Glass with improved toughness and preparation method thereof

Abstract

The invention discloses the technical field of layered materials, and relates to glass with improved toughness and a preparation method thereof. The preparation method comprises the following steps: providing a first glass substrate and a second glass substrate; a composite reinforcement layer material is provided and comprises a first stainless steel fiber layer, a first thin glass layer, a glass fiber layer, a second thin glass layer and a second stainless steel fiber layer which are sequentially stacked; sequentially stacking the first glass substrate, the composite reinforcement layer material and the second glass substrate to obtain a laminated body; the laminated body is put into a mold, hot-pressing fusion treatment is conducted on the laminated body, the glass is obtained, and hot-pressing fusion has two hot-pressing fusion stages. The glass disclosed by the invention is high in breaking strength, the breaking strength is basically kept unchanged at a high temperature, and the glass is simple in structure, simple in preparation process and low in cost.

Description

Technical Field

[0001] The present invention relates to the technical field of laminated materials, and particularly to a glass with improved toughness and a preparation method thereof. Background Art

[0002] A large number of glassware are required in chemical experiments. However, since glass is a brittle material, improving the toughness of glass is an important method to extend the service life of glassware.

[0003] Our company's previously authorized patent CN111572132B proposed a high-strength glass for laboratory glassware. However, during the manufacturing and use of the patented product, our company's researchers found the following problems: This type of glass is an anisotropic material, that is, when stresses are applied to the two surfaces of this type of glass, the mechanical property parameters of this type of glass are different. In other words, when a stress is applied to one surface of this type of glass, the strength of this type of glass is high, and when a stress is applied to the other surface, the strength of this type of glass is low. This causes users to often apply stress to the side with weaker mechanical properties due to mistakes when using flat glass products, resulting in glass breakage. In addition, there are limitations on the thickness relationships of the glass substrate, thin glass layer, and each fiber layer in this type of glass, which leads to a substantial increase in the manufacturing cost of the glass. In addition, our company found in the research that under high-temperature conditions, the flexural strength of this type of glass declines significantly, and this type of glass cannot be used in high-temperature chemical experiments. Summary of the Invention

[0004] The present invention provides a glass with improved toughness and a preparation method thereof. By using stainless steel fibers and glass fibers in combination, the layer structure of the present invention is greatly simplified compared with the prior art, and at the same time, the thickness relationships between the various layers of the glass of the present invention are greatly simplified, which reduces the production cost. In addition, the present invention adopts an improved two-stage hot pressing and fusing process, which greatly reduces the production cost and improves the production efficiency. Finally, the mechanical property decline of the glass prepared by the present invention at high temperatures is greatly slowed down.

[0005] The present invention provides a glass with improved toughness, characterized in that the glass is prepared by the following method:

[0006] Provide a first glass substrate and a second glass substrate;

[0007] Provide a composite reinforcement layer material, wherein the composite reinforcement layer material includes a first stainless steel fiber layer, a first thin glass layer, a glass fiber layer, a second thin glass layer, and a second stainless steel fiber layer stacked in sequence;

[0008] Stack the first glass substrate, the composite reinforcement layer material, and the second glass substrate in sequence to obtain a laminate;

[0009] Place the laminate in a mold and perform hot-pressing fusion treatment on the laminate to obtain glass, wherein the hot-pressing fusion has two hot-pressing fusion stages.

[0010] In a preferred embodiment, the first stainless steel fiber layer, the first thin glass layer, the glass fiber layer, the second thin glass layer, and the second stainless steel fiber layer have the same thickness.

[0011] In a preferred embodiment, the first glass substrate and the second glass substrate have the same thickness.

[0012] In a preferred embodiment, the hot-pressing fusion treatment is carried out in an argon atmosphere. The hot-pressing fusion treatment has a first hot-pressing fusion treatment stage and a second hot-pressing fusion treatment stage. Among them, the temperature of the first hot-pressing fusion treatment stage is 700 - 800 °C, the heat preservation time is 10 - 20 min, and the pressure is 15 - 25 MPa. The temperature of the second hot-pressing fusion treatment stage is 910 - 930 °C, the heat preservation time is 10 - 20 min, and the pressure is 25 - 30 MPa.

[0013] In a preferred embodiment, the total weight of the first glass substrate and the second glass substrate is the first weight, and the total weight of the first stainless steel fiber layer, the glass fiber layer, and the second stainless steel fiber layer is the second weight. Among them, the ratio of the first weight to the second weight is (15 - 20):1.

[0014] The present invention provides a method for preparing glass with improved toughness, characterized in that the method comprises:

[0015] Providing a first glass substrate and a second glass substrate;

[0016] Providing a composite reinforcement layer material, wherein the composite reinforcement layer material comprises a first stainless steel fiber layer, a first thin glass layer, a glass fiber layer, a second thin glass layer, and a second stainless steel fiber layer stacked in sequence;

[0017] Stacking the first glass substrate, the composite reinforcement layer material, and the second glass substrate in sequence to obtain a laminate;

[0018] Place the laminate in a mold and perform hot-pressing fusion treatment on the laminate to obtain glass, wherein the hot-pressing fusion has two hot-pressing fusion stages.

[0019] In a preferred embodiment, the first stainless steel fiber layer, the first thin glass layer, the glass fiber layer, the second thin glass layer, and the second stainless steel fiber layer have the same thickness.

[0020] In a preferred embodiment, the first glass substrate and the second glass substrate have the same thickness.

[0021] In a preferred embodiment, the hot pressing and fusing treatment is carried out in an argon atmosphere. The hot pressing and fusing treatment has a first hot pressing and fusing treatment stage and a second hot pressing and fusing treatment stage. Among them, the temperature in the first hot pressing and fusing treatment stage is 700 - 800 °C, the heat preservation time is 10 - 20 min, and the pressure is 15 - 25 MPa. The temperature in the second hot pressing and fusing treatment stage is 910 - 930 °C, the heat preservation time is 10 - 20 min, and the pressure is 25 - 30 MPa.

[0022] In a preferred embodiment, the total weight of the first glass substrate and the second glass substrate is the first weight, and the total weight of the first stainless steel fiber layer, the glass fiber layer, and the second stainless steel fiber layer is the second weight. Among them, the ratio of the first weight to the second weight is (15 - 20):1.

[0023] Compared with the prior art, the present invention has the following advantages. The present invention provides a glass with improved toughness and its preparation method. By using stainless steel fibers and glass fibers in combination, the layer structure of the present invention is greatly simplified compared with the prior art. At the same time, the thickness relationship between the layers of the glass of the present invention is greatly simplified, which reduces the production cost. In addition, the present invention adopts an improved two-stage hot pressing and fusing treatment, which greatly reduces the production cost and improves the production efficiency. Finally, the decline of the mechanical properties of the glass prepared by the present invention at high temperatures is greatly slowed down. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 is a schematic diagram of the glass layer structure of an embodiment of the present invention.

[0025] Figure 2 is a flowchart of the method of an embodiment of the present invention.

[0026] Figure 3 is a graph showing the change of the flexural strength of the glass prepared according to an embodiment with temperature.

[0027] Figure 4 is a graph showing the change of the flexural strength of the glass prepared according to another embodiment with temperature.

[0028] Figure 5 is a graph showing the change of the flexural strength of the glass prepared according to a comparative example with temperature.

[0029] Figure 6 is a graph showing the change of the flexural strength of the glass prepared according to another comparative example with temperature. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0030] The following will describe in detail the specific embodiments of the present invention with reference to the accompanying drawings. However, it should be understood that the protection scope of the present invention is not limited by the specific embodiments.

[0031] Figure 1 Schematic diagram of the glass layer structure of an embodiment of the present invention. As Figure 1 shown, the glass of the present invention sequentially includes a first glass substrate, a first stainless steel fiber layer, a first thin glass layer, a glass fiber layer, a second thin glass layer, a second stainless steel fiber layer, and a second glass substrate from top to bottom. Different from the prior art CN111572132B, the mechanical properties of the upper and lower surfaces of the glass of the present invention are consistent. Therefore, during use, it can be the first glass substrate facing outward (in the present invention, if the glass is made into a container for holding a solution, the direction in which the glass contacts the air is the outside; if the glass is made into a planar shape, the stress surface of the glass is the outside), or it can be the second glass substrate facing outward. While the prior art CN111572132B requires that the first glass substrate must face outward and the third glass substrate must face inward.

[0032] It should be pre-stated that since various laboratory utensils have inconsistent requirements for the glass thickness (some utensils require the glass thickness to be very thin, some utensils may require the glass thickness to reach 1 cm or even greater, and some laboratories also require the purchase of glass stirring rods, etc.), in order to cover these thickness ranges, the present application does not specifically limit the glass thickness, and the specific glass thickness needs to be adjusted according to customer requirements. Of course, the method of the present application is generally suitable for producing glass utensils with a relatively thick thickness, so that the characteristics of the present application can be fully exerted. The method of the present application has no special requirements for the glass composition, and it can be considered that the glass material used in the present application is the common glass material for ordinary laboratory glass utensils. For the comparability of the results, the examples and comparative examples of the present application both use the glass composition marked as AS1 in Section 3.1 of Chapter 3 of the reference document ("Research on the Structure and Properties of High-Strength and High-Modulus Glass", Ye Shiqian, Doctoral Thesis of Wuhan University of Technology) for experiments, and this glass can be directly purchased from the laboratory of Wuhan University of Technology. The flexural strength test method of the present invention refers to the reference document ("Research on the Structure and Properties of High-Strength and High-Modulus Glass", Ye Shiqian, Doctoral Thesis of Wuhan University of Technology). The alkali-free glass fiber used in the present invention is purchased from Toray Industries, Inc. of Japan, and the stainless steel fiber is purchased from Fujian Qianglun New Materials Co., Ltd.

[0033] Figure 2 is a flowchart of the method of an embodiment of the present invention. As shown in the figure, the method of the present invention includes the following steps:

[0034] Step 1: Provide a first glass substrate and a second glass substrate;

[0035] Step 2: Provide a composite reinforcement layer material, wherein the composite reinforcement layer material includes a first stainless steel fiber layer, a first thin glass layer, a glass fiber layer, a second thin glass layer, and a second stainless steel fiber layer stacked in sequence;

[0036] Step 3: Stack the first glass substrate, the composite reinforcement layer material, and the second glass substrate in sequence to obtain a laminate;

[0037] Step 4: Place the laminate into a mold and perform a hot pressing and fusing process on the laminate to obtain glass, wherein the hot pressing and fusing has two hot pressing and fusing stages.

[0038] Example 1

[0039] Glass is prepared through the following steps: Provide a first glass substrate and a second glass substrate; Provide a composite reinforcement layer material, wherein the composite reinforcement layer material includes a first stainless steel fiber layer, a first thin glass layer, a glass fiber layer, a second thin glass layer, and a second stainless steel fiber layer stacked in sequence; Stack the first glass substrate, the composite reinforcement layer material, and the second glass substrate in sequence to obtain a laminate; Place the laminate into a mold and perform a hot pressing and fusing process on the laminate to obtain glass, wherein the hot pressing and fusing has two hot pressing and fusing stages.

[0040] The first stainless steel fiber layer, the first thin glass layer, the glass fiber layer, the second thin glass layer, and the second stainless steel fiber layer have the same thickness.

[0041] The first glass substrate and the second glass substrate have the same thickness.

[0042] The hot pressing and fusing process is carried out in an argon atmosphere. The hot pressing and fusing process has a first hot pressing and fusing stage and a second hot pressing and fusing stage. Among them, the temperature of the first hot pressing and fusing stage is 700 °C, the heat preservation time is 10 min, the pressure is 15 MPa, the temperature of the second hot pressing and fusing stage is 910 °C, the heat preservation time is 10 min, and the pressure is 25 MPa.

[0043] The total weight of the first glass substrate and the second glass substrate is the first weight, and the total weight of the first stainless steel fiber layer, the glass fiber layer, and the second stainless steel fiber layer is the second weight. Among them, the ratio of the first weight to the second weight is 15:1. At room temperature, the flexural strength of Example 1 is 210 MPa. Compared with the prior art CN111572132B, the flexural strength has increased by about 5%. At the same time, the layer structure of the present invention is simpler than that of the prior art, and there is no strict and complex matching relationship between the thicknesses of each layer, which greatly reduces the manufacturing cost of the glass of the present invention. In addition, the special layer composition and layer structure of the present invention enable the present invention to adopt a two-stage short-time hot pressing and fusing process, which greatly improves the production efficiency of the glass of the present invention. A possible explanation for this result is that during the process of hot pressing and fusing to form a product, since the stainless steel fiber and the glass fiber are fibers with different compositions (the stainless steel fiber is a metal fiber, and the glass fiber is an inorganic non-metallic fiber), their wettabilities to the glass melt are different. After simulation by our researchers, the stainless steel fiber has better wettability to the glass melt. Therefore, the stainless steel fiber will attract the surrounding glass melt to form a firm contact interface with it. This phenomenon indirectly leads to a reduction in the glass melt near the glass fiber, which instead solves the problem of a large amount of glass melt accumulating around the glass fiber (a large amount of glass melt accumulating around the glass fiber during the hot pressing and fusing stage causes problems such as pores and defects, and the accumulation of the melt requires an extension of the hot pressing and fusing process). In short, through the layer structure design, the present invention forms a "gradient wetting" effect between the two fibers, which enables one fiber to quickly form a firm contact interface with the melt, and the other fiber, with the help of the previous fiber, can form a firm contact interface with the melt at a slower rate, which avoids the problem of melt accumulation, and thus avoids problems such as pores and defects. For the graph of the flexural strength of the glass prepared in Example 1 varying with temperature, see Figure 3 . As Figure 3 shown, below 260 °C, the flexural strength of the glass of the present invention remains almost unchanged. Only when the temperature is higher than 260 °C, the flexural strength decreases significantly. The glass of the present invention is more suitable for high-temperature chemical experiment applications. The reason for this result may be as follows: The interface between the glass fiber and the glass first undergoes slip under high-temperature action, but this slip is an endothermic reaction. Therefore, the interface slip between the glass fiber and the glass absorbs the nearby energy, which instead leads to insufficient driving force for the interface slip between the stainless steel fiber and the glass, which delays the interface slip between the stainless steel fiber and the glass, thereby maintaining the flexural strength of the glass.

[0044] Example 2

[0045] The glass is prepared through the following steps: providing a first glass substrate and a second glass substrate; providing a composite reinforcing layer material, wherein the composite reinforcing layer material includes a first stainless steel fiber layer, a first thin glass layer, a glass fiber layer, a second thin glass layer, and a second stainless steel fiber layer stacked in sequence; stacking the first glass substrate, the composite reinforcing layer material, and the second glass substrate in sequence to obtain a laminate; placing the laminate into a mold and performing a hot pressing and fusing treatment on the laminate to obtain the glass, wherein the hot pressing and fusing has two hot pressing and fusing stages.

[0046] The first stainless steel fiber layer, the first thin glass layer, the glass fiber layer, the second thin glass layer, and the second stainless steel fiber layer have the same thickness.

[0047] The first glass substrate and the second glass substrate have the same thickness.

[0048] The hot pressing and fusing treatment is carried out in an argon atmosphere. The hot pressing and fusing treatment has a first hot pressing and fusing treatment stage and a second hot pressing and fusing treatment stage. Among them, the temperature of the first hot pressing and fusing treatment stage is 800 °C, the heat preservation time is 20 min, and the pressure is 25 MPa. The temperature of the second hot pressing and fusing treatment stage is 930 °C, the heat preservation time is 20 min, and the pressure is 30 MPa.

[0049] The total weight of the first glass substrate and the second glass substrate is the first weight, and the total weight of the first stainless steel fiber layer, the glass fiber layer, and the second stainless steel fiber layer is the second weight. Among them, the ratio of the first weight to the second weight is 20:1. At room temperature, the flexural strength of Example 2 is 215 MPa. For the graph of the flexural strength of the glass prepared in Example 2 varying with temperature, see Figure 4 . As Figure 4 shown, the flexural strength of the glass of the present invention remains almost unchanged below 260 °C. Only when the temperature is higher than 260 °C does the flexural strength decrease significantly. The glass of the present invention is more suitable for high-temperature chemical experiment applications.

[0050] Example 3

[0051] The glass is prepared through the following steps: providing a first glass substrate and a second glass substrate; providing a composite reinforcing layer material, wherein the composite reinforcing layer material includes a first stainless steel fiber layer, a first thin glass layer, a glass fiber layer, a second thin glass layer, and a second stainless steel fiber layer stacked in sequence; stacking the first glass substrate, the composite reinforcing layer material, and the second glass substrate in sequence to obtain a laminate; placing the laminate into a mold and performing a hot pressing and fusing treatment on the laminate to obtain the glass, wherein the hot pressing and fusing has two hot pressing and fusing stages.

[0052] The first stainless steel fiber layer, the first thin glass layer, the glass fiber layer, the second thin glass layer, and the second stainless steel fiber layer have the same thickness.

[0053] The first glass substrate and the second glass substrate have the same thickness.

[0054] The hot pressing and fusing process is carried out in an argon atmosphere. The hot pressing and fusing process has a first hot pressing and fusing stage and a second hot pressing and fusing stage. Among them, the temperature of the first hot pressing and fusing stage is 750 °C, the heat preservation time is 15 min, the pressure is 20 MPa, the temperature of the second hot pressing and fusing stage is 920 °C, the heat preservation time is 15 min, and the pressure is 28 MPa.

[0055] The total weight of the first glass substrate and the second glass substrate is the first weight, and the total weight of the first stainless steel fiber layer, the glass fiber layer and the second stainless steel fiber layer is the second weight. Among them, the ratio of the first weight to the second weight is 18:1. At room temperature, the flexural strength of Example 3 is 212 MPa.

[0056] Comparative Example 1

[0057] Comparative Example 1 is Example 3 of the prior art CN111572132B. See the figure of the flexural strength of the glass prepared in Comparative Example 1 changing with temperature Figure 5 . As Figure 5 shown, the flexural strength of the glass in Comparative Example 1 begins to decline rapidly above 200 degrees Celsius, which makes the glass in Comparative Example 1 not suitable for high-temperature chemical experiments.

[0058] Comparative Example 2

[0059] The composite reinforcing layer material includes a first glass fiber layer, a first thin glass layer, a second glass fiber layer, a second thin glass layer and a third glass fiber layer stacked in sequence. The remaining parameters, processes and conditions are the same as those in Example 1. At room temperature, the flexural strength of Comparative Example 2 is 160 MPa.

[0060] Comparative Example 3

[0061] The composite reinforcing layer material includes a first stainless steel fiber layer, a first thin glass layer, a second stainless steel fiber layer, a second thin glass layer and a third stainless steel fiber layer stacked in sequence. The remaining parameters, processes and conditions are the same as those in Example 1. At room temperature, the flexural strength of Comparative Example 3 is 180 MPa. See the figure of the flexural strength of the glass prepared in Comparative Example 3 changing with temperature Figure 6 . As Figure 6 shown, the flexural strength of the glass in Comparative Example 3 begins to decline rapidly above 200 degrees Celsius.

[0062] Comparative Example 4

[0063] The composite reinforcing layer material includes a first copper fiber layer, a first thin glass layer, a glass fiber layer, a second thin glass layer, and a second copper fiber layer stacked in sequence. The remaining parameters, processes, and conditions are the same as those in Example 1. At room temperature, the flexural strength of Comparative Example 4 is 190 MPa. The reason for the result of Comparative Example 4 is that the difference in the wetting ability of the two fibers for glass should be within a suitable range. If the difference in wetting ability is too small or too large, the realization of the "gradient wetting" effect will be affected. Therefore, the mechanical properties of Comparative Example 4 are lower than those of Examples 1-3.

[0064] Comparative Example 5

[0065] The thickness of the first glass substrate is 10-20% larger than that of the second glass substrate. The remaining parameters, processes, and conditions are the same as those in Example 1. At room temperature, the flexural strength of Comparative Example 5 is 208 MPa.

[0066] Comparative Example 6

[0067] The hot pressing and fusing treatment is carried out in an argon atmosphere. The hot pressing and fusing treatment has a first hot pressing and fusing treatment stage and a second hot pressing and fusing treatment stage. Among them, the temperature of the first hot pressing and fusing treatment stage is 750 °C, the heat preservation time is 2 h, and the pressure is 20 MPa. The temperature of the second hot pressing and fusing treatment stage is 920 °C, the heat preservation time is 2 h, and the pressure is 28 MPa. The remaining parameters, processes, and conditions are the same as those in Example 1. At room temperature, the flexural strength of Comparative Example 6 is 167 MPa.

[0068] It should be understood that the above specific embodiments of the present invention are only used for exemplary illustration or explanation of the principle of the present invention, and do not constitute a limitation to the present invention. Therefore, any modifications, equivalent substitutions, improvements, etc. made without departing from the spirit and scope of the present invention shall be included within the protection scope of the present invention. In addition, the appended claims of the present invention are intended to cover all variations and modification examples falling within the scope and boundary of the appended claims, or equivalent forms of such scope and boundary.

Claims

1. A glass with improved toughness, characterized in that, The glass is prepared by the following method: Provide a first glass substrate and a second glass substrate; Provide a composite reinforcing layer material, wherein the composite reinforcing layer material includes a first stainless steel fiber layer, a first thin glass layer, a glass fiber layer, a second thin glass layer, and a second stainless steel fiber layer stacked in sequence; Stack the first glass substrate, the composite reinforcing layer material, and the second glass substrate in sequence to obtain a laminate; Place the laminate in a mold and perform a hot pressing and fusing treatment on the laminate to obtain the glass, wherein the hot pressing and fusing has two hot pressing and fusing stages.

2. The glass according to claim 1, wherein, The first stainless steel fiber layer, the first thin glass layer, the glass fiber layer, the second thin glass layer, and the second stainless steel fiber layer have the same thickness.

3. The glass according to claim 1, wherein, The first glass substrate and the second glass substrate have the same thickness.

4. The glass according to claim 1, wherein, The hot pressing and fusing treatment is carried out in an argon atmosphere. The hot pressing and fusing treatment has a first hot pressing and fusing treatment stage and a second hot pressing and fusing treatment stage. Among them, the temperature of the first hot pressing and fusing treatment stage is 700 - 800 °C, the heat preservation time is 10 - 20 min, the pressure is 15 - 25 MPa, the temperature of the second hot pressing and fusing treatment stage is 910 - 930 °C, the heat preservation time is 10 - 20 min, and the pressure is 25 - 30 MPa.

5. The glass according to claim 1, wherein, The total weight of the first glass substrate and the second glass substrate is the first weight, and the total weight of the first stainless steel fiber layer, the glass fiber layer, and the second stainless steel fiber layer is the second weight. Among them, the ratio of the first weight to the second weight is (15 - 20):

1.

6. A method for preparing glass with improved toughness, characterized in that, The method includes: Provide a first glass substrate and a second glass substrate; Provide a composite reinforcing layer material, wherein the composite reinforcing layer material includes a first stainless steel fiber layer, a first thin glass layer, a glass fiber layer, a second thin glass layer, and a second stainless steel fiber layer stacked in sequence; Stack the first glass substrate, the composite reinforcing layer material, and the second glass substrate in sequence to obtain a laminate; Place the laminate in a mold and perform a hot pressing and fusing treatment on the laminate to obtain the glass, wherein the hot pressing and fusing has two hot pressing and fusing stages.

7. The method according to claim 6, wherein, The first stainless steel fiber layer, the first thin glass layer, the glass fiber layer, the second thin glass layer, and the second stainless steel fiber layer have the same thickness.

8. The method according to claim 6, wherein The first glass substrate and the second glass substrate have the same thickness.

9. The method according to claim 6, wherein The hot pressing and fusing treatment is carried out in an argon atmosphere. The hot pressing and fusing treatment has a first hot pressing and fusing treatment stage and a second hot pressing and fusing treatment stage. Among them, the temperature of the first hot pressing and fusing treatment stage is 700 - 800 °C, the heat preservation time is 10 - 20 min, the pressure is 15 - 25 MPa, the temperature of the second hot pressing and fusing treatment stage is 910 - 930 °C, the heat preservation time is 10 - 20 min, and the pressure is 25 - 30 MPa.

10. The method according to claim 6, wherein, The total weight of the first glass substrate and the second glass substrate is the first weight, and the total weight of the first stainless steel fiber layer, the glass fiber layer, and the second stainless steel fiber layer is the second weight. Among them, the ratio of the first weight to the second weight is (15 - 20):1.

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