN108314315A (en) * | 2017-01-16 | 2018-07-24 | 中国南玻集团股份有限公司 | Glass, preparation method, strengthened glass, glass plate and application |
-
2018
- 2018-11-02 CN CN201811300198.XA patent/CN109342476A/en active Pending
Patent Citations (6)
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| KR20130075488A (en) * | 2011-12-27 | 2013-07-05 | 삼성전기주식회사 | Quantative analysys method for dielectric substance of multi-layer ceramic capacitor |
| CN103323479A (en) * | 2013-06-18 | 2013-09-25 | 芜湖东旭光电科技有限公司 | Glass mixed batch uniformity determination method |
| CN104280415A (en) * | 2013-10-31 | 2015-01-14 | 东旭集团有限公司 | Method for accurately detecting components of raw glass sheets |
| CN106470951A (en) * | 2014-07-04 | 2017-03-01 | 旭硝子株式会社 | Chemical enhanced use glass and chemically reinforced glass |
| CN108314315A (en) * | 2017-01-16 | 2018-07-24 | 中国南玻集团股份有限公司 | Glass, preparation method, strengthened glass, glass plate and application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114031292A (en) * | 2021-12-07 | 2022-02-11 | 中氢国储(杭州)精密制造有限公司 | Formula of high-alumina-silica glass tube and manufacturing method of high-alumina-silica glass tube |
| CN114295663A (en) * | 2021-12-28 | 2022-04-08 | 自然资源部第二海洋研究所 | Magnesium-based electron probe microbeam component analysis standard sample and preparation method thereof |
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Address after: 571924 Hainan Province Chengmai County Old Town High-tech Industrial Demonstration Zone Hainan Eco-Software Park A17 One Floor 2001 Applicant after: Hainan Haikong special glass technology Co., Ltd Address before: 571924 Hainan Chengmai County Chengmai County Economic Development Zone South First Ring Road Hainan Ecological Software Park incubator room Applicant before: AVIC (HAINAN) SPECIAL GLASS MATERIALS Co.,Ltd. |
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Application publication date: 20190215 |
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