CN108675633A - A kind of electronic glass and its shrinking percentage test method of low-shrinkage - Google Patents
A kind of electronic glass and its shrinking percentage test method of low-shrinkage Download PDFInfo
- Publication number
- CN108675633A CN108675633A CN201810820037.7A CN201810820037A CN108675633A CN 108675633 A CN108675633 A CN 108675633A CN 201810820037 A CN201810820037 A CN 201810820037A CN 108675633 A CN108675633 A CN 108675633A
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- Prior art keywords
- glass
- electronic
- glass plate
- shrinkage
- shrinking percentage
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
- C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/16—Investigating or analyzing materials by the use of thermal means by investigating thermal coefficient of expansion
Abstract
The invention discloses a kind of electronic glass of low-shrinkage and its shrinking percentage test methods.The electronic glass belongs to silicate glass containing boron and aluminium without alkali, by the optimization of component, achievees the purpose that reduce shrinking percentage, obtains the glass of high thermal stability；The sag of chain for reducing large-size substrate glass plate than elasticity modulus during Automatic Conveying is increased simultaneously, meets high-resolution display and requires.The method test deflection that test method is crossed by micrometering, high certainty of measurement, error are small；The test method can directly, quickly react percent thermal shrinkage of the glass in back-end fabrication processes, and what is be easy and fast to feeds back to production line by production result i.e. test result, adjusts the technological parameter in Improving Glass Manufacturing Processes.
Description
【Technical field】
The invention belongs to electronic glass fields, and in particular to a kind of electronic glass of low-shrinkage and its test of shrinking percentage
Method.
【Background technology】
With the continuous development of display technology, people pursue high-resolution and high grade picture increasingly, to thin film transistor (TFT)
(TFT) there are higher requirement in the size of display screen and response time.Low temperature polycrystalline silicon (LTPS) technology has due to it
Higher electron mobility (1,000 times higher than amorphous silicon technology), and allow to manufacture driving circuit and other electricity on the glass substrate
Sub- device reduces device cost, simplifies the module technique in later stage, improves yields, to manufacture skill as the TFT of current mainstream
Art.
LTPS techniques generally use laser annealing techniques to make amorphous silicon layer, most efficient polysilicon (p-Si) facture
It is to be operated at 600 DEG C or more of temperature, this method can be formed over a large area (to be used for fast with high electron mobility
Speed conversion) and fabulous TFT uniformities polycrystalline-Si films.This manufacturing method generally include using increase temperature method according to
Secondary deposition film simultaneously forms pattern, and this method makes the temperature that base material is heated to 500 DEG C or more, at this high temperature, base
Glass sheet easy tos produce contraction and deforms, and the raising of pixel is hindered, to prevent glass baseplate in hot procedure later
Contraction distortion, base plate glass need lower shrinking percentage；The shrinking percentage of general base plate glass is less than 40ppm, cannot be satisfied this
Demand of the method to substrate, further to solve the problems, such as to shrink, shrinking percentage needs further decrease.
On the other hand, the test method of glass plate percent thermal shrinkage directly determines the accuracy of its shrinkage results, in turn
Instruct producing line technological design.
Dilatometer is currently mainly used or annealing strain point instrument tests the thermal contraction of glass, but this measurement fills
Sample can be applied when measuring the power of certain load by setting, which can be such that sample size in entire heat treatment process becomes
Change, especially in holding stage, the thinner glass influence of or diameter smaller on thickness is bigger, so measurement result cannot be really anti-
The thermal contraction performance of glass is reflected, while different thermal contraction test conditions is needed to be made in advance using dilatometer before testing and is somebody's turn to do
The corresponding standard curve of test condition, increases measurement period, it is therefore desirable to which one kind being capable of accurate fast reaction low-shrinkage glass
Percent thermal shrinkage test method of the glass in the backend process process such as TFT.
【Invention content】
It is an object of the invention to overcome the above-mentioned prior art, provide a kind of low-shrinkage electronic glass and its
Shrinking percentage test method.The electronic glass belongs to silicate glass containing boron and aluminium without alkali, has very in display device preparation process
Low change in size, i.e. percent thermal shrinkage are low.
In order to achieve the above objectives, the present invention is achieved by the following scheme：
A kind of electronic glass of low-shrinkage, in mole percent, the oxide components content of electronic glass is：
SiO2：64.5-76.8%；Al2O3：7-14%；B2O3：3-5%；MgO：1-3%；CaO：7-9%；SrO：1.1-4.3%；BaO：
0-2%；Wherein：[BaO]/[SrO] ＜ 1.2.
Further improvement of the present invention is：
Preferably, percent thermal shrinkage≤10ppm；Glass viscosity reaches temperature of glass liquid≤1270 DEG C when 35000dPas；
Liquidus viscosity >=105dPa·s。
Preferably, density ＜ 2.6g/cm3；Than elasticity modulus >=32GPa/gcm3。
A kind of electronic glass shrinking percentage test method, includes the following steps：
1) rectangular glass is chosen, is crossed along glass plate longitudinal center, XY is labeled as, the sides XY are crossed as the first glass in center
Glass plate, the other side are the second glass plate；
2) two datum lines AB and CD are laterally drawn along glass plate, the vertical range between AB and CD is L；Datum line AB is with XY
It is divided into AA1 and BB1 for boundary, datum line CD is divided into CC1 and DD1 by boundary of XY；
3) the first glass plate and the second glass plate are separated along the directions XY；
4) by the first glass plate in Muffle furnace heating and thermal insulation postcooling to room temperature；
5) the first glass plate and the second glass plate are spliced along XY, measure vertical range a, CC1 between AA1 and BB1 and
Vertical range b between DD1；
6) percent thermal shrinkage is calculated；
If 6-1) AA1 and CC1 is in the homonymy of BB1 and DD1,
Percent thermal shrinkage=(∣ a ∣-∣ b ∣)/L
If 6-2) AA1 is in the side of BB1, CC1 is in the other side of DD1, then
Percent thermal shrinkage=(∣ a ∣+∣ b ∣)/L.
Preferably, rectangular glass length >=180mm, wide >=60mm in step 1).
Preferably, L >=150mm in step 2).
Preferably, heating temperature is 600 DEG C in step 4), heating time 10min.
Compared with prior art, the invention has the advantages that：
The invention discloses a kind of electronic glass of low-shrinkage, the electronic glass belongs to alkali-free boroaluminosilicate glass
Glass can get the glass of high thermal stability by the optimization of component, meets high-resolution display and requires.In the present invention, SiO is utilized2
Highly viscous characteristic can be put forward, by SiO2Molar percentage control in 64.5-76.8%, so that the electronic glass is had relatively strong
Durability and mechanical strength, while being not necessarily to the longer quartz raw material melting time again, it is difficult to reduce production.A12O3It can improve
The chemical stability of glass reduces devitrification of glass tendency, while can also improve glass hard (HRC65Yi Shang) and mechanical strength, is suitable for production ruler
Very little plate glass with high accuracy controls its total content 14% hereinafter, making the viscosity of glass melting liquid will not be excessively high, and melting is warm
Degree be less than 1650 DEG C, and can take into account glass melt quality, glass forming temperature, devitrification problems, glass machinery intensity and
Chemical stability.B2O3It has been a kind of component of fluxing action, the melting that viscosity promotes glass, such as B can be reduced2O3Content
Less than 3%, then it is as the not sufficiently effective of fluxing agent, and merely reduces B2O3Content easily causes other problems, including melting
The deterioration of ability and the increase of bubble；On the other hand, higher B2O3Content easily reduces acid resistance, while reducing answering for glass
Height, and then thermal stability declines.MgO can reduce the high temperature viscosity of glass, and will not strain point be declined, thus promote
The melting of glass, if the content of MgO is more than 3%, the tendency towards devitrification of glass increases；The effect of CaO is similar to MgO, if
The content of CaO is more than 9%, then devitrification of glass tendency increases；The influence of SrO is similar to BaO, is a kind of change not only improving glass
It learns tolerance and also improves the component of its tendency toward devitrification, the content of SrO is more than 4.3%, can increase the density of glass；BaO's
Content is more than 2%, then strain point declines so that the heat resistance of glass deteriorates.On the other hand, the contraction of electronic glass is main because disappearing
De-stress generates, and under conditions of same technique and production equipment, stress remnants are identical.The molding electronics of overflow downdraw
Glass, annealing furnace vertical design, annealing furnace height design space is limited, and base plate glass is limited in the annealing furnace residence time, generally
For 1min or so, stress cannot be completely eliminated, residual stress is more.The present invention is in the condition for not changing technique and production equipment
Under, achieve the purpose that reduce shrinking percentage by adjusting material side, reduces the requirement to glass annealing process, reduce subsequent anneal
The design difficulty of stove.
Further, the present invention by adjusting glass component so that percent thermal shrinkage≤10ppm of glass, be less than it is existing
The shrinking percentage of the shrinking percentage of electronic glass, substrate is low, and deformation rate is small, and thermal stability increases；Glass viscosity reaches 35000dPas
When temperature of glass liquid≤1270 DEG C, it is small to the high-temerature creep and corrosive effect of producing equipment.
Further, the glass of tie element of the present invention, than elasticity modulus >=32GPa/gcm3；The present invention by adjusting
Ingredient reduces sag of chain (amount of deflection) of large-size substrate glass plate during Automatic Conveying.
The invention discloses a kind of test method of corresponding electronic glass shrinking percentage, this method is different from existing by swollen
Swollen instrument or annealing strain point instrument test thermal stability, and the test method in the present invention is tested by the method for micrometering of crossing to be become
Shape amount, high certainty of measurement, error are small；The test method can directly, quickly react heat of the glass in back-end fabrication processes
Shrinking percentage, the technological parameter for feeding back to production line, adjusting in Improving Glass Manufacturing Processes being easy and fast to.
【Description of the drawings】
Fig. 1 is the glass plate schematic diagram of the present invention；
Fig. 2 is that the glass plate of the present invention cuts schematic diagram；
Fig. 3 is the datum line scribing line of the present invention and cuts rear schematic diagram；
Fig. 4 is schematic diagram after two pieces of cropped glass plates splice；
Fig. 5 is AA1 and CC1 in the glass plate close-up schematic view of BB1 and DD1 homonymies；
Fig. 6 is glass plate close-up schematic views of the AA1 and CC1 in BB1 and DD1 heteropleurals；
Wherein：The first glass plates of 1-；The second glass plates of 2-.
【Specific implementation mode】
The present invention is described in further detail below in conjunction with the accompanying drawings：
Referring to Fig. 1, the invention discloses a kind of electronic glasses of low-shrinkage, in mole percent, the electronic glass
Oxide components content be：SiO2：64.5-76.8%；Al2O3：7-14%；B2O3：3-5%；MgO：1-3%；CaO：7-
9%；SrO：1.1-4.3%；BaO：0-2%；Wherein：[BaO]/[SrO] ＜ 1.2, glass its physics in the compositional range are special
Property is：Percent thermal shrinkage≤10ppm；Glass viscosity reaches environment temperature≤1270 DEG C when 35000dPas；Liquidus viscosity >=
105dPa·s；Density ＜ 2.6g/cm3；Than elasticity modulus >=32GPa/gcm3；The glass is suitable for overflow downdraw producer
Method.
Electronic glass disclosed by the invention, ingredient correspond to two important physical characteristics of glass：Percent thermal shrinkage≤
10ppm, than elasticity modulus >=32GPa/gcm3；Percent thermal shrinkage directly affects electronic glass deposition film in LTPS techniques
Process；The elastic sag (amount of deflection) of Young's modulus can influence to be packed into, take out and divide in the babinet of transport glass between processing stand
Every the ability of glass plate；Sag of chain (amount of deflection) is the function of the geometry of the glass plate, the density of the glass and Young's modulus,
They can be collectively referred to as specific modulus.The geometry of sheet glass is determined by being processed requirement.For fixed density, Young mould
The increase of amount is advantageous, because this reduce the sag of chains that big glass plate is shown in transport, processing and hot procedure；
Similarly, any increase of density all should proportionally increase with Young's modulus, otherwise will lead to sagging increase；Therefore
The qualification rate of glass plate is improved, glass sheet sags amount (amount of deflection) is reduced, the specific modulus of glass baseplate should be controlled in 32Gp/g
cm3More than.Percent thermal shrinkage≤10ppm of the electronic glass and than elasticity modulus >=32GPa/gcm3, disclosure satisfy that electronic glass
The requirement that high-resolution is shown.
Quickly to measure the percent thermal shrinkage of above-mentioned electronic glass, convenient for quickly being fed back to production process, for this
The low glass of percent thermal shrinkage in invention designs a kind of shrinking percentage test method, includes the following steps：
1) length >=180mm, wide >=60mm rectangular glass, along glass plate longitudinal center glass referring to Fig. 1 and Fig. 2, are chosen
The sharp objects such as glass knife, sand paper are crossed, and XY is labeled as, and the sides XY are crossed as the first glass plate 1 in center, and the other side is the second glass plate
2；
2) referring to Fig. 3, two datum line AB and CD, AB and CD are drawn along the sharp objects such as glass plate transverse direction glass cutter or sand paper
Symmetrical relative to glass plate cross central line, the vertical range between AB and CD is L, L >=150mm；Datum line AB is using XY as boundary
Limit is divided into AA1 and BB1, and datum line CD is divided into CC1 and DD1 by boundary of XY；
3) the first glass plate 1 and the second glass plate 2 are separated along the directions XY；
4) the first glass plate 1 is heated in Muffle furnace, heat treatment temperature is 600 DEG C, and the time is
10min, heat treatment postcooling to room temperature；
5) referring to Fig. 4, the first glass plate 1 and the second glass plate 2 is spliced along the directions XY, measure two under an optical microscope
Vertical range a, the vertical range b between CC1 and DD1 between datum line AA1 and BB1；
6) percent thermal shrinkage is calculated；
6-1) referring to Fig. 5, if AA1 and CC1 are in the homonymy of BB1 and DD1, i.e. AA1 is in the left side of BB1, and CC1 is DD1's
Left side；Or AA1, on the right side of BB1, CC1 is on the right side of DD1, then：
Percent thermal shrinkage=(∣ a ∣-∣ b ∣)/L；
6-2) referring to Fig. 6, if AA1, in the side of BB1, and CC1 in the other side of DD1, i.e. AA1 is in the left side of BB1, CC1
On the right side of DD1；Or AA1, on the right side of BB1, CC1 is in the left side of DD1, then：
Percent thermal shrinkage=(∣ a ∣+∣ b ∣)/L；
Specific embodiment：
Table 1 is some embodiments in the present invention, carries out being melted for sample according to design component, obtains in present component
Glass in range carries out proportion, Young's modulus and liquidus viscosity performance test to the sample after being melted, and according to this hair
Shrinking percentage test method in bright carries out thermal contraction test, and the test is carried out according to industry testing standard method, specific to join
Number is as shown in table 1 below with result.
1 embodiment glass sample test result of table
In above table, the glass ingredient that preceding 29 embodiments are related to can be seen within the scope of the embodiment of the present invention
Go out, in the compositional range glass percent thermal shrinkage≤10ppm, specific modulus >=32Gp/gcm3.The last one comparative example is normal
The electronic glass ingredient of rule, wherein B2O3With SrO not within the scope of the glass ingredient of the present invention, percent thermal shrinkage 40ppm, poplar
Family name's modulus is 31.93Gp/gcm3。
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (7)
1. a kind of electronic glass of low-shrinkage, which is characterized in that in mole percent, the oxide components of electronic glass contain
Amount is：SiO2：64.5-76.8%；Al2O3：7-14%；B2O3：3-5%；MgO：1-3%；CaO：7-9%；SrO：1.1-
4.3%；BaO：0-2%；Wherein：[BaO]/[SrO] ＜ 1.2.
2. a kind of electronic glass of low-shrinkage according to claim 1, which is characterized in that percent thermal shrinkage≤10ppm；Glass
Glass viscosity reaches temperature of glass liquid≤1270 DEG C when 35000dPas；Liquidus viscosity >=105dPa·s。
3. a kind of electronic glass of low-shrinkage according to claim 1, which is characterized in that density ＜ 2.6g/cm3；Compare bullet
Property modulus >=32GPa/gcm3。
4. the electronic glass shrinking percentage test method described in a kind of claim 1-3 any one, which is characterized in that including following
Step：
1) rectangular glass is chosen, is crossed along glass plate longitudinal center, XY is labeled as, the sides XY are crossed as the first glass plate in center
(1), the other side is the second glass plate (2)；
2) two datum lines AB and CD are laterally drawn along glass plate, the vertical range between AB and CD is L；Datum line AB is using XY as boundary
Limit is divided into AA1 and BB1, and datum line CD is divided into CC1 and DD1 by boundary of XY；
3) the first glass plate (1) and the second glass plate (2) are separated along the directions XY；
4) by the first glass plate (1) in Muffle furnace heating and thermal insulation postcooling to room temperature；
5) the first glass plate (1) and the second glass plate (2) are spliced along XY, measures the vertical range a, CC1 between AA1 and BB1
Vertical range b between DD1；
6) percent thermal shrinkage is calculated；
If 6-1) AA1 and CC1 is in the homonymy of BB1 and DD1,
Percent thermal shrinkage=(∣ a ∣-∣ b ∣)/L
If 6-2) AA1 is in the side of BB1, CC1 is in the other side of DD1, then
Percent thermal shrinkage=(∣ a ∣+∣ b ∣)/L.
5. electronic glass shrinking percentage test method according to claim 4, which is characterized in that rectangular glass in step 1)
Length >=180mm, wide >=60mm.
6. electronic glass shrinking percentage test method according to claim 4, which is characterized in that L >=150mm in step 2).
7. electronic glass shrinking percentage test method according to claim 4, which is characterized in that heating temperature is in step 4)
600 DEG C, heating time 10min.
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Cited By (4)
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| CN109725019A (en) * | 2018-12-29 | 2019-05-07 | 东旭集团有限公司 | Detection device, measuring system and the measurement method that base plate glass is heat-shrinked |
| CN110054401A (en) * | 2019-03-06 | 2019-07-26 | 彩虹显示器件股份有限公司 | A kind of manufacturing method improving electronic glass dimensional stability |
| CN112777923A (en) * | 2020-12-28 | 2021-05-11 | 北京工业大学 | TFT substrate glass annealing process and TFT substrate glass prepared by adopting same |
| CN113183214A (en) * | 2021-05-28 | 2021-07-30 | 芜湖东旭光电科技有限公司 | Cutting device and cutting method for detecting heat wire shrinkage rate of substrate glass |
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