CN105651745A - Fluorescence detection method of zirconia content in TFT glass - Google Patents
Fluorescence detection method of zirconia content in TFT glass Download PDFInfo
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- CN105651745A CN105651745A CN201511015953.6A CN201511015953A CN105651745A CN 105651745 A CN105651745 A CN 105651745A CN 201511015953 A CN201511015953 A CN 201511015953A CN 105651745 A CN105651745 A CN 105651745A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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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
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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
- G01N2001/2866—Grinding or homogeneising
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Abstract
The invention discloses a fluorescence detection method of the zirconia content in TFT glass. The method comprises: a, finely grinding a glass sample to obtain glass powder; b, mixing the glass powder obtained from the step a with a fusing agent and a releasing agent for fusion sample preparation to obtain a fused glass sheet, wherein the mass ratio of the glass powder to the fusing agent to the releasing agent is 1: (0.5-2): (0.01-0.1), and the fusing agent is a mixture of lithium tetraborate and lithium metaborate with the mass ratio being (1-5): 1; and c, performing fluorescence detection of the fused glass sheet obtained from the step b to obtain the zirconia content in the glass sample. According to the method, the zirconia content in glass can be quickly, accurately, and efficiently measured.
Description
Technical field
The present invention relates to glass detection field, in particular it relates to the fluorescence detection method of zirconia content in a kind of TFT glass.
Background technology
Owing to various glass products have been widely applied to the every field of productive life, and the glass performance used in different field and production technology have very big difference, it is especially applicable to the TFT glass of high-end Display Technique, the equipment of production and manufacturing technique requirent is very harsh, and wherein product quality and product yield are had the greatest impact by the technology controlling and process ability of glass-melting furnace. The brick body of glass-melting furnace usually contains the refractory material of significantly high zirconia content, this refractory material can be subject to the erosion of vitreous humour in the case of a high temperature, the zirconium oxide major part eaten away can melt and be distributed in vitreous humour, or some is deposited on furnace bottom due to its higher density. Zirconia content in the vitreous humour flowed out from smelting furnace generally can reflect flow condition and the vitreous humour erosion degree to furnace refractories of inside furnace vitreous humour, also becoming the effective and important means to glass-melting furnace condition monitoring so the zirconia content in vitreous humour is monitored, in glass, the detection fast and accurately of zirconia content just seems particularly important.
In traditional glass, zirconic fluorescence analysis method is due to the existence of bead matrix effect, so the flux large percentage adopted, the mass ratio of usual glass dust and flux is 1:10, in so high dilution ratio situation, when in glass zirconia content lower than to a certain degree, zirconia content in melten glass sheet dilutes further and can be closer to or limit lower than the detection of fluorescence spectrophotometer, thus causing the accuracy of test result and measuring accuracy to significantly reduce, loses its meaning of monitoring.
If it addition, use the pressed disc method of glass dust hybrid adhesive to measure zirconia content, then because its granularity effect, skin effect and sample dispersion uniformity coefficient also can have a strong impact on stability and the accuracy of test result.
Summary of the invention
It is an object of the invention to provide the fluorescence detection method of zirconia content in a kind of TFT glass, the method can quickly, accurately and efficiently measure zirconic content in glass.
To achieve these goals, the present invention provides the fluorescence detection method of zirconia content in a kind of TFT glass, and the method includes: a, glass sample is carried out levigate process, obtains glass powder; B, gained glass powder in step a is mixed with flux, releasing agent after carry out molten sample film-making, obtain molten sample sheet glass; Wherein, the mass ratio of described glass powder, flux and releasing agent is 1:(0.5-2): (0.01-0.1), described flux is the mixture of lithium tetraborate and lithium metaborate, and in described solvent, lithium tetraborate is (1-5) with the mass ratio of lithium metaborate: 1; C, molten for gained in step b sample sheet glass is carried out fluoroscopic examination, obtain the zirconic content of glass sample.
Preferably, the mass ratio of described glass powder, flux and releasing agent is 1:(0.8-1.2): (0.02-0.05).
Preferably, in described flux, the mass ratio of lithium tetraborate and lithium metaborate is (1-3): 1.
Preferably, described levigate process carries out in oscillating mill, and the mould used by described oscillating mill is tungsten carbide material.
Preferably, the particle diameter of described glass powder is less than 45 microns.
Preferably, the particle diameter of described glass powder is 1-40 micron.
Preferably, described releasing agent is ammonium iodide and/or ammonium bromide.
Preferably, the condition of described molten sample film-making is: molten sample temperature is 1100-1250 DEG C, and the time of molten sample is 15-20 minute.
Preferably, molten model machine automatically is adopted to carry out described molten sample film-making.
Preferably, described molten sample film-making carries out in platinum yellow crucible.
What in TFT glass of the present invention, the fluorescence detection method of zirconia content can reduce flux makes consumption, improve detectable zirconia content in molten sample sheet glass to be measured, effectively eliminate mineral effect and granularity effect, significantly reduce matrix effect, thus expanding zirconic detection range in TFT glass, can not only accurately, quickly and efficiently measure the zirconia content in TFT glass, and smelting furnace can be realized and produce the monitoring of the zirconia content in TFT glass process, it is ensured that produce stable carrying out.
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently.
Detailed description of the invention
Hereinafter the specific embodiment of the present invention is described in detail. It should be appreciated that detailed description of the invention described herein is merely to illustrate and explains the present invention, it is not limited to the present invention.
The present invention provides the fluorescence detection method of zirconia content in a kind of TFT glass, and the method includes: a, glass sample is carried out levigate process, obtains glass powder; B, gained glass powder in step a is mixed with flux, releasing agent after carry out molten sample film-making, obtain molten sample sheet glass; Wherein, the mass ratio of described glass powder, flux and releasing agent is 1:(0.5-2): (0.01-0.1), described flux is the mixture of lithium tetraborate and lithium metaborate, and in described solvent, lithium tetraborate is (1-5) with the mass ratio of lithium metaborate: 1; C, molten for gained in step b sample sheet glass is carried out fluoroscopic examination, obtain the zirconic content of glass sample.
According to the present invention, the mass ratio of described glass powder, flux and releasing agent is preferably 1:(0.8-1.2): (0.02-0.05).
Present inventors discovered unexpectedly that, choose mass ratio for (1-5): the lithium tetraborate of 1 and lithium metaborate are used for melting glass powder as flux, good effect can be reached, and can reduce flux make consumption, further, in described flux, the mass ratio of lithium tetraborate and lithium metaborate is preferably (1-3): 1.
According to the present invention, described levigate process can carry out in oscillating mill, and the mould used by described oscillating mill is preferably tungsten carbide material.
According to the present invention, in order to make glass sample dissolve better, the particle diameter of described glass powder is preferably smaller than 45 microns, more preferably 1-40 micron.
According to the present invention, the effect of releasing agent is that the molten sample sheet glass making molten sample film-making gained more easily comes off, and described releasing agent can be ammonium iodide and/or ammonium bromide, it is preferred to ammonium iodide.
According to the present invention it is possible to adopt molten model machine automatically to carry out described molten sample film-making, molten sample film-making can carry out in platinum yellow crucible, and the condition of described molten sample film-making can be: molten sample temperature is 1100-1250 DEG C, and the time of molten sample is 15-20 minute.
Further illustrate the present invention following by embodiment, but the present invention is not therefore subject to any restriction.
Embodiment 1
In the TFT glass of the embodiment of the present invention 1, the fluorescence-detecting step of zirconia content is as follows:
(1), take 25 grams broken after glass sample (from Dong Xu Optoelectronics Technology limited company production line, zirconia content is 0.0040 mass %), it is placed in the vibromill of tungsten carbide material, and drip 8 dehydrated alcohol as dispersant, vibrate 30 seconds, the screen cloth post-drying of 400 orders crossed by sample after levigate process, obtains glass powder;
(2), accurately weigh 3.000g glass powder and 3.000g mixed flux (in this flux, lithium tetraborate and lithium metaborate mass ratio are 2:1), be placed in agate mortar and be sufficiently mixed uniformly;
(3), the 6g mixture of gained in step (2) is moved in platinum yellow crucible, the ammonium iodide solution of 10 0.2g/mL of dropping is as releasing agent, at 1200 DEG C, 15 minutes are founded in molten model machine automatically, after molten sample program end of run, take out crucible and be cooled to room temperature, take out the molten sample sheet glass founded, it is labeled as sample 1-a, properly preserves;
(4), using the glass powder of gained in (1), repetition step (2), (3) found two molten sample sheet glass again, are respectively labeled as 1-b, 1-c;
(5), adopting x-ray fluorescence analyzer that tri-samples of above-mentioned 1-a, 1-b, 1-c are tested, and use the fluorometric investigation curve made to be analyzed, result is as shown in table 1.
Embodiment 2
Embodiment 2 method of testing is identical with embodiment 1, is different in that, the addition of flux is 1.500 grams, and in flux, lithium tetraborate and lithium metaborate mass ratio are 1:1, and test result is as shown in table 1.
Embodiment 3
Embodiment 3 method of testing is identical with embodiment 1, is different in that, the addition of flux is 6.000 grams, and in flux, lithium tetraborate and lithium metaborate mass ratio are 5:1, and test result is as shown in table 1.
Comparative example 1
The method of testing of comparative example 1 is identical with embodiment 1, is different in that, the addition of flux is 3.000 grams, and flux is pure lithium tetraborate, and test result is as shown in table 1.
Comparative example 2
The method of testing of comparative example 2 is identical with embodiment 1, is different in that, the addition of flux is 6.000 grams, and flux is pure lithium metaborate, and test result is as shown in table 1.
Embodiment 4
Embodiment 4 provides the test result of zirconia content in one group of TFT glass.
Determination step is as follows:
(1), four not same date (A date, B date on Qu Dongxu Optoelectronics Technology limited company production line, date C, date D) glass sample appropriate, described in embodiment 1, step (1), (2), (3) are melting into the molten sample sheet glass of a, b, c, d tetra-, four glass samples of corresponding date A, B, C, D;
(2), by molten for a, b, c, d tetra-described in step (1) sample sheet glass using the fluorometric investigation curve made to test, test result is as shown in table 2.
From embodiment 1-4, even the method for the present invention is also fine to zirconia content test result repeatability very low in glass, so without same sample is repeatedly tested to determine the reliability of its result again, additionally zirconia content in the product of different time on product line is tested, test result may be used for the fluctuation situation of smelting furnace production technology being described or for adjusting production mode reform, it is possible to as steady production, the strong reference widening process bands.
Table 1
| Project | 1-a | 1-b | 1-c | Meansigma methods (quality %) |
| Embodiment 1 test result (quality %) | 0.0041 | 0.0038 | 0.0043 | 0.0041 |
| Embodiment 2 test result (quality %) | 0.0037 | 0.0046 | 0.0047 | 0.0042 |
| Embodiment 3 test result (quality %) | 0.0035 | 0.0041 | 0.0038 | 0.0038 |
| Comparative example 1 test result (quality %) | 0.0022 | 0.0057 | 0.0032 | 0.0037 |
| Comparative example 2 test result (quality %) | 0.0083 | 0.0075 | 0.0043 | 0.0067 |
Table 2
| The sample date | A | B | C | D |
| Sample number into spectrum | a | b | c | d |
| Zirconium oxide actual content (quality %) | 0.0071 | 0.0107 | 0.0134 | 0.0131 |
| Test result (quality %) | 0.0072 | 0.0105 | 0.0133 | 0.0131 |
Claims (10)
1. a fluorescence detection method for zirconia content in TFT glass, the method includes:
A, glass sample is carried out levigate process, obtain glass powder;
B, gained glass powder in step a is mixed with flux, releasing agent after carry out molten sample film-making, obtain molten sample sheet glass; Wherein, the mass ratio of described glass powder, flux and releasing agent is 1:(0.5-2): (0.01-0.1), described flux is the mixture of lithium tetraborate and lithium metaborate, and in described solvent, lithium tetraborate is (1-5) with the mass ratio of lithium metaborate: 1;
C, molten for gained in step b sample sheet glass is carried out fluoroscopic examination, obtain the zirconic content of glass sample.
2. method according to claim 1, wherein, the mass ratio of described glass powder, flux and releasing agent is 1:(0.8-1.2): (0.02-0.05).
3. method according to claim 1, wherein, in described flux, lithium tetraborate is (1-3) with the mass ratio of lithium metaborate: 1.
4. method according to claim 1, wherein, described levigate process carries out in oscillating mill, and the mould used by described oscillating mill is tungsten carbide material.
5. method according to claim 1, wherein, the particle diameter of described glass powder is less than 45 microns.
6. method according to claim 1, wherein, the particle diameter of described glass powder is 1-40 micron.
7. method according to claim 1, wherein, described releasing agent is ammonium iodide and/or ammonium bromide.
8. method according to claim 1, wherein, the condition of described molten sample film-making is: molten sample temperature is 1100-1250 DEG C, and the time of molten sample is 15-20 minute.
9. method according to claim 1, wherein, adopts molten model machine automatically to carry out described molten sample film-making.
10. method according to claim 1, wherein, described molten sample film-making carries out in platinum yellow crucible.
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| CN201511015953.6A CN105651745A (en) | 2015-12-29 | 2015-12-29 | Fluorescence detection method of zirconia content in TFT glass |
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| CN201511015953.6A CN105651745A (en) | 2015-12-29 | 2015-12-29 | Fluorescence detection method of zirconia content in TFT glass |
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Cited By (3)
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| CN106950205A (en) * | 2017-02-22 | 2017-07-14 | 歌尔股份有限公司 | The assay method of zirconia ceramics composition |
| 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 |
| CN108982563A (en) * | 2018-08-03 | 2018-12-11 | 武汉科技大学 | The preparation method of the XRF analysis sheet glass of demolding aids effect |
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| CN108982563B (en) * | 2018-08-03 | 2021-02-19 | 武汉科技大学 | Method for preparing glass sheet for XRF analysis of release aid effect |
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Application publication date: 20160608 |