CN110455798A - The test method of devitrification of glass temperature - Google Patents
The test method of devitrification of glass temperature Download PDFInfo
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- CN110455798A CN110455798A CN201910765909.9A CN201910765909A CN110455798A CN 110455798 A CN110455798 A CN 110455798A CN 201910765909 A CN201910765909 A CN 201910765909A CN 110455798 A CN110455798 A CN 110455798A
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- 239000011521 glass Substances 0.000 title claims abstract description 116
- 238000004031 devitrification Methods 0.000 title claims abstract description 22
- 238000010998 test method Methods 0.000 title claims abstract description 19
- 238000002425 crystallisation Methods 0.000 claims abstract description 68
- 230000008025 crystallization Effects 0.000 claims abstract description 68
- 238000010438 heat treatment Methods 0.000 claims abstract description 45
- 239000002245 particle Substances 0.000 claims abstract description 37
- 238000005530 etching Methods 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000012360 testing method Methods 0.000 claims abstract description 25
- 239000007921 spray Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 238000010791 quenching Methods 0.000 claims description 5
- 230000000171 quenching effect Effects 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 7
- 238000001514 detection method Methods 0.000 abstract description 3
- 229910052573 porcelain Inorganic materials 0.000 description 14
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 description 8
- 238000001816 cooling Methods 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 229910052863 mullite Inorganic materials 0.000 description 5
- 238000000926 separation method Methods 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000006396 nitration reaction Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000001907 polarising light microscopy Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012956 testing procedure Methods 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- 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
- G01N1/32—Polishing; Etching
-
- 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
- G01N1/34—Purifying; Cleaning
-
- 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
-
- 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
- G01N21/84—Systems specially adapted for particular applications
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Glass Compositions (AREA)
Abstract
The present invention relates to glass properties detection fields, a kind of test method of devitrification of glass temperature are disclosed, this method comprises: glass particle is heat-treated by S1.；S2. glass particle after heat treatment is subjected to surface etching process；S3. the crystallization temperature of petrographic microscope test glass is utilized.The test method of devitrification of glass temperature provided by the invention, pattern can be eliminated and bring the influence that impurity tests crystallization temperature into the process, it is etched simultaneously by the surface to crystallization, it is apparent significantly to observe crystallization pattern, it avoids crystallization too small and generates and fail to judge, greatly improve the credibility of the test result of crystallization temperature.
Description
Technical field
The present invention relates to glass properties detection fields, and in particular to a kind of test method of devitrification of glass temperature.
Background technique
The high product of clarity is capable of providing good visual experience, thus can more attract terminal client, and glass substrate
As the key basic material of electronic display unit, the clarity shown with product is closely related.As terminal user is to electricity
The promotion of sub- product display effect experience requirements, the requirement for glass substrate quality are also higher and higher.
Devitrification of glass is one of most common defect in process of glass, is the weight of glass production producer concern always
Point.In glass production manufacturing process, crystallization temperature is needed as important one of physical function parameter according to its temperature range
Reasonable technological parameter is formulated, the generation of devitrification of glass is avoided.
Test method one of of the temperature gradient furnace method as crystallization temperature, can not only test crystallization upper and lower bound temperature,
The degree of crystallization and crystallization pattern under different temperatures can also be understood, provided to solve the devitrification defects source in product of production line
Important evidence, most of existing glass production producer carry out the test of crystallization temperature using temperature gradient furnace method.
However, temperature gradient furnace method is readily incorporated impurity in sample making course, impurity can induce crystallization again, easily cause erroneous judgement,
Influence the test result of crystallization temperature；In addition, being in stagnation temperature when the crystallization sample after heat treatment is analyzed under the microscope
The crystallization quantity of degree is few, crystallization form is smaller, is easy to fail to judge.And a kind of measurement accurate detection side obvious it would therefore be desirable to have observation
Method detects the crystallization temperature of glass.
Summary of the invention
The purpose of the invention is to overcome the above problem existing for existing technology, the present invention provides a kind of devitrification of glass temperature
The test method of degree, this method comprises:
S1. glass particle is heat-treated；
S2. glass particle after heat treatment is subjected to surface etching process；
S3. the crystallization temperature of petrographic microscope test glass is utilized.
Preferably, the glass particle is prepared by the following method,
(1) glass to be measured melted, clarified, obtain glass metal；
(2) glass metal is subjected to Water Quenching in water, and sieves and obtains the glass particle.
Preferably, the partial size of the glass particle is 1-7mm, more preferably 2-5mm.
Preferably, in heat treatment process, the soaking time of the glass particle is 2-48h, more preferably 12-24h.
Preferably, the heat treatment is to be heat-treated the multistage.
Preferably, the heat treatment is to be heat-treated the two-stage.
Preferably, the condition of the two-stage heat treatment includes:
First stage: 700-900 DEG C is risen to 8-12 DEG C/min heating rate；
Second stage: 1180-1330 DEG C is risen to 4-6 DEG C/min heating rate, and keeps the temperature 2-48h.
Preferably, when heat treatment temperature is the highest point temperature of heat treatment, the viscosity of the glass is 103.2-
104.0DPas, more preferably 103.5-103.8dPa·s。
Preferably, the etching with a thickness of 1-15 μm, more preferably 2-10 μm.
Preferably, the etching solution for etching is HF and H2SO4Mixed solution.
Preferably, in mixed solution, the concentration of the HF is 2-6 weight %, the H2SO4Concentration be 4-10 weight %.
Preferably, in mixed solution, the concentration of the HF is 3-5 weight %, the H2SO4Concentration be 6-8 weight %.
Preferably, the etching solution is sprayed to the glass particle surface and is etched.
Preferably, the time of the spray etching is 1-5min.
Through the above technical solutions, the influence for bringing impurity in sample making course into crystallization temperature test result can be eliminated,
And amplifies small crystallization, keeps crystallization preferably exposed in glass surface, avoid crystallization too small and generate and fail to judge, greatly improve
The credibility of the test result of crystallization temperature；Meanwhile in the case where not separation of glasses and porcelain boat, crystallization feelings can be directly observed
Condition is further simplified operation, saves process.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Specific embodiment
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
The present invention provides a kind of test methods of devitrification of glass temperature, this method comprises:
S1. glass particle is heat-treated；
S2. glass particle after heat treatment is subjected to surface etching process；
S3. the crystallization temperature of petrographic microscope test glass is utilized.
According to the present invention, by selecting glass particle to be tested, hand breaking step is saved, to avoid hand breaking
When impurity introduce caused by erroneous judgement, ensure that the credibility of crystallization temperature test result；By carrying out surface to glass particle
Etching process, so that crystallization quantity is few, crystallization form is smaller etc. is not easy observation or the incomplete crystallization of crystallization is exposed to glass
Glass sample surfaces avoid failing to judge for small crystallization, ensure that the accuracy of crystallization temperature test, and in not separation of glasses and porcelain
In the case where boat, crystallization situation directly can be obtained under the microscope in polarized light microscopy, to simplify operation, save process.
In the present invention, in order to further eliminate by the factors bring limitation such as mixability, shape of sample, preferably
Ground, the glass particle are prepared by the following method,
(1) glass to be measured melted, clarified, obtain glass metal；
(2) glass metal is subjected to Water Quenching in water, and sieves and obtains the glass particle.
By melting, clarification after can all obtain ontology uniformly, the glass metal without internal flaw, eliminate sample state band
The limitation come, further by Water Quenching, acquisition particle is uniform, and the sample of moderate in grain size eliminates hand breaking glass
Operation, and any impurity will not be mixed into glass particle.
Preferably, in above-mentioned steps (2), the water is preferably deionized water.
For the temperature of above-mentioned melting, there is no particular limitation, can be adjusted according to the composition of specific glass to be measured,
Such as can be 1350-1580 DEG C, it can also be carried out using split-level, such as can be for the heating of 8-12 DEG C/min speed
Rate rises to 1400-1480 DEG C, after continuation rises to 1480-1520 DEG C with the heating rate of 6-10 DEG C/min, with 6-10 DEG C/min's
The mode that heating rate rises to 1520-1550 DEG C carries out, during above-mentioned heating melting stage by stage, after the completion of each step-up temperature
It can also carry out heat preservation operation.
In the present invention, above-mentioned steps (2) specifically: glass metal is poured into deionized water, Water Quenching is carried out, obtains
Glass particle, then will be spare after glass particle drying screening.
In the present invention, in order to further ensure the accuracy of test result and confidence level, it is preferable that the glass particle
Partial size be 1-7mm；It is highly preferred that the partial size of the glass particle is 2-5mm.
In the present invention, in order to further ensure the accuracy of test result and confidence level, it is preferable that heat treatment process
In, the soaking time of the glass particle is 2-48h；It is highly preferred that in heat treatment process, the soaking time of the glass particle
For 12-24h.
In the present invention, it is preferred to which the heat treatment is to be heat-treated the multistage.
For multistage heat treatment, there is no particular limitation, can be two-stage, three stages or four and the above stage
Heat treatment, it is preferable that it is described heat treatment be the two-stage be heat-treated.
In the present invention, in order to further ensure the accuracy of test result and confidence level, it is preferable that the two-stage heat
The condition of processing includes:
First stage: 700-900 DEG C is risen to 8-12 DEG C/min heating rate；
Second stage: 1180-1330 DEG C is risen to 4-6 DEG C/min heating rate, and keeps the temperature 2-48h.
In the prior art, before heat treatment, it in order to estimate test sample heating highest point temperature, needs to carry out more
Secondary test, in the present invention, it is preferable that when heat treatment temperature be the highest point temperature of heat treatment, the viscosity of the glass is 103.2-
104.0DPas, more preferably 103.5-103.8dPa·s.By the way that highest point temperature setting will be heated in glass viscosity 103.5-
103.8When the corresponding temperature range of dPas, devitrification of glass ceiling temperature can accurately be found by a heat treatment test,
Compared with the existing technology, reduce unnecessary test link.
In heat treatment step of the invention, specifically, glass particle is put into mullite porcelain boat, in thermal gradient furnace into
Row heat treatment, charge weight are no more than 4/5ths of mullite porcelain boat boat wall.
In the present invention, it in order to make crystallization be fully exposed to glass sample surface, avoids failing to judge, it is preferable that the etching
With a thickness of 1-15 μm, it is highly preferred that the etching with a thickness of 2-10 μm.
In the present invention, it is preferred to which the etching solution for etching is HF and H2SO4Mixed solution.
In the present invention, in order to guarantee etch effect, it is preferable that in mixed solution, the concentration of the HF is 2-6 weight
Measure %, the H2SO4Concentration be 4-10 weight %；It is highly preferred that the concentration of the HF is 3-5 weight % in mixed solution,
The H2SO4Concentration be 6-8 weight %.
In the present invention, in order to further ensure etch effect, it is preferable that by etching solution spray to the glass
Grain surface is etched.
In the present invention, in order to further ensure etch effect, it is preferable that the time of the spray etching is 1-5min.
In the present invention, it will be etched by using the nitration mixture aqueous solution that etching solution is hydrofluoric acid and sulfuric acid and using spray mode
Liquid spray is to crystallization sample surfaces, and spray etching 1-5min, etched thickness is 2-10 μm, it can be achieved that the optimal small crystallization of amplification
Effect keeps crystallization preferably exposed in glass surface, so that crystallization pattern is clearer, is directly heat-treated compared to existing
Sample is observing crystallization start region and when crystallization disappearance region, crystallization quantity is few, crystallization form is smaller, it is not easy to observation or
Crystallization is not exclusively exposed to glass sample surface and causes failing to judge for small crystallization.
In the prior art, it usually needs it will be observed after crystallization sample and porcelain boat separation, and high-temperature heat treatment can make
Sample and porcelain boat are adhered to each other, and cause the process separated after cooling to destroy crystallization sample, or even will cause the residual of crystallization sample
Scarce or sample mixing.In crystallization temperature step using petrographic microscope test glass of the invention, by the crystallization after heat treatment
Sample carries out surface etching process so that crystallization is easier to observe, can not separation of glasses and porcelain boat, directly make under petrographic microscope
Crystallization situation can be clearly observed with reflection source.
For the glass ingredient in the present invention, there is no particular limitation, for example, with the total weight of the glass, glass can
With the SiO containing 58-62 weight %2, 10-18 weight % Al2O3, 10-16 weight % Na2O, the K of 3-7 weight %2O、4-8
The ZrO of MgO, 0-3 weight % of weight %2With the CaO of 0-0.4 weight % or the glass of other components content.
The object of the present invention is to provide a kind of test methods of devitrification of glass temperature, can eliminate and bring impurity in sample making course into
Influence to crystallization temperature test, while being etched by the surface to crystallization sample, apparent apparent observation analysis
Crystalline form looks avoid crystallization too small and generate and fail to judge, greatly improve the credibility of the test result of crystallization temperature.
The present invention will be described in detail by way of examples below.It is unless otherwise instructed, used in following embodiment
Each material can be commercially available, and unless otherwise instructed, method used is the conventional method of this field.
Embodiment 1
1) sample to be tested is a, and sample state is the special-shaped glass block without defect, and adding up to weight is 450g.
2) glass blocks is put into platinum-rhodium crucible, platinum-rhodium crucible is put into high temperature furnace using crucible tongs, high temperature furnace is with 10
DEG C/min rises to 1440 DEG C, 1h is kept the temperature, then rise to 1520 DEG C with 8 DEG C/min, keeps the temperature 1h, then rise to 1550 DEG C with 8 DEG C/min, protect
Warm 2h melts glass blocks, is clarified.
3) glass metal is poured into the container equipped with pure water, obtains glass particle.
4) it will be fitted into sample disc after glass particle drainage, be put into baking oven and dry, oven temperature is 105 DEG C, keeps the temperature 2h.
Sample disc is taken out, is sieved after glass particle is cooling, the glass particle that partial size is 2-5mm is chosen and is fitted into sample sack.
5) glass particle 45g is weighed, is uniformly fitted into mullite porcelain boat, charge weight is no more than the five of mullite porcelain boat boat wall
/ tetra-.
6) horizontal plane that mullite porcelain boat is slowly pushed into D- type pipe is hit exactly using thermal gradient furnace front plug, i.e. sample face thermoelectricity
Even lower end.
7) heat treatment temperature system is arranged: thermal gradient furnace rises to 800 DEG C with 10 DEG C/min, then rises to 1200 DEG C with 8 DEG C/min,
Heat preservation is for 24 hours.
8) porcelain boat is taken out after keeping the temperature, is cooled to room temperature.
9) use lower spray mode by the H of the HF of 2.6% weight and 5.7% weight2SO4Etching solution spray is mixed to sample
Surface, spray etching 1.8min, etched thickness are 5.7 μm.With pure water cleaning sample 3 times, then dries, is cooling.
10) under petrographic microscope, using reflection source, the sample crystallization situation from porcelain boat one end to the other end is high
Temperature area, critical-temperature is labeled as crystallization ceiling temperature to crystallization from scratch, and low-temperature region, crystallization is from the stagnation temperature having to nothing
Scale is denoted as lower temperature of crystallization.
11) calculation formula of the temperature and thermocouple location corresponding relationship fitted according to thermal gradient furnace software, in conjunction with porcelain boat
The crystallization upper and lower limit position of upper label calculates temperature value corresponding to porcelain boat mark, as the crystallization upper and lower limit of glass
Temperature.
Embodiment 2
Other than following steps, other conditions carry out same as Example 1ly, obtain the crystallization upper and lower limit temperature of glass
Degree.
1) sample to be tested is a, and sample state is the batch that various raw materials are uniformly mixed, and batch weight adds up to 550g.
2) batch is put into platinum-rhodium crucible, platinum-rhodium crucible is put into high temperature furnace using crucible tongs, high temperature furnace is with 10
DEG C/min rises to 1440 DEG C, 2h is kept the temperature, then rise to 1520 DEG C with 8 DEG C/min, keeps the temperature 2h, then rise to 1550 DEG C with 8 DEG C/min, protect
Warm 3h melts batch, is clarified.
7) heat treatment temperature system is arranged: thermal gradient furnace rises to 800 DEG C with 10 DEG C/min, then rises to 1200 DEG C with 8 DEG C/min,
Keep the temperature 18h.
9) use lower spray mode by the H of the HF of 3.2% weight and 6.8% weight2SO4Etching solution spray is mixed to sample
Surface, spray etching 1.2min, etched thickness are 4.5 μm.With pure water cleaning sample 3 times, then dries, is cooling.
Embodiment 3
Other than following steps, other conditions carry out same as Example 1ly, obtain the crystallization upper and lower limit temperature of glass
Degree.
1) sample to be tested is a, and sample state is the column finished glass without defect, and adding up to weight is 400g.
2) sheet finished glass is put into platinum-rhodium crucible, platinum-rhodium crucible is put into high temperature furnace using crucible tongs, high temperature
Furnace rises to 1440 DEG C with 10 DEG C/min, keeps the temperature 1h, then rise to 1520 DEG C with 8 DEG C/min, keeps the temperature 2h, then rise to 8 DEG C/min
1550 DEG C, 2h is kept the temperature, sheet finished glass is melted, is clarified.
7) heat treatment temperature system is arranged: thermal gradient furnace rises to 800 DEG C with 10 DEG C/min, then rises to 1200 DEG C with 8 DEG C/min,
Keep the temperature 23h.
9) use lower spray mode by the H of the HF of 3.8% weight and 6.2% weight2SO4Etching solution spray is mixed to sample
Surface, spray etching 2.1min, etched thickness are 8.6 μm.With pure water cleaning sample 3 times, then dries, is cooling.
Embodiment 4
Other than following steps, other conditions carry out same as Example 1ly, obtain the crystallization upper and lower limit temperature of glass
Degree.
1) sample to be tested is a, and sample state is the sheet finished glass without defect, and adding up to weight is 400g.
2) sheet finished glass is put into platinum-rhodium crucible, platinum-rhodium crucible is put into high temperature furnace using crucible tongs, high temperature
Furnace rises to 1440 DEG C with 10 DEG C/min, keeps the temperature 1h, then rise to 1520 DEG C with 8 DEG C/min, keeps the temperature 2h, then rise to 8 DEG C/min
1550 DEG C, 2h is kept the temperature, sheet finished glass is melted, is clarified.
Embodiment 5
The glass particle that screening partial size is 7mm is tested, and other conditions are same as Example 1.
According to above embodiments testing procedure, respectively the sample crystallization temperature of four kinds of different components is carried out repeating to try three times
It is averaged after testing, test result is shown in Table 1.
Table 1
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In skill of the invention
In art conception range, can with various simple variants of the technical solution of the present invention are made, including each technical characteristic with it is any its
Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, is belonged to
Protection scope of the present invention.
Claims (10)
1. a kind of test method of devitrification of glass temperature, which is characterized in that this method comprises:
S1. glass particle is heat-treated；
S2. glass particle after heat treatment is subjected to surface etching process；
S3. the crystallization temperature of petrographic microscope test glass is utilized.
2. the test method of devitrification of glass temperature according to claim 1, which is characterized in that the glass particle is through following
Method is made,
(1) glass to be measured melted, clarified, obtain glass metal；
(2) glass metal is subjected to Water Quenching in water, and sieves and obtains the glass particle.
3. the test method of devitrification of glass temperature according to claim 1 or 2, which is characterized in that the glass particle
Partial size is 1-7mm, preferably 2-5mm.
4. the test method of devitrification of glass temperature according to claim 1 or 2, which is characterized in that in heat treatment process, institute
The soaking time for stating glass particle is 2-48h, preferably 12-24h.
5. the test method of devitrification of glass temperature according to claim 4, which is characterized in that the heat treatment is the multistage
Heat treatment；
Preferably, the heat treatment is to be heat-treated the two-stage；
Preferably, the condition of the two-stage heat treatment includes:
First stage: 700-900 DEG C is risen to 8-12 DEG C/min heating rate；
Second stage: 1180-1330 DEG C is risen to 4-6 DEG C/min heating rate, and keeps the temperature 2-48h.
6. the test method of devitrification of glass temperature according to claim 1 or 2, which is characterized in that heat treatment temperature is heat
When the highest point temperature of processing, the viscosity of the glass is 103.2-104.0DPas, preferably 103.5-103.8dPa·s。
7. the test method of devitrification of glass temperature according to claim 1 or 2, which is characterized in that the thickness of the etching
It is 1-15 μm, preferably 2-10 μm.
8. the test method of devitrification of glass temperature according to claim 7, which is characterized in that the etching solution for etching is
HF and H2SO4Mixed solution.
9. the test method of devitrification of glass temperature according to claim 8, which is characterized in that in mixed solution, the HF
Concentration be 2-6 weight %, the H2SO4Concentration be 4-10 weight %；
Preferably, in mixed solution, the concentration of the HF is 3-5 weight %, the H2SO4Concentration be 6-8 weight %.
10. the test method of devitrification of glass temperature according to claim 8 or claim 9, which is characterized in that spray the etching solution
The glass particle surface is poured to be etched；
Preferably, the time of the spray etching is 1-5min.
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| CN201910765909.9A CN110455798A (en) | 2019-08-19 | 2019-08-19 | The test method of devitrification of glass temperature |
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| CN201910765909.9A CN110455798A (en) | 2019-08-19 | 2019-08-19 | The test method of devitrification of glass temperature |
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| CN114518382A (en) * | 2021-12-27 | 2022-05-20 | 清远南玻节能新材料有限公司 | Glass liquidus temperature detection method |
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