A transparent microcrystalline glass and its preparation method

Abstract

The application discloses transparent microcrystalline glass and a preparation method thereof, relates to the technical field of microcrystalline glass preparation, and discloses a preparation method of transparent microcrystalline glass, which comprises the following steps: S1, placing a common glass sheet on a lifting loading platform in a high-temperature furnace, then driving a screw rod to rotate through a rotating motor, thereby driving a first nut block to move in an upward direction, and the first nut block drives a bottom base, the lifting loading platform and the glass sheet to move upward; when the outer surface of a heating rod in the high-temperature furnace is attached with a large amount of oxide layers, the cleaning mechanism can be used to open a vertical hydraulic rod to make a top frame descend into a microcrystalline chamber in the high-temperature furnace, at this time, a first motor is opened to drive a T-shaped sliding rail outside an upper arc-shaped brush to slide in an arc-shaped track, then the upper arc-shaped brush and a lower arc-shaped brush surround the heating rod, and the upper arc-shaped brush and the lower arc-shaped brush move up and down to clean the oxide layers on the heating rod in the microcrystalline chamber.

Description

Technical Field

[0001] This invention belongs to the field of microcrystalline glass preparation technology, specifically a transparent microcrystalline glass and its preparation method. Background Technology

[0002] With the upgrading of smart electronic devices and the popularization of intelligent driving in new energy vehicles, the requirements for display devices are becoming increasingly stringent. Display devices are evolving towards larger screen-to-body ratios and thinner, lighter designs. Therefore, the cover glass for display devices also needs to be thin, lightweight, and high-strength. However, glass itself is relatively brittle, and with the increasing thinness and lightness of glass sheets, it is prone to breakage. One of the most effective methods to improve the strength and toughness of the glass body is to microcrystallize it. Microcrystalline glass, also known as glass-ceramic, is a type of polycrystalline solid material containing a large number of microcrystalline and glassy phases, produced by adjusting the glass composition and heat-treating it under specific temperature conditions. Microcrystalline glass possesses high resistance to crack propagation and drop impacts, high chemical stability, and excellent thermal properties. Based on these advantages, transparent microcrystalline glass is applied to the field of cover glass for display devices with high strength requirements. The microcrystallization process involves placing the glass sheet in a high-temperature furnace for microcrystallization treatment, repeatedly moving it between the preheating chamber and the microcrystallization chamber within the furnace to achieve the microcrystallization process.

[0003] In existing technologies, high-temperature furnaces are generally heated by silicon carbide heating rods. However, after prolonged use, an oxide layer will adhere to the outer wall of the heating rod, affecting its resistance and lifespan. Moreover, the oxide layer on the outside of the heating rod needs to be removed regularly by personnel. This is usually done manually by personnel using tools such as brushes, which not only increases the workload of personnel but also reduces cleaning efficiency. To address this issue, we propose a transparent microcrystalline glass and its preparation method. Summary of the Invention

[0004] The purpose of this invention is to provide a transparent microcrystalline glass and its preparation method to solve the technical problems mentioned in the background art.

[0005] To achieve the above objectives, the present invention provides the following technical solution: a method for preparing transparent microcrystalline glass, comprising the following steps:

[0006] S1. Place the ordinary glass plate on the lifting platform in the high-temperature furnace, and then drive the lead screw to rotate through the rotary motor, thereby driving the first nut block to move in the upward direction. The first nut block drives the base, the lifting platform and the glass plate to rise, and then the glass plate enters the preheating chamber. Turn on the heating rod located in the preheating chamber to preheat the glass plate in the preheating chamber.

[0007] S2. After the glass sheet is preheated, turn on the lifting rod located in the base platform. The working end of the lifting rod drives the lifting platform to rise and move the glass sheet into the microcrystalline chamber. Turn on the heating rod located in the microcrystalline chamber.

[0008] S3. The glass sheet is heated and microcrystallized, then lowered into the microcrystallization chamber by a lifting rod. After repeating the steps multiple times, the temperature of the microcrystallization chamber is set to the annealing temperature and cooled with the furnace to complete the microcrystallization process of the glass sheet.

[0009] The raw materials for the glass slide, by mass percentage, include: SiO2 52-68%, Al2O3 8-25%, Na2O 5-19%, K2O 1-7%, Li2O 0.5-4%, MgO 1-5%, CaO 0.1-1%, ZnO 0.1-1%, ZrO2 0.1-2.5%, TiO2 0.1-2.5%, RO (MgO+CaO+ZnO) 3-6%, RO2 (ZrO2+TiO2) 0.4-1.5%, and clarifying agent 0.2%.

[0010] Preferably, the high-temperature furnace includes a support frame, a preheating chamber, and a microcrystalline chamber. Multiple sets of bases are fixedly installed on the inner walls of both the preheating chamber and the microcrystalline chamber. A heating rod is fixedly installed on the top of each base. A mounting frame is installed on the top of both the preheating chamber and the microcrystalline chamber. A concave slide rail is slidably installed on the mounting frame. A baffle is fixedly installed on the concave slide rail. A cleaning mechanism is installed on the top of the microcrystalline chamber. The cleaning mechanism includes a cleaning component and a lifting component.

[0011] The cleaning assembly includes an upper arc-shaped brush and a lower arc-shaped brush disposed outside the heating rod. A lower arc-shaped plate is fixedly disposed at the bottom of the lower arc-shaped brush. A T-shaped slide rail is fixedly disposed outside the upper arc-shaped brush. An arc-shaped track is disposed on one side of the upper arc-shaped brush, and the end of the T-shaped slide rail can pass into the interior of the arc-shaped track. Multiple sets of connecting rods are fixedly disposed between the lower arc-shaped brush and the arc-shaped track. An arc-shaped tooth is fixedly disposed at the top of the T-shaped slide rail. A first motor is fixedly disposed outside the lower arc-shaped brush. A gear is fixedly disposed at the working end of the first motor, and the gear meshes with the arc-shaped tooth.

[0012] Preferably, the lifting assembly includes a vertical hydraulic rod, a top frame, and four sets of concave frames. A horizontal bar is fixedly installed on the concave frame, and the lower arc plate is fixed on the horizontal bar. An outer ring is fitted around all four ends of the top frame, and a connecting block is fixedly installed between the outer ring and the concave frame.

[0013] Preferably, a top column is provided at the top of the top frame, the bottom working end of the vertical hydraulic rod is fixedly connected to the top of the top column, a fixing ring is fixedly provided on the outside of the vertical hydraulic rod, and an L-shaped frame is fixedly provided between the fixing ring and the mounting frame.

[0014] Preferably, the top frame is provided with a driving component for moving the outer ring. The driving component includes a mounting bearing sleeved and fixed to the outside of the top column. A rotating ring is sleeved and fixed to the outer wall of the mounting bearing. A rotating motor is fixedly provided on the top frame. A driving wheel is fixedly provided at the working end of the rotating motor. The outer wall of the driving wheel is in contact with the outer wall of the rotating ring.

[0015] Preferably, the top of the rotating ring is rotatably provided with four sets of rotating rods, the top of the connecting block is rotatably provided with a rotating column, and the rotating column and the rotating rods are provided with arc-shaped frames.

[0016] Preferably, a first hydraulic rod is fixedly mounted on the mounting bracket, and the working end of the first hydraulic rod is fixedly connected to the baffle.

[0017] Preferably, the support is provided with a movable component for lifting and lowering the glass sheet. The movable component includes a lifting platform and a base. Two sets of lifting rods are fixedly installed on the base. The working ends of the lifting rods are fixedly connected to the lifting platform. Two sets of lead screws are rotatably installed on the support. A first nut block is provided on the outside of the lead screw. A connecting frame is fixedly installed between the first nut block and the base. A rotary motor is provided on the top of the lead screw.

[0018] Another object of the present invention is to provide a transparent microcrystalline glass prepared by the above preparation method.

[0019] Compared with the prior art, the beneficial effects of the present invention are:

[0020] (1) The present invention, through the designed cleaning mechanism, when a lot of oxide layer is attached to the outer surface of the heating rod in the high temperature furnace, can open the vertical hydraulic rod to lower the top frame into the microcrystalline chamber in the high temperature furnace. At this time, the first motor is turned on, driving the T-shaped slide rail outside the upper arc brush to slide in the arc track. Then the upper arc brush and the lower arc brush surround the heating rod. The upper arc brush and the lower arc brush move up and down to remove the oxide layer on the heating rod in the microcrystalline chamber. Then the T-shaped slide rail on the upper arc brush moves into the arc track and then descends into the preheating chamber through the vertical hydraulic rod. The upper arc brush and the lower arc brush remove the oxide layer on the heating rod in the preheating chamber.

[0021] (2) The present invention uses a designed driving component to drive the rotating ring to rotate via a rotating motor, thereby causing the arc frame to rotate. This causes the upper and lower arc brushes to move towards or away from the top frame, allowing the upper and lower arc brushes to easily enter the preheating chamber from the microcrystalline chamber. This avoids the upper and lower arc brushes from being blocked by the base in the microcrystalline chamber as they are about to enter the preheating chamber, and facilitates the removal of the oxide layer on the heating rod located in the preheating chamber.

[0022] (3) Ordinary glass sheets are microcrystalline after being microcrystalline in a high-temperature furnace. The microcrystalline glass has excellent mechanical properties and transparency. It can also be further ion exchanged to improve its performance. It has high mechanical properties such as resistance to crack propagation and drop resistance, high chemical stability and excellent thermal properties. Attached Figure Description

[0023] Figure 1 This is a schematic diagram of the structure of the present invention;

[0024] Figure 2 This is a schematic diagram of the right-side structure of the present invention;

[0025] Figure 3 This is a schematic diagram of the left sectional view of the mounting bracket of the present invention;

[0026] Figure 4 This is a schematic cross-sectional view of the microcrystalline chamber and preheating chamber of the present invention;

[0027] Figure 5 This is a schematic diagram of the heating rod structure of the present invention;

[0028] Figure 6 This is a schematic diagram of the cleaning component structure of the present invention;

[0029] Figure 7 This is a bottom view of the cleaning component of the present invention;

[0030] Figure 8 This is a schematic diagram of the lower arc-shaped brush structure of the present invention;

[0031] Figure 9 This is a schematic diagram of the connection structure between the T-shaped slide rail and the arc track of the present invention;

[0032] Figure 10 This is a schematic diagram of the moving part structure of the present invention;

[0033] Figure 11 This is a bottom view of the moving part of the present invention;

[0034] In the diagram: 100, bracket; 101, first nut block; 102, lead screw; 103, mounting bracket; 104, first hydraulic rod; 105, microcrystalline chamber; 106, preheating chamber; 107, lifting platform; 108, base; 109, baffle; 110, concave slide rail; 111, heating rod; 112, base; 200, vertical hydraulic rod; 201, fixing ring; 202, L-shaped frame; 203, concave frame; 204, outer ring. ; 205, horizontal bar; 206, upper arc-shaped brush; 207, arc-shaped tooth; 208, first motor; 209, lower arc-shaped plate; 210, gear; 211, arc-shaped track; 212, lower arc-shaped brush; 213, T-shaped slide rail; 214, connecting rod; 215, top column; 216, top frame; 217, connecting block; 300, rotating ring; 301, mounting bearing; 302, rotating rod; 303, arc-shaped frame; 305, rotating motor. Detailed Implementation

[0035] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0036] Example 1

[0037] Please see Figures 1-11 This invention provides a technical solution: a method for preparing transparent microcrystalline glass, comprising the following steps:

[0038] S1. Place the ordinary glass plate on the lifting platform 107 in the high-temperature furnace, and then drive the lead screw 102 to rotate through the rotary motor, thereby driving the first nut block 101 to move in the upward direction. The first nut block 101 drives the base 108, the lifting platform 107 and the glass plate to rise. Then the glass plate enters the preheating chamber 106. Turn on the heating rod 111 located in the preheating chamber 106 to preheat the glass plate in the preheating chamber 106.

[0039] S2. After the glass sheet is preheated, turn on the lifting rod located in the base 108. Drive the lifting platform 107 to rise through the working end of the lifting rod, and move the glass sheet into the microcrystalline chamber 105. Turn on the heating rod 111 located in the microcrystalline chamber 105.

[0040] S3. The glass sheet is heated and microcrystallized, and then lowered into the microcrystallization chamber 105 by a lifting rod. After repeating the steps multiple times, the temperature of the microcrystallization chamber 105 is set to the annealing temperature and cooled with the furnace to complete the microcrystallization treatment of the glass sheet.

[0041] The raw materials for the glass slide, by mass percentage, include: SiO2 52-68%, Al2O3 8-25%, Na2O 5-19%, K2O 1-7%, Li2O 0.5-4%, MgO 1-5%, CaO 0.1-1%, ZnO 0.1-1%, ZrO2 0.1-2.5%, TiO2 0.1-2.5%, ROMgO+CaO+ZnO 3-6%, RO2ZrO2+TiO2 0.4-1.5%, and clarifying agent 0.2%.

[0042] The high-temperature furnace includes a support 100, a preheating chamber 106, and a microcrystal chamber 105. The preheating chamber 106 can preheat the glass slide. Multiple sets of bases 112 are fixedly installed on the inner walls of both the preheating chamber 106 and the microcrystal chamber 105. The microcrystal chamber 105 is used for microcrystallization treatment of the glass slide. A heating rod 111 is fixedly installed on the top of the base 112. The heating rod 111 can heat the preheating chamber 106 and the microcrystal chamber 105. A mounting bracket 103 is installed on the top of both the preheating chamber 106 and the microcrystal chamber 105. A concave slide rail 110 is slidably installed on the mounting bracket 103. A baffle 109 is fixedly installed on the concave slide rail 110. A cleaning mechanism is installed on the top of the microcrystal chamber 105. The cleaning mechanism includes a cleaning component and a lifting component.

[0043] The cleaning assembly includes an upper arc-shaped brush 206 and a lower arc-shaped brush 212 disposed outside the heating rod 111. A lower arc-shaped plate 209 is fixedly disposed at the bottom of the lower arc-shaped brush 212. A T-shaped slide rail 213 is fixedly disposed outside the upper arc-shaped brush 206. The T-shaped slide rail 213 can slide within the arc-shaped track 211. An arc-shaped track 211 is disposed on one side of the upper arc-shaped brush 206, and the end of the T-shaped slide rail 213 can pass into the interior of the arc-shaped track 211. Multiple sets of connecting rods 214 are fixedly disposed between the lower arc-shaped brush 212 and the arc-shaped track 211. An arc-shaped tooth 207 is fixedly disposed at the top of the T-shaped slide rail 213. A first motor 208 is fixedly disposed outside the lower arc-shaped brush 212. The first motor 208 can drive the upper arc-shaped brush 206 and the T-shaped slide rail 213 to rotate. A gear 210 is fixedly disposed at the working end of the first motor 208, and the gear 210 meshes with the arc-shaped tooth 207.

[0044] Example 2

[0045] Please refer to Example 1. Figure 1 , Figure 2 , Figure 4 , Figure 5The lifting assembly includes a vertical hydraulic rod 200, a top frame 216, and four sets of concave frames 203. The vertical hydraulic rod 200 can drive the top frame 216 and other components to move up and down. A horizontal bar 205 is fixedly installed on the concave frame 203, and a lower arc plate 209 is fixed on the horizontal bar 205. An outer ring 204 is fitted around the four ends of the top frame 216. The outer ring 204 can slide freely on the top frame 216. A connecting block 217 is fixedly installed between the outer ring 204 and the concave frame 203.

[0046] A top column 215 is provided on the top of the top frame 216. The bottom working end of the vertical hydraulic rod 200 is fixedly connected to the top of the top column 215. A fixing ring 201 is fixedly provided on the outside of the vertical hydraulic rod 200. An L-shaped frame 202 is fixedly provided between the fixing ring 201 and the mounting frame 103. The vertical hydraulic rod 200 and the mounting frame 103 are fixed together by the L-shaped frame 202.

[0047] This invention utilizes a designed cleaning mechanism. When a large amount of oxide layer adheres to the outer surface of the heating rod 111 in the high-temperature furnace, the vertical hydraulic rod 200 can be activated to lower the top frame 216 into the microcrystalline chamber 105 within the high-temperature furnace. At this time, the first motor 208 is activated, driving the T-shaped slide rail 213 outside the upper arc-shaped brush 206 to slide within the arc-shaped track 211. Then, the upper arc-shaped brush 206 and the lower arc-shaped brush 212 surround the heating rod 111, and the upper arc-shaped brush 206 and the lower arc-shaped brush 212 move up and down reciprocally to remove the oxide layer on the heating rod 111 in the microcrystalline chamber 105. Afterward, the T-shaped slide rail 213 on the upper arc-shaped brush 206 moves into the arc-shaped track 211, and then the vertical hydraulic rod 200 lowers it into the preheating chamber 106, where the upper arc-shaped brush 206 and the lower arc-shaped brush 212 remove the oxide layer on the heating rod 111 within the preheating chamber 106.

[0048] During use, when removing the oxide layer on the heating rod 111 in the high-temperature furnace, the baffle 109 at the top of the microcrystalline chamber 105 is opened by the driving action of the first hydraulic rod 104. At this time, the vertical hydraulic rod 200 is activated, which drives the cleaning assembly and top frame 216 to move downward and enter the microcrystalline chamber 105. Then, the lower arc-shaped brush 212 surrounds the heating rod 111. Next, the first motor 208 is activated to drive the gear 210 to rotate, which in turn drives the arc-shaped gear 207 to rotate, thereby driving the upper arc-shaped brush 206 and the T-shaped slide rail 213 to rotate. At this time, the T-shaped slide rail 213 located in the arc-shaped track 211 rotates and extends outward, driving the upper arc-shaped brush 206 to rotate and extend. Then, the upper arc-shaped brush 206 can surround the part of the heating rod 111 near the inner wall of the microcrystalline chamber 105. The upper arc-shaped brush 206 and the lower arc-shaped brush 212 surround the heating rod 111, and then the vertical hydraulic rod 200 drives it to move up and down repeatedly to clean the heating rod 111 located in the microcrystalline chamber 105. After the heating rod 111 in the microcrystalline chamber 105 is cleaned, the T-shaped slide rail 213 in the upper arc-shaped brush 206 is rotated into the arc-shaped track 211 according to the reverse principle. At this time, the upper arc-shaped brush 206, which is close to the inner wall of the microcrystalline chamber 105, rotates to a position above the lower arc-shaped brush 212. Then, the vertical hydraulic rod 200 can drive it to move down and enter the preheating chamber 106. Then the upper arc-shaped brush 206 unfolds, and the upper arc-shaped brush 206 and the lower arc-shaped brush 212 surround the heating rod 111 and move up and down repeatedly to clean the heating rod 111 located in the preheating chamber 106.

[0049] Example 3

[0050] Please refer to Example 2. Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 10 and Figure 11 The top frame 216 is provided with a driving component for moving the outer ring 204. The driving component includes a mounting bearing 301 sleeved and fixed to the outside of the top column 215. The mounting bearing 301 can support the rotating ring 300. The rotating ring 300 is sleeved and fixed to the outer wall of the mounting bearing 301. A rotating motor 305 is fixedly provided on the top frame 216. The rotating motor 305 can drive the rotating ring 300 to rotate. A drive wheel is fixedly provided at the working end of the rotating motor 305. The outer wall of the drive wheel contacts the outer wall of the rotating ring 300.

[0051] The top of the rotating ring 300 is rotatably equipped with four sets of rotating rods 302, and the top of the connecting block 217 is rotatably equipped with a rotating column. The rotating column and the rotating rods 302 are equipped with an arc frame 303. The rotating ring 300 can drive the connecting block 217 at the bottom of the concave frame 203 to move through the arc frame 303, thereby driving the lower arc brush 212 to move.

[0052] This invention utilizes a designed driving component, where a rotating motor 305 drives a rotating ring 300 to rotate, which in turn drives an arc-shaped frame 303 to rotate. This causes the upper arc-shaped brush 206 and the lower arc-shaped brush 212 to move closer to or further away from the top frame 216. This allows the upper arc-shaped brush 206 and the lower arc-shaped brush 212 to easily enter the preheating chamber 106 from the microcrystalline chamber 105, avoiding obstruction by the base 112 in the microcrystalline chamber 105. This facilitates the removal of the oxide layer on the heating rod 111 located in the preheating chamber 106.

[0053] During use, before the upper arc-shaped brush 206 and the lower arc-shaped brush 212 enter the preheating chamber 106 after cleaning the heating rod 111 located in the microcrystalline chamber 105, the rotating motor 305 is started, driving the rotating ring 300 to rotate counterclockwise. Then, the rotating ring 300 drives the arc-shaped frame 303 to rotate, thereby indirectly driving the upper arc-shaped brush 206, the lower arc-shaped brush 212 and other structures to move closer to the top frame 216. At this time, the inner wall of the lower arc-shaped brush 212 is no longer in contact with the heating rod 111. Then, it descends into the preheating chamber 106 by the action of the vertical hydraulic rod 200. At this time, the rotating motor 305 reverses, causing the upper arc-shaped brush 206, the lower arc-shaped brush 212 and other structures to extend away from the top frame 216. Then, the inner wall of the lower arc-shaped brush 212 contacts the heating rod 111 and begins to remove the oxide layer on the heating rod 111.

[0054] In this embodiment, a first hydraulic rod 104 is fixedly installed on the mounting bracket 103. The first hydraulic rod 104 can make the baffle 109 cover the top of the microcrystalline chamber 105 or the position between the preheating chamber 106 and the microcrystalline chamber 105, so as to facilitate preheating or microcrystallization treatment. The working end of the first hydraulic rod 104 is fixedly connected to the baffle 109.

[0055] In this embodiment, the support 100 is equipped with a movable component for lifting and lowering the glass sheet. The movable component includes a lifting platform 107 and a base 108. Two sets of lifting rods are fixedly installed on the base 108, and the working ends of the lifting rods are fixedly connected to the lifting platform 107. Two sets of lead screws 102 are rotatably installed on the support 100. The first nut block 101 rises or falls left and right with the rotating lead screw 102. When the glass sheet located at the top of the lifting platform 107 enters the microcrystalline chamber 105, it is lifted by the lifting rod in the baffle 109. The first nut block 101 is installed outside the lead screw 102, and a connecting frame is fixedly installed between the first nut block 101 and the base 108. A rotary motor is installed at the top of the rod 102. The glass sheet can be preheated in the preheating chamber 106 through the lead screw 102 and the first nut block 101. At this time, the bottom platform 108 blocks the bottom of the preheating chamber 106, and then the baffle 109 at the top of the preheating chamber 106 covers it, so that the glass sheet can be preheated. After preheating, the baffle 109 at the top of the preheating chamber 106 is opened, and the glass sheet is lifted by the lifting rod to raise the lifting platform 107 and drive the glass sheet into the microcrystal chamber 105. At this time, the baffle 109 at the top of the microcrystal chamber 105 is closed, and then the lifting platform 107 blocks the bottom of the microcrystal chamber 105, and then the microcrystallization treatment of the glass sheet begins.

[0056] Example 4

[0057] Please see Figures 1-5 This invention provides a technical solution: a method for preparing transparent microcrystalline glass, comprising the following steps:

[0058] (a) Weigh the raw materials of the batch according to the following mass percentages: SiO2 65%, Al2O3 14%, Na2O 11%, K2O 2%, Li2O 0.5-6%, MgO 2-8%, CaO 0.1-1%, ZnO 0.1-1%, ZrO2 0.1-2.5%, TiO2 0.1-2.5%, of which RO (MgO+CaO+ZnO) 3.5%; RO2 (ZrO2+TiO2) 1.2%; and clarifying agent 0.2%. Melt, homogenize and clarify the raw materials of the batch in a high-temperature heating furnace, cast into shape, anneal, cool to room temperature in the furnace, and then prepare a 2 mm thick glass sheet, which is then cleaned and dried.

[0059] (b) The glass slide prepared in (a) is placed into the ultra-microcrystallization experimental device for ultra-microcrystallization treatment. The ultra-microcrystallization experimental device consists of a preheating chamber 106, a slow-temperature section, a microcrystallization chamber 105, and a lifting platform 107.

[0060] The preheating chamber 106, the slow-temperature section, and the microcrystalline chamber 105 are on the same axis, so that they are connected vertically and vertically, which is used for the lifting platform 107 to move through.

[0061] The ultrafine crystallization process is as follows: A glass slide is vertically placed into the lifting stage 107 and raised to the preheating chamber 106 for pretreatment. The temperature in the preheating chamber 106 is set to T1 (T1: initial crystallization temperature), held for 5 minutes, and then moved to the microcrystal chamber 105 at an upward speed of v1. The temperature in the microcrystal chamber 105 is set to T2 (T2: maximum crystallization temperature), and the treatment time is t: 10 seconds. After treatment, the slide is moved back to the preheating chamber 106 at a downward speed of v2. This process is repeated multiple times. Finally, the temperature of the preheating chamber 106 is set to the annealing temperature, and the slide is cooled with the furnace. By setting the temperature within the crystallization temperature range of T1-T2 and adjusting the crystallization time at different temperatures, the crystal nucleation rate and grain growth rate can be effectively controlled.

[0062] The objectives of this invention and the technical problems it addresses can be further achieved by the following technical measures.

[0063] The glass batch material in step (a) has the following composition: RO (MgO+CaO+ZnO) value of 3.5% and RO2 (ZrO2+TiO2) value of 1.2%.

[0064] In step (b), v1: 0.5 m / min, v2: 2 m / min;

[0065] In step (b), the distance between the preheating chamber 106 and the microcrystalline chamber 105 is H, where H is 0.3 m.

[0066] Example 5

[0067] Please see Figures 1-5 This invention provides a technical solution: a method for preparing transparent microcrystalline glass, comprising the following steps:

[0068] (a) Weigh the raw materials of the batch according to the following mass percentages: SiO2 65%, Al2O3 14%, Na2O 11%, K2O 2%, Li2O 0.5-6%, MgO 2-8%, CaO 0.1-1%, ZnO 0.1-1%, ZrO2 0.1-2.5%, TiO2 0.1-2.5%, of which RO (MgO+CaO+ZnO) 4%; RO2 (ZrO2+TiO2) 1.0%; and clarifying agent 0.2%. Melt, homogenize and clarify the raw materials of the batch in a high-temperature heating furnace, cast into shape, anneal, cool to room temperature in the furnace, and then prepare 2 mm thick glass sheets, which are then cleaned and dried.

[0069] (b) The glass slide prepared in (a) is placed into the ultra-microcrystallization experimental device for ultra-microcrystallization treatment. The ultra-microcrystallization experimental device consists of a preheating chamber 106, a slow-temperature section, a microcrystallization chamber 105, and a lifting platform 107.

[0070] The preheating chamber 106, the slow-temperature section, and the microcrystalline chamber 105 are on the same axis, so that they are connected vertically and vertically, which is used for the lifting platform 107 to move through.

[0071] Ultrafine crystallization process: The glass slide is vertically placed into the lifting stage 107 and raised to the preheating chamber 106 for pretreatment. The temperature in the preheating chamber 106 is set to T1 (T1: initial crystallization temperature T1), held for 2 minutes, and then moved to the microcrystal chamber 105 at an upward speed of v1. The temperature in the microcrystal chamber 105 is set to T2 (T2: maximum crystallization temperature), and the treatment time is t: 45 seconds. After treatment, the slide is moved back to the preheating chamber 106 at a downward speed of v2. This process is repeated multiple times. Finally, the temperature of the preheating chamber 106 is set to the annealing temperature, and the slide is cooled with the furnace. By setting the temperature within the crystallization temperature range of T1-T2 and adjusting the crystallization time at different temperatures, the crystal nucleation rate and grain growth rate can be effectively controlled.

[0072] The objectives of this invention and the technical problems it addresses can be further achieved by the following technical measures.

[0073] The glass batch material in step (a) has an RO (MgO+CaO+ZnO) value of 4%.

[0074] The RO2 (ZrO2 + TiO2) value is 1.0%;

[0075] In step (b), v1: 0.8 m / min, v2: 1 m / min;

[0076] In step (b), the distance between the preheating chamber 106 and the microcrystalline chamber 105 is H, where H is 0.7m.

[0077] Example 6

[0078] Please see Figures 1-5 This invention provides a technical solution: a method for preparing transparent microcrystalline glass, comprising the following steps:

[0079] (a) Weigh the raw materials of the batch according to the following mass percentages: SiO2 65%, Al2O3 14%, Na2O 11%, K2O 2%, Li2O 0.5-6%, MgO 2.8%, CaO 1%, ZnO 0.2%, ZrO2 0.2%, TiO2 0.6%, of which RO (MgO+CaO+ZnO) 4.5%; RO2 (ZrO2+TiO2) 0.8%; and clarifying agent 0.2%. Melt, homogenize and clarify the raw materials of the batch in a high-temperature heating furnace, cast into shape, anneal, cool to room temperature in the furnace, and then prepare 2 mm thick glass sheets, which are then cleaned and dried.

[0080] (b) The glass slide prepared in (a) is placed into the ultra-microcrystallization experimental device for ultra-microcrystallization treatment. The ultra-microcrystallization experimental device consists of a preheating chamber 106, a slow-temperature section, a microcrystallization chamber 105, and a lifting platform 107.

[0081] The preheating chamber 106, the slow-temperature section, and the microcrystalline chamber 105 are on the same axis, so that they are connected vertically and vertically, which is used for the lifting platform 107 to move through.

[0082] The ultrafine crystallization process is as follows: A glass slide is vertically placed into the lifting stage 107 and raised to the preheating chamber 106 for pretreatment. The temperature in the preheating chamber 106 is set to T1 (T1: initial crystallization temperature), held for 3 minutes, and then moved to the microcrystal chamber 105 at an upward speed of v1. The temperature in the microcrystal chamber 105 is set to T2 (T2: maximum crystallization temperature), and the treatment time is t: 45 seconds. After treatment, the slide is moved back to the preheating chamber 106 at a downward speed of v2. This process is repeated multiple times. Finally, the temperature of the preheating chamber 106 is set to the annealing temperature, and the slide is cooled with the furnace. By setting the temperature within the crystallization temperature range of T1~T2 and adjusting the crystallization time at different temperatures, the crystal nucleation rate and grain growth rate can be effectively controlled.

[0083] The objectives of this invention and the technical problems it addresses can be further achieved by the following technical measures.

[0084] The glass batch material in step (a) has the following composition: RO (MgO+CaO+ZnO) value of 4.5% and RO2 (ZrO2+TiO2) value of 0.8%.

[0085] In step (b), v1: 1.2 m / min, v2: 2.5 m / min;

[0086] In step (b), the distance between the preheating chamber 106 and the microcrystalline chamber 105 is H, where H is 0.5 m.

[0087] Example 7

[0088] Please see Figures 1-5 This invention provides a technical solution: a method for preparing transparent microcrystalline glass, comprising the following steps:

[0089] (a) Weigh the following raw materials according to the following mass percentages: SiO2 65%, Al2O3 14%, Na2O 10%, K2O 2%, Li2O 1%, MgO 4%, CaO 0.6%, ZnO 1%, ZrO2 0.3%, TiO2 0.3%, of which RO (MgO+CaO+ZnO) 3-6%; RO2 (ZrO2+TiO2) 0.4-1.5%, and clarifying agent 0.2%. Melt, homogenize and clarify the raw materials in a high-temperature heating furnace, cast into shape, anneal, cool to room temperature in the furnace, and then prepare 2 mm thick glass sheets, which are then cleaned and dried.

[0090] (b) The glass slide prepared in (a) is placed into the ultra-microcrystallization experimental device for ultra-microcrystallization treatment. The ultra-microcrystallization experimental device consists of a preheating chamber 106, a slow-temperature section, a microcrystallization chamber 105, and a lifting platform 107.

[0091] The preheating chamber 106, the slow-temperature section, and the microcrystalline chamber 105 are on the same axis, so that they are connected vertically and vertically, which is used for the lifting platform 107 to move through.

[0092] The ultrafine crystallization process is as follows: A glass slide is vertically placed into the lifting stage 107 and raised to the preheating chamber 106 for pretreatment. The temperature in the preheating chamber 106 is set to T1 (T1: initial crystallization temperature), held for 3 minutes, and then moved to the microcrystal chamber 105 at an upward speed of v1: 2.0 m / min. The temperature in the microcrystal chamber 105 is set to T2 (T2: maximum crystallization temperature), and the treatment time is t: 60 s. After treatment, the slide is moved back to the preheating chamber 106 at a downward speed of v2: 3 m / min. This process is repeated multiple times. Finally, the temperature in the preheating chamber 106 is set to the annealing temperature, and the slide is cooled with the furnace. By setting the temperature within the crystallization temperature range of T1~T2 and adjusting the crystallization time at different temperatures, the crystal nucleation rate and grain growth rate can be effectively controlled.

[0093] The objectives of this invention and the technical problems it addresses can be further achieved by the following technical measures.

[0094] The glass batch material in step (a) has the following composition: RO (MgO+CaO+ZnO) value of 5.6% and RO2 (ZrO2+TiO2) value of 0.6%.

[0095] In step (b), v1: 2 m / min, v2: 3 m / min;

[0096] In step (b), the distance between the preheating chamber 106 and the microcrystalline chamber 105 is H, where H is 1.0 m.

[0097] Control group 1:

[0098] The sample composition remained the same as in Example 1. The raw materials for the batch were weighed according to the following mass percentages: SiO2 65%, Al2O3 14%, Na2O 11%, K2O 2%, Li2O 0.5-6%, MgO 2-8%, CaO 0.1-1%, ZnO 0.1-1%, ZrO2 0.1-2.5%, TiO2 0.1-2.5%, of which RO (MgO+CaO+ZnO) 4%; RO2 (ZrO2+TiO2) 1.0%; and clarifying agent 0.2%. The raw materials for the batch were melted, homogenized, and clarified in a high-temperature furnace, cast into shape, annealed, cooled to room temperature in the furnace, and then a 2 mm thick glass sheet was prepared, cleaned, and dried.

[0099] The sample was processed in the preheating chamber 106, and the temperature rise in the preheating chamber 106 was set to T1 (T1: initial crystallization temperature T1). The processing time was the same as the total processing time in Example 2, and the sample was processed in the preheating chamber 106 until the end.

[0100] Control group 2:

[0101] The sample composition remained the same as in Example 1. The raw materials for the batch were weighed according to the following mass percentages: SiO2 65%, Al2O3 14%, Na2O 11%, K2O 2%, Li2O 0.5-6%, MgO 2-8%, CaO 0.1-1%, ZnO 0.1-1%, ZrO2 0.1-2.5%, TiO2 0.1-2.5%, of which RO (MgO+CaO+ZnO) 4%; RO2 (ZrO2+TiO2) 1.0%; and clarifying agent 0.2%. The raw materials for the batch were melted, homogenized, and clarified in a high-temperature furnace, cast into shape, annealed, cooled to room temperature in the furnace, and then a 2 mm thick glass sheet was prepared, cleaned, and dried.

[0102] The sample was processed in the preheating chamber 106, and the temperature rise in the preheating chamber 106 was set to T1 (T1: initial crystallization temperature T1). The processing time was the same as the total processing time in Example 2, and the sample was processed in the preheating chamber 106 until the end.

[0103] Control group 3:

[0104] (a) Weigh the raw materials of the batch according to the following mass percentages: SiO2 64%, Al2O3 14%, Na2O 10%, K2O 2%, Li2O 0.5-6%, MgO 2-8%, CaO 0.1-1%, ZnO 0.1-1%, ZrO2 0.1-2.5%, TiO2 0.1-2.5%, of which RO (MgO+CaO+ZnO) 4.5%; clarifying agent 0.2%. Melt, homogenize and clarify the raw materials of the batch in a high-temperature furnace, cast into shape, anneal, cool to room temperature in the furnace, and then prepare 2 mm thick glass sheets, which are then cleaned and dried.

[0105] (b) The glass slide prepared in (a) is placed into the ultra-microcrystallization experimental device for ultra-microcrystallization treatment. The ultra-microcrystallization experimental device consists of a preheating chamber 106, a slow-temperature section, a microcrystallization chamber 105, and a lifting platform 107.

[0106] The preheating chamber 106, the slow-temperature section, and the microcrystalline chamber 105 are on the same axis, so that they are connected vertically and vertically, which is used for the lifting platform 107 to move through.

[0107] Ultrafine crystallization process: The glass slide is placed vertically into the lifting platform 107 and raised to the preheating chamber 106 for pretreatment. The temperature rise in the preheating chamber 106 is set to T1 (T1: initial crystallization temperature T1), and the temperature is held for 3 minutes. The temperature of the preheating chamber 106 is then set to the annealing temperature and cooled with the furnace.

[0108] The objectives of this invention and the technical problems it addresses can be further achieved by the following technical measures.

[0109] The glass batch material in step (a) has the following composition: RO (MgO+CaO+ZnO) value of 4.5% and RO2 (ZrO2+TiO2) value of 0.8%.

[0110] In step (b), v1: 1.2 m / min, v2: 2.5 m / min;

[0111] In step (b), the distance between the preheating chamber 106 and the microcrystalline chamber 105 is H, where H is 0.5 m.

[0112] Lithium silicate glasses were obtained according to the methods in Examples 5-7 and Comparative Groups 1-3, and their performance was tested and compared with the control group. The treatment conditions and test results are shown in Table 1 below:

[0113] Table 1: Process parameters and test performance of the examples

[0114]

[0115] The above embodiments are only used to illustrate the technical methods of the present invention and are not intended to limit it. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical methods of the present invention without departing from the spirit and scope of the technical methods of the present invention.

Claims

1. A method of making a transparent microcrystalline glass, characterized by: The method comprises the following steps: S1, the common glass sheet is placed on the lifting stage (107) in the high temperature furnace, then the screw rod (102) is driven to rotate by the rotating motor, so that the first nut block (101) moves upward, the first nut block (101) drives the base (108), the lifting stage (107) and the glass sheet to rise, and then the glass sheet enters the preheating chamber (106), the heating rod (111) in the preheating chamber (106) is turned on, and the glass sheet is preheated in the preheating chamber (106); S2, after the glass sheet is preheated, the lifting rod in the base (108) is turned on, the lifting stage (107) is driven to rise by the working end of the lifting rod, and the glass sheet enters the microcrystalline chamber (105), and the heating rod (111) in the microcrystalline chamber (105) is turned on; S3, the glass sheet is heated and microcrystallized, then it is lowered into the microcrystalline chamber (105), and the temperature of the microcrystalline chamber (105) is set to the annealing temperature after repeating the steps for several times, and the glass sheet is microcrystallized by cooling in the furnace; The high temperature furnace comprises a support (100), a preheating chamber (106) and a microcrystalline chamber (105), the inner walls of the preheating chamber (106) and the microcrystalline chamber (105) are fixedly provided with a plurality of bases (112), the top of the base (112) is fixedly provided with a heating rod (111), the top of the preheating chamber (106) and the microcrystalline chamber (105) is provided with a mounting bracket (103), the mounting bracket (103) is provided with a concave slide rail (110) which is slidably arranged on the mounting bracket (103), the concave slide rail (110) is fixedly provided with a baffle (109), and the top of the microcrystalline chamber (105) is provided with a cleaning mechanism. The cleaning mechanism comprises a cleaning assembly and a lifting assembly, the cleaning assembly comprises an upper arc-shaped brush (206) and a lower arc-shaped brush (212) which are arranged outside the heating rod (111), the bottom of the lower arc-shaped brush (212) is fixedly provided with a lower arc-shaped plate (209), the outside of the upper arc-shaped brush (206) is fixedly provided with a T-shaped slide rail (213), one side of the upper arc-shaped brush (206) is provided with an arc-shaped track (211), and the end of the T-shaped slide rail (213) penetrates into the inside of the arc-shaped track (211), a plurality of connecting rods (214) are fixedly arranged between the lower arc-shaped brush (212) and the arc-shaped track (211), the top of the T-shaped slide rail (213) is fixedly provided with an arc-shaped tooth (207), the outside of the lower arc-shaped brush (212) is fixedly provided with a first motor (208), the working end of the first motor (208) is fixedly provided with a gear (210), and the gear (210) is engaged with the arc-shaped tooth (207).

2. The method of claim 1, wherein the transparent microcrystalline glass is prepared by the steps of: The lifting assembly comprises a vertical hydraulic rod (200), a top frame (216) and four groups of concave frames (203), the horizontal bars (205) are fixedly arranged on the concave frames (203), the lower arc-shaped plates (209) are fixed on the horizontal bars (205), the outer rings (204) are sleeved on the four circumferential ends of the top frame (216), and the connecting blocks (217) are fixedly arranged between the outer rings (204) and the concave frames (203). ​ 3. The method of claim 2, wherein the transparent microcrystalline glass is prepared by the following steps: The top of the top frame (216) is provided with a top column (215), the bottom working end of the vertical hydraulic rod (200) is fixedly connected with the top of the top column (215), the outer portion of the vertical hydraulic rod (200) is fixedly provided with a fixing ring (201), and the fixing ring (201) and the mounting frame (103) are fixedly provided with an L-shaped frame (202). ​ 4. The method of claim 3, wherein the transparent microcrystalline glass is prepared by the following steps of: The top frame (216) is provided with a driving piece for moving the outer ring (204), the driving piece comprises a mounting bearing (301) fixedly sleeved on the outer portion of the top column (215), the outer wall of the mounting bearing (301) is fixedly sleeved with a rotating ring (300), the top frame (216) is fixedly provided with a rotating motor (305), the working end of the rotating motor (305) is fixedly provided with a driving wheel, and the outer wall of the driving wheel is in contact with the outer wall of the rotating ring (300). ​ 5. The method of claim 4, wherein the transparent microcrystalline glass is prepared by the following steps of: The top of the rotating ring (300) is rotatably provided with four groups of rotating rods (302), the top of the connecting block (217) is rotatably provided with a rotating column, and the rotating column and the arc-shaped frames (303) on the rotating rods (302) are provided. ​ 6. The method of claim 1, wherein the transparent microcrystalline glass is prepared by the steps of: The mounting frame (103) is fixedly provided with a first hydraulic rod (104), and the working end of the first hydraulic rod (104) is fixedly connected with the baffle (109). ​ 7. The method of claim 1, wherein the transparent microcrystalline glass is prepared by the steps of: The support (100) is provided with a moving piece for lifting the glass sheet, the moving piece comprises a lifting loading platform (107) and a bottom platform (108), two groups of lifting rods are fixedly arranged on the bottom platform (108), the working ends of the lifting rods are fixedly connected with the lifting loading platform (107), two groups of lead screws (102) are rotatably arranged on the support (100), the outer portion of the lead screw (102) is provided with a first nut block (101), the first nut block (101) and the bottom platform (108) are fixedly provided with a connecting frame, and the top of the lead screw (102) is provided with a rotating motor. ​ 8. The method of claim 1, wherein the transparent microcrystalline glass is prepared by the steps of: The glass sheet comprises, in percentage by mass: SiO2 52-68 %, Al2O3 8-25 %, Na2O 5-19 %, K2O 1-7 %, Li2O 0.5-4 %, MgO 1-5 %, CaO 0.1-1 %, ZnO 0.1-1 %, ZrO2 0.1-2.5 %, TiO2 0.1-2.5 %, and clarifying agent 0.2 %. ​ 9. A transparent microcrystalline glass, characterized by, Prepared according to the method of any one of claims 1-8. Prepared according to the method of any one of claims 1-8.

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