CN115159854A - Semitransparent SiO prepared based on low-carbon cold sintering process 2 Method for producing glass ceramics - Google Patents
Semitransparent SiO prepared based on low-carbon cold sintering process 2 Method for producing glass ceramics Download PDFInfo
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- CN115159854A CN115159854A CN202211045011.2A CN202211045011A CN115159854A CN 115159854 A CN115159854 A CN 115159854A CN 202211045011 A CN202211045011 A CN 202211045011A CN 115159854 A CN115159854 A CN 115159854A
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- 238000005245 sintering Methods 0.000 title claims abstract description 39
- 239000002241 glass-ceramic Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 33
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 12
- 239000012670 alkaline solution Substances 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 2
- 238000002834 transmittance Methods 0.000 abstract description 12
- 239000003513 alkali Substances 0.000 abstract description 11
- 239000007791 liquid phase Substances 0.000 abstract description 11
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 abstract description 9
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 9
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 72
- 239000000243 solution Substances 0.000 description 17
- 238000000280 densification Methods 0.000 description 10
- 239000000919 ceramic Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000009766 low-temperature sintering Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000006121 base glass Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- C03B19/066—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 for the production of quartz or fused silica articles
Abstract
The invention discloses a method for preparing semitransparent SiO based on a low-carbon cold sintering process 2 The method of glass ceramic adopts analytically pure silicic acid powder, takes 1-9 mol/L concentration, adds 5-50 wt% alkali solution and analytically pure H 2 SiO 3 Mixing the powders, grinding, pouring into a mold, applying 50-1000 MPa pressure, maintaining the pressure for 5 min, and mixing at 5-50 deg.C o Heating to 100-300 deg.c at C/min, and maintaining at 0.1-12 h. The invention adopts a cold sintering process, and adds a certain alkali solution as a liquid phase to carry out auxiliary sintering to obtain semitransparent SiO 2 The relative density of the glass ceramic can reach more than 95%, the light transmittance can reach more than 70%, and the glass ceramic has the advantages of simple and convenient preparation process, low energy consumption, short sintering time, safety and low pollution.
Description
Technical Field
The invention relates to a translucent SiO 2 A method for preparing glass ceramics, in particular to a method for preparing semitransparent SiO based on a cold sintering process 2 A method of glass-ceramic.
Background
SiO 2 Is an acidic oxide, is stable in chemical property, is insoluble in water, and can only react with a few substances such as hydrofluoric acid, concentrated ammonium hydroxide and the like. SiO 2 2 The product has the advantages of high hardness, acid and alkali corrosion resistance, friction resistance, good stability, good light transmission, good insulativity, high compatibility with human body and the like. At the same time, siO 2 The fertilizer is widely distributed in nature, has low price and is widely applied in many fields. SiO 2 2 The material is used for manufacturing glass materials, optical fibers, optical lenses and refractory materials, can also be used for manufacturing articles, living appliances and medical utensils, and is also an important material for scientific research. The most remarkable feature of glass ceramics is that they possess extremely fine-sized grains and extremely high degree of densification, in order to make SiO 2 Ceramics have a high degree of densification and certain mechanical properties, often requiring high sintering temperatures (above 1000 ℃) and/or extremely high pressures. However, high sintering temperatures result in high energy consumption, are neither economical nor environmentally friendly, and can cause a series of problems resulting from high sintering temperatures, such as excessive grain growth, failure to remove bubbles, and microcracking. In addition, high pressures place higher demands on the manufacturing process and equipment.
In order to improve and overcome the above problems, researchers at home and abroad have developed a series of low-temperature sintering techniques, such as Hydrothermal Reaction Sintering (HRS), hydrothermal Hot Pressing (HHP), reactive hydrothermal liquid phase densification (rllpd), and Cold Sintering Process (CSP). The specific densification mechanism of these processes is still under investigation, usually aided by an aqueous solution used as a reactant or transient liquid phase to achieve densification. One of their most notable features is that they all involve a series of dissolution precipitation changes and throughout the densification process. All of these methods are in phase with conventional sintering (excluding pressure-assisted sintering)The method is carried out at a lower temperature and a certain pressure. Among them, CSP has been used to develop hundreds of ceramic materials, but there is little research on optical materials such as transparent and translucent ceramics, glass ceramics and glass, especially on transparent/translucent SiO 2 The base glass ceramics have been studied yet.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the semitransparent SiO with low energy consumption and short sintering time 2 A glass ceramic sintering method.
In order to solve the technical problems, the invention adopts the following technical scheme: semitransparent SiO prepared based on low-carbon cold sintering process 2 A method of glass-ceramic comprising the steps of:
s1: using analytically pure H 2 SiO 3 Taking the powder, taking the powder with the concentration of 1-9 mol/L, adding alkaline solution accounting for 5-50 wt percent and analytically pure H 2 SiO 3 Mixing the powder materials;
s2: fully and uniformly grinding the mixed material in the step S1, and pouring the mixed material into a mold; applying pressure of 50-1000 MPa, maintaining for 5 min, and keeping the pressure for 5-50 min o Heating to 100-300 deg.C at C/min, and maintaining the temperature for 0.1-12 h to obtain translucent SiO 2 A glass-ceramic.
The method can sinter silicic acid powder into amorphous SiO at below 300 deg.C 2 Glass-ceramic, and the SiO obtained 2 The relative density of the glass ceramic sample can reach more than 95 percent, the light transmittance can reach 70 percent, and the preparation process is simple and convenient, low in energy consumption, short in sintering time, safe and low in pollution.
Compared with the prior art, the invention has at least the following advantages:
the invention adopts a low-temperature sintering mode, takes silicic acid powder as original powder, and adds KOH or NaOH/KOH alkali solution as auxiliary liquid phase for sintering, and the addition of KOH or NaOH/KOH alkali solution has great influence on the method of the invention as follows:
1) KOH or NaOH/KOH alkaline solution to SiO 2 The low-temperature sintering of the glass ceramic plays an important role, 300 o C below to complete high densificationThe sintering energy consumption is greatly reduced due to the low densification temperature (the relative density is more than 95%).
2) Cold sintering of SiO 2 The pressure applied in the process of the densification of the glass ceramic is 50-1000 MPa, the requirement can be met by a common manual press, and the method is simple to operate, safe and pollution-free.
3) Cold sintering of SiO 2 During the densification process of the glass ceramic, the excessive growth of the grain size can be avoided, and the fine glass ceramic with few microscopic defects and nano-scale grain size can be obtained.
4) Low temperature prepared high transparency SiO 2 The crystal structure of the glass ceramic is in an amorphous state, and other impurity phases are not detected.
5) Cold sintering of SiO 2 The glass ceramic has high transparency, and the visible light transmittance of the glass ceramic can reach more than 70%.
Drawings
FIG. 1 is SiO 2 Appearance of glass ceramic sample, wherein the thickness of the sample is 1.2 mm.
FIG. 2 is SiO 2 Transmittance of glass ceramic samples.
Detailed Description
The present invention is described in further detail below.
The NaOH/KOH alkaline solution in the present invention means a double alkaline solution of NaOH mixed with KOH.
The cold sintering technology adopted by the invention realizes the low-temperature sintering of the ceramic material in the true sense, and the sintering technology can be used at the extremely low temperature (less than or equal to 300℃) o C) The ceramic is densified within tens of minutes, and the sintering energy consumption is only 1/100 of that of the traditional sintering. The main mechanism of the sintering technology is that a proper amount of KOH solution or NaOH solution or double-alkali solution mixed by NaOH and KOH with a certain concentration is added into silicic acid powder, the silicic acid powder is fully contacted with the KOH solution or NaOH solution or double-alkali solution mixed by NaOH and KOH, a certain chemical reaction and partial wetting and dissolving of powder particles occur, then the solvent and the silicic acid powder are dehydrated and volatilized in the sintering and temperature rising process, highly saturated powder is precipitated and recrystallized, the supersaturation state of the whole powder and the double-alkali solution and silicon are mixedThe acid powder reacts to form SiO 2 The porcelain of the glass ceramic provides chemical driving force, and simultaneously applies uniaxial pressure to a sample in the sintering process, so that compact semitransparent SiO can be sintered at extremely low temperature in short time 2 A glass-ceramic.
The cold sintering technology of the invention prepares semitransparent SiO 2 The addition of KOH or NaOH/KOH alkaline solution with certain concentration to the glass ceramic has important influence on the sintering process. The results show that SiO is sintered in the cold sintering process by adding a proper amount of KOH solution or NaOH solution or mixed double-alkali solution of NaOH and KOH to the initial silicic acid powder 2 Glass ceramic sample 300 o The relative density below C can reach more than 95 percent, and the visible light transmittance can reach more than 70 percent.
Example 1: mixing 99.9% of commercial silicic acid powder with NaOH/KOH aqueous alkali with the concentration of 1 mol/L and the addition mass ratio of 50 wt% with the silicic acid powder; fully and uniformly grinding the mixed material in the step S1, and pouring the mixed material into a mold; applying 1000 MPa pressure, maintaining the pressure for 1 min, and starting to control the pressure to 5 o Heating to 100 ℃ at the rate of C/min, and preserving heat for 10 min to obtain SiO 2 Glass-ceramic, sample 1.
Examples 2-30 were prepared according to the same procedure as example 1, except for the formulation and process parameters, see in particular table 1:
TABLE 1 formulation and Process parameters for examples 1-30
| Selection of auxiliary liquid phase | The concentration of liquid phase/mol/l and the addition account for the ratio/wt% | Applied pressure/MPa | Dwell time/min | Rate of temperature rise- o C/min | Sintering temperature/. Degree.C | Holding time/h | Sample number | |
| Example 1 | NaOH/KOH | 1，50 | 1000 | 1 | 5 | 100 | 0.1 | Sample No. 1 |
| Example 2 | NaOH/KOH | 2，42 | 800 | 3 | 10 | 125 | 0.5 | Sample No. 2 |
| Example 3 | NaOH/KOH | 3，35 | 700 | 5 | 15 | 150 | 1 | Sample No. 3 |
| Example 4 | NaOH/ |
4，30 | 600 | 7 | 20 | 175 | 2 | Sample No. 4 |
| Example 5 | NaOH/KOH | 5，25 | 500 | 9 | 25 | 200 | 3 | Sample No. 5 |
| Example 6 | NaOH/ |
6，20 | 400 | 11 | 30 | 225 | 4 | Sample No. 6 |
| Example 7 | NaOH/KOH | 7，15 | 300 | 13 | 35 | 250 | 5 | Sample 7 |
| Example 8 | NaOH/ |
8，10 | 100 | 15 | 40 | 275 | 8 | Sample No. 8 |
| Example 9 | NaOH/KOH | 9，5 | 50 | 15 | 50 | 300 | 12 | Sample 9 |
| Example 10 | |
5，30 | 300 | 5 | 15 | 175 | 12 | |
| Example 11 | |
7，40 | 600 | 10 | 5 | 200 | 1 | Sample 11 |
For the double-alkali solution mixed by KOH or NaOH solution and KOH with different proportioning modes, the auxiliary liquid phase can achieve similar experimental effects by finely adjusting parameter indexes.
For the obtained SiO obtained in example 1 to example 30 2 And (3) carrying out performance test on the glass ceramic sample:
1.SiO 2 and (4) testing the density of the glass ceramic.
2.SiO 2 And (4) testing the optical performance of the glass ceramic.
To demonstrate the beneficial effects of the present invention, the inventors prepared SiO according to the present invention 2 The glass ceramics are tested and analyzed, and the main experimental data results are shown in table 2.
TABLE 2 different SiO 2 Relative Density and light transmittance of glass-ceramic samples
| Test specimen | Relative density/%) | Transmittance (a) |
| Sample No. 1 | 81.02 | 5.54 |
| Sample No. 2 | 78.02 | 23.71 |
| Sample No. 3 | 82.49 | 32.69 |
| Sample No. 4 | 95.82 | 73.47 |
| Sample No. 5 | 97.49 | 76.36 |
| Sample No. 6 | 93.12 | 65.88 |
| Sample 7 | 93.87 | 24.95 |
| Sample 8 | 89.72 | 20.47 |
| Sample No. 9 | 91.73 | 14.15 |
| Sample 10 | 97.37 | 74.88 |
| Sample 11 | 96.49 | 73.46 |
As is clear from tables 1 and 2, the sintering conditions (liquid phase, applied pressure, heating rate, sintering temperature, holding time, etc.) during the cold sintering process were applied to SiO 2 The degree of densification and transparency of the glass-ceramic have an important influence. The compactness of the composite material tends to be stable after reaching a certain value along with the increase of liquid phase concentration, pressure and temperature; the light transmittance is complicated by the sintering conditions, and the transparency is reduced due to the fact that the liquid phase concentration and the temperature are too high or too low, so that the light transmittance needs to be controlled within a proper liquid phase concentration and sintering temperature range.
FIG. 1 shows SiO prepared under the conditions of the present invention 2 The glass ceramic physical map can find that a part of samples have quite high light transmittance, and characters behind the samples can be clearly observed through the samples. FIG. 2 shows the light transmittances of samples 4, 5 and 6 in the visible light band (300-800 nm), and it can be seen that the visible light transmittance of sample 5 is 70% or more.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (1)
1. Semitransparent SiO prepared based on low-carbon cold sintering process 2 A method of making a glass-ceramic, comprising the steps of:
s1: using analytically pure H 2 SiO 3 Taking the powder, taking the powder with the concentration of 1-9 mol/L, adding alkaline solution accounting for 5-50 wt percent and analytically pure H 2 SiO 3 Mixing the powder materials;
s2: fully and uniformly grinding the mixed material in the step S1, and pouring the mixed material into a mold; applying pressure of 50-1000 MPa, maintaining the pressure for 1-15 min, and keeping the pressure for 5-50 min o Heating to 100-300 deg.C at C/min, and maintaining the temperature for 0.1-12 h to obtain translucent SiO 2 A glass-ceramic.
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| CN202211045011.2A CN115159854B (en) | 2022-08-30 | 2022-08-30 | Semitransparent SiO prepared based on low-carbon cold sintering process 2 Method for producing glass ceramics |
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| CN115159854B CN115159854B (en) | 2024-03-26 |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06279097A (en) * | 1993-03-26 | 1994-10-04 | Hitachi Ltd | Production of sintered glass ceramic and sintered glass ceramic |
| US20030209534A1 (en) * | 2002-05-09 | 2003-11-13 | Ferguson Lucian G. | Tapecast electro-conductive cermets for high temperature resistive heating systems |
| CN104402515A (en) * | 2014-11-19 | 2015-03-11 | 吉林大学 | Porous cordierite ceramic prepared by taking walnut hull powder as pore former |
| CN106830989A (en) * | 2017-01-11 | 2017-06-13 | 北京交通大学 | A kind of foam notes the method that shape low-temperature sintering of congealing into prepares iron tailings porous ceramics |
| US20190248707A1 (en) * | 2016-07-05 | 2019-08-15 | ETH Zürich | High performance ceramics from cold sintered nanoscale powders |
| CN111054929A (en) * | 2019-12-03 | 2020-04-24 | 南京汇聚新材料科技有限公司 | Low-temperature co-fired ceramic colloid and preparation method and application thereof |
| WO2020204952A1 (en) * | 2019-04-05 | 2020-10-08 | Halliburton Energy Services, Inc. | Cement composition and its relation with compressive strength |
| WO2022035552A1 (en) * | 2020-08-11 | 2022-02-17 | The Penn State Research Foundation | Process for cold sintering of calcium carbonate for precast construction materials |
-
2022
- 2022-08-30 CN CN202211045011.2A patent/CN115159854B/en active Active
Patent Citations (8)
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|---|---|---|---|---|
| JPH06279097A (en) * | 1993-03-26 | 1994-10-04 | Hitachi Ltd | Production of sintered glass ceramic and sintered glass ceramic |
| US20030209534A1 (en) * | 2002-05-09 | 2003-11-13 | Ferguson Lucian G. | Tapecast electro-conductive cermets for high temperature resistive heating systems |
| CN104402515A (en) * | 2014-11-19 | 2015-03-11 | 吉林大学 | Porous cordierite ceramic prepared by taking walnut hull powder as pore former |
| US20190248707A1 (en) * | 2016-07-05 | 2019-08-15 | ETH Zürich | High performance ceramics from cold sintered nanoscale powders |
| CN106830989A (en) * | 2017-01-11 | 2017-06-13 | 北京交通大学 | A kind of foam notes the method that shape low-temperature sintering of congealing into prepares iron tailings porous ceramics |
| WO2020204952A1 (en) * | 2019-04-05 | 2020-10-08 | Halliburton Energy Services, Inc. | Cement composition and its relation with compressive strength |
| CN111054929A (en) * | 2019-12-03 | 2020-04-24 | 南京汇聚新材料科技有限公司 | Low-temperature co-fired ceramic colloid and preparation method and application thereof |
| WO2022035552A1 (en) * | 2020-08-11 | 2022-02-17 | The Penn State Research Foundation | Process for cold sintering of calcium carbonate for precast construction materials |
Non-Patent Citations (1)
| Title |
|---|
| KANG, SL ET AL.: "Evolution from transparent SiO2 glass to ceramics enabled by cold sintering with a transient chemistry: H2SiO3", 《SCRIPTA MATERIALIA》, vol. 233 * |
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