CN113860745B - Microcrystalline glass and preparation method thereof - Google Patents
Microcrystalline glass and preparation method thereof Download PDFInfo
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- CN113860745B CN113860745B CN202111247394.7A CN202111247394A CN113860745B CN 113860745 B CN113860745 B CN 113860745B CN 202111247394 A CN202111247394 A CN 202111247394A CN 113860745 B CN113860745 B CN 113860745B
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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
- C03C10/0018—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 SiO2, Al2O3 and monovalent metal oxide as main constituents
Abstract
The invention provides microcrystalline glass and a preparation method thereof, wherein the microcrystalline glass comprises the following components in molar mass fraction: siO 2 2 50.0～65.0％，Al 2 O 3 10.0～24.0％，Li 2 O 2.0～15.0％，Na 2 O 5.0～15.0％，MgO 2.0～12.0％，TiO 2 3.0～11.0％，P 5 O 2 1.0 to 8.0 percent; the preparation method of the microcrystalline glass comprises the following steps: the raw materials are mixed and melted according to the proportion to obtain non-crystallized precursor glass, and then the precursor glass is subjected to heat treatment to obtain the microcrystalline glass. The glass matrix can grow magnesium phosphate, magnesium lithium phosphate, amorphous phosphate and a composition thereof, and needle-rod rutile with the length-diameter ratio more than 5, and crystals or polymers with two morphologies form an inter-stacking or interlocking structure, so that the hardness and toughness of the glass are greatly improved.
Description
Technical Field
The invention belongs to the technical field of glass materials, and particularly relates to microcrystalline glass capable of growing rod-shaped rutile and a preparation method thereof.
Background
At present, smart phones, tablet computers and wearable devices have become necessities of daily life of people, and the lightening, thinning and large-size display panels have become inevitable trends in development, so that cover plate glass has to be developed towards the direction of thinness, light weight and high strength. The 5G era is a new communication technology revolution, has the characteristics of low energy consumption, full network coverage and the like, and basically meets the requirement that people have networks everywhere when checking time. The 5G smart phone perfectly combines the 5G communication technology and the artificial intelligence, the 5G communication technology greatly improves the communication capability of the smart phone, and the maturity of the 5G communication technology also means great innovation of the smart phone and develops from the intelligent type to the intelligent type. Meanwhile, the 5G communication technology puts forward higher requirements on the network transmission capacity of the mobile phone, and the metal material has obvious absorption on electromagnetic signals and is unfavorable for the transmission of 5G high-frequency signals, so that the traditional metal material must be abandoned on the back plate of the 5G smart phone. In contrast, the glass has small dielectric loss, has little influence on the transmission of electromagnetic signals, and has good applicability to 5G communication.
Aluminosilicate glass has the advantages of light weight, high strength, stable chemical property and the like, and the excellent performance makes the aluminosilicate glass popular in the field of electronic communication. The structure of the aluminosilicate glass influences the mechanical property of the aluminosilicate glass, the aluminosilicate glass and the aluminosilicate glass are closely related, and the research on the relationship between the aluminosilicate glass and the aluminosilicate glass has instructive significance for the preparation of large-size glass. The cover plate material has high requirements on strength and has high falling resistance. The glass has larger brittleness and crack resistance toughness lower than 0.8Mpa/m 1/2 The glass plate is easily broken along with the thinning of the glass plate. One of the most effective ways to improve the fracture toughness of the glass body is to microcrystallize it, i.e. to grow a uniform growth in the glass matrixDistributed crystalline particles, which are generally spherical particles or ellipsoidal particles having a certain aspect ratio. However, the toughening method has the following problems: firstly, the growth direction of crystals in the microcrystalline glass is difficult to control, and needle crystals with large length-diameter ratio are difficult to grow; secondly, sometimes a single needle crystal is grown in the microcrystalline glass, and the toughening effect of the matrix glass is not obvious. Therefore, how to grow the bulk crystal and the crystal with the length-diameter ratio larger than 5 in the microcrystalline glass and obviously improve the crack resistance and toughness of the microcrystalline glass is a difficult problem faced by the high-strength microcrystalline glass for the cover plate at present.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the microcrystalline glass, wherein a stack or interlocking structure formed by magnesium phosphate, magnesium lithium phosphate, amorphous phosphate, a composition or a polymer of the amorphous phosphate and needle-rod-shaped rutile with the length-diameter ratio more than 5 grows in the microcrystalline glass, so that the hardness and the toughness of the glass are greatly improved.
In order to solve the technical problem, the invention adopts the following technical scheme:
the microcrystalline glass is characterized by comprising the following components in molar mass fraction:
SiO 2 50.0～65.0％，
Al 2 O 3 10.0～24.0％，
Li 2 O 2.0～15.0％，
Na 2 O 5.0～15.0％，
MgO 2.0～12.0％，
TiO 2 3.0～11.0％，
P 5 O 2 1.0～8.0％。
furthermore, phosphate crystals and needle-rod-shaped rutile crystals grow in the glass ceramics.
Further, the rutile crystals in the glass-ceramic account for 5-15wt%, and the magnesium phosphate, the magnesium lithium phosphate, the amorphous phosphate and the composition thereof account for 15-40wt%.
Further, the needle-like rutile crystal has a length of not less than 100nm and a cross-sectional average diameter of not more than 20nm.
Further, [ Li ] 2 O+Na 2 O+MgO]/Al 2 O 3 The molar ratio is 1.1-2.5.
Further, [ Li 2 O+Na 2 O-Al2O3]/TiO 2 The molar ratio is-1 to 1.
Further, P 2 O 5 /[MgO+TiO 2 ]The molar ratio is 0.1-0.8.
Furthermore, the fracture toughness of the microcrystalline glass is more than or equal to 5Mpa/m 1/2 。
Furthermore, the Vickers hardness of the microcrystalline glass is more than or equal to 7GPa.
Another object of the present invention is to provide a method for preparing the above microcrystalline glass, which comprises the following steps: the raw materials are mixed and melted according to the proportion to obtain non-crystallized precursor glass, and then the precursor glass is subjected to heat treatment to obtain the microcrystalline glass, wherein the heat treatment method comprises the following steps: the precursor glass is kept at 750-900 ℃ for 2-4 h.
Among the above raw materials, siO 2 The oxide is an oxide related to glass forming, can be used for stabilizing the network structure of glass, but the excessive content can cause the excessive melting temperature and the difficulty in the melting process, and is not beneficial to environmental protection and energy conservation.
Al 2 O 3 The network can also be stabilized and also provide improved mechanical properties and chemical durability; but Al 2 O 3 Too high a content results in a glass sample that is too viscous to melt.
Li 2 O is used to lower the melting temperature of the glass while providing a lithium source during chemical strengthening; however, li 2 Too high an amount of O can destabilize the glass melt and affect the physical properties of the article.
Na 2 O is used to lower the melting temperature of the glass while providing a source of sodium during chemical strengthening. But Na 2 Too high an amount of O may deteriorate the stability of the glass melt and affect the physical properties of the article.
MgO is used to lower the melting temperature of the glass and at the same time the system stability is greatly improved compared to the addition of alkali metal oxides.
P 2 O 5 For lowering the melting temperature of the glass and promoting the phase separation of the glass in the early stage. But P is 2 O 5 Too high a content deteriorates glass stability.
TiO 2 The crystal nucleus agent can promote the crystallization of the glass, avoid the surface crystallization of the glass and provide sufficient oxide source for the growth of rutile crystal.
After a plurality of creative efforts of the inventor, the molar mass fractions of the components are obtained finally, as mentioned above, and the microcrystalline glass with needle-rod-shaped rutile can be manufactured by adopting the formula and the heat treatment method, and the nano crystals of the microcrystalline glass are uniformly distributed in a glass sample. The invention is in SiO 2 -Al 2 O 3 -MgO-TiO 2 Adding P into the system 2 O 5 Following P 2 O 5 Increase in content of PO in glass 4 3+ The number of ions increases at P 5+ Under the action of high ionic field strength of 2- 、Mg 2+ And Li + The plasma preferentially migrates to the phosphorus-rich region, forming spontaneous phase separation, forming magnesium phosphate, magnesium lithium phosphate, amorphous phosphate, and combinations or polymers thereof, resulting in a reduction of cations in the glass matrix and titanium-rich region, and acicular rutile with a high aspect ratio grows from the titanium-rich region in the sample. The microcrystalline glass prepared by the invention is characterized in that phosphate crystals and rutile crystals are dispersed in a silicon-aluminum-rich glass matrix, the phosphate crystals form bulk particles, the rutile crystals form needle-rod-shaped nanowires, and the silicon-aluminum-rich phase forms a glass matrix.
Compared with the prior art, the invention has the beneficial effects that: the invention adjusts the formula and the heat treatment method, namely, P with larger ion field intensity is introduced into the formula 5+ For competing for Ti 4+ Ambient cations, eventually Ti 4+ Needle-like rutile crystals are separated out and have higher length-diameter ratio, wherein the length-diameter ratio of the rutile crystals is more than 5, the length-diameter ratio of partial crystals can reach more than 10, and simultaneously, the conglobate magnesium phosphate, magnesium lithium phosphate and amorphous phosphorus are formedThe acid salt and the composition or the polymer thereof, and the bulk crystal and the needle-rod crystal are stacked mutually, so that the hardness and the toughness of the glass ceramics are greatly improved.
Drawings
FIG. 1 is an XRD pattern of a sample of precursor glass made in accordance with example 2 of the present invention at various heat treatment temperatures;
FIG. 2 is an SEM photograph of a glass sample obtained in example 2 of the present invention;
FIG. 3 is a TEM element distribution diagram of a glass sample in example 2 of the present invention;
FIG. 4 is a graph showing the hardness of the precursor glass obtained in example 2 of the present invention as a function of the heat treatment temperature.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
The screening method of the salt-tolerant rhizosphere growth-promoting bacteria comprises the following steps:
example 1:
the following components are taken in mol%: siO 2 2 54.5％，Al 2 O 3 11.5％，Li 2 O 5.0％，Na 2 O
11.0％，MgO 8.0％，TiO 2 5.0％，P 2 O 5 5.0％。
Weighing and mixing the raw materials containing the oxides in proportion, melting at 1550 ℃ to obtain non-crystallized precursor glass, and putting the precursor glass into a crystallization furnace for heat treatment to ensure thatThe rutile crystal grows, the heat treatment condition is that the temperature is kept for 4 hours at 850 ℃, thereby obtaining the microcrystalline glass with the rutile crystal phase with high length-diameter ratio and the phosphate crystal in a cluster shape, the two crystals are mutually stacked, the Vickers hardness reaches 7.28GPa, the fracture toughness reaches 5.1Mpa/m 1/2 。
Example 2:
the following components are taken in mol%: siO 2 2 56.5％，Al 2 O 3 11.5％,Li 2 O 5.0％,Na 2 O 11.0％，MgO 8.0％，TiO 2 4.0％，P 2 O 5 4.0％。
Weighing and mixing the raw materials containing the oxides in proportion, melting at 1600 ℃ to obtain non-crystallized precursor glass, then putting the precursor glass into a crystallization furnace for heat treatment to enable rutile crystals to grow, wherein the heat treatment condition is that the temperature is kept at 850 ℃ for 2 hours, so that the microcrystalline glass with the rutile crystal phase with high length-diameter ratio and the phosphate crystal in a bulk shape is obtained, the two crystals are mutually stacked, the Vickers hardness reaches 7.18GPa, and the fracture toughness reaches 5.32Mpa/m 1/2 。
Example 3:
taking the following components in mol percent: siO 2 2 50％，Al 2 O 3 13％，Li 2 O 2.0％，Na 2 O 12.0％，MgO 12.0％，TiO 2 3.0％，P 2 O 5 8.0％。
The raw materials containing the oxides are weighed and mixed in proportion, and then are melted at 1600 ℃ to obtain non-crystallized precursor glass, then the precursor glass is put into a crystallization furnace for heat treatment to enable rutile crystals to grow, the heat treatment condition is that the temperature is kept at 900 ℃ for 2 hours, so that the microcrystalline glass with rutile crystal phase with high length-diameter ratio and phosphate crystal in a bulk shape is obtained, the two crystals are mutually stacked, the Vickers hardness reaches 7.10GPa, and the fracture toughness reaches 5.02Mpa/m 1/2 。
Example 4:
the following components are taken in mol%: siO 2 2 65％，Al 2 O 3 10％，Li 2 O 4.0％，Na 2 O 10.0％，MgO 6.0％，TiO 2 4.0％，P 2 O 5 1.0％。
The raw materials containing the oxides are weighed and mixed in proportion, then the raw materials are melted at 1550 ℃ to obtain non-crystallized precursor glass, then the precursor glass is put into a crystallization furnace for heat treatment to enable rutile crystals to grow, the heat treatment condition is that the temperature is kept for 3 hours at 870 ℃, so that the microcrystalline glass with rutile crystal phase with high length-diameter ratio and bulk phosphate polymer is obtained, the two crystals are mutually stacked, the Vickers hardness reaches 7.00GPa, and the fracture toughness reaches 5.02Mpa/m 1/2 。
Example 5:
the following components are taken in mol%: siO 2 2 58％，Al 2 O 3 12％，Li 2 O 4.0％，Na 2 O 9.0％，MgO 9.0％，TiO 2 3.0％，P 2 O 5 5.0％。
Weighing and mixing the raw materials containing the oxides in proportion, melting at 1620 ℃ to obtain non-crystallized precursor glass, putting the precursor glass into a crystallization furnace for heat treatment to grow rutile crystals, wherein the heat treatment condition is that the temperature is kept at 900 ℃ for 3 hours to obtain the microcrystalline glass with rutile crystal phase with high length-diameter ratio and phosphate crystal in a bulk shape, the two crystals are mutually stacked to ensure that the Vickers hardness reaches 7.05GPa and the fracture toughness reaches 5.06Mpa/m 1/2 。
Example 6:
taking the following components in mol percent: siO 2 2 57％，Al 2 O 3 11％，Li 2 O 5.00％，Na 2 O 11.0％，MgO 8.0％，TiO 2 5.0％，P 2 O 5 3.0％。
Weighing and mixing the raw materials containing the oxides in proportion, melting at 1600 ℃ to obtain non-crystallized precursor glass, then putting the precursor glass into a crystallization furnace for heat treatment to enable rutile crystals to grow, wherein the heat treatment condition is that the temperature is kept at 870 ℃ for 3 hours to obtain microcrystalline glass with a rutile crystal phase with a high length-diameter ratio and bulk phosphate crystals, and the two crystals are stacked to ensure that the dimension is increasedThe hardness reaches 7.26GPa, and the fracture toughness reaches 5.10Mpa/m 1/2 。
Example 7:
taking the following components in mol percent: siO 2 2 57％，Al 2 O 3 11％，Li 2 O 3.0％，Na 2 O 13.0％，MgO 8.0％，TiO 2 5.0％，P 2 O 5 3.0％。
Weighing and mixing the raw materials containing the oxides in proportion, melting at 1600 ℃ to obtain non-crystallized precursor glass, then putting the precursor glass into a crystallization furnace for heat treatment to enable rutile crystals to grow, wherein the heat treatment condition is that the temperature is kept for 3 hours at 870 ℃, so that the microcrystalline glass with rutile crystal phase with high length-diameter ratio and phosphate crystal clusters is obtained, the two crystals are mutually stacked, the Vickers hardness reaches 7.50GPa, and the fracture toughness reaches 5.43Mpa/m 1/2 。
Example 8:
the following components are taken in mol%: siO 2 2 54％，Al 2 O 3 12％，Li 2 O 3.0％，Na 2 O 13.0％，MgO 4.0％，TiO 2 8.0％，P 2 O 5 6.0％。
Weighing and mixing the raw materials containing the oxides in proportion, melting at 1600 ℃ to obtain non-crystallized precursor glass, then putting the precursor glass into a crystallization furnace for heat treatment to enable rutile crystals to grow, wherein the heat treatment condition is that the temperature is kept for 3 hours at 870 ℃, so that the microcrystalline glass with rutile crystal phase with high length-diameter ratio and phosphate crystal clusters is obtained, the two crystals are mutually stacked, the Vickers hardness reaches 7.50GPa, and the fracture toughness reaches 5.43Mpa/m 1/2 。
Example 9:
the following components are taken in mol%: siO 2 2 53％，Al 2 O 3 12％，Li 2 O 6.0％，Na 2 O 10.0％，MgO 3.0％，TiO 2 10.0％，P 2 O 5 6.0％。
The raw materials containing the above oxides are weighed and mixed at 1600 deg.CMelting to obtain non-crystallized precursor glass, placing the precursor glass into a crystallization furnace to carry out heat treatment to grow rutile crystals, wherein the heat treatment condition is that the temperature is kept at 870 ℃ for 3h, so that the microcrystalline glass with rutile crystal phase with high length-diameter ratio and phosphate crystal clusters is obtained, the two crystals are mutually stacked, the Vickers hardness reaches 7.32GPa, and the fracture toughness reaches 5.23Mpa/m 1/2 。
Example 10:
the following components are taken in mol%: siO 2 2 56％，Al 2 O 3 11％，Li 2 O 5.0％，Na 2 O 11.0％，MgO 5.0％，TiO 2 8.0％，P 2 O 5 4.0％。
Weighing and mixing the raw materials containing the oxides in proportion, melting at 1600 ℃ to obtain non-crystallized precursor glass, then putting the precursor glass into a crystallization furnace for heat treatment to enable rutile crystals to grow, wherein the heat treatment condition is that the temperature is kept at 870 ℃ for 3 hours, so that the microcrystalline glass with the rutile crystal phase with high length-diameter ratio and the phosphate crystal in a bulk shape is obtained, the two crystals are stacked mutually, the Vickers hardness reaches 7.61GPa, and the fracture toughness reaches 5.14Mpa/m 1/2 。
In order to verify the influence of the heat treatment temperature on the microcrystalline glass, the precursor glass prepared in example 2 is taken and placed at different temperatures for heat treatment, and the sample after heat treatment is subjected to XRD (X-ray diffraction) and hardness test; in addition, in order to better illustrate the beneficial effects of the present invention, the inventors performed SEM scanning electron microscope analysis and element distribution analysis on the microcrystalline glass sample obtained in example 2, and the above tests respectively obtained the results shown in fig. 1, fig. 2, fig. 3 and fig. 4.
Fig. 1 is an XRD pattern of the precursor glass sample prepared in example 2 at different heat treatment temperatures, and it can be seen from fig. 1 that when the heat treatment temperature exceeds 730 c, there are distinct crystallization peaks of rutile and phosphate crystals in the XRD pattern, and thus it can be seen that rutile crystals and phosphate crystals are grown in the glass sample. LiMgPO can be obtained by XRD refinement 4 21wt% and 6wt% rutile crystal.
FIG. 2 is an SEM photograph of a glass sample obtained in example 2. From FIG. 2, it can be seen that needle-like crystals having a relatively large major axis appear in the glass sample, and the needle-like crystals are rutile crystals. In addition, it can be seen from FIG. 2 that the length of rutile crystal in the glass sample is greater than or equal to 100nm, the length of partial crystal is greater than 300nm, the diameter of the cross section of rutile crystal is less than or equal to 20nm, the length-diameter ratio of rutile crystal in the glass sample is greater than 5, and the length-diameter ratio of partial crystal is greater than 10.
FIG. 3 is a TEM element distribution diagram of a glass sample in example 2. As can be seen from fig. 3 (a), two morphologies of crystals were present in the sample, one being needle-rod-shaped crystals and one being bulk-shaped crystals. In FIG. 3 (B-F), it was found that the needle-like crystals were rich in Ti 4+ The bulk crystal is rich in P 5+ ，Mg 2+ And Si 4+ ，Al 3+ Mainly exists in a glass matrix, and according to the XRD pattern, the needle rod-shaped crystals are rutile crystals, and the bulk crystals are phosphate crystals (LiMgPO) 4 )。
FIG. 4 is a graphical representation of hardness as a function of heat treatment temperature for the glass samples of example 2. As can be seen from FIG. 4, the Vickers hardness of the glass sample gradually increases with the temperature of the heat treatment, and when the heat treatment temperature reaches above 800 ℃, the hardness of the glass sample is obviously increased, and the Vickers hardness is more than or equal to 7GPa, because when the heat treatment temperature reaches 800 ℃, needle-rod-shaped rutile crystals and bulk-shaped phosphate crystals grow simultaneously in the sample, and the two crystals form a stacked or interlocked structure, so that the hardness and the toughness of the glass are greatly improved.
In conclusion, the invention can grow needle-shaped rutile crystals with high length-diameter ratio, and nodular magnesium phosphate, magnesium lithium phosphate, amorphous phosphate and the composition or polymer thereof in the glass matrix by adjusting the formula and the heat treatment method, wherein the length-diameter ratio of the needle-shaped rutile crystals is more than 5, the length-diameter ratio of partial rutile crystals can reach 10, and the two crystals or polymers are stacked with each other, thereby obviously increasing the hardness and toughness of the glass.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (8)
1. The microcrystalline glass is characterized by comprising the following components in mole fraction:
SiO 2 50.0～65.0%，
Al 2 O 3 10.0～24.0 %，
Li 2 O 2.0～15.0 %，
Na 2 O 5.0～15.0 %，
MgO 2.0～12.0 %，
TiO 2 8.0～11.0 %，
P 2 O 5 5.0～8.0 %；
wherein, P 2 O 5 /[MgO+TiO 2 ]The molar ratio is 0.1-0.8;
phosphate crystals and needle-shaped rutile crystals grow in the microcrystalline glass, the diameter of the cross section of each rutile crystal is less than or equal to 20nm, and the length-diameter ratio of each needle-shaped rutile crystal is greater than 5.
2. A glass-ceramic according to claim 1, wherein the rutile crystals constitute 5-15wt% of the glass-ceramic, and the glass-ceramic further comprises phosphate crystals selected from the group consisting of magnesium phosphate, magnesium lithium phosphate, amorphous phosphates, and combinations thereof, wherein the magnesium phosphate, magnesium lithium phosphate, amorphous phosphates, and combinations thereof constitute 15-40wt%.
3. The glass-ceramic according to claim 1, wherein the needle-like rutile crystal has a length of not less than 100nm.
4. The glass-ceramic according to claim 1, wherein [ Li [ ] 2 O+Na 2 O +MgO]/Al 2 O 3 The molar ratio is 1.1-2.5.
5. The glass-ceramic according to claim 1, wherein [ Li [ ] 2 O+Na 2 O -Al 2 O 3 ]/ TiO 2 The molar ratio is-1 to 1.
6. The microcrystalline glass according to claim 1, wherein the microcrystalline glass has a fracture toughness of 5MPa/m or more 1 /2 。
7. The glass-ceramic according to claim 1, wherein the glass-ceramic has a Vickers hardness of 7GPa or more.
8. A method for preparing a glass-ceramic according to any one of claims 1 to 7, characterized by comprising the steps of: the method comprises the following steps of mixing and melting raw materials according to the component ratio to obtain non-crystallized precursor glass, and carrying out heat treatment on the precursor glass to obtain microcrystalline glass, wherein the heat treatment method comprises the following steps: the precursor glass is insulated for 2 to 4 hours at the temperature of 750 to 900 ℃.
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