CN110451806A - A kind of uniform crystallization control method of glass ceramics - Google Patents
A kind of uniform crystallization control method of glass ceramics Download PDFInfo
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- CN110451806A CN110451806A CN201910821009.1A CN201910821009A CN110451806A CN 110451806 A CN110451806 A CN 110451806A CN 201910821009 A CN201910821009 A CN 201910821009A CN 110451806 A CN110451806 A CN 110451806A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0009—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing silica as main constituent
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Abstract
The present invention relates to a kind of uniform crystallization control methods of glass ceramics, comprising: partial size≤100nm high-purity zirconia is added in glass ceramics raw material.The uniform crystallization control method of glass ceramics of the invention is controlled by using high-purity zirconia and to initial size, is easily dispersed in it in glass melt, is kept glass smelting uniform, so that uniformly crystallization promotes material overall performance；Simultaneously by controlling high-purity zirconia initial size, and then the size of material nucleus is controlled, makes its homogeneous nucleation in controlled range.
Description
Technical field
The present invention relates to glass ceramics technical fields, more particularly, to a kind of uniform crystallization control method of glass ceramics.
Background technique
Glass ceramics is also known as devitrified glass, is by high temperature melt, molding, heat treatment and manufactured a kind of crystal phase and glass
The composite material combined, with high mechanical strength, hot expansibility is adjustable, heat shock resistance, resistant to chemical etching, low-dielectric loss
Etc. superior functions.Glass ceramics is widely used in machine-building, optics, electronics and microelectronics, space flight and aviation, chemistry, industry, life
The fields such as object medicine and building.
The manufacturing process of glass ceramics is complicated, and technical requirements are high.Research glass ceramic material is just kept away not open to its crystallization mistake
The control of journey is studied.Good Crystallization method and process can promote the transformation efficiency of crystal effectively to reinforcing material
The whole uniformity of mechanical property and material, the method for most study is that heterogeneous nucleation process controls material crystallization at present, that is, is existed
Nucleating agent is added in parent glass.Common nucleating agent has precious metal colloid Nucleating Agent (gold, silver, platinum, copper etc.), such Nucleating Agent
It is expensive, and the coloring of part metals colloidal ion is serious, it is excessive to the Color influences that material is final to be difficult to control, it is not suitable for big
Mass industrial production.The influence for reducing colloidal ion color simultaneously for control cost, is studied in being suitable for quantitatively producing
Nucleating Agent be of great immediate significance.
Common nucleating agent has oxide Nucleating Agent, such as zirconium oxide in industrialized production, such Nucleating Agent is cheap, answers
With extensive, the variation of material color not will cause substantially, controllable method is more skilled and degree of controllability is high, and pole is suitable for modern chemical industry
Industry production, can replace precious metal colloid Nucleating Agent substantially.But due to the physical features and preparing craft of zirconium oxide itself,
It will cause parent glass and difficulty be melted, quality unevenness occur, it is uneven so as to cause crystallization, seriously affect the entirety of glass ceramics
Performance.
Summary of the invention
The object of the present invention is to provide a kind of uniform crystallization control methods of glass ceramics, solve glass in the prior art
Ceramic crystallization unevenness during the preparation process leads to the problem of glass ceramics overall performance difference.
The technical proposal for solving the technical problem of the invention is: a kind of uniform crystallization control method of glass ceramics,
It include: addition partial size≤100nm high-purity zirconia in glass ceramics raw material.
In the uniform crystallization control method of glass ceramics of the invention, the average grain diameter of high-purity zirconia is 40-60nm；
Purity >=99.9% of the high-purity zirconia.
In the uniform crystallization control method of glass ceramics of the invention, the raw material of glass ceramics includes following mass parts
The component of number ratio: 30-80 parts of SiO2, 20-45 parts of Li2CO3, 1-15 parts of alkali metal salt, 1-10 parts of Al (OH)3And 0-
10 parts of rare earth oxide, while the mass fraction for the high-purity zirconia being added is 1-10 parts.
In the uniform crystallization control method of glass ceramics of the invention, the high-purity zirconia, SiO2、Li2CO3, alkali gold
Belong to salt, Al (OH)3Mass parts ratio with rare earth oxide is: 1-5 parts of high-purity zirconia, 48-60 parts of SiO2, 28-32 parts
Li2CO3, 4.8-8 parts of alkali metal salt, 2-5 parts of Al (OH)3With 0-10 parts of rare earth oxide.
In the uniform crystallization control method of glass ceramics of the invention, the uniform crystallization control method of the glass ceramics
Further include: glass ceramics raw material and high-purity zirconia are settled to dry extremely hardening agglomeration after mixing, to the material after drying
It carries out boiling to be melted, the liquid material after boiling is melted is placed in molding in molding die and obtains sample blocks, then to sample blocks
It is treated with heat such that nucleation crystallization.
It is described that nucleation is treated with heat such that sample blocks in the uniform crystallization control method of glass ceramics of the invention
The process of crystallization specifically includes:
A1, nucleation stage: 5-15min is kept the temperature at 450-550 DEG C；
A2, crystallization stage: it is warming up to 600-700 DEG C, and keeps the temperature 15-60min at 600-700 DEG C；
A3, it is fully crystallized the stage: being warming up to 820-880 DEG C, and keep the temperature 10-30min at 820-880 DEG C.
In the uniform crystallization control method of glass ceramics of the invention, in A2 and A3 step, heating rate control exists
50-90℃/min。
In the uniform crystallization control method of glass ceramics of the invention, the material after described pair of drying carries out boiling and is melted
Process specifically include:
B1, first stage: material of the sedimentation after dry is put into 1200 DEG C -1250 DEG C of temperature of melted utensil；
B2, second stage: it is warming up to 1300-1400 DEG C, and keeps the temperature 2-4h at 1300-1400 DEG C；
B3, phase III: it is warming up to 1500-1600 DEG C, and keeps the temperature 2-6h at 1500-1600 DEG C；
B4,1300-1400 DEG C that second stage is cooled to from 1500-1600 DEG C of the phase III；Repeat second stage and
Phase III.
In the uniform crystallization control method of glass ceramics of the invention, in B2 step, heating rate is controlled in 10-20
℃/min；In B3 step, heating rate is controlled in 20-40 DEG C/min；In B4 step, second-order is cooled to from the phase III
The rate of temperature fall of section is controlled in 25-35 DEG C/min.
In the uniform crystallization control method of glass ceramics of the invention, using ball mill by glass ceramics raw material and high-purity
Zirconium oxide is uniformly mixed, and drying temperature when sedimentation is dry after mixing is controlled at 90-100 DEG C.
The uniform crystallization control method for implementing glass ceramics of the invention, has the advantages that glass of the invention
The uniform crystallization control method of ceramics is controlled by using high-purity zirconia and to initial size, it is made to be easily dispersed in glass
In melt, keep glass smelting uniform, so that uniformly crystallization promotes material overall performance；Simultaneously by the original grain of high-purity zirconia
Diameter is controlled, and then controls the size of material nucleus, makes its homogeneous nucleation in controlled range.
Specific embodiment
Below with reference to embodiment, the uniform crystallization control method of glass ceramics of the invention is described further:
The crystallization for being rich in zirconium oxygen is first precipitated from parent phase, and then induces nucleation for the nucleation of zirconium oxide, in LiO-
Al2O3-SiO2In glass ceramics system, the main induced synthesis principal crystalline phase β-quartz solid solution of zirconium oxide, secondary crystal phase is fine grain
Cube ZrO2Solid.The present invention provides a kind of uniform crystallization controlling party of glass ceramics using zirconium oxide as nucleating agent
Method.
The uniform crystallization control method of glass ceramics includes:
S1, high-purity zirconia, partial size integrally requirement≤100nm, average grain diameter 40-60nm, in above range are chosen
Interior particle size is preferably more dispersed, to form interlocking structure, the purity of high-purity zirconia preferably >=99.9%, more preferably >=
99.99%, without other auxiliary agents；
S2, the raw material of glass ceramics and high-purity zirconia are mixed by mass parts ratio, it is mixed to carry out ball milling using ball mill
It closes uniformly, drum's speed of rotation 300-500r/min, runing time 1-5h；
Wherein, the raw material of glass ceramics includes the component of following mass parts ratio: 30-80 parts of SiO2, 20-45 parts
Li2CO3, 1-15 parts of alkali metal salt, 1-10 parts of Al (OH)3With 0-10 parts of rare earth oxide, while be added high pure zirconia
The mass fraction of zirconium is 1-10 parts；Preferably, the high-purity zirconia, SiO2、Li2CO3, alkali metal salt, Al (OH)3And rare earth
The mass parts ratio of oxide is: 1-5 parts of high-purity zirconia, 48-60 parts of SiO2, 28-32 parts of Li2CO3, 4.8-8 parts
Alkali metal salt, 2-5 parts of Al (OH)3With 0-10 parts of rare earth oxide；Wherein, alkali metal salt uses chemical element Biao Zhong IA race
Salt corresponding with Group IIA metal oxide, it is preferable that alkali metal salt is in potassium carbonate, sodium sulphate, magnesium carbonate, strontium carbonate
It is at least one；Rare earth oxide is preferably selected from least one of cerium oxide, bismuth oxide, yttrium oxide, for improving the beauty of material
Sight degree, such as color and corresponding saturation degree；
S3, material after mixing is settled to drying, temperature when sedimentation is dry is 90-100 DEG C, settles drying time
For 5-10h, agglomerate until hardening；
S4, boil to the material after drying is melted, and process specifically includes:
S41, first stage: material of the sedimentation after dry is put into 1200 DEG C -1250 DEG C of temperature of melted utensil, i.e.,
Melted utensil is preheated to 1200 DEG C -1250 DEG C in advance, and wherein by material investment of the sedimentation after dry, melted utensil can be various
Heat-resisting utensil, including but unlimited crucible, molten cellar, smelting furnace etc.；
S42, second stage: it is warming up to 1300-1400 DEG C, and keeps the temperature 2-4h at 1300-1400 DEG C；Heating rate control
In 10-20 DEG C/min；
S43, phase III: it is warming up to 1500-1600 DEG C, and keeps the temperature 2-6h at 1500-1600 DEG C；Heating rate control
In 20-40 DEG C/min；
S44,1300-1400 DEG C that second stage is cooled to from 1500-1600 DEG C of the phase III, rate of temperature fall control exist
25-35 DEG C/min, it is preferably controlled in 30 DEG C/min；It repeats second stage and keeps the temperature 2-4h and phase III at 1300-1400 DEG C
It is warming up to 1500-1600 DEG C, and keeps the temperature 2-6h at 1500-1600 DEG C；
S5, the liquid material after being melted that will boil are placed in molding in molding die and obtain sample blocks；Wherein, molding die exists
30min or so need to be preheated before use under the conditions of 500 DEG C；
S6, sample blocks are treated with heat such that with nucleation crystallization, process specifically includes:
S61, nucleation stage: 5-15min is kept the temperature at 450-550 DEG C；Wherein, sample blocks after molding are not completely cooling
Before be heat-treated, about 450 DEG C of the temperature of sample blocks at this time or so；
S62, crystallization stage: it is warming up to 600-700 DEG C, heating rate is controlled in 50-90 DEG C/min, and at 600-700 DEG C
Lower heat preservation 15-60min；
S63, it is fully crystallized the stage: being warming up to 820-880 DEG C, heating rate is controlled in 50-90 DEG C/min, and in 820-
10-30min is kept the temperature at 880 DEG C.
It is handled by accurately multistage temperature, makes the crystalline substance for growing different-grain diameter size and length in certain homogeneity range
Core, so that perfect interlocking structure is formed, with performances such as the flexural strength of reinforcing glass ceramics and toughness.
It is described in detail below by specific embodiment.
Embodiment 1
By the SiO of 3kg2, 2kg Li2CO3, the magnesium carbonate of 0.1kg, 0.1kg Al (OH)3, 0.1kg zirconium oxide be added
Into ball mill, drum's speed of rotation 500r/min, runing time 4h；The dry 5h of sedimentation after mixing, 90 DEG C of drying temperature, greatly
Cause hardening agglomeration；Boiling is carried out later to be melted, and material of the sedimentation after dry is put into 1200 DEG C -1250 DEG C of temperature of melted device
In tool, it is warming up to 1300-1400 DEG C, heating rate control keeps the temperature 2h in 10 DEG C/min, and at 1300-1400 DEG C, after of continuing rising
For temperature to 1500-1600 DEG C, heating rate control keeps the temperature 2h in 20 DEG C/min, and at 1500-1600 DEG C；From 1500-1600 DEG C
Be cooled to 1300-1400 DEG C, rate of temperature fall control in 25 DEG C/min, repeat second stage keep the temperature at 1300-1400 DEG C 2h with
Phase III is warming up to 1500-1600 DEG C, and keeps the temperature 2h at 1500-1600 DEG C；；Liquid material after boiling is melted later
Molding in the molding die of 30min or so is preheated under the conditions of being placed in 500 DEG C obtains sample blocks；Sample blocks are heat-treated later
So that nucleation crystallization, keeps the temperature 5min at 450-550 DEG C；It is warming up to 600-700 DEG C, heating rate is controlled in 50 DEG C/min, and
15min is kept the temperature at 600-700 DEG C；It is warming up to 820-880 DEG C, heating rate is controlled in 50 DEG C/min, and at 820-880 DEG C
Keep the temperature 10min.Referring to table 1, difference leads to performance difference for the purity and partial size of zirconium oxide, using high-purity Nano-class zirconium oxide
(partial size integrally requirement≤100nm, average grain diameter 40-60nm), the various aspects of performance of glass ceramics is superior.
Table 1:
Embodiment 2
By the SiO of 4.8kg2, 2.8kg Li2CO3, the potassium carbonate of 0.48kg, 0.2kg Al (OH)3, 0.3kg oxidation
Cerium, 0.1kg zirconium oxide be added into ball mill, drum's speed of rotation 400r/min, runing time 1h；Sedimentation is dry after mixing
Dry 8h, 95 DEG C of drying temperature, substantially hardening agglomeration；Boiling is carried out later to be melted, and material of the sedimentation after dry is put into temperature
In 1200 DEG C -1250 DEG C of melted utensil, it is warming up to 1300-1400 DEG C, heating rate is controlled in 15 DEG C/min, and in 1300-
3h is kept the temperature at 1400 DEG C, is continuously heating to 1500-1600 DEG C, heating rate is controlled in 25 DEG C/min, and at 1500-1600 DEG C
Keep the temperature 4h；1300-1400 DEG C is cooled to from 1500-1600 DEG C, rate of temperature fall control repeats second stage and exist in 30 DEG C/min
3h is kept the temperature at 1300-1400 DEG C and the phase III is warming up to 1500-1600 DEG C, and keeps the temperature 4h at 1500-1600 DEG C；Later will
Liquid material after boiling is melted preheats molding in the molding die of 30min or so and obtains sample blocks under the conditions of being placed in 500 DEG C；It
Nucleation crystallization is treated with heat such that sample blocks afterwards, keeps the temperature 10min at 450-550 DEG C；It is warming up to 600-700 DEG C, heating
Rate control keeps the temperature 40min in 70 DEG C/min, and at 600-700 DEG C；It is warming up to 820-880 DEG C, heating rate is controlled 70
DEG C/min, and 20min is kept the temperature at 820-880 DEG C.Referring to table 2, difference causes performance poor to the purity and partial size of zirconium oxide
Not, using high-purity Nano-class zirconium oxide (partial size integrally requirement≤100nm, average grain diameter 40-60nm), each side of glass ceramics
Face performance is superior.
Table 2:
Embodiment 3
By the SiO of 6kg2, 3.2kg Li2CO3, the potassium carbonate of 0.8kg, 0.5kg Al (OH)3, 0.5kg cerium oxide,
The zirconium oxide of 0.5kg is added into ball mill, drum's speed of rotation 400r/min, runing time 3h；Drying is settled after mixing
8h, 95 DEG C of drying temperature, substantially hardening agglomeration；Boiling is carried out later to be melted, and material of the sedimentation after dry is put into temperature
In 1200 DEG C -1250 DEG C of melted utensil, it is warming up to 1300-1400 DEG C, heating rate is controlled in 15 DEG C/min, and in 1300-
3h is kept the temperature at 1400 DEG C, is continuously heating to 1500-1600 DEG C, heating rate is controlled in 25 DEG C/min, and at 1500-1600 DEG C
Keep the temperature 4h；1300-1400 DEG C is cooled to from 1500-1600 DEG C, rate of temperature fall control repeats second stage and exist in 30 DEG C/min
3h is kept the temperature at 1300-1400 DEG C and the phase III is warming up to 1500-1600 DEG C, and keeps the temperature 4h at 1500-1600 DEG C；Later will
Liquid material after boiling is melted preheats molding in the molding die of 30min or so and obtains sample blocks under the conditions of being placed in 500 DEG C；It
Nucleation crystallization is treated with heat such that sample blocks afterwards, keeps the temperature 10min at 450-550 DEG C；It is warming up to 600-700 DEG C, heating
Rate control keeps the temperature 40min in 70 DEG C/min, and at 600-700 DEG C；It is warming up to 820-880 DEG C, heating rate is controlled 70
DEG C/min, and 20min is kept the temperature at 820-880 DEG C.Referring to table 3, difference causes performance poor to the purity and partial size of zirconium oxide
Not, using high-purity Nano-class zirconium oxide (partial size integrally requirement≤100nm, average grain diameter 40-60nm), each side of glass ceramics
Face performance is superior.
Table 3:
Embodiment 4
By the SiO of 8kg2, 4.5kg Li2CO3, the potassium carbonate of 8kg, 1.5kg Al (OH)3, the bismuth oxide of 1kg, 1kg
Zirconium oxide is added into ball mill, drum's speed of rotation 500r/min, runing time 5h；Dry 10h is settled after mixing, it is dry
100 DEG C of temperature, substantially hardening agglomeration；Boiling is carried out later to be melted, will sedimentation it is dry after material put into 1200 DEG C of temperature-
In 1250 DEG C of melted utensil, it is warming up to 1300-1400 DEG C, heating rate is controlled in 20 DEG C/min, and at 1300-1400 DEG C
4h is kept the temperature, is continuously heating to 1500-1600 DEG C, heating rate control keeps the temperature 6h in 40 DEG C/min, and at 1500-1600 DEG C；
1300-1400 DEG C is cooled to from 1500-1600 DEG C, rate of temperature fall control repeats second stage in 1300-1400 in 35 DEG C/min
4h is kept the temperature at DEG C and the phase III is warming up to 1500-1600 DEG C, and keeps the temperature 6h at 1500-1600 DEG C；Boiling is melted later
Liquid material afterwards preheats molding in the molding die of 30min or so and obtains sample blocks under the conditions of being placed in 500 DEG C；Later to sample
Block is treated with heat such that nucleation crystallization, keeps the temperature 15min at 450-550 DEG C；It is warming up to 600-700 DEG C, heating rate control
60min is kept the temperature in 90 DEG C/min, and at 600-700 DEG C；It is warming up to 820-880 DEG C, heating rate is controlled in 90 DEG C/min, and
30min is kept the temperature at 820-880 DEG C.Referring to table 4, difference leads to performance difference for the purity and partial size of zirconium oxide, using height
Pure nanoscale zirconia (partial size integrally requirement≤100nm, average grain diameter 40-60nm), the various aspects of performance of glass ceramics is equal
It is superior.
Table 4:
It should be understood that for those of ordinary skills, it can be modified or changed according to the above description,
Within all these improvement or transformation should all belong to the protection domain of appended claims of the present invention.
Claims (10)
1. a kind of uniform crystallization control method of glass ceramics characterized by comprising partial size is added in glass ceramics raw material
The high-purity zirconia of≤100nm.
2. the uniform crystallization control method of glass ceramics according to claim 1, which is characterized in that high-purity zirconia is put down
Equal partial size is 40-60nm；Purity >=99.9% of the high-purity zirconia.
3. the uniform crystallization control method of glass ceramics according to claim 1, which is characterized in that the raw material of glass ceramics
It include the component of following mass parts ratio: 30-80 parts of SiO2, 20-45 parts of Li2CO3, 1-15 parts alkali metal salt, 1-10
The Al (OH) of part3With 0-10 parts of rare earth oxide, while the mass fraction of high-purity zirconia being added is 1-10 parts.
4. the uniform crystallization control method of glass ceramics according to claim 3, which is characterized in that the high pure zirconia
Zirconium, SiO2、Li2CO3, alkali metal salt, Al (OH)3Mass parts ratio with rare earth oxide is: 1-5 parts of high-purity zirconia,
48-60 parts of SiO2, 28-32 parts of Li2CO3, 4.8-8 parts of alkali metal salt, 2-5 parts of Al (OH)3With 0-10 parts of rare earth oxygen
Compound.
5. the uniform crystallization control method of glass ceramics according to claim 1, which is characterized in that the glass ceramics
Uniform crystallization control method further include: settle glass ceramics raw material and high-purity zirconia after mixing dry to hardening knot
Block carries out boiling to the material after drying and is melted, and the liquid material after boiling is melted is placed in molding in molding die and obtains sample
Then product block is treated with heat such that nucleation crystallization to sample blocks.
6. the uniform crystallization control method of glass ceramics according to claim 5, which is characterized in that it is described to sample blocks into
Row is heat-treated so that the process of nucleation crystallization specifically includes:
A1, nucleation stage: 5-15min is kept the temperature at 450-550 DEG C；
A2, crystallization stage: it is warming up to 600-700 DEG C, and keeps the temperature 15-60min at 600-700 DEG C；
A3, it is fully crystallized the stage: being warming up to 820-880 DEG C, and keep the temperature 10-30min at 820-880 DEG C.
7. the uniform crystallization control method of glass ceramics according to claim 6, which is characterized in that in A2 and A3 step
In, heating rate is controlled in 50-90 DEG C/min.
8. the uniform crystallization control method of glass ceramics according to claim 5, which is characterized in that after described pair of drying
Material carries out the melted process of boiling and specifically includes:
B1, first stage: material of the sedimentation after dry is put into 1200 DEG C -1250 DEG C of temperature of melted utensil；
B2, second stage: it is warming up to 1300-1400 DEG C, and keeps the temperature 2-4h at 1300-1400 DEG C；
B3, phase III: it is warming up to 1500-1600 DEG C, and keeps the temperature 2-6h at 1500-1600 DEG C；
B4,1300-1400 DEG C that second stage is cooled to from 1500-1600 DEG C of the phase III；Repeat second stage and third
Stage.
9. the uniform crystallization control method of glass ceramics according to claim 8, which is characterized in that in B2 step, rise
Warm rate control is in 10-20 DEG C/min；In B3 step, heating rate is controlled in 20-40 DEG C/min；In B4 step, from
The rate of temperature fall that three stages were cooled to second stage is controlled in 25-35 DEG C/min.
10. the uniform crystallization control method of glass ceramics according to claim 5, which is characterized in that utilize ball mill will
Glass ceramics raw material and high-purity zirconia are uniformly mixed, and drying temperature when sedimentation is dry after mixing is controlled in 90-100
℃。
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1383201A (en) * | 1971-02-19 | 1975-02-05 | Pilkington Brothers Ltd | Glass ceramic material |
| CN102730970A (en) * | 2012-06-27 | 2012-10-17 | 华南理工大学 | Red silicate glass and preparation method thereof |
| CN106277800A (en) * | 2016-08-26 | 2017-01-04 | 湖北戈碧迦光电科技股份有限公司 | Li2o Al2o3siO2the preparation method and application of system glass ceramics |
| CN106927819A (en) * | 2017-03-14 | 2017-07-07 | 南京云启金锐新材料有限公司 | Hot pressed sintering high-purity zirconia composite ceramics and preparation method thereof |
| CN107056071A (en) * | 2017-04-25 | 2017-08-18 | 福州大学 | ZrO2, HfO2The gear division devitrified glass being co-doped with |
| CN108840569A (en) * | 2018-06-29 | 2018-11-20 | 安徽新瑞重工股份有限公司 | A kind of novel nucleated glass and preparation method thereof |
-
2019
- 2019-08-30 CN CN201910821009.1A patent/CN110451806B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1383201A (en) * | 1971-02-19 | 1975-02-05 | Pilkington Brothers Ltd | Glass ceramic material |
| CN102730970A (en) * | 2012-06-27 | 2012-10-17 | 华南理工大学 | Red silicate glass and preparation method thereof |
| CN106277800A (en) * | 2016-08-26 | 2017-01-04 | 湖北戈碧迦光电科技股份有限公司 | Li2o Al2o3siO2the preparation method and application of system glass ceramics |
| CN106927819A (en) * | 2017-03-14 | 2017-07-07 | 南京云启金锐新材料有限公司 | Hot pressed sintering high-purity zirconia composite ceramics and preparation method thereof |
| CN107056071A (en) * | 2017-04-25 | 2017-08-18 | 福州大学 | ZrO2, HfO2The gear division devitrified glass being co-doped with |
| CN108840569A (en) * | 2018-06-29 | 2018-11-20 | 安徽新瑞重工股份有限公司 | A kind of novel nucleated glass and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112876214A (en) * | 2021-01-22 | 2021-06-01 | 北京科技大学 | Microcrystalline foamed ceramic and preparation method and application thereof |
| CN112876214B (en) * | 2021-01-22 | 2022-07-19 | 北京科技大学 | Microcrystalline foamed ceramic and preparation method and application thereof |
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| CN110451806B (en) | 2022-03-08 |
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