CN105973927A - Method for determining shrinkage rate of glass - Google Patents
Method for determining shrinkage rate of glass Download PDFInfo
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- CN105973927A CN105973927A CN201610284112.3A CN201610284112A CN105973927A CN 105973927 A CN105973927 A CN 105973927A CN 201610284112 A CN201610284112 A CN 201610284112A CN 105973927 A CN105973927 A CN 105973927A
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B21/00—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant
- G01B21/02—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness
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- Health & Medical Sciences (AREA)
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- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention relates to the technical field of glass production, and discloses a method for determining the shrinkage rate of glass. The method comprises the following steps: 1, preparing glass fibers to be determined, and determining the length L1 of heat treated glass fibers in the glass fibers to be determined; 2, carrying out heat treatment on the glass fibers to be determined, and determining the length change deltaL of the glass fibers before and after the heat treatment; and 3, determining the shrinkage rate C of the glass fibers to be determined, wherein C = deltaL/L1. The method has the advantages of accurate determination result, high reappearance, high precision, high result credibility, and provision of a shrinkage determination reference standard for the research and development process of plate glass.
Description
Technical field
The present invention relates to field of glass production technology, in particular it relates to a kind of side measuring also retract rate
Method.
Background technology
Fast development and portable type electronic product such as notebook computer, flat board along with flat panel display
Popularizing rapidly of computer, smart mobile phone and Intelligent worn device, liquid crystal display role wherein
More and more important, there is lightening, the lcd products more market institute of high-resolution, high image quality
Accept.
Glass substrate is the important component part of liquid crystal display device (LCD), recently as LCD
The development of technology, proposes the highest requirement to the performance of glass substrate material.These requirements are main
Depend on mode and the manufacturing process of liquid crystal display.As shown in (AM-LCD) at active matrix liquid crystal,
Thin film transistor (TFT) (TFT) and chromatic filter layer are through heating for multiple times and to be accurate to micron-sized photoetching process straight
Connect and formed on the glass substrate.Therefore, in order to ensure repeatedly the suitable coincidence of photoetching process, to glass base
The thermal dimensional stability of plate proposes important requirement.In the manufacture process of display device, thermal contraction will
Cause the change of substrate size, it is therefore desirable to also retract rate can be measured more accurately.
At present, the method for testing of plate glass shrinkage factor, roughly the same, it is all to use at glass sample two ends
Diamant or sand paper make marks；Keep flat and anneal into annealing furnace；Measure heat treatment the most under the microscope
Rear labelling changes.Product glass sizes is regular and relatively big, and thickness degree is uniform, and thermal contraction test easily realizes
And repeatability is high；But in the R&D process of plate glass, the glass existing defects founded is (such as glass
There is bubble, in irregular shape etc.), it is impossible to produce the most relatively large sized on production line, surface matter
Amount is high, the uniform plate glass of thickness provides laboratory reference data, and the most aforementioned thermal contraction assay method is difficult
To measure the shrinkage factor of glass in irregular shape, size is little.Current glass substrate maximize, frivolous
Change under the overall situation that direction is developed, need a kind of method easily to weigh more different material sides and technique
The percent thermal shrinkage of the glass produced.
Summary of the invention
The invention aims to overcome drawbacks described above of the prior art, it is provided that a kind of glass that measures is received
The method of shrinkage.
To achieve these goals, the invention provides a kind of method measuring also retract rate, the method
Including:
(1) prepare glass fiber to be measured, and determine the glass fiber length carrying out heat treatment in glass fiber to be measured
Value L1；
(2) glass fiber to be measured is carried out heat treatment, and determine the length change of glass fiber before and after heat treatment
Value Δ L；
(3) shrinkage factor C of glass fiber to be measured, wherein, C=Δ L/L1 are determined.
Under preferable case, in step (1), the preparation method of glass fiber to be measured includes: by glass-pulling
Become glass fiber, after intercepting, the two ends of glass fiber are fired into spherical.
Under preferable case, in step (1), a diameter of 0.3-1mm of the glass fiber being drawn into, enters one
Step is preferably 0.5-0.8mm.
Under preferable case, in step (1), a length of 300-550mm of the glass fiber of intercepting.
Under preferable case, in step (1), spherical a diameter of 2-8mm that glass fiber two ends are fired.
Under preferable case, in step (2), described heat-treating methods includes: depended on by glass fiber to be measured
Secondary carry out hyperthermic treatment, isothermal holding and cooling process.
Under preferable case, the method for described hyperthermic treatment includes: by glass fiber with the intensification of 8-30 DEG C/min
Ramp is to design temperature, it is further preferred that heating rate is 10-20 DEG C/min.
Under preferable case, the method for described isothermal holding includes: be incubated at design temperature by glass fiber
0.01-10h。
Under preferable case, the method that described cooling processes includes: by glass fiber with the cooling of 3-20 DEG C/min
Speed is cooled to room temperature or glass fiber is naturally cooling to room temperature.
Under preferable case, in step (2), determine that the method for length varying value Δ L includes: burnt at two ends
Make glomerate glass fiber vertical hanging to be measured in test device, by the displacement sensing of described test device
System determines length varying value Δ L, and wherein, described test device includes the resistance for heating glass fiber
Stove, for resistance furnace heat up, be incubated or lower the temperature control system, for monitoring the thermoelectricity of glass fiber temperature
Even summation is for monitoring the displacement sensing system of the length change of glass fiber.
Under preferable case, the method determining length varying value Δ L by the displacement sensing system of test device
Including: before hyperthermic treatment and after cooling process, record the position that the sensor of displacement sensing system shows respectively
Shifting value Δ L0 and Δ L1, length varying value Δ L=Δ L0-Δ L1.
Under preferable case, before carrying out heat treatment, glass fiber to be measured is made annealing treatment；Further
Preferably, the method for described annealing includes: by glass fiber to be measured with the heating rate of 8-30 DEG C/min
It is warming up to annealing temperature, and is incubated 30-60min in annealing temperature, be then cooled to room temperature, described annealing
Temperature is that annealing point temperature is to annealing point temperature+5 DEG C；It is further preferred that glass fiber to be measured is incubated
The bale of cotton makes annealing treatment after wrapping up in.
Under preferable case, described glass is glass substrate for flat display, more preferably TFT-LCD
Glass substrate, cover-plate glass or PDP glass, the most preferably TFT-LCD glass substrate.
The method measuring also retract rate of the present invention, by glass-pulling is become glass fiber, measures its heat
Length varying value before and after process determines shrinkage factor, solves in plate glass R&D process due to glass
In irregular shape little so that also retract rate cannot be measured to provide laboratory reference data, nothing with glass size
Method weighs the problem of the performance of glass in development process, the measurement result of the method is accurate, repeatability is high,
Precision is high, credible result degree is high, glass properties research is had huge practical value, for flat board glass
The R&D process of glass provides the reference standard of a shrinkage determination, can depend on as the theory of research and development
According to.
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 detailed description of the invention of the present invention is described in detail.It should be appreciated that this place is retouched
The detailed description of the invention stated is merely to illustrate and explains the present invention, is not limited to the present invention.
The invention provides a kind of method measuring also retract rate, the method includes:
(1) prepare glass fiber to be measured, and determine the glass fiber length carrying out heat treatment in glass fiber to be measured
Value L1；
(2) glass fiber to be measured is carried out heat treatment, and determine the length change of glass fiber before and after heat treatment
Value Δ L；
(3) shrinkage factor C of glass fiber to be measured, wherein, C=Δ L/L1 are determined.
In the case of process of the present invention it is preferred, in step (1), the preparation method of glass fiber to be measured
Including: glass-pulling is become glass fiber, after intercepting, the two ends of glass fiber is fired into spherical.
The glass wire drawing machine founded difference material side pulls into uniform diameter and the identical glass fiber of diameter, excellent
Selection of land, a diameter of 0.3-1mm of the glass fiber being drawn into, more preferably 0.5-0.8mm.Pass through
The method of the present invention measures shrinkage factor, for measuring the performance of glass in development process, when measuring, and choosing
Take the glass fiber of even thickness as experimental subject, the most accurately measure its diameter, same batch
The glass fiber diameter making to measure is close to identical, and error control is within 0.1mm.
Preferably, a length of 300-550mm of the glass fiber of intercepting.The length of concrete intercepting can basis
Practical situation selects.
Preferably, spherical a diameter of 2-8mm that glass fiber two ends are fired.
In the method for the present invention, for determining the glass fiber length value carrying out heat treatment in glass fiber to be measured
There is no particular limitation for the method for L1, can be various methods commonly used in the art, such as, can be:
On glass fiber to be measured, two datum lines are demarcated at interval, and the glass fiber between two datum lines is for carrying out
The glass fiber part of heat treatment, measures the length value between two datum lines, and this value is L1.
In the case of process of the present invention it is preferred, in step (2), heat-treating methods includes: will
Glass fiber to be measured carries out hyperthermic treatment, isothermal holding and cooling successively and processes.
In the method for the present invention, for the heating rate not particularly requirement of hyperthermic treatment, as long as by glass
Glass silk is warming up to design temperature, and under preferable case, the method for hyperthermic treatment includes: by glass fiber with
The heating rate of 8-30 DEG C/min is warming up to design temperature, it is further preferred that heating rate is
10-20℃/min。
In the method for the present invention, for the time not particularly requirement of isothermal holding, as long as setting temperature
Degree insulation a period of time, under preferable case, the method for isothermal holding includes: set by glass fiber
Temperature 0.01-10h.
In the method for the present invention, the cooldown rate not particularly requirement processed for cooling, as long as by glass
Glass silk carries out cooling after hyperthermic treatment and isothermal holding and processes, and under preferable case, cooling processes
Method includes: with the cooldown rate of 3-20 DEG C/min, glass fiber is cooled to room temperature or is naturally dropped by glass fiber
Warm to room temperature.
In the method for the present invention, it will be understood by those skilled in the art that the setting described in heat treatment
Temperature is the temperature needed during downstream process process, and this design temperature is according to different downstream processes the most not
With, can determine according to practical situation.Such as, design temperature can be 350 DEG C, 400 DEG C, 500 DEG C
Or 600 DEG C.
In the case of process of the present invention it is preferred, in step (2), determine the side of length varying value Δ L
Method includes: two ends are fired glomerate glass fiber vertical hanging to be measured in test device, by described survey
The displacement sensing system of electricity testing device determines length varying value Δ L, wherein, described test device include for
Heating glass fiber resistance furnace, for resistance furnace heat up, be incubated or lower the temperature control system, for monitoring
The thermocouple of glass fiber temperature and for monitoring the displacement sensing system of the length change of glass fiber.
In the case of process of the present invention it is preferred, determine length by the displacement sensing system of test device
The method of changing value Δ L includes: before hyperthermic treatment and after cooling process, record displacement sensing system respectively
The shift value Δ L0 that shows of sensor and Δ L1, length varying value Δ L=Δ L0-Δ L1.
When it will be understood by those skilled in the art that the aforementioned test device of use, in step (1),
The glass fiber length value L 1 carrying out heat treatment in glass fiber to be measured is in the burner hearth of the stove of test device
Carry out the glass fiber length value of heat treatment, be also furnace height.
In the case of process of the present invention it is preferred, before carrying out heat treatment, glass fiber to be measured is carried out
Annealing.
Preferably, the method for annealing includes: by glass fiber to be measured with the heating rate of 8-30 DEG C/min
It is warming up to annealing temperature, and is incubated 30-60min in annealing temperature, be then cooled to room temperature, described annealing
Temperature is that annealing point temperature is to annealing point temperature+5 DEG C.It is further preferred that glass fiber to be measured is incubated
The bale of cotton makes annealing treatment after wrapping up in, and heat-preservation cotton can be that resistance toization is cotton, is used for ensureing that glass fiber to be measured is in annealing
Process is heated evenly.Wherein, the method being cooled to room temperature can be with 3-20 DEG C/min's by glass fiber
Cooldown rate is cooled to room temperature or glass fiber is naturally cooling to room temperature.It is naturally cooling to room temperature be appreciated that
For cooling to room temperature with the furnace.Room temperature can be 15-25 DEG C.
In the case of process of the present invention it is preferred, glass is glass substrate for flat display, the most excellent
Elect TFT-LCD glass substrate, cover-plate glass or PDP glass, the most preferably TFT-LCD as
Glass substrate.
Embodiment
Hereinafter will be described the present invention by embodiment, but and be not so limited the present invention.With
In lower embodiment, if no special instructions, each material and reagent all can be by commercially available, and each method is
This area conventional method.
Test device is annealing point strain point instrument, including the resistance furnace for heating glass fiber, for resistance
Stove heat up, be incubated or lower the temperature control system, for monitoring the thermocouple of glass fiber temperature and for monitoring
The displacement sensing system of the length change of glass fiber, wherein, the furnace height of resistance furnace is 350mm.
The annealing point temperature of glass is measured according to standard ASTM C-336.
Embodiment 1-12
The present embodiment is for illustrating the method measuring also retract rate of the present invention.
(1), after being melted by TFT-LCD glass substrate to be measured, it is drawn into a diameter of D (mm) with wire drawing machine
Glass fiber, be L (mm) by glass fiber intercepted length, and the two ends of the glass fiber that intercepting is obtained
It is fired into the spherical shape of a diameter of 7mm, obtains glass fiber to be measured, and glass fiber to be measured being carried out at heat
The glass fiber length value L 1 of reason is 350mm；
(2) put in fine annealing stove, by glass fiber to be measured after glass fiber heat-preservation cotton to be measured being wrapped up
It is warming up to annealing point temperature with heating rate V1 (DEG C/min), and in annealing point temperature insulation T1 (min),
Then 25 DEG C are cooled to the furnace；
(3) glomerate glass fiber vertical hanging to be measured is fired at the two ends obtained after step (2) being annealed
In test device, lower end chain is connected to displacement sensing system, the biography of the displacement sensing system of record test device
The shift value Δ L0 that sensor shows；
(4) glass fiber to be measured is warming up to design temperature with heating rate V2 (DEG C/min), and in setting
Fixed temperature insulation T2 (min), then cools to 25 DEG C, and the displacement sensing of record test device with the furnace
The shift value Δ L1 that the sensor of system shows, obtains the length varying value Δ L of glass fiber before and after heat treatment,
Wherein, Δ L=Δ L0-Δ L1；
(5) shrinkage factor C of glass fiber to be measured, wherein, C=Δ L/L1 are calculated.
The diameter D (mm) of the glass fiber being drawn into, length L (mm) of glass fiber intercepted, setting
Temperature (DEG C), heating rate V1 (DEG C/min), annealing point temperature temperature retention time T1 (min), heat up
Speed V2 (DEG C/min), design temperature temperature retention time T2 (min), shrinkage factor (ppm) are shown in Table 1.
(6) accuracy analysis
According in patent application CN103454302A embodiment method and with phase in the embodiment of the present invention
The program answered carries out heat treatment, measures the finished glass shrinkage factor of TFT-LCD glass substrate.
Wherein, the thickness (mm) of finished glass, length (mm), design temperature (DEG C), shrinkage factor
(ppm) 2 it are shown in Table.
Table 1
Table 2
From Tables 1 and 2, with the existing essence being measured for testing sample with finished glass substrate
Really method is compared, the method measuring also retract rate of the present invention, and accuracy is high.
(7) Precision Analyze
According to step (1)-(5), the difference of the diameter D of the glass fiber that step (1) is drawn into is little
In 0.1mm, sample X1 is carried out 11 parallel analysis (the most corresponding 1#-11# of sample number into spectrum), if
Fixed temperature is that measurement result when 350 DEG C is as shown in table 3, and design temperature is measurement result when 600 DEG C
As shown in table 4.
Table 3
Table 4
From table 3 and table 4 data, the method measuring also retract rate of the present invention, discreteness is good,
Precision is high, and relative standard deviation (less than 5%) is the least, and repeatability is high, and credible result degree is high, complete
The demand of production all can be met.
The method measuring also retract rate of the present invention, by glass-pulling is become glass fiber, measures its heat
Length varying value before and after process determines shrinkage factor, solves in plate glass R&D process due to glass
In irregular shape little so that also retract rate cannot be measured to provide laboratory reference data, nothing with glass size
Method measures the problem of the performance of glass in development process, the measurement result of the method is accurate, repeatability is high,
Precision is high, credible result degree is high, glass properties research is had huge practical value, for flat board glass
The R&D process of glass provides the reference standard of a shrinkage determination.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited to above-mentioned reality
Execute the detail in mode, in the technology concept of the present invention, can be to the technical side of the present invention
Case carries out multiple simple variant, and these simple variant belong to protection scope of the present invention.
It is further to note that each the concrete technology described in above-mentioned detailed description of the invention is special
Levy, in the case of reconcilable, can be combined by any suitable means, in order to avoid need not
The repetition wanted, various possible compound modes are illustrated by the present invention the most separately.
Additionally, combination in any can also be carried out between the various different embodiment of the present invention, as long as its
Without prejudice to the thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. the method measuring also retract rate, it is characterised in that the method includes:
(1) prepare glass fiber to be measured, and determine the glass fiber length carrying out heat treatment in glass fiber to be measured
Value L1；
(2) glass fiber to be measured is carried out heat treatment, and determine the length change of glass fiber before and after heat treatment
Value Δ L；
(3) shrinkage factor C of glass fiber to be measured, wherein, C=Δ L/L1 are determined.
Method the most according to claim 1, it is characterised in that in step (1), glass to be measured
The preparation method of silk includes: glass-pulling is become glass fiber, after intercepting, is fired at the two ends of glass fiber
Glomeration；
Preferably, a diameter of 0.3-1mm of the glass fiber being drawn into, more preferably 0.5-0.8mm；
Preferably, a length of 300-550mm of the glass fiber of intercepting；
Preferably, spherical a diameter of 2-8mm that glass fiber two ends are fired.
Method the most according to claim 2, it is characterised in that in step (2), at described heat
The method of reason includes: glass fiber to be measured carries out hyperthermic treatment, isothermal holding and cooling successively and processes.
Method the most according to claim 3, it is characterised in that the method bag of described hyperthermic treatment
Include: glass fiber is warming up to design temperature with the heating rate of 8-30 DEG C/min, it is preferable that heating rate
For 10-20 DEG C/min.
Method the most according to claim 3, it is characterised in that the method bag of described isothermal holding
Include: glass fiber is incubated 0.01-10h at design temperature.
Method the most according to claim 3, it is characterised in that the method bag that described cooling processes
Include: glass fiber is cooled to room temperature with the cooldown rate of 3-20 DEG C/min or glass fiber is naturally cooling to room
Temperature.
Method the most according to claim 3, it is characterised in that in step (2), determine length
The method of changing value Δ L includes: two ends are fired glomerate glass fiber vertical hanging to be measured in test dress
Put, determine length varying value Δ L, wherein, described survey by the displacement sensing system of described test device
Electricity testing device includes the resistance furnace for heating glass fiber, the control heating up for resistance furnace, being incubated or lower the temperature
System, for monitor glass fiber temperature thermocouple and for monitor glass fiber length change displacement pass
Sensing system.
Method the most according to claim 7, it is characterised in that passed by the displacement of test device
Sensing system determines that the method for length varying value Δ L includes: before hyperthermic treatment and after cooling process, remember respectively
The shift value Δ L0 that shows of sensor of record displacement sensing system and Δ L1, length varying value
Δ L=Δ L0-Δ L1.
9. according to the method described in any one in claim 1-8, it is characterised in that carrying out heat
Before process, glass fiber to be measured is made annealing treatment；
Preferably, the method for described annealing includes: by glass fiber to be measured with the intensification of 8-30 DEG C/min
Ramp is to annealing temperature, and is incubated 30-60min in annealing temperature, is then cooled to room temperature, described
Annealing temperature is that annealing point temperature is to annealing point temperature+5 DEG C；It is further preferred that glass fiber to be measured is used
Make annealing treatment after heat-preservation cotton parcel.
10. according to the method described in any one in claim 1-9, it is characterised in that described glass
For glass substrate for flat display, preferably TFT-LCD glass substrate, cover-plate glass or PDP glass,
More preferably TFT-LCD glass substrate.
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| CN201610284112.3A CN105973927A (en) | 2016-05-03 | 2016-05-03 | Method for determining shrinkage rate of glass |
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| CN106950119A (en) * | 2017-04-18 | 2017-07-14 | 东旭科技集团有限公司 | Determine method and its application of glass flexibility |
| CN107228876A (en) * | 2017-06-26 | 2017-10-03 | 东旭科技集团有限公司 | A kind of method for evaluating glass substrate thermal contraction |
| CN108152324A (en) * | 2018-01-31 | 2018-06-12 | 彩虹显示器件股份有限公司 | A kind of method tested glass and be heat-shrinked |
| CN108426913A (en) * | 2018-06-19 | 2018-08-21 | 四川旭虹光电科技有限公司 | A kind of test method of also retract rate |
| CN108802088A (en) * | 2018-06-22 | 2018-11-13 | 北京冶科磁性材料有限公司 | The assay method and tooling of soft magnetism band Length after heat treatment constriction coefficient |
| CN109164131A (en) * | 2018-07-24 | 2019-01-08 | 彩虹显示器件股份有限公司 | A kind of electronic plane glass heat contraction measuring device and method |
| CN109187622A (en) * | 2018-07-24 | 2019-01-11 | 彩虹显示器件股份有限公司 | A kind of measurement method that high-resolution display is shunk with electronics glass heat |
| CN109507225A (en) * | 2018-10-29 | 2019-03-22 | 彩虹显示器件股份有限公司 | A kind of percent thermal shrinkage measuring device and measuring method of high strain-point electronic glass |
| WO2018232153A3 (en) * | 2017-06-14 | 2019-04-11 | Corning Incorporated | Method for controlling compaction |
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| CN106950119A (en) * | 2017-04-18 | 2017-07-14 | 东旭科技集团有限公司 | Determine method and its application of glass flexibility |
| WO2018232153A3 (en) * | 2017-06-14 | 2019-04-11 | Corning Incorporated | Method for controlling compaction |
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| US11827553B2 (en) | 2017-06-14 | 2023-11-28 | Corning Incorporated | Method for controlling compaction |
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