Transparent microcrystalline glass and preparation method thereof

Abstract

The invention discloses transparent microcrystalline glass and a preparation method, and relates to the technical field of microcrystalline glass preparation, and the preparation method of the transparent microcrystalline glass comprises the following steps: S1, placing a common glass sheet on a lifting objective table in a high-temperature furnace, and then driving a screw rod to rotate through a rotating motor so as to drive a first nut block to move in the ascending direction, the first nut block drives the bottom table, the lifting objective table and the glass sheet to ascend; through the designed cleaning mechanism, when many oxide layers are attached to the outer surface of a heating rod in the high-temperature furnace in the using process, a vertical hydraulic rod can be started to enable a top frame to descend into a microcrystal chamber in the high-temperature furnace, and at the moment, a first motor is started to drive a T-shaped sliding rail outside an upper arc-shaped brush to slide in an arc-shaped rail; and then the upper arc-shaped brush and the lower arc-shaped brush surround the heating rod, and the upper arc-shaped brush and the lower arc-shaped brush move up and down in a reciprocating manner to remove an oxide layer on the heating rod in the microcrystal chamber.

Description

Technical Field

[0001] The present invention belongs to the technical field of microcrystalline glass preparation, and in particular relates to a transparent microcrystalline glass and a preparation method thereof. Background Art

[0002] With the replacement of smart electronic devices and the popularization of smart driving of new energy vehicles, the requirements for display devices are getting higher and higher. Display devices are developing towards a larger screen-to-body ratio and being thinner and lighter. Therefore, the cover glass of display devices also needs to have the characteristics of thin thickness, light weight, and high strength. However, glass itself is relatively brittle, and it is easy to break as the glass plate becomes thinner and lighter. One of the most effective ways to improve the strength and toughness of the glass body is to make it microcrystalline. Microcrystalline glass, also known as glass ceramics, is a type of polycrystalline solid material containing a large amount of microcrystalline phase and glass phase obtained by adjusting the glass composition, heat treatment under specific temperature conditions, and controlling crystallization during the heating process. Microcrystalline glass has high mechanical properties such as resistance to crack propagation and resistance to falling, high chemical stability and excellent thermal properties. Based on the above advantages, transparent microcrystalline glass is applied to the field of cover glass of display devices with high strength requirements. In the process of microcrystallization, the glass sheet is placed in a high-temperature furnace for microcrystallization treatment, and repeatedly moved in the preheating chamber and microcrystallization chamber in the high-temperature furnace to make the glass microcrystalline.

[0003] In the prior art, high-temperature furnaces are generally heated by carbon-silicon heating rods. After the heating rods are used for a long time, an oxide layer will adhere to the outer wall, which affects the resistance value and service life of the heating rods. In addition, personnel are required to regularly remove the oxide layer on the outside of the heating rods during cleaning. During cleaning, personnel generally use tools such as brushes to manually remove the oxide layer on the outside of the heating rods. This not only increases the workload of personnel, but also reduces the cleaning efficiency. For this reason, we propose a transparent microcrystalline glass and a preparation method. Summary of the invention

[0004] The object of the present invention is to provide a transparent microcrystalline glass and a preparation method thereof to solve the technical problems raised in the above-mentioned background technology.

[0005] To achieve the above object, the present invention provides the following technical solution: a method for preparing transparent microcrystalline glass, comprising the following steps: S1. Place an ordinary glass sheet on the lifting platform in the high-temperature furnace, and then drive the 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 bottom platform, the lifting platform and the glass sheet to rise, and then the glass sheet enters the preheating chamber, and the heating rod in the preheating chamber is turned on to preheat the glass sheet in the preheating chamber; S2, after the glass piece is preheated, the lifting rod located in the bottom platform is turned on, and the lifting platform is driven up by the working end of the lifting rod to drive the glass piece into the microcrystalline chamber, and the heating rod located in the microcrystalline chamber is turned on; S3, heating the glass sheet for microcrystallization treatment, and then lowering it into the microcrystallization chamber through the lifting rod. After repeating the steps for many times, the temperature of the microcrystallization chamber is set to the annealing temperature, and the glass sheet is cooled with the furnace to complete the microcrystallization treatment.

[0006] The raw materials of the glass sheet include, by mass percentage, 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 clarifier 0.2%.

[0007] Preferably, the high temperature furnace comprises a support, a preheating chamber and a microcrystal chamber, the inner walls of the preheating chamber and the microcrystal chamber are fixedly provided with a plurality of groups of bases, the tops of the bases are fixedly provided with heating rods, the tops of the preheating chamber and the microcrystal chamber are provided with mounting frames, the mounting frames are slidably provided with concave slide rails, the concave slide rails are fixedly provided with baffles, the top of the microcrystal chamber is provided with a cleaning mechanism, and the cleaning mechanism comprises a cleaning component and a lifting component; The cleaning assembly includes an upper arc brush and a lower arc brush arranged on the outside of the heating rod, a lower arc plate is fixedly arranged on the bottom of the lower arc brush, a T-shaped slide rail is fixedly arranged on the outside of the upper arc brush, an arc track is arranged on one side of the upper arc brush, and the end of the T-shaped slide rail can be inserted into the interior of the arc track, a plurality of groups of connecting rods are fixedly arranged between the lower arc brush and the arc track, an arc tooth is fixedly arranged on the top of the T-shaped slide rail, a first motor is fixedly arranged on the outside of the lower arc brush, a gear is fixedly arranged on the working end of the first motor, and the gear is meshed with the arc tooth.

[0008] Preferably, the lifting assembly includes a vertical hydraulic rod, a top frame and four groups of concave frames, a horizontal bar is fixedly provided on the concave frame, the lower arc plate is fixed on the horizontal bar, the four ends of the top frame are sleeved with an outer ring, and a connecting block is fixedly provided between the outer ring and the concave frame.

[0009] Preferably, a top column is provided on 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.

[0010] Preferably, a driving member for moving the outer ring is provided on the top frame, and the driving member includes a mounting bearing sleeved and fixed on the outside of the top column, and a rotating ring is sleeved and fixed on the outer wall of the mounting bearing. A rotating motor is fixed on the top frame, and a driving wheel is fixed on the working end of the rotating motor, and the outer wall of the driving wheel is in contact with the outer wall of the rotating ring.

[0011] Preferably, four groups of rotating rods are rotatably provided on the top of the rotating ring, a rotating column is rotatably provided on the top of the connecting block, and arc frames are provided on the rotating column and the rotating rods.

[0012] Preferably, a first hydraulic rod is fixedly provided on the mounting frame, and a working end of the first hydraulic rod is fixedly connected to the baffle.

[0013] Preferably, the bracket is provided with a moving part for lifting the glass sheet, and the moving part includes a lifting platform and a base platform, two groups of lifting rods are fixedly provided on the base platform, and the working ends of the lifting rods are fixedly connected to the lifting platform, and two groups of screw rods are rotatably provided on the bracket, a first nut block is provided on the outside of the screw rod, a connecting frame is fixedly provided between the first nut block and the base platform, and a rotating motor is provided on the top of the screw rod.

[0014] Another object of the present invention is to provide a transparent microcrystalline glass produced by the above preparation method.

[0015] Compared with the prior art, the present invention has the following beneficial effects: (1) The cleaning mechanism designed in the present invention can be used to open the vertical hydraulic rod to lower the top frame into the microcrystalline chamber of the high-temperature furnace when a lot of oxide layers adhere to the outer surface of the heating rod in the high-temperature furnace. At this time, the first motor is turned on to drive the T-shaped slide rail outside the upper arc brush to slide in the arc track, and then the upper arc brush and the lower arc brush surround the heating rod. The upper arc brush and the lower arc brush reciprocate 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 it is lowered into the preheating chamber through the vertical hydraulic rod, and the oxide layer on the heating rod in the preheating chamber is removed by the upper arc brush and the lower arc brush.

[0016] (2) The present invention uses a designed driving member to drive the rotating ring to rotate by rotating the motor to drive the arc frame to rotate, thereby driving the upper arc brush and the lower arc brush to move toward or away from the top frame, so that the upper arc brush and the lower arc brush can easily enter the preheating chamber from the microcrystalline chamber, avoiding the situation where the upper arc brush and the lower arc brush about to enter the preheating chamber are blocked by the base in the microcrystalline chamber, and facilitating the removal of the oxide layer on the heating rod in the preheating chamber.

[0017] (3) Ordinary glass sheets are microcrystallized in a high-temperature furnace to obtain transparent microcrystalline glass. This microcrystalline glass has excellent mechanical properties and transparency. It can also be further treated with ion exchange 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. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 It is a structural schematic diagram of the present invention; Figure 2 It is a right view structural schematic diagram of the present invention; Figure 3 It is a schematic diagram of the cross-sectional structure of the mounting frame of the present invention from the left side; Figure 4 It is a schematic cross-sectional structure diagram of a microcrystal chamber and a preheating chamber of the present invention; Figure 5 It is a schematic diagram of the heating rod structure of the present invention; Figure 6 It is a schematic diagram of the structure of the cleaning component of the present invention; Figure 7 It is a bottom view structural schematic diagram of the cleaning assembly of the present invention; Figure 8 It is a schematic diagram of the structure of the lower arc-shaped brush of the present invention; Fig. 9 It is a schematic diagram of the connection structure of the T-shaped slide rail and the arc track of the present invention; Fig.10 It is a schematic diagram of the structure of the moving part of the present invention; Fig.11 It is a bottom view structural diagram of the moving part of the present invention; In the figure: 100, bracket; 101, first nut block; 102, screw rod; 103, mounting frame; 104, first hydraulic rod; 105, microcrystal chamber; 106, preheating chamber; 107, lifting platform; 108, bottom platform; 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 brush; 207, arc teeth; 208, first motor; 209, lower arc plate; 210, gear; 211, arc track; 212, lower arc 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 frame; 305, rotating motor. DETAILED DESCRIPTION

[0019] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0020] Embodiment 1 See also Figure 1-Figure 11 The present invention provides a technical solution: a method for preparing a transparent microcrystalline glass, comprising the following steps: S1. Place an ordinary glass sheet on the lifting platform 107 in the high-temperature furnace, and then drive the 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 bottom platform 108, the lifting platform 107 and the glass sheet to rise, and then the glass sheet enters the preheating chamber 106, and the heating rod 111 located in the preheating chamber 106 is turned on to preheat the glass sheet in the preheating chamber 106; S2, after the glass piece is preheated, the lifting rod located in the bottom platform 108 is turned on, and the lifting platform 107 is driven up by the working end of the lifting rod to drive the glass piece into the microcrystalline chamber 105, and the heating rod 111 located in the microcrystalline chamber 105 is turned on; S3, heating the glass sheet for microcrystallization treatment, and then lowering it into the microcrystallization chamber 105 through the lifting rod, repeating the steps for multiple times, setting the temperature of the microcrystallization chamber 105 to the annealing temperature, and cooling with the furnace, completing the microcrystallization treatment of the glass sheet; The raw materials of the glass sheet include, by mass percentage, 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 clarifier 0.2%.

[0021] 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 sheet. The inner walls of the preheating chamber 106 and the microcrystal chamber 105 are fixedly provided with multiple groups of bases 112. The microcrystal chamber 105 performs microcrystalization on the glass sheet. A heating rod 111 is fixedly provided on the top of the base 112. The preheating chamber 106 and the microcrystal chamber 105 can be heated by the heating rod 111. The tops of the preheating chamber 106 and the microcrystal chamber 105 are provided with a mounting frame 103. A concave slide rail 110 is slidably provided on the mounting frame 103. A baffle 109 is fixedly provided on the concave slide rail 110. A cleaning mechanism is provided on the top of the microcrystal chamber 105. The cleaning mechanism includes a cleaning component and a lifting component. The cleaning assembly includes an upper arc brush 206 and a lower arc brush 212 arranged on the outside of the heating rod 111, a lower arc plate 209 is fixedly arranged at the bottom of the lower arc brush 212, a T-shaped slide rail 213 is fixedly arranged on the outside of the upper arc brush 206, and the T-shaped slide rail 213 can slide in the arc track 211, a side of the upper arc brush 206 is provided with an arc track 211, and the end of the T-shaped slide rail 213 can penetrate into the interior of the arc track 211, a plurality of groups of connecting rods 214 are fixedly arranged between the lower arc brush 212 and the arc track 211, an arc tooth 207 is fixedly arranged on the top of the T-shaped slide rail 213, and a first motor 208 is fixedly arranged on the outside of the lower arc brush 212, and the upper arc brush 206 and the T-shaped slide rail 213 can be driven to rotate by the first motor 208, and a gear 210 is fixedly arranged on the working end of the first motor 208, and the gear 210 is meshed with the arc tooth 207.

[0022] Embodiment 2 Based on Example 1, please refer to Figure 1 , Figure 2 , Figure 4 , Figure 5 The lifting assembly includes a vertical hydraulic rod 200, a top frame 216 and four groups of concave frames 203. The vertical hydraulic rod 200 can drive the top frame 216 to move up and down. A horizontal bar 205 is fixed on the concave frame 203, and the lower arc plate 209 is fixed on the horizontal bar 205. The four ends of the top frame 216 are sleeved with an outer ring 204. The outer ring 204 can slide on the top frame 216 at will. A connecting block 217 is fixed between the outer ring 204 and the concave frame 203; A top column 215 is provided on the top of the top frame 216, and 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, and 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 through the L-shaped frame 202.

[0023] The present invention has a designed cleaning mechanism. When a lot of oxide layers are attached to the outer surface of the heating rod 111 in the high-temperature furnace during use, the vertical hydraulic rod 200 can be opened to make the top frame 216 descend into the microcrystalline chamber 105 in the high-temperature furnace. At this time, the first motor 208 is turned on to drive the T-shaped slide rail 213 outside the upper arc brush 206 to slide in the arc track 211, and then the upper arc brush 206 and the lower arc brush 212 surround the heating rod 111. The upper arc brush 206 and the lower arc brush 212 reciprocate up and down to remove the oxide layer on the heating rod 111 in the microcrystalline chamber 105. Then the T-shaped slide rail 213 on the upper arc brush 206 moves into the arc track 211, and then descends into the preheating chamber 106 through the vertical hydraulic rod 200, and the oxide layer on the heating rod 111 in the preheating chamber 106 is removed by the upper arc brush 206 and the lower arc brush 212.

[0024] During use, when the oxide layer on the heating rod 111 in the high-temperature furnace is to be removed, the baffle 109 located at the top of the microcrystal chamber 105 is opened by the driving action of the first hydraulic rod 104, and then the vertical hydraulic rod 200 is started, and the cleaning assembly and the top frame 216 and other structures are driven to move downward and enter the microcrystal chamber 105 by the action of the vertical hydraulic rod 200, and then the lower arc brush 212 surrounds the heating rod 111, and then the first motor 208 is started to drive the gear 210 to rotate, driving the arc gear 207 to rotate, and then the upper arc brush 206 and the T-shaped slide rail 213 to rotate, and at this time the T-shaped slide rail 213 located in the arc track 211 rotates and extends outward, driving the upper arc brush 206 to rotate and extend, and then the upper arc brush 206 can surround the portion of the heating rod 111 close to the inner wall of the microcrystal chamber 105, and at this time The upper arc brush 206 and the lower arc brush 212 can surround the heating rod 111, and then the vertical hydraulic rod 200 drives them to move up and down repeatedly to clean the heating rod 111 located in the microcrystal chamber 105. When the heating rod 111 in the microcrystal chamber 105 is cleaned, the T-shaped slide rail 213 in the upper arc brush 206 is rotated into the arc track 211 according to the above-mentioned reverse principle. At this time, the upper arc brush 206 of the heating rod 111 close to the inner wall of the microcrystal chamber 105 rotates to the position above the lower arc brush 212. At this time, the vertical hydraulic rod 200 can drive it to move downward and enter the preheating chamber 106, and then the upper arc brush 206 is unfolded, and the upper arc brush 206 and the lower arc 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.

[0025] Embodiment 3 Based on Example 2, please refer to Figure 1 , Figure 2 , Figure 3 , Figure 4 , Fig.10 and Fig.11The top frame 216 is provided with a driving member for moving the outer ring 204, and the driving member includes a mounting bearing 301 sleeved and fixed on the outside of the top column 215, and the rotating ring 300 can be supported by the mounting bearing 301, and the outer wall of the mounting bearing 301 is sleeved and fixed with the rotating ring 300, and a rotating motor 305 is fixedly provided on the top frame 216, and the rotating ring 300 can be driven to rotate by the rotating motor 305, and a driving wheel is fixedly provided on the working end of the rotating motor 305, and the outer wall of the driving wheel is in contact with the outer wall of the rotating ring 300; Four sets of rotating rods 302 are rotatably arranged on the top of the rotating ring 300, and a rotating column is rotatably arranged on the top of the connecting block 217. An arc frame 303 is arranged on the rotating column and the rotating rod 302. The rotating 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.

[0026] The present invention uses a designed driving member to drive the rotating ring 300 to rotate by rotating the motor 305, thereby driving the arc frame 303 to rotate, thereby driving the upper arc brush 206 and the lower arc brush 212 to move toward or away from the top frame 216, so that the upper arc brush 206 and the lower arc brush 212 can easily enter the preheating chamber 106 from the microcrystalline chamber 105, avoiding the situation where the upper arc brush 206 and the lower arc brush 212 about to enter the preheating chamber 106 are blocked by the base 112 in the microcrystalline chamber 105, and facilitating the removal of the oxide layer on the heating rod 111 located in the preheating chamber 106.

[0027] During use, after the upper arc brush 206 and the lower arc brush 212 have finished cleaning the heating rod 111 in the microcrystal chamber 105 and before entering the preheating chamber 106, the rotating motor 305 is started to drive the rotating ring 300 to rotate counterclockwise, and then the rotating ring 300 drives the arc frame 303 to rotate, thereby indirectly driving the upper arc brush 206, the lower arc brush 212 and other structures to move toward the top frame 216. At this time, the inner wall of the lower arc brush 212 no longer contacts the heating rod 111, and then it is lowered into the preheating chamber 106 under the action of the vertical hydraulic rod 200. At this time, the rotating motor 305 is reversed, so that the upper arc brush 206, the lower arc brush 212 and other structures extend away from the top frame 216, and then the inner wall of the lower arc brush 212 contacts the heating rod 111, and the oxide layer on the heating rod 111 is removed.

[0028] In this embodiment, a first hydraulic rod 104 is fixedly provided on the mounting frame 103, and the baffle 109 can be used to cover the top of the microcrystal chamber 105 or the position between the preheating chamber 106 and the microcrystal chamber 105 to facilitate preheating or microcrystallization treatment. The working end of the first hydraulic rod 104 is fixedly connected to the baffle 109.

[0029] In this embodiment, a moving part for lifting the glass piece is arranged on the bracket 100, and the moving part includes a lifting platform 107 and a base 108. Two sets of lifting rods are fixedly arranged on the base 108, and the working ends of the lifting rods are fixedly connected to the lifting platform 107. Two sets of screw rods 102 are rotatably arranged on the bracket 100, and the first nut block 101 rises or falls left and right with the rotating screw rod 102. When the glass piece located on 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 arranged on the outside of the screw rod 102, and a connecting frame is fixedly arranged between the first nut block 101 and the base 108. A rotating motor is provided at the top of the rod 102. The glass sheet can be preheated in the preheating chamber 106 through the screw rod 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 the preheating is completed, the baffle 109 at the top of the preheating chamber 106 is opened, and the glass sheet makes the lifting stage 107 rise through the lifting rod and drives the glass sheet into the microcrystalline chamber 105. At this time, the baffle 109 at the top of the microcrystalline chamber 105 is covered, and then the lifting stage 107 blocks the bottom of the microcrystalline chamber 105, and then the microcrystallization treatment of the glass sheet begins.

[0030] Embodiment 4 See also Figure 1-Figure 5 The present invention provides a technical solution: a method for preparing a transparent microcrystalline glass, comprising the following steps: (a) Weigh the following batch materials 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 clarifier 0.2%. Melt, homogenize and clarify the batch materials in a high-temperature heating furnace, cast them into shape, anneal them, cool them to room temperature with the furnace, and prepare 2 mm thick glass sheets, which are then cleaned and dried.

[0031] (b) The glass sheet prepared in (a) is placed in an ultra-micro-crystallization experimental device for ultra-micro-crystallization treatment. The ultra-micro-crystallization experimental device includes: a preheating chamber 106, a slow temperature section, a micro-crystallization chamber 105 and a lifting stage 107.

[0032] The preheating chamber 106, the slow temperature section, and the microcrystal chamber 105 are located in the same axis, so that they are connected up and down, and are used for the lifting stage 107 to move through; Ultra-microcrystallization process: put the glass sheet vertically into the lifting stage 107, and rise to the preheating chamber 106 for pretreatment. The temperature rise in the preheating chamber 106 is set to T1 (T1: starting crystallization temperature T1), keep warm for 5 minutes, and then move to the microcrystallization chamber 105 at a rising speed of v1. The temperature of the microcrystallization chamber 105 is set to T2 (T2: maximum crystallization temperature), and the treatment time is t: 10s. After the treatment is completed, move to the preheating chamber 106 at a descending speed of v2. After repeating the steps many times, set the temperature of the preheating chamber 106 to the annealing temperature and cool with the furnace. The temperature is set in the crystallization temperature range: T1-T2, and by adjusting the crystallization time at different temperatures, the crystal nucleation rate and grain growth rate can be effectively controlled.

[0033] The purpose of the present invention and the solution to its technical problems can be further achieved by adopting the following technical measures.

[0034] In step (a), the raw materials of the glass batch are: RO (MgO + CaO + ZnO) value is 3.5%, RO2 (ZrO2 + TiO2) value is 1.2%; In step (b), v1: 0.5 m / min, v2: 2 m / min; In step (b), the distance between the preheating chamber 106 and the microcrystal chamber 105 is H, H: 0.3 m; Embodiment 5 See also Figure 1-Figure 5 The present invention provides a technical solution: a method for preparing a transparent microcrystalline glass, comprising the following steps: (a) Weigh the following batch materials in percentage by mass: 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 clarifier 0.2%. Melt, homogenize and clarify the batch materials in a high-temperature heating furnace, cast them into shape, anneal them, cool them to room temperature with the furnace, prepare 2 mm thick glass sheets, wash them and dry them.

[0035] (b) The glass sheet prepared in (a) is placed in an ultra-micro-crystallization experimental device for ultra-micro-crystallization treatment. The ultra-micro-crystallization experimental device includes: a preheating chamber 106, a slow temperature section, a micro-crystallization chamber 105 and a lifting stage 107.

[0036] The preheating chamber 106, the slow temperature section, and the microcrystal chamber 105 are located in the same axis, so that they are connected up and down, and are used for the lifting stage 107 to move through; Ultra-microcrystallization process: put the glass sheet vertically into the lifting stage 107, and rise to the preheating chamber 106 for pretreatment. The temperature rise in the preheating chamber 106 is set to T1 (T1: starting crystallization temperature T1), keep warm for 2 minutes, and then move to the microcrystallization chamber 105 at a rising speed of v1. The temperature of the microcrystallization chamber 105 is set to T2 (T2: maximum crystallization temperature), and the treatment time is t: 45s. After the treatment is completed, move to the preheating chamber 106 at a descending speed of v2. After repeating the steps many times, set the temperature of the preheating chamber 106 to the annealing temperature and cool with the furnace. The temperature is set in the crystallization temperature range: T1-T2, and by adjusting the crystallization time at different temperatures, the crystal nucleation rate and grain growth rate can be effectively controlled.

[0037] The purpose of the present invention and the solution to its technical problems can be further achieved by adopting the following technical measures.

[0038] The raw materials of the glass batch in step (a) are: RO (MgO+CaO+ZnO) value is 4%, RO2 (ZrO2+TiO2) value is 1.0%; In step (b), v1: 0.8 m / min, v2: 1 m / min; In step (b), the distance between the preheating chamber 106 and the microcrystallization chamber 105 is H, H: 0.7m; Embodiment 6 See also Figure 1-Figure 5 The present invention provides a technical solution: a method for preparing a transparent microcrystalline glass, comprising the following steps: (a) Weigh the following batch materials 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 clarifier 0.2%. Melt, homogenize and clarify the batch materials in a high-temperature heating furnace, cast them into shape, anneal them, cool them to room temperature with the furnace, and prepare 2 mm thick glass sheets, which are then cleaned and dried.

[0039] (b) The glass sheet prepared in (a) is placed in an ultra-micro-crystallization experimental device for ultra-micro-crystallization treatment. The ultra-micro-crystallization experimental device includes: a preheating chamber 106, a slow temperature section, a micro-crystallization chamber 105 and a lifting stage 107.

[0040] The preheating chamber 106, the slow temperature section, and the microcrystal chamber 105 are located in the same axis, so that they are connected up and down, and are used for the lifting stage 107 to move through; Ultra-microcrystallization process: put the glass sheet vertically into the lifting stage 107, and rise to the preheating chamber 106 for pretreatment. The temperature rise in the preheating chamber 106 is set to T1 (T1: starting crystallization temperature T1), keep warm for 3 minutes, and then move to the microcrystallization chamber 105 at a rising speed of v1. The temperature of the microcrystallization chamber 105 is set to T2 (T2: maximum crystallization temperature), and the treatment time is t: 45s. After the treatment is completed, move to the preheating chamber 106 at a descending speed of v2. After repeating the steps many times, set the temperature of the preheating chamber 106 to the annealing temperature and cool with the furnace. The temperature is set in the crystallization temperature range: T1~T2, and by adjusting the crystallization time at different temperatures, the crystal nucleation rate and grain growth rate can be effectively controlled.

[0041] The purpose of the present invention and the solution to its technical problems can be further achieved by adopting the following technical measures.

[0042] In step (a), the raw materials of the glass batch are: RO (MgO + CaO + ZnO) value is 4.5%, RO2 (ZrO2 + TiO2) value is 0.8%; In step (b), v1: 1.2 m / min, v2: 2.5 m / min; In step (b), the distance between the preheating chamber 106 and the microcrystallization chamber 105 is H, H: 0.5 m; Embodiment 7 See also Figure 1-Figure 5 The present invention provides a technical solution: a method for preparing a transparent microcrystalline glass, comprising the following steps: (a) Weigh the following batch materials in percentage by mass: 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 clarifier 0.2%. Melt, homogenize and clarify the batch materials in a high-temperature heating furnace, cast them into shape, anneal them, cool them to room temperature with the furnace, and prepare 2 mm thick glass sheets, which are then cleaned and dried.

[0043] (b) The glass sheet prepared in (a) is placed in an ultra-micro-crystallization experimental device for ultra-micro-crystallization treatment. The ultra-micro-crystallization experimental device includes: a preheating chamber 106, a slow temperature section, a micro-crystallization chamber 105 and a lifting stage 107.

[0044] The preheating chamber 106, the slow temperature section, and the microcrystal chamber 105 are located in the same axis, so that they are connected up and down, and are used for the lifting stage 107 to move through; Ultra-microcrystallization process: put the glass sheet vertically into the lifting stage 107, and rise to the preheating chamber 106 for pretreatment. The temperature rise in the preheating chamber 106 is set to T1 (T1: starting crystallization temperature T1), keep warm for 3 minutes, and then move to the microcrystallization chamber 105 at a rising speed of v1: 2.0 m / min. The temperature of the microcrystallization chamber 105 is set to T2 (T2: maximum crystallization temperature), and the treatment time is t: 60s. After the treatment is completed, move to the preheating chamber 106 at a descending speed of v2: 3 m / min. After repeating the steps many times, set the temperature of the preheating chamber 106 to the annealing temperature and cool with the furnace. The temperature is set in the crystallization temperature range: T1~T2, and by adjusting the crystallization time at different temperatures, the crystal nucleation rate and grain growth rate can be effectively controlled.

[0045] The purpose of the present invention and the solution to its technical problems can be further achieved by adopting the following technical measures.

[0046] In step (a), the raw materials of the glass batch are: RO (MgO + CaO + ZnO) value is 5.6%, RO2 (ZrO2 + TiO2) value is 0.6%; In step (b), v1: 2 m / min, v2: 3 m / min; In step (b), the distance between the preheating chamber 106 and the microcrystallization chamber 105 is H, H: 1.0 m; Control group 1: The composition of the sample is the same as that of Example 1, and the batch raw materials are 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 clarifier 0.2%. The batch raw materials are melted, homogenized and clarified in a high-temperature furnace, cast into shape, and then annealed. The mixture is cooled to room temperature with the furnace, and then a 2 mm thick glass sheet is prepared, which is cleaned and dried.

[0047] The sample is processed in the preheating chamber 106 , the temperature rise in the preheating chamber 106 is set to T1 (T1: starting crystallization temperature T1), the processing time is the same as the total processing time of Example 2, and the processing is completed in the preheating chamber 106 .

[0048] Control group 2: The composition of the sample is the same as that of Example 1, and the batch raw materials are 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 clarifier 0.2%. The batch raw materials are melted, homogenized and clarified in a high-temperature furnace, cast into shape, and then annealed. The mixture is cooled to room temperature with the furnace, and then a 2 mm thick glass sheet is prepared, which is cleaned and dried.

[0049] The sample is processed in the preheating chamber 106 , the temperature rise in the preheating chamber 106 is set to T1 (T1: starting crystallization temperature T1), the processing time is the same as the total processing time of Example 2, and the processing is completed in the preheating chamber 106 .

[0050] Control group 3: (a) Weigh the following batch materials 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%; clarifier 0.2%, melt, homogenize and clarify the batch materials in a high-temperature furnace, cast and mold, anneal, cool to room temperature with the furnace, and prepare a 2 mm thick glass sheet, which is then cleaned and dried.

[0051] (b) The glass sheet prepared in (a) is placed in an ultra-micro-crystallization experimental device for ultra-micro-crystallization treatment. The ultra-micro-crystallization experimental device includes: a preheating chamber 106, a slow temperature section, a micro-crystallization chamber 105 and a lifting stage 107.

[0052] The preheating chamber 106, the slow temperature section, and the microcrystal chamber 105 are located in the same axis, so that they are connected up and down, and are used for the lifting stage 107 to move through; Ultra-microcrystallization treatment process: the glass sheet is placed vertically on 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: the starting crystallization temperature T1), and the temperature is kept for 3 minutes. The temperature of the preheating chamber 106 is set to the annealing temperature and cooled with the furnace.

[0053] The purpose of the present invention and the solution to its technical problems can be further achieved by adopting the following technical measures.

[0054] In step (a), the raw materials of the glass batch are: RO (MgO + CaO + ZnO) value is 4.5%, RO2 (ZrO2 + TiO2) value is 0.8%; In step (b), v1: 1.2 m / min, v2: 2.5 m / min; In step (b), the distance between the preheating chamber 106 and the microcrystallization chamber 105 is H, H: 0.5 m; According to the methods of Examples 5-7 and Comparative Groups 1-3, lithium silicate glasses were obtained respectively, and their performances were tested and compared with those of the control group. The processing conditions and test results are shown in Table 1 below: Table 1: Example process parameters and test performance The above embodiments are only used to illustrate the technical method of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical method of the present invention may be modified or replaced by equivalents without departing from the spirit and scope of the technical method of the present invention.

Claims

1. A method for preparing transparent microcrystalline glass, characterized in that: The following steps are involved: S1. Place an ordinary glass sheet on a lifting platform (107) in a high-temperature furnace, then drive the screw rod (102) to rotate by a rotary motor, thereby driving the first nut block (101) to move in an upward direction, and the first nut block (101) drives the bottom platform (108), the lifting platform (107) and the glass sheet to rise, and then the glass sheet enters a preheating chamber (106), and turns on a heating rod (111) in the preheating chamber (106) to preheat the glass sheet in the preheating chamber (106); S2, after the glass piece is preheated, the lifting rod located in the bottom platform (108) is turned on, and the lifting platform (107) is driven upward by the working end of the lifting rod to drive the glass piece into the microcrystalline chamber (105), and the heating rod (111) located in the microcrystalline chamber (105) is turned on; S3, heating the glass sheet for microcrystallization treatment, and then lowering it into the microcrystallization chamber (105) through the lifting rod. After repeating the steps for multiple times, the temperature of the microcrystallization chamber (105) is set to the annealing temperature, and the glass sheet is cooled with the furnace to complete the microcrystallization treatment of the glass sheet.

2. The method for preparing a transparent microcrystalline glass according to claim 1, characterized in that: The high-temperature furnace comprises a support (100), a preheating chamber (106) and a microcrystal chamber (105); the inner walls of the preheating chamber (106) and the microcrystal chamber (105) are fixedly provided with a plurality of groups of bases (112); the tops of the bases (112) are fixedly provided with heating rods (111); the tops of the preheating chamber (106) and the microcrystal chamber (105) are provided with mounting frames (103); the mounting frames (103) are slidably provided with concave slide rails (110); the concave slide rails (110) are fixedly provided with baffles (109); the top of the microcrystal chamber (105) is provided with a cleaning mechanism; the cleaning mechanism comprises a cleaning component and a lifting component; 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); a lower arc-shaped plate (209) is fixedly arranged at the bottom of the lower arc-shaped brush (212); a T-shaped slide rail (213) is fixedly arranged outside the upper arc-shaped brush (206); a curved track (211) is arranged on one side of the upper arc-shaped brush (206); and an end of the T-shaped slide rail (213) can be inserted into the curved track (211). A plurality of connecting rods (214) are fixedly arranged inside the lower arc-shaped brush (212) and the arc-shaped track (211), arc-shaped teeth (207) are fixedly arranged on the top of the T-shaped slide rail (213), a first motor (208) is fixedly arranged outside the lower arc-shaped brush (212), a gear (210) is fixedly arranged at the working end of the first motor (208), and the gear (210) is meshed with the arc-shaped teeth (207).

3. The method for preparing a transparent microcrystalline glass according to claim 2, characterized in that: The lifting assembly comprises a vertical hydraulic rod (200), a top frame (216) and four groups of concave frames (203); a horizontal bar (205) is fixedly provided on the concave frame (203); the lower arc-shaped plate (209) is fixed on the horizontal bar (205); the four ends of the top frame (216) are sleeved with an outer ring (204); and a connecting block (217) is fixedly provided between the outer ring (204) and the concave frame (203).

4. The method for preparing a transparent microcrystalline glass according to claim 3, characterized in that: A top column (215) is provided at the top of the top frame (216); a 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); and an L-shaped frame (202) is fixedly provided between the fixing ring (201) and the mounting frame (103).

5. The method for preparing a transparent microcrystalline glass according to claim 4, characterized in that: The top frame (216) is provided with a driving member for moving the outer ring (204), the driving member comprising a mounting bearing (301) sleeved and fixed on the outside of the top column (215), a rotating ring (300) sleeved and fixed on the outer wall of the mounting bearing (301), a rotating motor (305) is fixedly provided on the top frame (216), a driving wheel is fixedly provided on the working end of the rotating motor (305), and the outer wall of the driving wheel contacts the outer wall of the rotating ring (300).

6. The method for preparing a transparent glass-ceramic according to claim 5, characterized in that: Four groups of rotating rods (302) are rotatably provided at the top of the rotating ring (300), a rotating column is rotatably provided at the top of the connecting block (217), and an arc frame (303) is provided on the rotating column and the rotating rods (302).

7. The method for preparing a transparent glass-ceramic according to claim 2, characterized in that: A first hydraulic rod (104) is fixedly arranged on the mounting frame (103), and a working end of the first hydraulic rod (104) is fixedly connected to the baffle (109).

8. The method for preparing a transparent glass-ceramic according to claim 1, characterized in that: The support (100) is provided with a moving part for lifting the glass sheet, the moving part comprising a lifting platform (107) and a base (108), two groups of lifting rods are fixedly provided on the base (108), the working ends of the lifting rods are fixedly connected to the lifting platform (107), two groups of screw rods (102) are rotatably provided on the support (100), a first nut block (101) is provided outside the screw rod (102), a connecting frame is fixedly provided between the first nut block (101) and the base (108), and a rotating motor is provided on the top of the screw rod (102).

9. The method for preparing a transparent glass-ceramic according to claim 1, characterized in that: The raw materials of the glass sheet include, by mass percentage, 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 clarifier 0.2%.

10. A transparent microcrystalline glass, characterized in that: Prepared according to the method according to any one of claims 1 to 9.

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