CN104280415A - Method for accurately detecting components of raw glass sheets - Google Patents

Method for accurately detecting components of raw glass sheets Download PDF

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Publication number
CN104280415A
CN104280415A CN201310528625.0A CN201310528625A CN104280415A CN 104280415 A CN104280415 A CN 104280415A CN 201310528625 A CN201310528625 A CN 201310528625A CN 104280415 A CN104280415 A CN 104280415A
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China
Prior art keywords
original sheet
sheet glass
glass
sample
measured
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Pending
Application number
CN201310528625.0A
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Chinese (zh)
Inventor
李刚
张广涛
李俊锋
闫冬成
王丽红
侯建伟
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Tunghsu Group Co Ltd
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Tunghsu Group Co Ltd
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Application filed by Tunghsu Group Co Ltd filed Critical Tunghsu Group Co Ltd
Priority to CN201310528625.0A priority Critical patent/CN104280415A/en
Publication of CN104280415A publication Critical patent/CN104280415A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a method for accurately detecting the components of raw glass sheets. The method for accurately detecting the components of the raw glass sheets comprises the following steps: A, designing a standard curve by the steps of (1) designing a group of specific embodiment formulas for preparing the raw glass sheets according to a design formula of a glass production line, (2) melting the glass according to the formula of the embodiment and preparing a series of standard sample sheets by the molten glass and (3) putting the standard sample sheets on an X fluorescence tester to establish a standard curve; and B, detecting the components of to-be-detected raw glass sheets, namely testing the to-be-detected raw glass sheets by the standard curve obtained by the step A to obtain percentages of the components in the to-be-detected raw glass sheets. According to the method for accurately detecting the components of the raw glass sheets, standard substances are not used; the raw materials for producing the raw glass sheets are directly used; the influence of a reagent and a machine body and the influence of a thermal process and weighing on the test are greatly alleviated; the method is accurate and quick, and has a relatively great guiding significance.

Description

A kind of method of accurate detection original sheet glass composition
Technical field
The invention belongs to glass ingredient detection technique field, relate to a kind of method using X-fluorescence Criterion curve accurately to detect original sheet glass composition.
Background technology
The former slice assembly line of TFT-LCD uses material quality higher, and most starting material dry basis purity is all more than 99.5%, and the fluctuation of producing line glass ingredient mainly comes from: during (1) hot charging kiln, heterogeneity glass pollutes; (2) fire resistive material pollutes; (3) adjustment of glass ingredient; (4) raw material the reason such as to be vaporized and to cause.
Traditional X-ray fluorescence Criterion curve test method to mix with flux found standard sample of photo by weighing often kind of primary standard substance, in standard sample of photo preparation process, various primary standard substance (some also needs many times of dilutions) the less error of weigh is larger, and molten sample is distributed to separately in flux for often kind of primary standard substance, different from glass history of forming to be measured, be distributed to structure in flux also not identical.Therefore test result is difficult to close to actual value, and whole result or certain element result often exceed standard allowed band, need could obtain exact value through standard model comparison.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method of accurate detection original sheet glass composition, can more accurate testing producing lines glass ingredient, reduce standard sample of photo and prepare primary standard substance weighing matrix difference, reduce in glass melting process the impact polluted and be vaporized, realize accurate Instructing manufacture.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A method for accurate detection original sheet glass composition, comprises the following steps:
A, design standards curve
1. according to the design material side of glass production line, the specific embodiment material side that a group is prepared original sheet glass is designed;
2. according to embodiment material side fusion cast glass, with the glass preparation series standard print founded;
3. by standard sample of photo Criterion curve on X-fluorescence tester;
The mensuration of B, original sheet glass composition to be measured
Prepare testing sample with original sheet glass to be measured, with the typical curve obtained in steps A, testing sample is tested, to obtain the percentage composition of each composition in original sheet glass to be measured.
There is provided the preparation method of two kinds of standard sample of photo below: the first is flux fusion process; Namely the preparation section of step 2. Plays print comprises: the glass grinding founded is become glass dust, glass dust flux is founded series standard print, on this basis, correspondingly in step B, with above-mentioned identical flux, testing sample is founded to original sheet glass abrasive dust to be measured, with the typical curve obtained in steps A, testing sample is tested again, be the percentage composition of each composition in original sheet glass to be measured with the percentage composition obtaining each composition in testing sample.
2nd kind is abrasive disc method, the preparation section of step 2. Plays print comprises: by the glass-cutting of founding, grind, be polished to the series standard print of the thickness identical with testing sample and roughness, correspondingly, in step B, original sheet glass to be measured cut, grind, be polished to the thickness identical with standard sample of photo and the testing sample of roughness.
Step 2. in the operation of fusion cast glass comprise: according to embodiment material side feeding, then by get various raw material blendings, division, then the raw material after division is placed in crucible, puts into sample-melting stove melting preparation.
Pure lithium tetraborate analyzed by described flux.
The operation of founding series standard print comprises: glass dust, solvent are fully mixed in platinum crucible, then the iodate ammonia solution that 5 ~ 8 concentration are 10 ~ 20% is dripped, series standard print is founded in 1100-1150 DEG C of sample-melting stove, correspondingly, founding testing sample is also original sheet glass powder to be measured, flux are fully mixed in platinum crucible, then drip the iodate ammonia solution that 5 ~ 8 concentration are 10 ~ 20%, found in 1100-1150 DEG C of sample-melting stove and form.
The invention has the beneficial effects as follows: no matter (1) the present invention adopts flux to found standard sample of photo method or use abrasive disc method to detect original sheet glass composition, comparatively classic method is high for its testing result confidence level, and the inventive method is simple and convenient, is monitoring glass quality, produces the reliable method of line glass ingredient; (2) standard sample of photo and glass sample to be measured generate approximate thermal history therefore test result more close to actual value; (3) first the present invention solves primary standard substance and uses raw-material difference, and the unified starting material that use remove Criterion curve, eliminate primary standard substance and bring uncertain impact.
Embodiment
Be described in detail with embodiment below.
Embodiment one
A method for accurate detection original sheet glass composition, comprises the following steps:
A, design standards curve
1. according to the design material side of glass production line, the specific embodiment material side that a group is prepared original sheet glass is designed.
2. according to embodiment material side fusion cast glass, with the glass preparation series standard print founded.
Respectively according to the material side of the design standards sample of 5 in table 1, calculate the consumption of each component in 500 grams of frits, simultaneously by displayed in Table 1 for the original sheet glass material side to be measured of known each component concentration:
Table 1
Get production raw material weighing respectively according to the consumption of each component of above-mentioned calculating gained to mix, contracting is got 160g and is poured in the 200ml corundum crucible cleaned up;
Five standard sample of photo are placed on molten sample in stove by setting high temperature melting sample furnace temperature curve simultaneously;
After molten sample terminates, the glass metal in each crucible is poured out respectively annealing cooling, the particle grinding to form less than 45 μm is for subsequent use;
Take 6g lithium tetraborate in platinum crucible (this step utensil used reagent is all supporting with X-fluorescence instrument), add the mixing of 0.6g standard sample of photo, add 8 200mg/ml ammonium iodides, under 1100 DEG C of high temperature, on molten model machine, be melting into series standard print according to standing 5min, wave 15min curve of founding;
3. by standard sample of photo Criterion curve on X-fluorescence tester.
The mensuration of B, original sheet glass composition to be measured
Take three parts of equivalent original sheet glass abrasive dust to be measured, molten, wherein fuse piece process, fuse piece condition are identical with the molten sample's condition of above-mentioned standard sample of photo.After fuse piece terminates, the glass metal in each crucible is poured out respectively annealing cooling, the particle grinding to form less than 45 μm is for subsequent use;
Take 6g lithium tetraborate in platinum crucible (this step utensil used reagent is all supporting with X-fluorescence instrument), add the mixing of 0.6g testing sample, add 8 200mg/ml ammonium iodides, under 1100 DEG C of high temperature, on molten model machine, be melting into testing sample according to standing 5min, wave 15min curve of founding;
Test testing sample with the typical curve obtained in steps A, to obtain the percentage composition of each composition in original sheet glass to be measured, test result is as shown in table 2.
Table 2
Embodiment two
A method for accurate detection original sheet glass composition, comprises the following steps:
A, design standards curve
1. according to the design material side of glass production line, the specific embodiment material side that a group is prepared original sheet glass is designed.
2. according to embodiment material side fusion cast glass, with the glass preparation series standard print founded.
Still according to the material side of the design standards sample of 5 in table 1, the consumption of each component in 500 grams of frits is calculated;
Get production raw material weighing respectively according to the consumption of each component of above-mentioned calculating gained to mix, pour in 750ml platinum crucible;
Five standard samples are placed on molten sample in high temperature furnace by setting high temperature melting sample furnace temperature curve respectively;
After molten sample terminates, glass metal is poured out respectively annealing cooling, by the glass blocks melted cutting, grind to form the series standard print being polished to the thickness identical with testing sample and roughness: thickness 0.5mm, long * are wide is 50mm*50mm;
3. by standard sample of photo Criterion curve on X-fluorescence tester.
Analytical approach set up by X-fluorescence instrument, test listing standard print Criterion curve.
The mensuration of B, original sheet glass composition to be measured
Original sheet glass to be measured cut, grinds, be polished to the thickness identical with standard sample of photo and the testing sample of roughness: thickness 0.5mm, long * are wide is 50mm*50mm, and testing sample also prepares three;
Test testing sample with the typical curve obtained in steps A, to obtain the percentage composition of each composition in original sheet glass to be measured, test result is as shown in table 3.
Table 3
In sum, be can visually see by table 2, table 3, utilize the mensuration degree of accuracy of method of testing of the present invention to original sheet glass composition higher, error is little, with a high credibility, in addition, with the typical curve set up in the present invention, daily test is carried out to product line glass ingredient, for the glass quality monitoring of product line and the adjustment of material side provide basic data, the research of frit side is had great importance.

Claims (6)

1. accurately detect a method for original sheet glass composition, it is characterized in that comprising the following steps:
A, design standards curve
1. according to the design material side of glass production line, the specific embodiment material side that a group is prepared original sheet glass is designed;
2. according to embodiment material side fusion cast glass, with the glass preparation series standard print founded;
3. by standard sample of photo Criterion curve on X-fluorescence tester;
The mensuration of B, original sheet glass composition to be measured
Prepare testing sample with original sheet glass to be measured, with the typical curve obtained in steps A, testing sample is tested, to obtain the percentage composition of each composition in original sheet glass to be measured.
2. the method for a kind of accurate detection original sheet glass composition according to claim 1, it is characterized in that: the preparation section of step 2. Plays print comprises: the glass grinding founded is become glass dust, glass dust solvent is founded series standard print, on this basis, correspondingly, in step B, with above-mentioned identical flux, testing sample is founded to original sheet glass abrasive dust to be measured, with the typical curve obtained in steps A, testing sample is tested again, be the percentage composition of each composition in original sheet glass to be measured with the percentage composition obtaining each composition in testing sample.
3. the method for a kind of accurate detection original sheet glass composition according to claim 1, it is characterized in that: the preparation section of step 2. Plays print comprises: by the glass-cutting of founding, grind, be polished to the series standard print of the thickness identical with testing sample and roughness, correspondingly, in step B, original sheet glass to be measured cut, grind, be polished to the thickness identical with standard sample of photo and the testing sample of roughness.
4. the method for a kind of accurate detection original sheet glass composition according to claim 1, it is characterized in that: step 2. in the operation of fusion cast glass comprise: according to embodiment material side feeding, again by get various raw material blendings, division, then the raw material after division is placed in crucible, puts into sample-melting stove melting preparation.
5. the method for a kind of accurate detection original sheet glass composition according to claim 2, is characterized in that: pure lithium tetraborate analyzed by described solvent.
6. the method for a kind of accurate detection original sheet glass composition according to claim 2, it is characterized in that: the operation of founding series standard print comprises: by glass dust, flux fully mixes in platinum crucible, then the iodate ammonia solution that 5 ~ 8 concentration are 10 ~ 20% is dripped, series standard print is founded in 1100-1150 DEG C of sample-melting stove, correspondingly, founding testing sample is also by original sheet glass powder to be measured, flux fully mixes in platinum crucible, then the iodate ammonia solution that 5 ~ 8 concentration are 10 ~ 20% is dripped, found in 1100-1150 DEG C of sample-melting stove and form.
CN201310528625.0A 2013-10-31 2013-10-31 Method for accurately detecting components of raw glass sheets Pending CN104280415A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107367521A (en) * 2017-06-29 2017-11-21 苏州浪声科学仪器有限公司 Pass through the method for impurity in x-ray fluorescence spectrometry glass
CN109342476A (en) * 2018-11-02 2019-02-15 海南中航特玻科技有限公司 A kind of test method that glass is carried out using high aluminosilicate glass standard specimen

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102401756A (en) * 2010-09-07 2012-04-04 鞍钢股份有限公司 Preparation method for ferromolybdenum sample melting glass body
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102401756A (en) * 2010-09-07 2012-04-04 鞍钢股份有限公司 Preparation method for ferromolybdenum sample melting glass body
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

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王毅民: "荧光分析地质样品时的制样方法", 《岩矿测试》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107367521A (en) * 2017-06-29 2017-11-21 苏州浪声科学仪器有限公司 Pass through the method for impurity in x-ray fluorescence spectrometry glass
CN109342476A (en) * 2018-11-02 2019-02-15 海南中航特玻科技有限公司 A kind of test method that glass is carried out using high aluminosilicate glass standard specimen

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