CN109179987A - A kind of preparation method of counter-bending glass ceramics - Google Patents
A kind of preparation method of counter-bending glass ceramics Download PDFInfo
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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
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
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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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Abstract
The invention discloses a kind of preparation methods of counter-bending glass ceramics, belong to technical field of function materials.The present invention according to parts by weight, by 20~30 parts of ethyl orthosilicates, 30~40 parts of organic acids, 30~40 parts of alcohol, 3~5 parts of methylpotassiums, 8~10 parts of butyl lithiums, 3~5 parts of phosphorus pentoxides, 3~5 parts of potassium permanganate, 3~5 parts of modified additives, 4~6 parts of isocyanates mixing, are then passed through the nitrogen containing triethyl aluminum, heating stirring reaction, obtains mixed powder；By mixed powder compression moulding, blank is obtained；By blank ice crystal steam steaming, modified blank is obtained；Modified blank is subjected to one section of high temperature crystallization, heats up step by step, carries out two sections of high temperature crystallization, cool down to get counter-bending glass ceramics.The counter-bending glass ceramics of technical solution of the present invention preparation has the characteristics that excellent mechanical property, has broad prospects in the development of the technology of preparing industry of functional material.
Description
Technical field
The invention discloses a kind of preparation methods of counter-bending glass ceramics, belong to technical field of function materials.
Background technique
Glass ceramics is the polycrystalline ceramic obtained by controlling vitreum crystallization.It has concurrently glass and ceramics it is excellent
Point is often better than metal and organic polymer material in terms of calorifics, chemistry, biology, optics and electric property.Glass pottery
Porcelain is a kind of material belonged between unorganic glass and ceramics, is that a kind of intensity is high, chemical stability is good, hardness is high and electrical isolation
The good new inorganic material of property.The structure and performance of glass ceramics and Tao Ci, glass are different, are a kind of special materials.By
In it internal crystallization construction carefully much than the crystal in many ceramic materials, and more uniform densification, almost without residual
Stomata, performance is also more far better than the ceramics of same material, thus is widely used in national defence sophisticated technology, industry, building
And the every field such as biological medicine, it has also become one of new material and the hot spot of new industrial research.It is similar to traditional ceramics material, glass
The toughness of glass ceramics is generally lower, what fracture often happened suddenly, and its intensity is also difficult to and the engineering ceramics such as aluminium oxide, silicon carbide
Material matches in excellence or beauty.Therefore, how to improve the mechanical property of glass ceramics is the key that the material is made to obtain broader applications.Composition and
Microstructure is two major influence factors of glass ceramics ingredient design.Principal component determines its glass forming ability and using feelings
The determinant of condition and internal nucleation or surface nucleation.It is micro- for having for the glass ceramics of mechanical and optical property
Structure is more crucial influence factor.But it is not independent variable, related with principal component and crystallite phase aggregation situation, different
Heat treating regime great influence can be also generated to structure.Microstructure is to determine the basis of material property, and glass ceramics is multiple
Condensation material has microstructure more better than glass ceramics, defect can be eliminated, to reach reinforcing glass Mechanical Property of Ceramics
Purpose.Generally acknowledged effective way is to carry out fibrous reinforcement to glass ceramics at present.Fiber reinforced ceramic matrix composites not only has
Conducive to the intensity for improving basis material, it is also beneficial to improve the CraCk extenslon reslstsnce of material, can effectively reduce material and disaster occurs
Property fracture a possibility that, the fatigue resistance of reinforcing material.Fiber/glass ceramic composite material is in mechanical property, high temperature resistant energy
All have the advantages that its uniqueness in terms of power and chemical stability, has broad application prospects in high-tech sector.
Therefore, when how to improve the counter-bending glass ceramics of tradition and preparing product using sol-gel method, gel is sintered
Easy contraction distortion in journey, leads to the disadvantage that product mechanical property is bad, to obtain the counter-bending glass ceramics of more high combination property,
It is that it is promoted and is applied to broader field, meets industrial production demand urgent problem to be solved.
Summary of the invention
The present invention solves the technical problem of: it is prepared for the counter-bending glass ceramics of tradition using sol-gel method
When product, gel easy contraction distortion during the sintering process leads to the problem that product mechanical property is bad, provides a kind of counter-bending
The preparation method of glass ceramics.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of counter-bending glass ceramics, specific preparation process is as follows:
(1) according to parts by weight, by 20~30 parts of ethyl orthosilicates, 30~40 parts of organic acids, 30~40 parts of alcohol, 3~5 parts of methyl
Potassium, 8~10 parts of butyl lithiums, 3~5 parts of phosphorus pentoxides, 3~5 parts of potassium permanganate, 3~5 parts of modified additives and 4~6 parts of isocyanides
Acid esters mixing, is then passed through the nitrogen containing triethyl aluminum, and heating stirring reaction obtains mixed powder；
(2) by mixed powder compression moulding, blank is obtained；
(3) by blank ice crystal steam steaming, modified blank is obtained；
(4) modified blank is subjected to one section of high temperature crystallization, heats up step by step, carry out two sections of high temperature crystallization, cools down to get counter-bending glass
Glass ceramics.
Step (1) organic acid is tartaric acid, oxalic acid, any one in malic acid or citric acid.
Step (1) alcohol is ethylene glycol, glycerine, any one in methanol or benzyl alcohol.
The volume content of triethyl aluminum is 3~5% in nitrogen containing triethyl aluminum described in step (1).
The preparation process of step (1) the modified additive are as follows: by (N- amidino groups) dodecylacrylamide and poly- second two
Alcohol phosphate 20:1~30:1 in mass ratio mixing, and be added 0.2~0.4 times of polyethylene glycol phosphate quality paracide and
Polyethylene glycol phosphate quality 0.06~0.08 times of ferrocene, constant temperature are stirred to react, and discharging is to get modified additive.
Step (1) isocyanates is toluene di-isocyanate(TDI), methyl diphenylene diisocyanate or trimethyl cyclohexane
Any one in diisocyanate.
Step (2) the compression moulding pressure is 200~220MPa.
Step (4) one section of high temperature crystallization condition are as follows: temperature is 750~850 DEG C, and crystallization time is 6~8h.
Step (4) heating rate step by step is 5~8 DEG C/min.
Step (4) two sections of high temperature crystallization conditions are；Temperature is 950~1050 DEG C, and crystallization time is 6~8h.
The beneficial effects of the present invention are:
(1) technical solution of the present invention, during the preparation process, firstly, by ethyl orthosilicate, organic acid, alcohol, methylpotassium, butyl lithium,
Phosphorus pentoxide, potassium permanganate, modified additive and isocyanates mixing, in the process, ester can occur for organic acid and alcohol
Change reaction, reaction, which generates water, to generate nano silica, nanometer respectively with ethyl orthosilicate, methylpotassium and butyl lithium reaction
Potassium oxide and nano oxidized lithium, simultaneously as the consumption of moisture is then passed through so that esterification is carried out to positive direction containing three
The nitrogen of aluminium ethide, triethyl aluminum can generate aluminium oxide with the reaction of moisture in system, secondly, isocyanates in system with
Water reaction, generates carbon dioxide and amine substance, the carbon dioxide of generation are conducive to the nano silica in system, nano oxygen
Change the dispersion of potassium and nano oxidized lithium, the amine substance of generation can adsorb the nano silica just generated, nano oxidized potassium
With nano oxidized lithium, nano silica, nano oxidized potassium and nano oxidized lithium nucleus continued growth are avoided, so that nano particle
Formation obtain good control, the uniformity of material can reach molecular level, the bulk density of the nano particle in system
It gets a promotion, so that the consistency of system is further promoted, effectively prevents blank contraction distortion during the sintering process, from
And the mechanical property of product is got a promotion, again, blank passes through ice crystal steam steaming, and ice crystal steam decomposes generation
Free state fluorine can generate mullite crystal whisker, the mullite crystal whisker dispersion of generation with silica, the oxidation reactive aluminum in system
In system, so that the mechanical property of product is further promoted；
(2) present invention is modified additive by adding, firstly, in ethyl orthosilicate, organic acid, alcohol, methylpotassium, butyl lithium, five
Two phosphorus are aoxidized, potassium permanganate is modified in additive and isocyanates mixed process, and modified additive can be self-assembly of vesica knot
Structure, the imitated vesicle structure can with carbon dioxide reaction, thus make in segment amidine group because make with like charges imitated vesicle structure into
The expansion of one step, simultaneously as expansion vesica is electrically charged, the nano particle that can be generated in absorption system, so that receiving in system
Rice grain obtains good dispersion, and during heating stirring, imitated vesicle structure is heated to release carbon dioxide, so that vesica is gradually
It shrinks, so that the densification degree of blank is promoted, blank contraction distortion during the sintering process is effectively prevented, so that the power of product
Performance is learned to get a promotion.
Specific embodiment
(N- amidino groups) dodecylacrylamide is mixed with polyethylene glycol phosphate 20:1~30:1 in mass ratio, and is added
Enter 0.2~0.4 times of polyethylene glycol phosphate quality paracide and 0.06~0.08 times of polyethylene glycol phosphate quality two
Luxuriant iron is then 35~40 DEG C in temperature, and under the conditions of revolving speed is 600~800r/min, constant temperature is stirred to react 3~5h, and discharging is
Additive must be modified；According to parts by weight, by 20~30 parts of ethyl orthosilicates, 30~40 parts of organic acids, 30~40 parts of alcohol, 3~5
Part methylpotassium, 8~10 parts of butyl lithiums, 3~5 parts of phosphorus pentoxides, 3~5 parts of potassium permanganate, 3~5 parts of modified additives and 4~6
Part isocyanates is placed in reaction kettle, under the conditions of revolving speed is 300~500r/min, 40~60min is stirred, then to anti-
It answers and is passed through the nitrogen containing triethyl aluminum in kettle, be 120~160 DEG C in temperature, revolving speed is 400~600r/min, and heating stirring is anti-
2~3h is answered, mixed powder is obtained；Mixed powder is poured into static pressure machine, under the conditions of pressure is 200~220MPa, compression moulding is obtained
Blank；By blank with ice crystal steam steaming 3~5 days, modified blank is obtained；Modified blank is placed in crystallization furnace, is in temperature
Under the conditions of 750~850 DEG C, after carrying out one section of 6~8h of high temperature crystallization, in-furnace temperature is risen to 5~8 DEG C/min heating rate
950~1050 DEG C, it is 950~1050 DEG C in temperature, after carrying out two sections of 6~8h of high temperature crystallization, is down to room temperature with furnace to get bending resistance
Bent glass ceramics.The organic acid is tartaric acid, oxalic acid, any one in malic acid or citric acid.The alcohol is ethylene glycol,
Any one in glycerine, methanol or benzyl alcohol.In the nitrogen containing triethyl aluminum the volume content of triethyl aluminum be 3~
5%.The isocyanates is toluene di-isocyanate(TDI), in methyl diphenylene diisocyanate or trimethylhexane diisocyanate
Any one.
Example 1
(N- amidino groups) dodecylacrylamide is mixed with polyethylene glycol phosphate 30:1 in mass ratio, and polyethylene glycol is added
The ferrocene of 0.08 times of the paracide and polyethylene glycol phosphate quality that 0.4 times of phosphate quality, then in temperature be 40 DEG C,
Under the conditions of revolving speed is 800r/min, constant temperature is stirred to react 5h, discharges up to modified additive；According to parts by weight, just by 30 parts
Silester, 40 parts of organic acids, 40 parts of alcohol, 5 parts of methylpotassiums, 10 parts of butyl lithiums, 5 parts of phosphorus pentoxides, 5 parts of potassium permanganate, 5 parts
Modified additive and 6 parts of isocyanates are placed in reaction kettle, under the conditions of revolving speed is 500r/min, are stirred 60min, then
It is passed through the nitrogen containing triethyl aluminum into reaction kettle, is 160 DEG C, revolving speed 600r/min in temperature, heating stirring reacts 3h, obtains
Mixed powder；Mixed powder is poured into static pressure machine, under the conditions of pressure is 220MPa, compression moulding obtains blank；By blank ice
Spar steam steaming 5 days, obtain modified blank；Modified blank is placed in crystallization furnace, under the conditions of temperature is 850 DEG C, carries out one
After Duan Gaowen crystallization 8h, in-furnace temperature is risen to 1050 DEG C with 8 DEG C/min heating rate, is 1050 DEG C in temperature, carries out two sections
After high temperature crystallization 8h, room temperature is down to get counter-bending glass ceramics with furnace.The organic acid is tartaric acid.The alcohol is second two
Alcohol.The volume content of triethyl aluminum is 5% in the nitrogen containing triethyl aluminum.The isocyanates is toluene di-isocyanate(TDI).
Example 2
(N- amidino groups) dodecylacrylamide is mixed with polyethylene glycol phosphate 30:1 in mass ratio, and polyethylene glycol is added
The ferrocene of 0.08 times of the paracide and polyethylene glycol phosphate quality that 0.4 times of phosphate quality, then in temperature be 40 DEG C,
Under the conditions of revolving speed is 800r/min, constant temperature is stirred to react 5h, discharges up to modified additive；According to parts by weight, just by 30 parts
Silester, 40 parts of alcohol, 5 parts of methylpotassiums, 10 parts of butyl lithiums, 5 parts of phosphorus pentoxides, 5 parts of potassium permanganate, 5 parts of modified additives
It is placed in reaction kettle with 6 parts of isocyanates, under the conditions of revolving speed is 500r/min, 60min is stirred, then into reaction kettle
It is passed through the nitrogen containing triethyl aluminum, is 160 DEG C, revolving speed 600r/min in temperature, heating stirring reacts 3h, obtains mixed powder；
Mixed powder is poured into static pressure machine, under the conditions of pressure is 220MPa, compression moulding obtains blank；By blank ice crystal steam
It is 5 days stifling, obtain modified blank；Modified blank is placed in crystallization furnace, under the conditions of temperature is 850 DEG C, carries out one section of high temperature crystalline substance
After changing 8h, in-furnace temperature is risen to 1050 DEG C with 8 DEG C/min heating rate, is 1050 DEG C in temperature, carries out two sections of high temperature crystallization
After 8h, room temperature is down to get counter-bending glass ceramics with furnace.The alcohol is ethylene glycol.Three in the nitrogen containing triethyl aluminum
The volume content of aluminium ethide is 5%.The isocyanates is toluene di-isocyanate(TDI).
Example 3
(N- amidino groups) dodecylacrylamide is mixed with polyethylene glycol phosphate 30:1 in mass ratio, and polyethylene glycol is added
The ferrocene of 0.08 times of the paracide and polyethylene glycol phosphate quality that 0.4 times of phosphate quality, then in temperature be 40 DEG C,
Under the conditions of revolving speed is 800r/min, constant temperature is stirred to react 5h, discharges up to modified additive；According to parts by weight, just by 30 parts
Silester, 40 parts of organic acids, 5 parts of methylpotassiums, 10 parts of butyl lithiums, 5 parts of phosphorus pentoxides, 5 parts of potassium permanganate, 5 parts of modifications add
Charging and 6 parts of isocyanates are placed in reaction kettle, under the conditions of revolving speed is 500r/min, 60min are stirred, then to reaction
It is passed through the nitrogen containing triethyl aluminum in kettle, is 160 DEG C, revolving speed 600r/min in temperature, heating stirring reacts 3h, obtains mixed powder
Body；Mixed powder is poured into static pressure machine, under the conditions of pressure is 220MPa, compression moulding obtains blank；Blank is steamed with ice crystal
Gas is 5 days stifling, obtains modified blank；Modified blank is placed in crystallization furnace, under the conditions of temperature is 850 DEG C, carries out one section of high temperature
After crystallization 8h, in-furnace temperature is risen to 1050 DEG C with 8 DEG C/min heating rate, is 1050 DEG C in temperature, carries out two sections of high temperature crystalline substances
After changing 8h, room temperature is down to get counter-bending glass ceramics with furnace.The organic acid is tartaric acid.The nitrogen containing triethyl aluminum
The volume content of triethyl aluminum is 5% in gas.The isocyanates is toluene di-isocyanate(TDI).
Example 4
(N- amidino groups) dodecylacrylamide is mixed with polyethylene glycol phosphate 30:1 in mass ratio, and polyethylene glycol is added
The ferrocene of 0.08 times of the paracide and polyethylene glycol phosphate quality that 0.4 times of phosphate quality, then in temperature be 40 DEG C,
Under the conditions of revolving speed is 800r/min, constant temperature is stirred to react 5h, discharges up to modified additive；According to parts by weight, just by 30 parts
Silester, 40 parts of organic acids, 40 parts of alcohol, 5 parts of methylpotassiums, 10 parts of butyl lithiums, 5 parts of phosphorus pentoxides, 5 parts of modified additives and
6 parts of isocyanates are placed in reaction kettle, under the conditions of revolving speed is 500r/min, are stirred 60min, are then led into reaction kettle
Enter the nitrogen containing triethyl aluminum, is 160 DEG C, revolving speed 600r/min in temperature, heating stirring reacts 3h, obtains mixed powder；It will
Mixed powder pours into static pressure machine, and under the conditions of pressure is 220MPa, compression moulding obtains blank；Blank is smoked with ice crystal steam
It steams 5 days, obtains modified blank；Modified blank is placed in crystallization furnace, under the conditions of temperature is 850 DEG C, carries out one section of high temperature crystallization
After 8h, in-furnace temperature is risen to 1050 DEG C with 8 DEG C/min heating rate, is 1050 DEG C in temperature, carries out two sections of high temperature crystallization 8h
Afterwards, room temperature is down to get counter-bending glass ceramics with furnace.The organic acid is tartaric acid.The alcohol is ethylene glycol.It is described to contain three
The volume content of triethyl aluminum is 5% in the nitrogen of aluminium ethide.The isocyanates is toluene di-isocyanate(TDI).
Example 5
According to parts by weight, by 30 parts of ethyl orthosilicates, 40 parts of organic acids, 40 parts of alcohol, 5 parts of methylpotassiums, 10 parts of butyl lithiums, 5 parts
Phosphorus pentoxide, 5 parts of potassium permanganate and 6 parts of isocyanates are placed in reaction kettle, and under the conditions of revolving speed is 500r/min, stirring is mixed
60min is closed, the nitrogen containing triethyl aluminum is then passed through into reaction kettle, is 160 DEG C, revolving speed 600r/min in temperature, heats
It is stirred to react 3h, obtains mixed powder；Mixed powder is poured into static pressure machine, under the conditions of pressure is 220MPa, compression moulding obtains base
Material；By blank with ice crystal steam steaming 5 days, modified blank is obtained；Modified blank is placed in crystallization furnace, in temperature be 850 DEG C
Under the conditions of, after carrying out one section of high temperature crystallization 8h, in-furnace temperature is risen to 1050 DEG C with 8 DEG C/min heating rate, is in temperature
1050 DEG C, after carrying out two sections of high temperature crystallization 8h, room temperature is down to get counter-bending glass ceramics with furnace.The organic acid is winestone
Acid.The alcohol is ethylene glycol.The volume content of triethyl aluminum is 5% in the nitrogen containing triethyl aluminum.The isocyanates is
Toluene di-isocyanate(TDI).
Example 6
(N- amidino groups) dodecylacrylamide is mixed with polyethylene glycol phosphate 30:1 in mass ratio, and polyethylene glycol is added
The ferrocene of 0.08 times of the paracide and polyethylene glycol phosphate quality that 0.4 times of phosphate quality, then in temperature be 40 DEG C,
Under the conditions of revolving speed is 800r/min, constant temperature is stirred to react 5h, discharges up to modified additive；According to parts by weight, just by 30 parts
Silester, 40 parts of organic acids, 40 parts of alcohol, 5 parts of methylpotassiums, 10 parts of butyl lithiums, 5 parts of phosphorus pentoxides, 5 parts of potassium permanganate, 5 parts
Modified additive is placed in reaction kettle, under the conditions of revolving speed is 500r/min, is stirred 60min, is then led into reaction kettle
Enter the nitrogen containing triethyl aluminum, is 160 DEG C, revolving speed 600r/min in temperature, heating stirring reacts 3h, obtains mixed powder；It will
Mixed powder pours into static pressure machine, and under the conditions of pressure is 220MPa, compression moulding obtains blank；Blank is smoked with ice crystal steam
It steams 5 days, obtains modified blank；Modified blank is placed in crystallization furnace, under the conditions of temperature is 850 DEG C, carries out one section of high temperature crystallization
After 8h, in-furnace temperature is risen to 1050 DEG C with 8 DEG C/min heating rate, is 1050 DEG C in temperature, carries out two sections of high temperature crystallization 8h
Afterwards, room temperature is down to get counter-bending glass ceramics with furnace.The organic acid is tartaric acid.The alcohol is ethylene glycol.It is described to contain three
The volume content of triethyl aluminum is 5% in the nitrogen of aluminium ethide.
Example 7
(N- amidino groups) dodecylacrylamide is mixed with polyethylene glycol phosphate 30:1 in mass ratio, and polyethylene glycol is added
The ferrocene of 0.08 times of the paracide and polyethylene glycol phosphate quality that 0.4 times of phosphate quality, then in temperature be 40 DEG C,
Under the conditions of revolving speed is 800r/min, constant temperature is stirred to react 5h, discharges up to modified additive；According to parts by weight, just by 30 parts
Silester, 40 parts of organic acids, 40 parts of alcohol, 5 parts of methylpotassiums, 10 parts of butyl lithiums, 5 parts of phosphorus pentoxides, 5 parts of potassium permanganate, 5 parts
Modified additive and 6 parts of isocyanates are placed in reaction kettle, under the conditions of revolving speed is 500r/min, are stirred 60min, then
It is passed through the nitrogen containing triethyl aluminum into reaction kettle, is 160 DEG C, revolving speed 600r/min in temperature, heating stirring reacts 3h, obtains
Mixed powder；Mixed powder is poured into static pressure machine, under the conditions of pressure is 220MPa, compression moulding obtains blank；Blank is placed in
In crystallization furnace, under the conditions of temperature is 850 DEG C, after carrying out one section of high temperature crystallization 8h, with 8 DEG C/min heating rate by in-furnace temperature
1050 DEG C are risen to, is 1050 DEG C in temperature, after carrying out two sections of high temperature crystallization 8h, is down to room temperature with furnace and makes pottery to get counter-bending glass
Porcelain.The organic acid is tartaric acid.The alcohol is ethylene glycol.The volume content of triethyl aluminum in the nitrogen containing triethyl aluminum
It is 5%.The isocyanates is toluene di-isocyanate(TDI).
Comparative example: the counter-bending glass ceramics of Foshan material production Co., Ltd production.
Example 1 to the resulting counter-bending glass ceramics of example 7 and comparative example product are subjected to performance detection, specific detection side
Method is as follows:
Bar shaped test specimen after taking each material die casting, it is enterprising in AGS-10kNG universal material test machine (Shimadzu company, Japan)
The measurement of row three-point bending strength, every group of 12 samples.Pressure head loading velocity is 0.5mm/min, span 20mm.
Specific testing result is as shown in table 1:
The 1 specific testing result of counter-bending glass ceramics of table
| Detection project | Bending strength/MPa |
| Example 1 | 348 |
| Example 2 | 345 |
| Example 3 | 341 |
| Example 4 | 337 |
| Example 5 | 314 |
| Example 6 | 326 |
| Example 7 | 301 |
| Comparative example | 294 |
By 1 testing result of table it is found that the counter-bending glass ceramics of technical solution of the present invention preparation has excellent mechanical property
Feature has broad prospects in the development of the technology of preparing industry of functional material.
Claims (10)
1. a kind of preparation method of counter-bending glass ceramics, it is characterised in that specific preparation process is as follows:
(1) according to parts by weight, by 20~30 parts of ethyl orthosilicates, 30~40 parts of organic acids, 30~40 parts of alcohol, 3~5 parts of methyl
Potassium, 8~10 parts of butyl lithiums, 3~5 parts of phosphorus pentoxides, 3~5 parts of potassium permanganate, 3~5 parts of modified additives and 4~6 parts of isocyanides
Acid esters mixing, is then passed through the nitrogen containing triethyl aluminum, and heating stirring reaction obtains mixed powder；
(2) by mixed powder compression moulding, blank is obtained；
(3) by blank ice crystal steam steaming, modified blank is obtained；
(4) modified blank is subjected to one section of high temperature crystallization, heats up step by step, carry out two sections of high temperature crystallization, cools down to get counter-bending glass
Glass ceramics.
2. a kind of preparation method of counter-bending glass ceramics according to claim 1, it is characterised in that: step (1) is described to be had
Machine acid is tartaric acid, oxalic acid, any one in malic acid or citric acid.
3. a kind of preparation method of counter-bending glass ceramics according to claim 1, it is characterised in that: step (1) described alcohol
For ethylene glycol, glycerine, any one in methanol or benzyl alcohol.
4. a kind of preparation method of counter-bending glass ceramics according to claim 1, it is characterised in that: step (1) is described to be contained
The volume content of triethyl aluminum is 3~5% in the nitrogen of triethyl aluminum.
5. a kind of preparation method of counter-bending glass ceramics according to claim 1, it is characterised in that: step (1) is described to be changed
Property additive preparation process are as follows: by (N- amidino groups) dodecylacrylamide and polyethylene glycol phosphate 20:1 in mass ratio~
30:1 mixing, and the paracide and polyethylene glycol phosphate quality 0.06 of 0.2~0.4 times of polyethylene glycol phosphate quality is added
~0.08 times of ferrocene, constant temperature are stirred to react, and discharging is to get modified additive.
6. a kind of preparation method of counter-bending glass ceramics according to claim 1, it is characterised in that: step (1) is described different
Cyanate is toluene di-isocyanate(TDI), any one in methyl diphenylene diisocyanate or trimethylhexane diisocyanate
Kind.
7. a kind of preparation method of counter-bending glass ceramics according to claim 1, it is characterised in that: step (2) described pressure
Briquetting pressure processed is 200~220MPa.
8. a kind of preparation method of counter-bending glass ceramics according to claim 1, it is characterised in that: step (4) described one
Duan Gaowen crystallization condition are as follows: temperature is 750~850 DEG C, and crystallization time is 6~8h.
9. a kind of preparation method of counter-bending glass ceramics according to claim 1, it is characterised in that: step (4) it is described by
Grade heating rate is 5~8 DEG C/min.
10. a kind of preparation method of counter-bending glass ceramics according to claim 1, it is characterised in that: step (4) described two
Duan Gaowen crystallization condition is；Temperature is 950~1050 DEG C, and crystallization time is 6~8h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110156328A (en) * | 2019-04-28 | 2019-08-23 | 江苏华鸥玻璃有限公司 | A kind of novel fire resistant glass tube and its processing technology |
-
2018
- 2018-09-20 CN CN201811098608.7A patent/CN109179987A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110156328A (en) * | 2019-04-28 | 2019-08-23 | 江苏华鸥玻璃有限公司 | A kind of novel fire resistant glass tube and its processing technology |
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