CN105842119A - Method for determining viscosity of glass - Google Patents
Method for determining viscosity of glass Download PDFInfo
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- CN105842119A CN105842119A CN201610158039.5A CN201610158039A CN105842119A CN 105842119 A CN105842119 A CN 105842119A CN 201610158039 A CN201610158039 A CN 201610158039A CN 105842119 A CN105842119 A CN 105842119A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
- G01N11/10—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material
- G01N11/14—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material by using rotary bodies, e.g. vane
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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Abstract
The invention relates to the field of determining thermodynamic properties of glass, and discloses a method for determining the viscosity of glass. The method comprises the steps: crushing to-be-detected glass into broken glass, and heating the broken glass from room temperature to the melting temperature Tm+/-100 DEG C to obtain molten glass; and then making the molten glass in a heat preservation process and a cooling process successively, and continuously determining the viscosity of the molten glass from the melting temperature Tm+/-100 DEG C in the cooling process to the temperature of not less than Tm-500 DEG C in the cooling process. The method for determining the viscosity of the glass has the advantages of simple operation, high efficiency, high accurate degree, high precision, good repeatability, and high reliability of results, and has an important guiding significance on control of a technology for successful production of qualified glass.
Description
Technical field
The present invention relates to glass heat mechanics performance determining field, measure glass viscosity in particular it relates to a kind of
Method.
Background technology
Glass viscosity (glass viseosity): measuring of glass melt viscosity.Representing with η, unit is
Pa Sec (Pa s).The founding of glass viscosity and glass, clarify, homogenizing, molding, heat treatment, processing
Close relationship is had etc. process.The structure of glass and melt can be studied by viscosity, and glass is formed
Kinetics etc..Additionally, the crystallize of glass is also relevant with viscosity with some mechanical performances.Determine glass viscosity
Factor be mainly chemical composition and the temperature of glass.The generally chemical composition of glass is different, its differences in viscosity
Not bigger.To Single component glass, the relation of its viscosity and component depends on the bonding force between zwitterion, joins
Figure place and the contiguity of glass structure network.To multicomponent glass, viscosity also with the kind of Network modifier
Class, content and ligancy are relevant.The glass certain to chemical constituent, the rising of its viscosity with temperature and drop
Low.
In actual applications, empirical equation (Fulcher formula) T=T of viscosity is often used0+B/(log10η
+ A), A, B, T in formula0It is constant.Characteristic temperature: the temperature corresponding to particular viscosity is referred to as spy
Levy temperature.Characteristic temperature, as glass molding, the substantially standard of processing, is widely used, often aborning
Characteristic temperature have following 6 kinds: 1. strain point: viscosity is 1013.6Temperature time Pa Sec (Pa s).
At this temperature, glass is little to produce VISCOUS FLOW.Less than this temperature, the stress in glass cannot
Eliminate.Strain point determines that the foundation of annealing lower limit temperature, with symbol TstRepresent.2. transition point: viscous
Degree is 1012.4Temperature during Pa s.Also known as glass transformation temperature, with symbol TgRepresent.As glass
The ceiling temperature of middle elimination stress, can eliminate major part internal stress at such a temperature in a few minutes.The softest
Change point: viscosity is 3 × 106-1.5×107Temperature during Pa s, with symbol TsRepresent.4. pour point:
Viscosity is 104Pa s, the temperature that glass launches under self gravitation effect, with symbol TfRepresent.Glass
Draw forming operation on the basis of this temperature.5. operating point: viscosity is 103Temperature during Pa s, with symbol
Number TwRepresent.Approximately correspond to mechanical-moulded temperature.Be suitable to range of viscosities during glass molding
(102-104Pa s) corresponding to temperature be referred to as operating temperature range, forming method has drawing, suppresses, blows
System, press-blow, casting, float glass process etc..Generally distinguish frit with the width of this temperature range
Length.The title slow-setting glass that temperature range is wide, narrow title short-nature glass or weighing are short.6. fusion temperature:
Can realize the temperature that glass biodissolution is discharged with clarification, bubble, viscosity is 10Pa s, with symbol TmRepresent.
The viscosity of glass is most important, so the viscosity that Accurate Determining is at each temperature seems for producing
Increasingly important.The method of existing mensuration viscosity has following several: falling ball method, bending method, plunging and
Fiber elongation method, but the step of aforementioned each assay method is complex, and accuracy has much room for improvement.
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 glues
The method of degree, the method is simple to operate, and efficiently, accuracy is high, and precision is high, reproducible, result
With a high credibility, the technology controlling and process successfully producing grade glass is had important directive significance.
To achieve these goals, the invention provides a kind of method measuring glass viscosity, the method bag
Include: being pulverized by glass to be measured is cullet, and from room temperature, cullet are heated to Tm± 100 DEG C to obtain glass
Glass liquid, then makes this vitreous humour be in insulating process and temperature-fall period successively, and from described temperature-fall period
Tm± 100 DEG C start to being not less than T in described temperature-fall periodsmThe temperature cutoff of-500 DEG C, continuously
Ground measures the viscosity of vitreous humour, described TmFor fusion temperature.
Preferably, cullet are heated to T from room temperaturemThe method of ± 100 DEG C includes: first by cullet from
Room temperature is warming up to softening point with the heating rate of 5-15 DEG C/min, then from softening point with 3-7 DEG C/min's
Heating rate is warming up to Tm±100℃；It is further preferred that first by cullet from room temperature with 8-12 DEG C/min
Heating rate be warming up to softening point, be then warming up to T from softening point with the heating rate of 4-6 DEG C/minm
±100℃。
Preferably, the condition of described insulating process includes: temperature is Tm±100℃；Time is 10-30min,
More preferably 15-25min.
Preferably, the method for described temperature-fall period includes: first with the rate of temperature fall of 1-5 DEG C/min from Tm
± 100 DEG C are cooled to be not less than TmThe temperature of-500 DEG C, after viscosimetric analysis terminates, then with 7-12 DEG C
The heating rate of/min is warming up to Tm-100 DEG C, finally naturally cool to room temperature.
It is further preferred that the method for described temperature-fall period includes: first with the rate of temperature fall of 1-3 DEG C/min
From Tm± 100 DEG C are cooled to be not less than TmThe temperature of-400 DEG C, after viscosimetric analysis terminates, then with 9-11
DEG C/heating rate of min is warming up to Tm-100 DEG C, finally naturally cool to room temperature.
Preferably, the particle diameter of cullet is not more than 10mm.
Preferably, the method for described pulverizing includes loading in valve bag glass to be measured crushing.
Preferably, 210-270g cullet are heated.
Preferably, rotation high-temperature viscosimeter is used to measure the viscosity of vitreous humour.
Preferably, on the basis of the weight of described glass to be measured, described glass to be measured contains 60-70 weight
The SiO of %2, the Al of 16-20 weight %2O3, 3-10 weight % CaO, 0-8 weight % BaO,
The SnO of ZnO, 0-0.3 weight % of SrO, 0-2 weight % of 2-8 weight %2With 2-12 weight %
B2O3；It is further preferred that described glass to be measured contains the SiO of 60-65 weight %2, 17-19 weight %
Al2O3, SrO, 0.2-1.2 of BaO, 2.1-4 weight % of CaO, 0.01-2 weight % of 7-8 weight %
The SnO of ZnO, 0.05-0.2 weight % of weight %2B with 9-11 weight %2O3。
Preferably, on the basis of the weight of described glass to be measured, described glass to be measured contains 60-70 weight
The SiO of %2, the Al of 16-20 weight %2O3, 3-10 weight % CaO, 1-8 weight % MgO,
The SnO of BaO, 0-0.3 weight % of SrO, 0-10 weight of 0-3 weight %2With 1-11 weight %
B2O3；It is further preferred that described glass to be measured contains the SiO of 61-63 weight %2, 18-19 weight %
Al2O3, SrO, 4-9 of MgO, 0.01-2 weight % of CaO, 2-5 weight % of 4-6 weight %
The SnO of BaO, 0.05-0.2 weight % of weight %2B with 2-8 weight %2O3。
The method of the mensuration glass viscosity of the present invention, simple to operate, efficiently, accuracy is high, and precision is high,
Reproducible, credible result degree is high, and the technology controlling and process successfully producing grade glass is had important finger
Lead meaning.
One according to the present invention preferred embodiment, uses the rotation prepared according to circumgyration principle high
Temperature viscometer measures vitreous humour viscosity, and it utilizes Fulcher formula (torsion angle or twisting resistance) to calculate
To viscosity, measurement range is 1-107Pa s, has higher accuracy, precision and credibility, right
Produce line production and there is certain directive significance, be conducive to produce to be smoothed 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 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.
End points and any value of scope disclosed in this article are not limited to this accurate scope or value, this
A little scopes or value should be understood to the value comprised close to these scopes or value.For numerical range, respectively
Between the endpoint value of individual scope, between the endpoint value of each scope and single point value, and individually point
Can obtain one or more new numerical range between value with combination with one another, these numerical rangies should be regarded
For the most specifically disclosing.
The invention provides a kind of method measuring glass viscosity, the method includes: pulverized by glass to be measured
For cullet, cullet are heated to T from room temperaturem± 100 DEG C (are preferably heated to Tm± 50 DEG C) to obtain
Obtain vitreous humour, then make this vitreous humour be in insulating process and temperature-fall period successively, and lowered the temperature from described
T in journeym± 100 DEG C of (preferably Tm± 50 DEG C) start to described temperature-fall period is not less than Tm-
The temperature cutoff of 500 DEG C, measures the viscosity of vitreous humour, described T continuouslymFor fusion temperature.
In the method for the present invention, in order to improve the accuracy of method, glass to be measured is being pulverized as cullet
Shi Buying introduces impurity, and glass the most to be measured should be the glass cleaned up, and crushing process the most should not introduce
Impurity.Under preferable case, the method for pulverizing includes loading in valve bag glass to be measured crushing；Enter
Preferably, the particle diameter of cullet is not more than 10mm to one step.
In the case of process of the present invention it is preferred, 210-270g cullet are heated.In order to carry
210-270g cullet can be put into the platinum rhodium earthenware cleaning up and drying by the accuracy of high method
Crucible heats.Wherein, glass to be measured can be stand-by by washes of absolute alcohol post-drying, platinum-rhodium crucible
First it is heated to boiling with the hydrochloric acid solution of 50%, after soaking a period of time (such as 20-30min), outwells hydrochloric acid
Solution, with stand-by after deionized water cleaning, drying.
In the method for the present invention, in order to improve accuracy and the precision of method, under preferable case, by broken
Glass is heated to T from room temperaturemThe method of ± 100 DEG C includes: first by cullet from room temperature with 5-15 DEG C/min
Heating rate be warming up to softening point, be then warming up to T from softening point with the heating rate of 3-7 DEG C/minm
±100℃；It is further preferred that first cullet are heated up with the heating rate of 8-12 DEG C/min from room temperature
To softening point, then it is warming up to T from softening point with the heating rate of 4-6 DEG C/minm±100℃.This
In bright, room temperature can be 15-30 DEG C, can be bound according to actual temp during practical operation.
In the method for the present invention, in order to improve accuracy and the precision of method, under preferable case, insulation
The condition of process includes: temperature is Tm±100℃；Time is 10-30min, more preferably
15-25min。
In the method for the present invention, in order to improve accuracy and the precision of method, under preferable case, cooling
The method of process includes: first with the rate of temperature fall of 1-5 DEG C/min from Tm± 100 DEG C are cooled to be not less than Tm
The temperature of-500 DEG C, after viscosimetric analysis terminates, then is warming up to T with the heating rate of 7-12 DEG C/minm
-100 DEG C, finally naturally cool to room temperature.It is further preferred that the method for temperature-fall period includes: first
With the rate of temperature fall of 1-3 DEG C/min from Tm± 100 DEG C are cooled to be not less than TmThe temperature of-400 DEG C, treats
After viscosimetric analysis terminates, then it is warming up to T with the heating rate of 9-11 DEG C/minm-100 DEG C, finally natural
It is cooled to room temperature.
In the method for the present invention, in order to improve accuracy and the precision of method, under preferable case, use
Rotate high-temperature viscosimeter and measure the viscosity of vitreous humour.
In the method for the present invention, may be used for the mensuration of the viscosity number of the glass of any composition, especially suitable
In the mensuration of viscosity number of the glass of consisting of, under preferable case, with the weight of described glass to be measured it is
Benchmark, described glass to be measured contains the SiO of 60-70 weight %2, the Al of 16-20 weight %2O3、3-10
ZnO, 0-0.3 of SrO, 0-2 weight % of BaO, 2-8 weight % of CaO, 0-8 weight % of weight %
The SnO of weight %2B with 2-12 weight %2O3；It is further preferred that described glass to be measured contains 60-65
The SiO of weight %2, the Al of 17-19 weight %2O3, CaO, 0.01-2 weight % of 7-8 weight %
The SnO of ZnO, 0.05-0.2 weight % of SrO, 0.2-1.2 weight % of BaO, 2.1-4 weight %2With
The B of 9-11 weight %2O3。
Preferably, on the basis of the weight of described glass to be measured, described glass to be measured contains 60-70 weight
The SiO of %2, the Al of 16-20 weight %2O3, 3-10 weight % CaO, 1-8 weight % MgO,
The SnO of BaO, 0-0.3 weight % of SrO, 0-10 weight of 0-3 weight %2With 1-11 weight %
B2O3；It is further preferred that described glass to be measured contains the SiO of 61-63 weight %2, 18-19 weight %
Al2O3, SrO, 4-9 of MgO, 0.01-2 weight % of CaO, 2-5 weight % of 4-6 weight %
The SnO of BaO, 0.05-0.2 weight % of weight %2B with 2-8 weight %2O3。
In the method for the present invention, for the glass of aforementioned particular make-up, when entering according to following heat treatment condition
When row processes, accuracy and the precision of method can be improved further: first by cullet from room temperature with 8-12
DEG C/heating rate of min is warming up to softening point, then from softening point with the heating rate liter of 4-6 DEG C/min
Warm to Tm± 100 DEG C, and at Tm15-25min it is incubated, then with the fall of 1-3 DEG C/min at ± 100 DEG C
Temperature speed is from Tm± 100 DEG C are cooled to be not less than TmThe temperature of-400 DEG C, after viscosimetric analysis terminates,
It is warming up to T again with the heating rate of 9-11 DEG C/minm-100 DEG C mention rotate high-temperature viscosimeter rotor from
Open vitreous humour, finally naturally cool to room temperature.
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.
The composition of glass sample to be measured: on the basis of the weight of glass to be measured, glass to be measured contains 62 weights
The SiO of amount %2, the Al of 17.7 weight %2O3, the CaO of 7 weight %, the BaO of 1 weight %, 2.1
The SrO of weight %, the ZnO of 0.5 weight %, the SnO of 0.2 weight %2B with 9.5 weight %2O3,
Its fusion temperature is 1550 DEG C, and softening point is 1000 DEG C.
Embodiment 1
The present embodiment is for the method that the mensuration glass viscosity of the present invention is described.
(1) flawless glass sample to be measured is cleaned up with dehydrated alcohol and deionized water successively,
Then 2h is dried at 120 DEG C.
(2) weigh the glass sample in 300g step (1) to load in valve bag, smash into hammer
Particle diameter is the cullet of 1-10mm, it is ensured that not contaminated samples.
(3) weigh the cullet obtained in 220g step (2), put into the platinum cleaning up and drying
In rhodium crucible, it is warming up to the softening point 1000 DEG C of cullet with the heating rate of 10 DEG C/min from 25 DEG C,
Then it is warming up to 1550 DEG C with the heating rate of 5 DEG C/min from 1000 DEG C, obtains vitreous humour, to glass
Liquid is put into the rotor rotating high-temperature viscosimeter, is incubated 20min at 1550 DEG C, then with 2 DEG C/min's
Rate of temperature fall is cooled to 1250 DEG C from 1550 DEG C, completes test process, then with 10 DEG C/min heating rate
Mention rotor after being warming up to 1450 DEG C and leave vitreous humour, and naturally cool to 25 DEG C.Lowered the temperature aforementioned
Cheng Zhong, starts during from temperature-fall period 1550 DEG C to measure vitreous humour continuously with rotating high-temperature viscosimeter
Viscosity, until stopping during in temperature-fall period 1250 DEG C measuring the viscous of vitreous humour with rotating high-temperature viscosimeter
Degree.The measured value of the viscosity of the glass sample to be measured under concrete different temperatures and this glass sample to be measured
The viscosity criterion value dispatched from the factory in reporting under the different temperatures of display is shown in Table 1.
Table 1
| Temperature | 1250℃ | 1300℃ | 1350℃ | 1400℃ | 1450℃ |
| Viscosity measurement (logPa s) | 3.390 | 3.031 | 2.702 | 2.399 | 2.124 |
| Viscosity criterion value (logPa s) | 3.392 | 3.032 | 2.704 | 2.398 | 2.126 |
| | standard value-measured value |/standard value | 0.059% | 0.033% | 0.074% | 0.042% | 0.094% |
As can be seen from Table 1, under the different temperatures that the method for the present invention measures, the viscosity number ratio of glass is calibrated
Really.It addition, the method for the present invention is applied in producing line, the control of each characteristic temperature point and product
Line design technology is coincide, and has higher credibility, can direct Instructing manufacture.
(4) Precision Analyze
Repeat step (1)-(3), carry out 11 times repeating test, the hyaloid to be measured under different temperatures
The measured value of the viscosity of product is shown in Table 2.
Table 2
As can be seen from Table 2, same glass sample to be measured is carried out 11 parallel analysis, the present invention's
The equal ＜ of relative standard deviation 1% of viscosity number under the different temperatures that method measures, the method showing the present invention,
Discreteness is little, and precision is high, with a high credibility, reproducible, can meet production and application completely.
Embodiment 2
According to the method for embodiment 1, except for the difference that, in step (3), from 25 DEG C with 8 DEG C/min's
Heating rate is warming up to the softening point 1000 DEG C of cullet, then with the heating rate of 6 DEG C/min from 1000
DEG C it is warming up to 1500 DEG C, obtains vitreous humour, in vitreous humour, put into the rotor rotating high-temperature viscosimeter,
1500 DEG C of insulation 25min, are then cooled to 1200 DEG C with the rate of temperature fall of 3 DEG C/min from 1500 DEG C, complete
Become test process, then mention rotor after being warming up to 1450 DEG C with 9 DEG C/min heating rate and leave vitreous humour,
And naturally cool to 25 DEG C.In aforementioned temperature-fall period, start during from temperature-fall period 1500 DEG C to use
Rotate high-temperature viscosimeter and measure the viscosity of vitreous humour continuously, until stopping during in temperature-fall period 1200 DEG C
By the viscosity rotating high-temperature viscosimeter mensuration vitreous humour.Glass sample to be measured under concrete different temperatures
Viscosity mark under the different temperatures of display in the report of dispatching from the factory of the measured value of viscosity and this glass sample to be measured
Quasi-value is shown in Table 3.
Table 3
| Temperature | 1250℃ | 1300℃ | 1350℃ | 1400℃ | 1450℃ |
| Viscosity measurement (logPa s) | 3.391 | 3.031 | 2.706 | 2.401 | 2.125 |
| Viscosity criterion value (logPa s) | 3.392 | 3.032 | 2.704 | 2.398 | 2.126 |
| | standard value-measured value |/standard value | 0.029% | 0.033% | 0.074% | 0.125% | 0.047% |
Embodiment 3
According to the method for embodiment 1, except for the difference that, in step (3), from 25 DEG C with 12 DEG C/min's
Heating rate is warming up to the softening point 1000 DEG C of cullet, then with the heating rate of 4 DEG C/min from 1000
DEG C it is warming up to 1600 DEG C, obtains vitreous humour, in vitreous humour, put into the rotor rotating high-temperature viscosimeter,
1600 DEG C of insulation 15min, are then cooled to 1300 DEG C with the rate of temperature fall of 1 DEG C/min from 1600 DEG C, complete
Become test process, then mention rotor after being warming up to 1450 DEG C with 11 DEG C/min heating rate and leave vitreous humour,
And naturally cool to 25 DEG C.In aforementioned temperature-fall period, start during from temperature-fall period 1600 DEG C to use
Rotate high-temperature viscosimeter and measure the viscosity of vitreous humour continuously, until stopping during in temperature-fall period 1300 DEG C
By the viscosity rotating high-temperature viscosimeter mensuration vitreous humour.Glass sample to be measured under concrete different temperatures
Viscosity mark under the different temperatures of display in the report of dispatching from the factory of the measured value of viscosity and this glass sample to be measured
Quasi-value is shown in Table 4.
Table 4
| Temperature | 1300℃ | 1350℃ | 1400℃ | 1450℃ |
| Viscosity measurement (logPa s) | 3.031 | 2.708 | 2.400 | 2.123 |
| Viscosity criterion value (logPa s) | 3.032 | 2.704 | 2.398 | 2.126 |
| | standard value-measured value |/standard value | 0.033% | 0.148% | 0.083% | 0.141% |
Embodiment 4
According to the method for embodiment 1, except for the difference that, in step (3), from 25 DEG C with 15 DEG C/min's
Heating rate is warming up to the softening point 1000 DEG C of cullet, then with the heating rate of 7 DEG C/min from 1000
DEG C it is warming up to 1550 DEG C, obtains vitreous humour, in vitreous humour, put into the rotor rotating high-temperature viscosimeter,
1550 DEG C of insulation 30min, are then cooled to 1250 DEG C with the rate of temperature fall of 4 DEG C/min from 1550 DEG C, complete
Become test process, then mention rotor after being warming up to 1450 DEG C with 12 DEG C/min heating rate and leave vitreous humour,
And naturally cool to 25 DEG C.In aforementioned temperature-fall period, start during from temperature-fall period 1550 DEG C to use
Rotate high-temperature viscosimeter and measure the viscosity of vitreous humour continuously, until stopping during in temperature-fall period 1250 DEG C
By the viscosity rotating high-temperature viscosimeter mensuration vitreous humour.Glass sample to be measured under concrete different temperatures
Viscosity mark under the different temperatures of display in the report of dispatching from the factory of the measured value of viscosity and this glass sample to be measured
Quasi-value is shown in Table 5.
Table 5
| Temperature | 1250℃ | 1300℃ | 1350℃ | 1400℃ | 1450℃ |
| Viscosity measurement (logPa s) | 3.361 | 3.005 | 2.721 | 2.427 | 2.146 |
| Viscosity criterion value (logPa s) | 3.392 | 3.032 | 2.704 | 2.398 | 2.126 |
| | standard value-measured value |/standard value | 0.914% | 0.891% | 0.629% | 1.209% | 0.941% |
The data of the data of embodiment 1-3 with embodiment 4 are compared and understands, measuring treating of specific composition
When surveying glass, by first cullet being warming up to softening point from room temperature with the heating rate of 8-12 DEG C/min,
Then it is warming up to T from softening point with the heating rate of 4-6 DEG C/minm± 100 DEG C, and at Tm±100℃
Lower insulation 15-25min, then with the rate of temperature fall of 1-3 DEG C/min from Tm± 100 DEG C are cooled to be not less than
TmThe temperature of-400 DEG C, after viscosimetric analysis terminates, then is warming up to the heating rate of 9-11 DEG C/min
Tm-100 DEG C of rotors mentioning rotation high-temperature viscosimeter leave vitreous humour, finally naturally cool to room temperature
Heat treatment mode, it is possible to put forward accuracy and the precision of full-bodied measured value further.
The method of the mensuration glass viscosity of the present invention, simple to operate, efficiently, accuracy is high, and precision is high,
Reproducible, credible result degree is high, and the technology controlling and process successfully producing grade glass is had important finger
Lead meaning.
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 glass viscosity, it is characterised in that the method includes: by glass to be measured
Pulverizing is cullet, and from room temperature, cullet are heated to Tm± 100 DEG C, to obtain vitreous humour, then make this
Vitreous humour is in insulating process and temperature-fall period, and the T from described temperature-fall period successivelymOpen for ± 100 DEG C
Begin to described temperature-fall period is not less than TmThe temperature cutoff of-500 DEG C, measures vitreous humour continuously
Viscosity, described TmFor fusion temperature.
Method the most according to claim 1, it is characterised in that cullet are heated to from room temperature
TmThe method of ± 100 DEG C includes: be first warming up to the heating rate of 5-15 DEG C/min from room temperature by cullet
Softening point, is then warming up to T from softening point with the heating rate of 3-7 DEG C/minm±100℃；
Preferably, first cullet are warming up to softening point from room temperature with the heating rate of 8-12 DEG C/min, so
After be warming up to T from softening point with the heating rate of 4-6 DEG C/minm±100℃。
Method the most according to claim 1 and 2, it is characterised in that the bar of described insulating process
Part includes: temperature is Tm±100℃；Time is 10-30min, preferably 15-25min.
4. according to the method described in any one in claim 1-3, it is characterised in that described cooling
The method of process includes: first with the rate of temperature fall of 1-5 DEG C/min from Tm± 100 DEG C are cooled to be not less than Tm
The temperature of-500 DEG C, after viscosimetric analysis terminates, then is warming up to T with the heating rate of 7-12 DEG C/minm
-100 DEG C, finally naturally cool to room temperature.
Method the most according to claim 4, it is characterised in that the method bag of described temperature-fall period
Include: first with the rate of temperature fall of 1-3 DEG C/min from Tm± 100 DEG C are cooled to be not less than TmThe temperature of-400 DEG C
Degree, after viscosimetric analysis terminates, then is warming up to T with the heating rate of 9-11 DEG C/minm-100 DEG C,
After naturally cool to room temperature.
6. according to the method described in any one in claim 1-5, it is characterised in that cullet
Particle diameter is not more than 10mm；
Preferably, the method for described pulverizing includes loading in valve bag glass to be measured crushing.
7. according to the method described in any one in claim 1-6, it is characterised in that by 210-270g
Cullet heat.
8. according to the method described in any one in claim 1-7, it is characterised in that use and rotate
High-temperature viscosimeter measures the viscosity of vitreous humour.
9. according to the method described in any one in claim 1-8, it is characterised in that treat with described
On the basis of surveying the weight of glass, described glass to be measured contains the SiO of 60-70 weight %2, 16-20 weight %
Al2O3, 3-10 weight % CaO, 0-8 weight % BaO, 2-8 weight % SrO, 0-2 weight
The SnO of ZnO, 0-0.3 weight % of amount %2B with 2-12 weight %2O3；
Preferably, described glass to be measured contains the SiO of 60-65 weight %2, the Al of 17-19 weight %2O3、
SrO, 0.2-1.2 weight % of BaO, 2.1-4 weight % of CaO, 0.01-2 weight % of 7-8 weight %
The SnO of ZnO, 0.05-0.2 weight %2B with 9-11 weight %2O3。
10. according to the method described in any one in claim 1-8, it is characterised in that treat with described
On the basis of surveying the weight of glass, described glass to be measured contains the SiO of 60-70 weight %2, 16-20 weight %
Al2O3, SrO, 0-10 of MgO, 0-3 weight % of CaO, 1-8 weight % of 3-10 weight %
The SnO of BaO, 0-0.3 weight % of weight2B with 1-11 weight %2O3；
Preferably, described glass to be measured contains the SiO of 61-63 weight %2, the Al of 18-19 weight %2O3、
SrO, 4-9 weight % of MgO, 0.01-2 weight % of CaO, 2-5 weight % of 4-6 weight %
The SnO of BaO, 0.05-0.2 weight %2B with 2-8 weight %2O3。
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