CN111423105A - A glass composite reinforcement device and method thereof - Google Patents

Abstract

The invention discloses a glass composite strengthening device and a method thereof. The device comprises a preheating unit, a dispersion strengthening unit, an ion exchange unit and a post-processing unit which are connected in sequence; and further comprises a preheating unit, a dispersion strengthening unit, an ion The control unit to which the exchange unit and the post-processing unit are connected. In the invention, nano-scale crystal grains are precipitated in the glass matrix through nucleation and crystallization to achieve dispersion strengthening; through the ion exchange unit, compressive stress is generated on the glass surface to achieve chemical toughening enhancement. The device and the method can effectively solve the continuous preparation of glass "dispersion strengthening + chemical tempering strengthening" composite reinforcement, which can significantly improve the glass reinforcement efficiency; at the same time, the process parameters can be adjusted and optimized according to the glass type to achieve multi-type glass composite reinforcement.

Description

A glass composite reinforcement device and method thereof

technical field

The invention relates to the technical field of glass processing, in particular to a glass composite reinforcing device and a method thereof.

Background technique

Glass strengthening methods mainly include physical tempering, chemical tempering and dispersion strengthening. Both physical tempering and chemical tempering are enhanced by compressive stress on the glass surface. Compared with physical tempering, chemical tempering is mainly aimed at special-shaped, small thickness (≤ 5mm), large size (≥1000×1000mm) glass products, and the glass must contain a certain amount (≥3wt.%) of Li ₂ O or Na ₂ O in order to achieve enhanced ion exchange with K ₂ O with a large ionic radius For this reason, chemical tempered glass is widely used in building curtain walls, aircraft and high-speed rail windshields, bulletproof windows and transparent plank roads.

With the improvement of the level of industrial equipment and the quality of people's life, traditional chemical tempered glass is difficult to meet high-end manufacturing, such as anti-drop mobile phone cover, high-end display and new bulletproof, etc., which puts forward higher requirements for glass strength.

SUMMARY OF THE INVENTION

The main purpose of the present invention is to provide a glass composite strengthening device and a method thereof. The technical problem to be solved is to break the drawback that the current glass dispersion strengthening process and chemical tempering strengthening process cannot be automatically connected, and develop a "dispersion strengthening + chemical tempering strengthening" composite Automated equipment to achieve continuous production and improve glass enhancement efficiency.

The purpose of the present invention and the solution to its technical problems are achieved by adopting the following technical solutions.

A glass composite strengthening device proposed according to the present invention includes a preheating unit, a dispersion strengthening unit, an ion exchange unit and a post-processing unit connected in sequence; it also includes a preheating unit, a dispersion strengthening unit, an ion exchange unit and a post-processing unit, respectively. the control unit to which the unit is connected;

The preheating unit includes a first transmission guide rail and a preheating furnace; the first transmission guide rail is located above the preheating furnace;

The dispersion strengthening unit includes a second transmission guide rail, a nucleation furnace, a crystallization furnace and a cooling furnace; the second transmission guide rail is located above the nucleation furnace, the crystallization furnace and the cooling furnace; the nucleation furnace and the preheating furnace The furnace is connected through an isolation valve; the crystallization furnace is located on the side of the nucleation furnace away from the preheating furnace, and is connected with the nucleation furnace through an isolation valve; the cooling furnace is located on the side of the crystallization furnace away from the nucleation furnace, and It is connected with the crystallization furnace through the isolation valve;

The ion exchange unit includes a third transmission guide rail, a heat-resistant stainless steel molten salt tank and an ion exchange furnace; the heat-resistant stainless steel molten salt tank is filled with molten salt, and the heat-resistant stainless steel molten salt tank is placed in the ion exchange furnace ;

The post-processing unit includes a fourth transmission guide rail, a heat-resistant stainless steel water tank, a post-processing furnace, an ultrasonic generator and a fan; the heat-resistant stainless steel water tank is filled with deionized water, and the heat-resistant stainless steel water tank is placed in the post-processing furnace ; The ultrasonic generator is located on the outside of the post-processing furnace and is symmetrically distributed; the blower is fixed on the top wall in the post-processing furnace.

Preferably, in the aforementioned glass composite strengthening device, the preheating unit, the dispersion strengthening unit, the ion exchange unit and the post-processing unit are all connected through an isolation valve.

Preferably, in the aforementioned glass composite strengthening device, the first transmission guide rail, the second transmission guide rail, the third transmission guide rail and the fourth transmission guide rail are connected in sequence to form a guide rail mechanism.

Preferably, the aforementioned glass composite strengthening device further comprises a resistance-resistant device that can be suspended below the guide rail mechanism and move along the directions of the first transmission guide rail, the second transmission guide rail, the third transmission guide rail and the fourth transmission guide rail. Hot tooling.

Preferably, in the aforementioned glass composite reinforcing device, at least eight running positioners are installed in the guide rail mechanism.

Preferably, in the aforementioned glass composite reinforcement device, the preheating furnace is composed of a heat-resistant stainless steel furnace shell, a heat insulating material, a heating element and a thermocouple, the heating element is a resistance wire, and the heating element is embedded in the heat insulating material , and is connected with the control unit; the thermocouple is inserted into the insulation material and connected with the control unit; the preheating furnace adopts a four-stage temperature control, with a gradient temperature distribution.

Preferably, in the aforementioned glass composite reinforcing device, a glass product is placed in the heat-resistant tooling, and the material of the heat-resistant tooling is titanium aluminum alloy.

Preferably, in the aforementioned glass composite strengthening device, wherein the nucleation furnace, the crystallization furnace and the cooling furnace all include a heat-resistant stainless steel furnace shell, a heat insulating material, a heating element and a thermocouple, and the heating element and the thermocouple are all connected with the control unit connection.

Preferably, in the aforementioned glass composite reinforcement device, the ion exchange furnace is composed of a heat-resistant stainless steel furnace shell, a heat insulating material, a heating element and a thermocouple, and the heating element is a resistance wire, which is embedded in the heat insulating material and is connected with the heat insulating material. The control unit is connected; the thermocouple is inserted into the insulation material and connected with the control unit.

Preferably, in the aforementioned glass composite reinforcing device, wherein the post-processing furnace is composed of a heat-resistant stainless steel furnace shell, a heat insulating material, a heating element and a thermocouple, and the heating element is a resistance wire, which is embedded in the heat insulating material and is connected with the heat insulating material. The control unit is connected; the thermocouple is inserted into the insulation material and connected with the control unit.

Preferably, in the aforementioned glass composite strengthening device, the control unit is an electronic display panel, which is connected with the guide rail, the heating element and the thermocouple.

The purpose of the present invention and the solution to its technical problems can be achieved by adopting the following technical solutions.

A glass composite strengthening method proposed according to the present invention includes:

1) Start the first transmission rail of the preheating unit, the second transmission rail of the dispersion strengthening unit and the third transmission rail of the ion exchange unit and the control unit;

2) After each unit rises to the set temperature, place the glass product in the heat-resistant tooling, and move it into the preheating unit through the first transmission guide rail;

3) When the glass product enters the dispersion strengthening unit, the control unit is used for timing, and it moves under the second transmission guide rail, and at the same time, the control unit ensures the nucleation and crystallization time of the glass product in the dispersion strengthening unit;

4) After the dispersion strengthening, the glass products enter the ion exchange unit through the third transmission guide rail for chemical strengthening treatment;

5) After the ion exchange, the glass product enters the post-processing unit through the fourth transmission guide rail, and is subjected to ultrasonic cleaning and blast drying in sequence;

6) After exiting the post-processing unit, the glass article is cooled to room temperature.

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

Preferably, in the aforementioned glass composite strengthening method, the preheating unit, the dispersion strengthening unit, the ion exchange unit and the post-processing unit are all heated by heating elements.

Preferably, in the aforementioned glass composite strengthening method, wherein the preheating unit adopts four-point temperature control, heating up, down, left, right and four sides, and the maximum heating temperature is higher than the glass transition point temperature and lower than its expansion softening point temperature by 30-50°C. Temperature distribution≤100℃/m.

Preferably, in the aforementioned glass composite strengthening method, wherein the heating temperature of the nucleation furnace of the dispersion strengthening unit is the same as the maximum temperature of the preheating unit, the temperature is controlled at three points on the upper and lower sides of the furnace body, and the temperature uniformity is ±1°C; The running speed of the second transmission rail is to ensure that the nucleation time is 1-3h.

Preferably, in the aforementioned glass composite strengthening method, the heating temperature of the crystallization furnace of the dispersion strengthening unit is 100-150°C higher than the heating temperature of the nucleation furnace, and the temperature of the upper and lower furnace body of the crystallization furnace is controlled at three points. The uniformity is ±1°C, and the crystallization time of the glass product is guaranteed to be 2-5h by controlling the running speed of the second transmission guide rail.

Preferably, the aforementioned glass composite strengthening method, wherein the heating temperature of the ion exchange unit is 380-440 ° C, the molten salt composition in the heat-resistant stainless steel molten salt tank is KNO ₃ and NaNO ₃ mixed salt, and CsNO ₃ is added to promote The temperature uniformity is ±2°C; the ion exchange time is 6-15h by controlling the running speed of the third transmission guide rail.

Preferably, the aforementioned glass composite strengthening method, wherein the weight ratio of KNO ₃ and NaNO ₃ in the KNO ₃ and NaNO ₃ mixed salt is x: (100-x), wherein 85<x<100; the CsNO ₃ promotes The added amount of the agent is less than or equal to 1% based on the weight of the mixed salt of KNO ₃ and NaNO ₃ .

Preferably, in the aforementioned glass composite strengthening method, the parameters of the ultrasonic cleaning in step 5) are set as follows: the temperature is 100°C, the time is 1-2h, and the ultrasonic frequency is 1000-2000KHz, so as to remove the residual molten salt on the glass surface thing.

With the above technical solutions, a glass composite reinforcing device and method thereof of the present invention have at least the following advantages:

1. The device of the present invention can realize the continuous preparation of "dispersion strengthening + chemical tempering strengthening" composite strengthening of glass, which can significantly improve the glass strengthening efficiency; at the same time, it can adjust and optimize the process parameters according to the glass species, so as to realize multi-variety glass. strengthen.

2. The method of the present invention effectively solves the temperature uniformity of the glass dispersion strengthening unit through the isolation valve and the upper and lower multi-point temperature control; accurately controls the nucleation and crystallization time of glass products through the guide rail mechanism and the running positioner , the synergy of the above measures ensures the precipitation of nanocrystalline grains with controllable size after dispersion strengthening of glass products.

3. The device and method of the present invention, through nucleation and crystallization, the nano-scale grains are precipitated in the glass matrix to achieve dispersion strengthening; through ion exchange, compressive stress is generated on the glass surface to achieve chemical toughening enhancement.

4. The device and method of the present invention not only improve the flexural strength of the glass (the flexural strength can be increased by 7-8 times), but also improve the microhardness of the glass (the microhardness can be increased by 10-20%).

The above description is only an overview of the technical solution of the present invention. In order to understand the technical means of the present invention more clearly, and implement it according to the content of the description, the preferred embodiments of the present invention are described in detail below with the accompanying drawings.

Description of drawings

FIG. 1 is a schematic structural diagram of a glass composite reinforcing device provided by an embodiment of the present invention.

1-preheating unit, 2-dispersion strengthening unit, 3-ion exchange unit, 4-post-processing unit, 5-control unit, 101-isolation valve, 102-glass products, 103-heat-resistant tooling, 104-thermocouple, 105-heating element, 106-rail mechanism, 107-preheating furnace; 201-isolation valve, 204-thermocouple, 205-heating element, 207-nuclearizing furnace, 208-crystallization furnace, 209-cooling furnace, 301- Isolation valve, 304-thermocouple, 305-heating element, 307-ion exchange furnace, 310-heat-resistant stainless steel molten salt tank, 401-isolation valve, 404-thermocouple, 405-heating element, 407-post-treatment furnace, 410 - Ultrasonic generator, 411- Heat-resistant stainless steel sink, 412- Positioner, 413- Fan.

Detailed ways

The above description is only an overview of the technical solution of the present invention. In order to understand the technical means of the present invention more clearly, and to implement according to the content of the description, the preferred embodiments of the present invention are described in detail below.

The present invention provides a glass composite strengthening device. As shown in FIG. 1 , the glass composite strengthening device includes a preheating unit 1 , a dispersion strengthening unit 2 , an ion exchange unit 3 and a post-processing unit 4 connected in sequence; The control unit 5 connected with the preheating unit 1, the dispersion strengthening unit 2, the ion exchange unit 3 and the post-processing unit 4;

The preheating unit 1 includes a first transmission guide rail, a preheating furnace 107 and an isolation valve 101; the first transmission guide rail is located above the preheating furnace 107, and the preheating furnace 107 is made of a heat-resistant stainless steel furnace shell, heat-insulating material. , a heating element 105 and a thermocouple 104, the heating element 105 is a resistance wire, the heating element 105 is embedded in the thermal insulation material, and is connected with the control unit; the thermocouple 104 is inserted into the thermal insulation material for monitoring the preheating The temperature of the hot furnace 107 is connected to the control unit 5; the preheating furnace 107 adopts a four-stage temperature control, and the temperature control is controlled by the thermocouple 104 and the control unit 5. The internal temperature is graded and used to preheat the glass article 102 for dispersion strengthening.

The dispersion strengthening unit 2 includes a second transmission guide rail, a nucleation furnace 207, a crystallization furnace 208 and a cooling furnace 209; the nucleation furnace 207 is connected to the preheating furnace 107, which is used to achieve nucleation of glass products. A large number of crystal nuclei are bred in the matrix; the crystallization furnace 208 is located on the side of the nucleation furnace 207 away from the preheating furnace 107, and is connected to the nucleation furnace 207 through the isolation valve 201, which is used to realize the crystallization of glass products and control the The crystal nucleus grows; the cooling furnace 209 is located on the side of the crystallization furnace 208 away from the nucleation furnace 207, and is connected to the crystallization furnace 208 through the isolation valve 201 to prevent the crystallization temperature and the ion exchange temperature from being greatly different and bursting . The nucleation furnace 207, the crystallization furnace 208 and the cooling furnace 209 all include a heat-resistant stainless steel furnace shell, a heat insulating material, a heating element 205 and a thermocouple 204, and they are all heated by the heating element 205 and the temperature of the thermocouple 204 is controlled. The heating element 205 and the thermocouple 204 are connected to the control unit 5 to control the temperature of the nucleating furnace 207, the crystallization furnace 208, the cooling furnace 209 and the residence time of the second transmission guide rail in each furnace body.

The ion exchange unit 3 includes a third transmission guide rail, a heat-resistant stainless steel molten salt tank 310 and an ion-exchange furnace 307; The heating element 305 is a resistance wire embedded in the heat insulating material and connected to the control unit 5 ; a thermocouple 304 is inserted into the heat insulating material for monitoring the temperature of the furnace body and connected to the control unit 5 . The heat-resistant stainless steel molten salt tank 310 is filled with molten salt, and the temperature of the molten salt is kept stable to ensure the quality of micro-crystallization; and the heat-resistant stainless steel molten salt tank 310 is placed in the ion exchange furnace 307, and the heat-resistant stainless steel molten salt tank 310 is The molten salt tank 310 is an important place for ion exchange of glass products.

The post-processing unit 4 includes a fourth transmission guide rail, a heat-resistant stainless steel water tank 411, a post-processing furnace 407, an ultrasonic generator 410, a fan 413 and an isolation valve 401; , a heating element 405, and a thermocouple 404, the heating element 405 is a resistance wire, which is embedded in the thermal insulation material and connected to the control unit 5; the thermocouple 404 is inserted into the thermal insulation material to monitor the temperature of the furnace body and connect The control unit 5 is connected. The heat-resistant stainless steel water tank 411 is filled with deionized water, and the heat-resistant stainless steel water tank 411 is placed in the post-processing furnace 407; the ultrasonic generator 410 is located outside the post-processing furnace 407, and is symmetrically distributed for ion exchange. The surface of the cleaned glass product is subjected to ultrasonic cleaning; the fan 413 is fixed on the top wall of the post-processing furnace 407 for fast drying of the cleaned glass product to prevent water marks from being left.

The preheating unit 1 , the dispersion strengthening unit 2 , the ion exchange unit 3 and the post-processing unit 4 are all connected by isolation valves to prevent heat exchange at the connection and ensure that the temperature fields of the units do not affect each other.

The first transmission guide rail, the second transmission guide rail, the third transmission guide rail and the fourth transmission guide rail are sequentially connected as a whole to form a guide rail mechanism 106 . The function of the guide rail mechanism 106 is to control the running speed and residence time of the heat-resistant tooling 103 in each unit.

The control unit 5 is an electronic display panel, which is connected with the guide rail mechanism 106 , heating elements and thermocouples of each unit, and intelligently controls the running speed and preheating temperature of the guide rail mechanism 106 . Isolation valves are located at both ends of each unit to isolate the heat flow between the units, prevent heat loss in the unit, and ensure the stability and uniformity of the temperature field of each unit; different units are connected by isolation valves.

The glass composite strengthening device also includes a heat-resistant tooling that can be suspended below the guide rail mechanism 106 and move along the directions of the first transmission guide rail, the second transmission guide rail, the third transmission guide rail and the fourth transmission guide rail 103. The guide rail mechanism 106 provides power for the heat-resistant tool 103 with glass products, and cooperates with the control unit 5 to adjust the running time of the heat-resistant tool 103 . The material of the heat-resistant tooling 103 is titanium aluminum alloy.

At least eight running positioners 412 are installed in the guide rail mechanism for controlling the running time of the heat-resistant tooling 103 in each unit.

As shown in FIG. 1, an embodiment of the present invention provides a glass composite strengthening method, including:

1) Start the first transmission guide rail of the preheating unit 1, the second transmission guide rail of the dispersion strengthening unit 2, the third transmission guide rail of the ion exchange unit 3 and the control unit 5;

2) After each unit reaches the set temperature, place the glass product 102 in the heat-resistant tooling 103, and move it into the preheating unit 1 through the first transmission guide rail;

3) After the glass product enters the dispersion strengthening unit 2, the control unit 5 is used to time the timing and move under the second transmission guide rail. At the same time, the control unit 5 ensures the nucleation and crystallization of the glass product 1 in the dispersion strengthening unit 2. time;

4) After the dispersion strengthening, the glass product enters the ion exchange unit 3 through the third transmission guide rail for chemical strengthening treatment;

5) After the ion exchange, the glass products enter the post-processing unit 4 through the fourth transmission guide rail, and are sequentially subjected to ultrasonic cleaning (temperature is 100°C, time is 1-2h, ultrasonic frequency is 1000-2000KHz) and blast drying (wind pressure). 1-10L/min) to remove the molten salt residue on the glass surface;

6) After exiting the post-processing unit 4, the glass article 102 is cooled to room temperature.

The preheating unit 1 , the dispersion strengthening unit 2 , the ion exchange unit 3 and the post-processing unit 4 are all heated by heating elements; the heating elements are resistance wires.

The preheating unit 1 adopts four-point temperature control, heating up, down, left, right and four sides. The maximum heating temperature should be higher than the glass transition point temperature and lower than its expansion softening point temperature by 30-50°C, and the gradient temperature distribution should be ≤100°C/m.

The heating temperature of the nucleation furnace of the dispersion strengthening unit 2 is the same as the maximum temperature of the preheating unit, and the temperature is controlled at three points on the upper and lower sides of the furnace body, and the temperature uniformity is ±1°C; by controlling the running speed of the second transmission guide rail to ensure the nucleation Chemical time 1-3h.

The heating temperature of the crystallization furnace 208 of the dispersion strengthening unit 2 is 100-150°C higher than the heating temperature of the nucleation furnace 209, and the temperature of the upper and lower furnace bodies of the crystallization furnace 208 is controlled at three points, and the temperature uniformity is ±1 ℃, by controlling the running speed of the second transmission guide rail to ensure that the crystallization time of the glass product is 2-5h.

The heating temperature of the ion exchange unit 3 is 380-440° C. The molten salt composition in the heat-resistant stainless steel molten salt tank 310 is KNO ₃ and NaNO ₃ mixed salt, plus CsNO ₃ accelerator, and the temperature uniformity is ±2° C. ; By controlling the running speed of the third transmission guide rail to ensure that the ion exchange time is 6-15h.

The weight ratio of KNO ₃ and NaNO ₃ in the KNO ₃ and NaNO ₃ mixed salt is x: (100-x), wherein 85<x<100; the addition amount of the CsNO ₃ accelerator is based on the KNO ₃ and NaNO 3 ₃ The weight of the mixed salt is less than or equal to 1%.

The flexural strength test of glass is based on "Test Method for Flexural Strength of Glass Materials" (JC/T676-1997); the glass microhardness test is based on "Standard Test Method for Microhardness of Materials" (ASTM 384-1999)

Example 1

The glass product of this embodiment adopts the following components by weight: 55% SiO ₂ ; 20% Al ₂ O ₃ ; 4% Li ₂ O; 10% Na ₂ O; 5% B ₂ O ₃ ; 5.5% ZnO and 0.5% Sb ₂ O ₃ glass, size 120×20×5mm, polished on all sides, free from defects such as bubbles, streaks and stones inside.

As shown in FIG. 1 , the first transmission guide rail of the preheating unit 1 , the second transmission guide rail of the dispersion strengthening unit 2 , the third transmission guide rail of the ion exchange unit 3 and the control unit are activated to heat each unit. The maximum temperature of the preheating unit 1 is set to 720°C, and the preheating time is 4h; the nucleation temperature of the dispersion strengthening unit 2 is 720°C, and the nucleation time is 2h; the crystallization temperature is 840°C, and the crystallization time is 2h; The temperature of the ion exchange unit 3 was 400° C., and the exchange time was 10 h.

After the preheating unit 1 and the dispersion strengthening unit 2 are raised to the set temperature, the glass product 102 is placed in the heat-resistant tool 103 and moved into the preheating unit 1 through the first guide rail. When the glass product enters the dispersion strengthening unit 2 , the positioning device 412 is used for timing, and moves under the guide rail, while the control unit 5 ensures the nucleation and crystallization time of the glass product in the dispersion strengthening unit 2 . After the dispersion strengthening is completed, the glass products pass through the isolation valve and enter the ion exchange unit 3 for chemical strengthening and strengthening, and the post-processing unit 4 is activated at the same time. Then the glass products enter the heat-resistant stainless steel water tank 411 for ultrasonic cleaning. The ultrasonic cleaning temperature is 100°C, the time is 1h, the ultrasonic frequency is 1000KHz, and finally it is dried by blasting (wind pressure 1L/min). The inspection of apparent quality shows that the appearance of the glass after composite reinforcement is not deformed, and the apparent quality is good. After testing, the flexural strength of the glass is 620MPa, and the microhardness is 652MPa.

Example 2

The glass product of this embodiment adopts the following components by weight: 72.5% SiO ₂ ; 10% Al ₂ O ₃ ; 15% Na ₂ O; 2% ZrO ₂ and 0.5% Sb ₂ O ₃ glass, with a size of 120 ×20×5mm, all surfaces are polished, and there are no defects such as bubbles, streaks and stones inside.

As shown in FIG. 1 , the first transmission guide rail of the preheating unit 1 , the second transmission guide rail of the dispersion strengthening unit 2 , the third transmission guide rail of the ion exchange unit 3 and the control unit 5 are activated to heat each unit. The maximum temperature of the preheating unit 1 is set to 700°C, and the preheating time is 2.5h; the nucleation temperature of the dispersion strengthening unit 2 is 700°C, and the nucleation time is 3h; the crystallization temperature is 800°C, and the crystallization time is 5h. ; The temperature of the ion exchange unit 3 is 380°C, and the exchange time is 15h.

After the preheating unit 1 and the dispersion strengthening unit 2 are raised to the set temperature, the glass product 102 is placed in a heat-resistant tool and moved into the preheating unit 1 through the guide rail. When the glass product enters the dispersion strengthening unit 2 , the positioning device 412 counts the time and moves under the guide rail mechanism, while the control unit 5 ensures the nucleation and crystallization time of the glass product in the dispersion strengthening unit 2 . After the dispersion strengthening is completed, the glass product passes through the isolation valve and enters the ion exchange unit for chemical strengthening and strengthening, and the post-processing unit 4 is activated at the same time. Then the glass products enter the heat-resistant stainless steel water tank 411 for ultrasonic cleaning. The ultrasonic cleaning temperature is 80°C, the time is 2h, the ultrasonic frequency is 2000KHz, and finally it is dried by blasting (wind pressure 10L/min). The inspection of apparent quality shows that the appearance of the glass after composite reinforcement is not deformed, and the apparent quality is good. After testing, the flexural strength of the glass is 540MPa, and the microhardness is 585MPa.

Example 3

The glass product of this embodiment adopts the following components by weight: 65% SiO ₂ ; 21.3% Al ₂ O ₃ ; 3.5% Li ₂ O; 0.5% MgO; 1.5% ZnO; 0.6% Na ₂ O; 0.5% K ₂ O; 2.5% BaO; 0.2% CaO; 2.3% TiO ₂ ; 1.6% ZrO ₂ and 0.5% Sb ₂ O ₃ glass, size 120 x 20 x 5 mm, polished on all sides, free of bubbles, streaks and stones inside and other defects.

As shown in FIG. 1 , the first transmission guide rail of the preheating unit 1 , the second transmission guide rail of the dispersion strengthening unit 2 , the third transmission guide rail of the ion exchange unit 3 and the control unit 5 are activated to heat each unit. The maximum temperature of the preheating unit 1 is set to 780°C, and the preheating time is 4h; the nucleation temperature of the dispersion strengthening unit 2 is 780°C, and the nucleation time is 1h; the crystallization temperature is 930°C, and the crystallization time is 2h; The temperature of the ion exchange unit 3 was 440°C, and the exchange time was 6h.

After the preheating unit 1 and the dispersion strengthening unit 2 are raised to the set temperature, the glass products are placed in the heat-resistant tooling and moved into the preheating unit 1 through the guide rail. When the glass product 102 enters the dispersion strengthening unit 2 , the positioning device 412 is used for timing, and moves under the guide rail, while the control unit 5 ensures the nucleation and crystallization time of the glass product in the dispersion strengthening unit 2 . After the dispersion strengthening is completed, the glass products pass through the isolation valve and enter the ion exchange unit 3 for chemical strengthening and strengthening, and the post-processing unit 4 is activated at the same time. Then the glass products enter the heat-resistant stainless steel water tank 411 for ultrasonic cleaning. The ultrasonic cleaning temperature is 90°C, the time is 1h, the ultrasonic frequency is 1500KHz, and finally it is dried by blasting (air pressure is 3L/min). The inspection of apparent quality shows that the appearance of the glass after composite reinforcement is not deformed, and the apparent quality is good. After testing, the flexural strength of the glass is 660MPa, and the microhardness is 664MPa.

Example 4

The glass product of this embodiment adopts the following components by weight: 55.5% SiO ₂ ; 25% Al ₂ O ₃ ; 4.1% Li ₂ O; 1% MgO; 1.5% ZnO; 5.4% P ₂ O ₅ ; 2.5% BaO; 2% TiO ₂ ; 2.5% ZrO ₂ and 0.5% Sb ₂ O ₃ glass, the size is 120×20×5mm, all surfaces are polished, and there are no internal defects such as bubbles, streaks and stones.

As shown in FIG. 1 , the first transmission guide rail of the preheating unit 1 , the second transmission guide rail of the dispersion strengthening unit 2 , the third transmission guide rail of the ion exchange unit 3 and the control unit 5 are activated to heat each unit. The maximum temperature of the preheating unit 1 is set to 700°C, and the preheating time is 2.5h; the nucleation temperature of the dispersion strengthening unit 2 is 700°C, and the nucleation time is 3h; the crystallization temperature is 800°C, and the crystallization time is 5h. ; The temperature of the ion exchange unit 3 is 420°C, and the exchange time is 9h.

After the preheating unit 1 and the dispersion strengthening unit 2 are raised to the set temperature, the glass product 102 is placed in a heat-resistant tool and moved into the preheating unit 1 through the guide rail. When the glass product 102 enters the dispersion strengthening unit 3 , the positioning device 412 is used for timing, and moves under the guide rail, while the control unit 5 ensures the nucleation and crystallization time of the glass product in the dispersion strengthening unit 2 . After the dispersion strengthening is completed, the glass products pass through the isolation valve and enter the ion exchange unit 3 for chemical strengthening and strengthening, and the post-processing unit 4 is activated at the same time. Then the glass products enter the heat-resistant stainless steel water tank 411 for ultrasonic cleaning. The ultrasonic cleaning temperature is 100°C, the time is 1h, the ultrasonic frequency is 2000KHz, and finally it is dried by blasting (wind pressure is 8L/min). The inspection of apparent quality shows that the appearance of the glass after composite reinforcement is not deformed, and the apparent quality is good. After testing, the flexural strength of the glass is 640MPa, and the microhardness is 676MPa.

Comparative Example 1

The glass product of this comparative example adopts the following components by weight: 55% SiO ₂ ; 20% Al ₂ O ₃ ; 4% Li ₂ O; 10% Na ₂ O; 5% B ₂ O ₃ ; 5.5% ZnO and 0.5% Sb ₂ O ₃ glass, size 120×20×5mm, polished on all sides, free from defects such as bubbles, streaks and stones inside.

As shown in FIG. 1 , the first transmission guide rail of the preheating unit 1 , the second transmission guide rail of the dispersion strengthening unit 2 , and the control unit 5 are activated to heat each unit. The maximum temperature of the preheating unit 1 was set to 720 °C, and the preheating time was 4 h; the nucleation temperature of the dispersion strengthening unit 2 was 720 °C, and the nucleation time was 2 h; the crystallization temperature was 840 °C, and the crystallization time was 2 h.

After the preheating unit 1 and the dispersion strengthening unit 2 are raised to the set temperature, the glass product is placed in the heat-resistant tooling 103 and moved into the preheating unit 1 through the first transmission guide rail. When the glass product enters the dispersion strengthening unit 2 , the positioning device 410 is used for timing, and moves under the guide rail mechanism, and the control unit 5 ensures the nucleation and crystallization time of the glass product in the dispersion strengthening unit 2 . After the dispersion strengthening is completed, the glass products pass through the isolation valve and enter the heat-resistant stainless steel water tank 411 of the post-processing unit 4 for ultrasonic cleaning. The ultrasonic cleaning temperature is 100 ° C, the time is 1 h, and the ultrasonic frequency is 1000 KHz. The wind pressure is 8L/min). The inspection of apparent quality shows that the appearance of the glass after composite reinforcement is not deformed, and the apparent quality is good. After testing, the glass has a flexural strength of 400 MPa and a microhardness of 582 MPa.

Comparative Example 2

The glass product of this comparative example adopts the following components by weight: 55% SiO ₂ ; 20% Al ₂ O ₃ ; 4% Li ₂ O; 10% Na ₂ O; 5% B ₂ O ₃ ; 5.5% ZnO and 0.5% Sb ₂ O ₃ glass, size 120×20×5mm, polished on all sides, free from defects such as bubbles, streaks and stones inside.

As shown in FIG. 1 , the first transmission guide rail of the preheating unit 1 , the second transmission guide rail of the dispersion strengthening unit 2 , the third transmission guide rail of the ion exchange unit 3 and the control unit 5 are activated to heat each unit. The maximum temperature of the preheating unit 1 is set to 400°C, and the preheating time is 4h; the nucleation temperature of the dispersion strengthening unit 2 is 720°C, and the nucleation time is 2h; the crystallization temperature is 840°C, and the crystallization time is 2h; The temperature of the ion exchange unit 3 was 400° C., and the exchange time was 10 h.

After the preheating unit 1 and the dispersion strengthening unit are raised to the set temperature, the glass product is placed in the heat-resistant tooling 103 and moved into the preheating unit 1 through the first transmission guide rail. After the glass products pass through the isolation valve and enter the ion exchange unit 3 for chemical toughening enhancement, the post-processing unit 4 is activated at the same time. Then the glass products enter the heat-resistant stainless steel water tank 411 of the post-processing unit 4 for ultrasonic cleaning. The ultrasonic cleaning temperature is 100°C, the time is 1h, the ultrasonic frequency is 1000KHz, and finally it is dried by blasting (air pressure is 8L/min), that is, Can. The inspection of apparent quality shows that the appearance of the glass after composite reinforcement is not deformed, and the apparent quality is good. After testing, the flexural strength of the glass is 520MPa, and the microhardness is 600MPa.

To sum up, in Example 1, after the composite reinforcement of "microcrystallization + chemical toughening", the flexural strength of the glass is increased by 7.29 times from 85MPa to 620MPa, and the microhardness is increased by 16% from 564MPa to 652MPa. In Example 2, after the composite reinforcement of "microcrystallization + chemical toughening", the flexural strength of the glass is increased by 7.1 times from 76MPa to 540MPa, and the microhardness is increased by 11% from 528MPa to 585MPa. In Example 3, after the composite reinforcement of "microcrystallization + chemical toughening", the flexural strength of the glass is increased from 88MPa, 7.5 times to 660MPa, and the microhardness is increased by 10% from 602MPa to 664MPa. In Example 4, after the composite reinforcement of "microcrystallization + chemical toughening", the flexural strength of the glass was increased by 7.8 times from 82MPa to 640MPa, and the microhardness was increased by 19.6% from 565MPa to 676MPa.

In Comparative Example 1 (compared to Example 1), the flexural strength of the glass was increased by 4.7 times from 85MPa to 400MPa after only microcrystallization was used, and the microhardness was increased by 3.2% from 564MPa to only 582MPa. In Comparative Example 2 (compared to Example 1), the flexural strength of the glass is increased by 6.1 times from 85MPa to 520MPa after only chemical toughening is used, and the microhardness is increased by 6.4% from 564MPa to only 600MPa.

It can be seen from the above data that the composite reinforcement of "dispersion strengthening + chemical tempering" of the present invention is more helpful for improving the flexural strength and microhardness of the glass than microcrystallization. After dispersion strengthening, a certain amount of nano-scale grains are controlled and precipitated from the glass matrix, and these grains are uniformly distributed in the glass, which can effectively improve the strength of the glass. Therefore, using the composite process of "dispersion strengthening + chemical tempering strengthening" can achieve two-step strengthening of glass, thereby significantly improving the strength of glass.

The above embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and the protection scope of the present invention is defined by the claims. Those skilled in the art can make various modifications or equivalent replacements to the present invention within the spirit and protection scope of the present invention, and such modifications or equivalent replacements should also be regarded as falling within the protection scope of the present invention.

Claims (10)

1. A glass composite strengthening device is characterized in that, comprising a preheating unit, a dispersion strengthening unit, an ion exchange unit and a post-processing unit connected in sequence; also include a preheating unit, a dispersion strengthening unit, an ion exchange unit and a post-processing unit respectively. The control unit to which the processing unit is connected; The preheating unit includes a first transmission guide rail and a preheating furnace; the first transmission guide rail is located above the preheating furnace; The dispersion strengthening unit includes a second transmission guide rail, a nucleation furnace, a crystallization furnace and a cooling furnace; the second transmission guide rail is located above the nucleation furnace, the crystallization furnace and the cooling furnace; the nucleation furnace and the preheating furnace The furnace is connected through an isolation valve; the crystallization furnace is located on the side of the nucleation furnace away from the preheating furnace, and is connected with the nucleation furnace through an isolation valve; the cooling furnace is located on the side of the crystallization furnace away from the nucleation furnace, and It is connected with the crystallization furnace through the isolation valve; The ion exchange unit includes a third transmission guide rail, a heat-resistant stainless steel molten salt tank and an ion exchange furnace; the heat-resistant stainless steel molten salt tank is filled with molten salt, and the heat-resistant stainless steel molten salt tank is placed in the ion exchange furnace ; The post-processing unit includes a fourth transmission guide rail, a heat-resistant stainless steel water tank, a post-processing furnace, an ultrasonic generator and a fan; the heat-resistant stainless steel water tank is filled with deionized water, and the heat-resistant stainless steel water tank is placed in the post-processing furnace ; The ultrasonic generator is located on the outside of the post-processing furnace and is symmetrically distributed; the blower is fixed on the top wall in the post-processing furnace. 2 . The glass composite strengthening device according to claim 1 , wherein the preheating unit, the dispersion strengthening unit, the ion exchange unit and the post-processing unit are all connected by an isolation valve; the first transmission guide rail, The second transmission guide rail, the third transmission guide rail and the fourth transmission guide rail are connected in sequence to form a guide rail mechanism. 3 . The glass composite strengthening device according to claim 2 , further comprising a device that can be suspended below the guide rail mechanism and along the first transmission guide rail, the second transmission guide rail, the third transmission guide rail and the fourth transmission guide rail. 4 . A heat-resistant tool that drives the directional movement of the guide rail; at least eight running positioners are installed in the guide rail mechanism. 4. The glass composite reinforcing device according to claim 1, wherein the preheating furnace is composed of a heat-resistant stainless steel furnace shell, a heat insulating material, a heating element and a thermocouple, the heating element is a resistance wire, and the heating element is a resistance wire. The heating element is embedded in the thermal insulation material and is connected with the control unit; the thermocouple is inserted into the thermal insulation material and connected with the control unit; the preheating furnace adopts a four-stage temperature control with a gradient temperature distribution. 5. The glass composite strengthening device according to claim 1, wherein the nucleation furnace, the crystallization furnace and the cooling furnace all comprise a heat-resistant stainless steel furnace shell, a heat insulating material, a heating element and a thermocouple, and the heating The element and the thermocouple are all connected to the control unit; the ion exchange furnace is composed of a heat-resistant stainless steel furnace shell, a thermal insulation material, a heating element and a thermocouple, and the heating element is a resistance wire, which is embedded in the thermal insulation material and is connected to the control unit. unit connection; the thermocouple is inserted into the thermal insulation material and connected to the control unit; the post-processing furnace is composed of a heat-resistant stainless steel furnace shell, thermal insulation material, a heating element and a thermocouple, the heating element is a resistance wire, which is inlaid In the heat preservation material, and connected with the control unit; the thermocouple is inserted into the heat preservation material and connected with the control unit; the control unit is an electronic display panel, and is connected with the guide rail, the heating element and the thermocouple. 6. A glass composite strengthening method, characterized in that, comprising the following steps: 1) Start the first transmission guide rail of the preheating unit, the second transmission guide rail of the dispersion strengthening unit and the third transmission guide rail of the ion exchange unit and the control unit; 2) After each unit rises to the set temperature, place the glass product in the heat-resistant tooling, and move it into the preheating unit through the first transmission guide rail; 3) When the glass product enters the dispersion strengthening unit, the control unit is used for timing, and it moves under the second transmission guide rail, and at the same time, the control unit ensures the nucleation and crystallization time of the glass product in the dispersion strengthening unit; 4) After the dispersion strengthening, the glass products enter the ion exchange unit through the third transmission guide rail for chemical strengthening treatment; 5) After the ion exchange, the glass product enters the post-processing unit through the fourth transmission guide rail, and is subjected to ultrasonic cleaning and blast drying in sequence; 6) After exiting the post-processing unit, the glass article is cooled to room temperature. 7 . The glass composite strengthening method according to claim 6 , wherein the preheating unit, the dispersion strengthening unit, the ion exchange unit and the post-processing unit are all heated by heating elements; the preheating unit adopts a four-point control The maximum heating temperature is higher than the glass transition point temperature and lower than its expansion softening point temperature by 30-50℃, and the gradient temperature distribution is less than or equal to 100℃/m. 8 . The glass composite strengthening method according to claim 7 , wherein the heating temperature of the nucleation furnace of the dispersion strengthening unit is the same as the maximum temperature of the preheating unit, and the temperature is controlled at three points on the upper and lower sides of the furnace body, and the temperature is uniform. 9 . is ±1°C; the nucleation time is 1-3h by controlling the running speed of the second transmission guide rail; the heating temperature of the crystallization furnace of the dispersion strengthening unit is 100-150°C higher than the heating temperature of the nucleation furnace, the crystallization The temperature is controlled at three points on the upper and lower sides of the furnace body, and the temperature uniformity is ±1°C. The crystallization time of the glass product is guaranteed to be 2-5h by controlling the running speed of the second transmission guide rail; the heating temperature of the ion exchange unit is 380-440 ℃, the molten salt composition in the heat-resistant stainless steel molten salt tank is KNO ₃ and NaNO ₃ mixed salt, plus CsNO ₃ accelerator, the temperature uniformity is ± 2 ℃; by controlling the running speed of the third transmission guide rail to Make sure the ion exchange time is 6-15h. 9. _The glass composite strengthening method according to claim ₈ , wherein the weight ratio _of KNO and NaNO in the KNO and NaNO mixed salt is x: (100 _- x), wherein 85<x<100; the added amount of the CsNO ₃ accelerator is less than or equal to 1% based on the weight of the KNO ₃ and NaNO ₃ mixed salt. 10. The glass composite strengthening method according to claim 6, wherein the parameters of the ultrasonic cleaning in step 5) are set as follows: the temperature is 100°C, the time is 1-2h, the ultrasonic frequency is 1000-2000KHz, and Remove molten salt residues from the glass surface.

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