CN105588797A - Method for detecting chemical resistance of TFT-LCD (thin film transistor-liquid crystal display) glass and method for measuring lithium content of glass - Google Patents
Method for detecting chemical resistance of TFT-LCD (thin film transistor-liquid crystal display) glass and method for measuring lithium content of glass Download PDFInfo
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- CN105588797A CN105588797A CN201511023467.9A CN201511023467A CN105588797A CN 105588797 A CN105588797 A CN 105588797A CN 201511023467 A CN201511023467 A CN 201511023467A CN 105588797 A CN105588797 A CN 105588797A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
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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
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
Abstract
The invention discloses a method for detecting chemical resistance of TFT-LCD (thin film transistor-liquid crystal display) glass and a method for measuring lithium content of the glass. The method for detecting the chemical resistance of the TFT-LCD glass comprises the following steps: the content of lithium in a glass sample is measured, and under the condition that the content proportions of other elements in the glass sample are consistent, the lower the lithium content, the better the chemical resistance of TFT-LCD glass. According to the method, not only can the lithium content of the TFT-LCD glass be measured rapidly, but also the chemical resistance of TFT-LCD glass can be detected, so that allocation can be performed on a glass formula in a formula development process.
Description
Technical field
The present invention relates to glass detection method, particularly, relate to a kind of TFT-LCD glass chemical resistanceThe assay method of lithium content in the detection method of energy and this glass.
Background technology
TFT (ThinFilmTransistor)-LCD glass, i.e. TFT LCD glass,It is the one in active matrix type liquid crystal display glass (AM-LCD). Liquid crystal flat panel display, spyOther TFT-LCD is at present unique comprehensive at brightness, contrast, power consumption, life-span, volume and weight etc.In performance, catch up with comprehensively and exceed the display device of CRT monitor, its function admirable, raw on a large scaleProduct characteristic is good, and automaticity is high, and the cost of raw material is cheap, and development space is wide, will become rapidly newThe main product in century is a bright spot of 21 century global economic growth.
Highly basic metal is the coefficient of expansion to TFT-LCD glass, corrosion resistance, machinery and thermodynamics not onlyPerformance impact is larger, and even more serious to the corrosion of kiln in TFT-LCD glass production. KnownBe, two kinds of elements of sodium and potassium can be to TFT-LCD glass production negative effect, and lithium is as finished product in the industryUncommon highly basic metallic element does not draw attention.
In addition, chemical-resistance is an important performance indexes of glass, has aobvious to the etching attenuate of glassThe impact of work. Learn glass chemical-resistance and frit side's relevance but do not exist in prior artMethod, so that just can control the chemical resistance of glass by the material side's allotment in frit side's development processEnergy.
Summary of the invention
The object of this invention is to provide a kind of detection method and this glass of TFT-LCD glass chemical-resistanceThe assay method of lithium content in glass, the lithium content of the method in can not only fast detecting TFT-LCD glass,And can measure the chemical-resistance of glass, thereby the glass formula in the side's of expecting development process is adjustedJoin.
To achieve these goals, first aspect present invention: a kind of TFT-LCD glass chemically-resistant is providedThe detection method of performance, the method comprises: measure the content of elemental lithium in glass sample, at glass sampleIn, in the consistent situation of the ratio of other constituent content, the content of elemental lithium is lower, this glass chemically-resistantPerformance is better.
Preferably, according to a first aspect of the invention, the method also comprises: measure sodium unit in glass sampleThe content of element, in glass sample, in the consistent situation of the ratio of other constituent content, elemental lithium and sodiumThe content of element is lower, and this glass chemical-resistance is better.
Preferably, according to a first aspect of the invention, the method also comprises: measure potassium unit in glass sampleThe content of element, in glass sample, in the consistent situation of the ratio of other constituent content, elemental lithium, sodiumThe content of element and potassium element is lower, and this glass chemical-resistance is better.
Preferably, according to a first aspect of the invention, adopt ICP-OES method to measure in glass sampleLithium content.
Preferably, according to a first aspect of the invention, after being adopted to dissolution with solvents, glass sample carries out constant volume,Then adopt ICP-OES method to measure lithium content in the solution of constant volume.
Preferably, according to a first aspect of the invention, described solvent is the water of hydrofluoric acid and/or perchloric acidSolution.
Preferably, according to a first aspect of the invention, in described course of dissolution, described glass sample, water,The mass ratio of hydrofluoric acid and perchloric acid is (0.01-0.1): (0.2-20): 1:(0.5-2).
Preferably, according to a first aspect of the invention, described dissolving comprises: by described glass sample and moltenAgent is heated to stop heating after Mao Baiyan, then glass sample and solvent is cooled to room temperature, adds 1-3The water of times solvent quality, heats again, until glass sample dissolves.
Preferably, according to a first aspect of the invention, described glass sample is crushed to below 80 micronsCarry out again described dissolving.
Preferably, according to a first aspect of the invention, adopt XRF method or Spectrophotometric DeterminationDetermine the content of sodium element in glass sample.
Preferably, according to a first aspect of the invention, adopt XRF method or Spectrophotometric DeterminationDetermine the content of potassium element in glass sample.
Second aspect present invention: the assay method of lithium content in a kind of TFT-LCD glass is provided, comprises:After glass sample is adopted to dissolution with solvents, carry out constant volume, then adopt ICP-OES method to measure the molten of constant volumeLithium content in liquid.
Preferably, according to a second aspect of the invention, described solvent is the water of hydrofluoric acid and/or perchloric acidSolution.
Preferably, according to a second aspect of the invention, in described course of dissolution, described glass sample, water,The mass ratio of hydrofluoric acid and perchloric acid is (0.01-0.1): (0.2-20): 1:(0.5-2).
Preferably, according to a second aspect of the invention, described dissolving comprises: by described glass sample and moltenAgent is heated to stop heating after Mao Baiyan, then glass sample and solvent is cooled to room temperature, adds 1-3The water of times solvent quality, heats again, until glass sample dissolves.
Preferably, according to a second aspect of the invention, described glass sample is crushed to below 80 micronsCarry out again described dissolving.
Compared with prior art, advantage of the present invention is as follows:
1, adopt a kind of easy method, for detection of the chemical-resistance of glass, and further facilitateThe allotment of frit side;
2, the assay method of elemental lithium of the present invention, in glass, elemental lithium dissolves fully, and measurement result is accurate.
Other features and advantages of the present invention are described in detail the detailed description of the invention part subsequently.
Detailed description of the invention
Below the specific embodiment of the present invention is elaborated. Should be understood that, retouch in this placeThe detailed description of the invention of stating only, for description and interpretation the present invention, is not limited to the present invention.
First aspect present invention: a kind of detection method of TFT-LCD glass chemical-resistance is provided, shouldMethod comprises: measure the content of elemental lithium in glass sample, and in glass sample, other constituent contentIn the consistent situation of ratio, the content of elemental lithium is lower, and this glass chemical-resistance is better.
According to a first aspect of the invention, the method can also comprise: measure sodium element in glass sampleContent, in glass sample, in the consistent situation of the ratio of other constituent content, elemental lithium and sodium elementContent lower, this glass chemical-resistance is better.
According to a first aspect of the invention, the method can also comprise: measure potassium element in glass sampleContent, in glass sample, in the consistent situation of the ratio of other constituent content, elemental lithium, sodium elementLower with the content of potassium element, this glass chemical-resistance is better.
According to a first aspect of the invention, the ratio of described other constituent content unanimously refers to except alkali goldThe quality sum that belongs to other element outside element is benchmark, and in glass sample, the ratio of other element is identical.
According to a first aspect of the invention, lithium is the auxiliary flux of X-fluorescence test pieces, therefore cannot adoptX-fluorescence method is measured the content of lithium, and the present invention preferably adopts ICP-OES, and (inductively coupled plasma is sent outPenetrate spectrum) method measures the lithium content in glass sample.
According to a first aspect of the invention, because glass sample dissolves difficulty, therefore glass sample can be adoptedWith carrying out constant volume after dissolution with solvents, the lithium that then adopts ICP-OES method to measure in the solution of constant volume containsAmount, wherein, described solvent is preferably the aqueous solution of hydrofluoric acid and/or perchloric acid, in described course of dissolution,The mass ratio of described glass sample, water, hydrofluoric acid and perchloric acid is preferably (0.01-0.1): (0.2-20):1：(0.5-2)。
According to a first aspect of the invention, for glass sample is fully dissolved, described dissolving preferably includes:Described glass sample and solvent are heated to stop heating after Mao Baiyan, then by cold to glass sample and solventBut to room temperature, add the water of 1-3 times of solvent quality, again heat, until glass sample dissolving,In addition, also preferably described glass sample is crushed to 80 microns and carries out again below described dissolving.
According to a first aspect of the invention, well-known to those skilled in the art, can adopt X rayThe content of sodium element in fluorescent method or spectrophotometry glass sample, also can adopt X ray glimmeringThe content of potassium element in light method or spectrophotometry glass sample.
Second aspect present invention: the assay method of lithium content in a kind of TFT-LCD glass is provided, comprises:After glass sample is adopted to dissolution with solvents, carry out constant volume, then adopt ICP-OES method to measure the molten of constant volumeLithium content in liquid, wherein, described solvent is preferably the aqueous solution of hydrofluoric acid and/or perchloric acid, described moltenIn solution process, the mass ratio of described glass sample, water, hydrofluoric acid and perchloric acid is preferably (0.01-0.1):(0.2-20)：1：(0.5-2)。
According to a second aspect of the invention, for glass sample is fully dissolved, described dissolving preferably includes:Described glass sample and solvent are heated to stop heating after Mao Baiyan, then by cold to glass sample and solventBut to room temperature, add the water of 1-3 times of solvent quality, again heat, until glass sample dissolving,In addition, also preferably described glass sample is crushed to 80 microns and carries out again below described dissolving.
To further illustrate the present invention by embodiment below, but therefore the present invention is not taken officeWhat restriction.
The embodiment of the present invention adopts the light splitting in GB/T1347-2008 soda-lime-silica glass chemical analysis methodThe content of sodium and potassium in photometry mensuration TFT-LCD glass.
The embodiment of the present invention adopts the method for the glass in ICP-OES mensuration TFT-LCD glass as follows:
(1), TFT-LCD glass sample is carried out being ground to below 80 microns after division, be then placed inIn the baking oven of 110 DEG C, be dried 2 hours, obtain glass powder;
(2), take 0.1000g glass powder and 5g hydrofluoric acid solution (40 quality %), the pure high chlorine of 3gAcid solution (70 quality %) is put into platinum crucible heating for dissolving, when liquid volume in crucible is less than 3mLLeft and right, a large amount of white cigarettes of emerging, crucible is cooling after, put into 15mL water, continue afterwards crucible to carry outHeating, until liquid clarification wherein;
(3), will after the liquid cools in crucible, be transferred to constant volume in 50mL polytetrafluoroethylene (PTFE) volumetric flask,And by crucible washing 8 times, washings are transferred in volumetric flask;
(4), adopt ICP-OES to detect solution in volumetric flask, and and standard working curve(adopting respectively the standard liquid of 0ppm, 1ppm and 2ppm to measure production standard curve) carries outContrast, calculates lithium content in glass, and wherein, analysis spectral line is 670.784 nanometers, RF powerFor 800KW, assisted gas flow is 0.5L/min, and be 5s the time of integration, and atomizer flow is 0.80L/min,Pump speed is 30r/min, and pump stabilization time is 0s.
The chemical-resistance detection method of TFT-LCD glass of the present invention is as follows: the hydrogen that adopts 10 quality %Fluorspar acid solution carries out chemical etching attenuate to glass sample, measures the etching speed of glass.
Embodiment 1-8
The inspection of lithium content in the detection method of embodiment 1-8 explanation glass chemical-resistance of the present invention and glassSurvey method.
Choose glass sample 1-8 (from Dong Xu Optoelectronics Technology limited company production line, glass sampleExcept alkali metal, the ratio of other constituent content is consistent) carry out respectively ICP-OES mensuration, light splitting lightDegree method is measured and chemical-resistance detects, and lithium content, sodium content and the potassium measured respectively in glass sample containThe chemical-resistance of amount and glass sample, concrete data are as shown in table 1.
Embodiment 9-10
The impact of the solvent difference of embodiment 9-10 explanation dissolving glass on lithium content measurement result.
The condition determination of lithium content is substantially the same manner as Example 1, and unique difference is hydrogen fluorine in solventAcid solution and perchloric acid solution add quality (concentration of hydrofluoric acid solution and perchloric acid solution and embodiment1 is identical), concrete solvent data are in table 2.
Comparative example 1-4
The impact of the solvent difference of comparative example 1-4 explanation dissolving glass on lithium content measurement result.
The condition determination of lithium content is substantially the same manner as Example 1, and unique difference is hydrogen fluorine in solventAcid solution and perchloric acid solution add quality (concentration of hydrofluoric acid solution and perchloric acid solution and embodiment1 is identical), concrete solvent data are in table 2.
From the data of table 1, can find out, in the case of the ratio of other constituent content is identical, glassIn sample, elemental lithium content is higher, and the etching speed of glass is faster, and chemical-resistance is poorer; Glass sampleMiddle elemental lithium and sodium element content are higher, and the etching speed of glass is faster, and chemical-resistance is poorer; GlassIn sample, elemental lithium, sodium element and Determination of Potassium are higher, and the etching speed of glass is faster, chemical resistanceCan be poorer.
Can find out from the data of table 2, in glass course of dissolution, add hydrofluoric acid and high chlorine as solventThe ratio difference of acid, the solute effect of glass is also different, specifically, at hydrofluoric acid of the present invention and heightIn the scope of chloric acid additional proportion, the solute effect of glass is good, and exceeds ratio of the present invention, glassSolute effect variation, thus cause the lithium content that can detect also to reduce.
Table 1
| Project | Lithium content, ppm | Sodium content, ppm | Potassium content, ppm | Etching speed, micro-m/min |
| Embodiment 1 | 26.71 | 0 | 0 | 7.3 |
| Embodiment 2 | 14.35 | 0 | 0 | 6.5 |
| Embodiment 3 | 18.51 | 7.2 | 0 | 11.6 |
| Embodiment 4 | 18.51 | 6.7 | 0 | 11.3 |
| Embodiment 5 | 15.36 | 6.3 | 0 | 10.2 |
| Embodiment 6 | 23.73 | 45.64 | 32.17 | 15.3 |
| Embodiment 7 | 23.73 | 45.64 | 29.84 | 14.2 |
| Embodiment 8 | 19.46 | 36.54 | 19.28 | 12.3 |
Table 2
| Project | Hydrofluoric acid solution adds quality, g | Perchloric acid solution adds quality, g | Lithium content, ppm |
| Standard value | / | / | 26.73 |
| Embodiment 1 | 5 | 3 | 26.71 |
| Embodiment 9 | 4.1 | 3.47 | 26.65 |
| Embodiment 10 | 5.98 | 2.24 | 26.67 |
| Comparative example 1 | / | 5.87 | 23.84 |
| Comparative example 2 | 10.08 | / | 24.77 |
| Comparative example 3 | 3.3 | 3.87 | 25.33 |
| Comparative example 4 | 7.23 | 1.81 | 25.17 |
Claims (16)
1. a detection method for TFT-LCD glass chemical-resistance, the method comprises: measure glassThe content of elemental lithium in sample, in glass sample, in the consistent situation of the ratio of other constituent content,The content of elemental lithium is lower, and this glass chemical-resistance is better.
2. according to the detection method of the TFT-LCD glass chemical-resistance of claim 1, wherein, be somebody's turn to doMethod also comprises: measure the content of sodium element in glass sample, and in glass sample, other constituent contentThe consistent situation of ratio under, the content of elemental lithium and sodium element is lower, this glass chemical-resistance is better.
3. according to the detection method of the TFT-LCD glass chemical-resistance of claim 2, wherein, be somebody's turn to doMethod also comprises: measure the content of potassium element in glass sample, and in glass sample, other constituent contentThe consistent situation of ratio under, the content of elemental lithium, sodium element and potassium element is lower, this glass chemically-resistantPerformance is better.
4. according to the detection method of the TFT-LCD glass chemical-resistance of claim 1, wherein, adoptWith the lithium content in ICP-OES method mensuration glass sample.
5. according to the detection method of the TFT-LCD glass chemical-resistance of claim 4, wherein, incite somebody to actionGlass sample carries out constant volume after adopting dissolution with solvents, then adopts ICP-OES method to measure the solution of constant volumeIn lithium content.
6. according to the detection method of the TFT-LCD glass chemical-resistance of claim 5, wherein, instituteState the aqueous solution that solvent is hydrofluoric acid and/or perchloric acid.
7. according to the detection method of the TFT-LCD glass chemical-resistance of claim 6, wherein, instituteState in course of dissolution, the mass ratio of described glass sample, water, hydrofluoric acid and perchloric acid is (0.01-0.1):(0.2-20)：1：(0.5-2)。
8. according to the detection method of the TFT-LCD glass chemical-resistance of claim 5, wherein, instituteState to dissolve and comprise: described glass sample and solvent are heated to stop heating after Mao Baiyan, then by glassSample and solvent are cooled to room temperature, add the water of 1-3 times of solvent quality, again heat, until glassGlass sample dissolution.
9. according to the detection method of the TFT-LCD glass chemical-resistance of claim 5, wherein, incite somebody to actionDescribed glass sample is crushed to 80 microns and carries out below described dissolving again.
10. according to the detection method of the TFT-LCD glass chemical-resistance of claim 2 or 3, itsIn, the content of sodium element in employing XRF method or spectrophotometry glass sample.
11. according to the detection method of the TFT-LCD glass chemical-resistance of claim 3, wherein,Adopt the content of potassium element in XRF method or spectrophotometry glass sample.
The assay method of lithium content in 12. 1 kinds of TFT-LCD glass, comprising: glass sample is adoptedAfter dissolution with solvents, carry out constant volume, then adopt ICP-OES method to measure the lithium content in the solution of constant volume.
13. according to the assay method of lithium content in the TFT-LCD glass of claim 12, wherein, and instituteState the aqueous solution that solvent is hydrofluoric acid and/or perchloric acid.
14. according to the assay method of lithium content in the TFT-LCD glass of claim 13, wherein, and instituteState in course of dissolution, the mass ratio of described glass sample, water, hydrofluoric acid and perchloric acid is (0.01-0.1):(0.2-20)：1：(0.5-2)。
15. according to the assay method of lithium content in the TFT-LCD glass of claim 12, wherein, and instituteState to dissolve and comprise: described glass sample and solvent are heated to stop heating after Mao Baiyan, then by glassSample and solvent are cooled to room temperature, add the water of 1-3 times of solvent quality, again heat, until glassGlass sample dissolution.
16. according to the assay method of lithium content in the TFT-LCD glass of claim 12, wherein, and willDescribed glass sample is crushed to 80 microns and carries out below described dissolving again.
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