Quartz crucible repair material and methods of making and using same

Abstract

This invention discloses a quartz crucible repair material, its preparation method, and its application method. The material is made from ultrafine quartz powder, kaolin, aluminum hydroxide, phosphoric acid, a naphthalene-based water-reducing agent, and water. In preparation, aluminum hydroxide and phosphoric acid are first heated to react and generate a transparent, viscous liquid of aluminum dihydrogen phosphate. Then, ultrafine quartz powder and kaolin are mixed evenly and poured into the viscous liquid. The pH of the system is then adjusted to 6.5-7.5. Finally, the naphthalene-based water-reducing agent and water are added, and the mixture is stirred into a thick paste and repeatedly kneaded to obtain the final product. In application, the material is applied to the area requiring repair and dried in an oven. It is then placed in a heating furnace for sintering, and finally cooled and removed to obtain a fully repaired crucible. The quartz crucible repair material of this invention has a scientifically sound composition, a simple and safe preparation process, and is easily implemented industrially, thus solving the problem of recycling and reusing damaged crucibles.

Description

Technical Field

[0001] This invention belongs to the field of crucible repair technology, specifically a quartz crucible repair material and its preparation and application methods. Background Technology

[0002] Crucibles, as common items in industrial production, have been rapidly promoted and popularized in industrial and experimental teaching fields since their invention due to their good refractoriness, high thermal stability, and readily available raw materials. However, because crucibles are exposed to extreme temperatures, dragging, and impacts in industrial production, they are prone to wear and cracks, which reduces their strength or renders them unusable. With the rapid development of industrial production, the number of broken crucibles is increasing.

[0003] Industrial crucibles are very large, and even minor damage can render them unusable, causing leaks in industrial products and leading to production accidents. Worn crucible material can easily fall into industrial products, affecting their purity.

[0004] The current method for dealing with broken crucibles is to discard them. A large number of broken crucibles accumulate, occupying ground resources. Even small breaks require the production of a new crucible, increasing carbon emissions. Repurchasing new crucibles also increases production costs.

[0005] Therefore, if the damaged crucibles can be repaired and used for a period of time, it can not only reduce the floor space occupied, but also reduce carbon emissions and financial expenditures. Summary of the Invention

[0006] The purpose of this invention is to address the problems existing in the prior art by providing a quartz crucible repair material, its preparation method, and its application method. The quartz crucible repair material of this invention has a scientifically sound composition, a simple and safe preparation process, and is easily implemented industrially, thus solving the problem of recycling and reusing damaged crucibles.

[0007] This invention is achieved through the following technical solution:

[0008] This invention provides a quartz crucible repair material, which is mainly made of the following raw materials in parts by weight: 40-50 parts of ultrafine quartz powder, 20-30 parts of kaolin, 1.5-2.0 parts of aluminum hydroxide, 5-7.5 parts of phosphoric acid, 2-3 parts of naphthalene-based water-reducing agent, and 16-20 parts of water.

[0009] The present invention also provides a method for preparing the above-mentioned quartz crucible repair material, comprising the following steps:

[0010] 1) Heating aluminum hydroxide and phosphoric acid produces a transparent, viscous liquid, aluminum dihydrogen phosphate;

[0011] 2) After mixing the ultrafine quartz powder and kaolin evenly, slowly pour the mixture into the liquid obtained in step 1) while stirring; then slowly add an appropriate amount of sodium hydroxide to adjust the pH value of the system to between 6.5 and 7.5; then add naphthalene-based water-reducing agent and water, and gradually stir until it becomes a thick paste. Knead the paste repeatedly to obtain the quartz crucible repair material.

[0012] The present invention also provides a method for using the above-mentioned quartz crucible repair material, comprising the following steps:

[0013] 1) Apply the quartz crucible repair material to the area of ​​the crucible that needs repair, then put it in an oven to dry. After taking it out, you will get an incompletely repaired crucible.

[0014] 2) Place the partially repaired crucible into a heating furnace, heat it to sinter, and then cool it down and remove it to obtain a fully repaired crucible.

[0015] Furthermore, in step 1) of the method, the drying temperature is 80℃. Comparative experiments show that the optimal drying temperature is 80℃. Because the quartz crucible and repair material are not fully fused, excessively high temperatures can easily cause secondary cracking during rapid heating, affecting the repair effect; excessively low temperatures result in low drying efficiency.

[0016] Furthermore, in step 1) of the method, the drying time is 720 min. Comparative experiments show that the optimal drying time is 720 min. The naphthalene-based water-reducing agent in the quartz crucible repair material has a certain water-retention effect. If the drying time is too short, moisture residue is likely to remain, which can easily cause cracks during rapid calcination in step 2). If the drying time is too long, the crucible repair material is likely to deform and energy will be wasted.

[0017] Furthermore, in step 2) of the method, the furnace temperature is raised to 1500℃. Comparative experiments show that the optimal sintering temperature is 1500℃. At 1500℃, aluminum dihydrogen phosphate can fuse and bond the ultrafine quartz powder and kaolin in the ceramic repair material with the quartz crucible matrix, forming a new dense body. Excessive temperature can easily affect the bonding properties of aluminum dihydrogen phosphate; excessively low temperature can affect the fusion effect between kaolin and the quartz crucible matrix.

[0018] Furthermore, in step 2) of the method, sintering is performed in the heating furnace for 20-30 minutes. Comparative experiments show that the optimal sintering time is 20-30 minutes. Sintering for 20-30 minutes ensures the fusion and bonding effect between the ultrafine quartz powder and kaolin and the quartz crucible matrix. If the time is too short, some repair areas may not bond completely, affecting the uniformity and density of the repair; if the time is too long, over-burning may occur, leading to local deformation of the repair area.

[0019] Furthermore, in step 2) of the method, the cooling process involves first mechanically cooling to 300°C, followed by natural cooling. Comparative experiments show that this method ensures the repaired area is smooth and dense, preventing crack formation. Excessive cooling can lead to uneven internal and external temperatures, resulting in greater thermal stress and increasing the risk of microcracks or even open cracking; conversely, excessively slow cooling affects repair efficiency.

[0020] Furthermore, in step 2) of the method of use, allow it to cool naturally to room temperature.

[0021] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0022] 1) The quartz crucible repair material of this invention can improve the recycling rate of crucibles. By forming a thick paste with a specific ratio of ultrafine quartz powder and kaolin, the viscosity is increased to repair cracks and damage to the crucible. The expansion coefficients of kaolin and ultrafine quartz powder are similar to those of the crucible, preventing detachment during post-repair use. The recycling of crucibles reduces carbon emissions and financial expenditure in crucible production.

[0023] 2) The present invention is first dried before use to prevent the crucible repair material from cracking.

[0024] 3) The present invention is subjected to high-temperature calcination during use, so that the crucible repair material and the crucible form a new dense body.

[0025] 4) This invention utilizes the adhesive effect of aluminum hydroxide and phosphoric acid to form a transparent and viscous liquid of aluminum dihydrogen phosphate, which avoids the crucible repair material from falling into powder after drying, making the crucible repair material easy to shape and adhere.

[0026] 5) This invention utilizes the high-temperature resistance properties of kaolin and ultrafine quartz powder to ensure that the repaired crucible remains resistant to high temperatures.

[0027] 6) This invention only requires mixing, drying and calcining the raw materials and then cooling and shaping them. The preparation process is simple, safe and reliable, easy to implement in industry, and can be widely promoted. Detailed Implementation

[0028] The technical solution of the present invention will be clearly and completely described below with reference to specific embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Example 1

[0029] A quartz crucible repair material is made from the following raw materials in parts by weight: 45g ultrafine quartz powder, 25g kaolin, 2.0g aluminum hydroxide, 7.5g phosphoric acid, 3g naphthalene-based water-reducing agent, and 20g water.

[0030] The preparation method of the above-mentioned quartz crucible repair material includes the following steps:

[0031] 1) 2.0g of aluminum hydroxide and 7.5g of phosphoric acid are heated to react and produce a transparent, viscous liquid of aluminum dihydrogen phosphate;

[0032] 2) Mix 45g of ultrafine quartz powder and 25g of kaolin evenly, and slowly pour the mixture into the liquid in step 1) while stirring. Then slowly add an appropriate amount of sodium hydroxide to adjust the pH of the system to between 6.5 and 7.5. Add 20g of water and 3g of naphthalene-based water-reducing agent, and gradually stir until it becomes a thick paste. Knead the paste repeatedly to obtain the quartz crucible repair material.

[0033] The method of using the above-mentioned quartz crucible repair material includes the following steps:

[0034] 1) Apply the quartz crucible repair material to the area of ​​the quartz crucible that needs repair, put it in an oven and dry it at 80°C for 720 minutes, then take it out to obtain an incompletely repaired quartz crucible;

[0035] 2) Place the partially repaired crucible into a heating furnace and heat it to 1500℃ for sintering for 20 minutes. Then cool it down to room temperature and remove it to obtain a fully repaired quartz crucible. Example 2

[0036] A quartz crucible repair material is made from the following raw materials in parts by weight: 40g of ultrafine quartz powder, 30g of kaolin, 1.5g of aluminum hydroxide, 5g of phosphoric acid, 2g of naphthalene-based water-reducing agent, and 16g of water.

[0037] The preparation method of the above-mentioned quartz crucible repair material includes the following steps:

[0038] 1) 1.5g of aluminum hydroxide and 5g of phosphoric acid are heated to react and produce a transparent, viscous liquid of aluminum dihydrogen phosphate;

[0039] 2) Mix 40g of ultrafine quartz powder and 30g of kaolin evenly, and slowly pour the mixture into the liquid in step 1) while stirring. Then slowly add an appropriate amount of sodium hydroxide to adjust the pH of the system to between 6.5 and 7.5. Then add 16g of water and 2g of naphthalene-based water-reducing agent, and gradually stir until it becomes a thick paste. Knead the paste repeatedly to obtain the quartz crucible repair material.

[0040] The method of using the above-mentioned quartz crucible repair material includes the following steps:

[0041] 1) Apply the quartz crucible repair material to the area of ​​the quartz crucible that needs repair, put it in an oven and dry it at 80°C for 720 minutes, then take it out to obtain an incompletely repaired quartz crucible;

[0042] 2) Place the partially repaired quartz crucible into a heating furnace and heat it to 1500℃ for sintering for 30 minutes. Then cool it down to room temperature and remove it to obtain a fully repaired quartz crucible. Example 3

[0043] A quartz crucible repair material is made from the following raw materials in parts by weight: 50g of ultrafine quartz powder, 20g of kaolin, 1.7g of aluminum hydroxide, 6.5g of phosphoric acid, 2.5g of naphthalene-based water-reducing agent, and 18g of water.

[0044] The preparation method of the above-mentioned quartz crucible repair material includes the following steps:

[0045] 1) 1.7g of aluminum hydroxide and 6.5g of phosphoric acid are heated to react and produce a transparent, viscous liquid of aluminum dihydrogen phosphate;

[0046] 2) Mix 50g of ultrafine quartz powder and 20g of kaolin evenly, and slowly pour the mixture into the liquid in step 1) while stirring. Then slowly add an appropriate amount of sodium hydroxide to adjust the pH of the system to between 6.5 and 7.5. Then add 18g of water and 2.5g of naphthalene-based water-reducing agent, and gradually stir until it becomes a thick paste. Knead the paste repeatedly to obtain the quartz crucible repair material.

[0047] The method of using the above-mentioned quartz crucible repair material includes the following steps:

[0048] 1) Apply the quartz crucible repair material to the area of ​​the quartz crucible that needs repair, put it in an oven and dry it at 80°C for 720 minutes, then take it out to obtain an incompletely repaired quartz crucible;

[0049] 2) Place the partially repaired quartz crucible into a heating furnace and heat it to 1500℃ for sintering for 30 minutes. Then cool it down to room temperature and remove it to obtain a fully repaired quartz crucible. Example 4

[0050] A quartz crucible repair material is made from the following raw materials in parts by weight: 42g of ultrafine quartz powder, 24g of kaolin, 1.6g of aluminum hydroxide, 5.5g of phosphoric acid, 2.1g of naphthalene-based water-reducing agent, and 17g of water.

[0051] The preparation method of the above-mentioned quartz crucible repair material includes the following steps:

[0052] 1) 1.6g of aluminum hydroxide and 5.5g of phosphoric acid are heated to react and produce a transparent, viscous liquid of aluminum dihydrogen phosphate;

[0053] 2) Mix 42g of ultrafine quartz powder and 24g of kaolin evenly, and slowly pour the mixture into the liquid in step 1) while stirring. Then slowly add an appropriate amount of sodium hydroxide to adjust the pH of the system to between 6.5 and 7.5. Then add 17g of water and 2.1g of naphthalene-based water-reducing agent, and gradually stir until it becomes a thick paste. Knead the paste repeatedly to obtain the quartz crucible repair material.

[0054] The method of using the above-mentioned quartz crucible repair material includes the following steps:

[0055] 1) Apply the quartz crucible repair material to the area of ​​the quartz crucible that needs repair, put it in an oven and dry it at 80°C for 720 minutes, then take it out to obtain an incompletely repaired quartz crucible;

[0056] 2) Place the partially repaired quartz crucible into a heating furnace and heat it to 1500℃ for sintering for 20 minutes. Then cool it down to room temperature and remove it to obtain a fully repaired quartz crucible. Example 5

[0057] A quartz crucible repair material is made from the following raw materials in parts by weight: 48g of ultrafine quartz powder, 26g of kaolin, 1.8g of aluminum hydroxide, 7g of phosphoric acid, 2.4g of naphthalene-based water-reducing agent, and 17g of water.

[0058] The preparation method of the above-mentioned quartz crucible repair material includes the following steps:

[0059] 1) 1.8g of aluminum hydroxide and 7g of phosphoric acid are heated to react and produce a transparent, viscous liquid of aluminum dihydrogen phosphate;

[0060] 2) Mix 48g of ultrafine quartz powder and 26g of kaolin evenly, and slowly pour the mixture into the liquid in step 1) while stirring. Then slowly add an appropriate amount of sodium hydroxide to adjust the pH of the system to between 6.5 and 7.5. Then add 17g of water and 2.4g of naphthalene-based water-reducing agent, and gradually stir until it becomes a thick paste. Knead the paste repeatedly to obtain the quartz crucible repair material.

[0061] The method of using the above-mentioned quartz crucible repair material includes the following steps:

[0062] 1) Apply the quartz crucible repair material to the area of ​​the quartz crucible that needs repair, put it in an oven and dry it at 80°C for 720 minutes, then take it out to obtain an incompletely repaired quartz crucible;

[0063] 2) Place the partially repaired quartz crucible into a heating furnace and heat it to 1500℃ for sintering for 20 minutes. Then cool it down to room temperature and remove it to obtain a fully repaired quartz crucible. Example 6

[0064] A quartz crucible repair material is made from the following raw materials in parts by weight: 49g of ultrafine quartz powder, 24g of kaolin, 1.8g of aluminum hydroxide, 7.2g of phosphoric acid, 2.8g of naphthalene-based water-reducing agent, and 19g of water.

[0065] The preparation method of the above-mentioned quartz crucible repair material includes the following steps:

[0066] 1) 1.8g of aluminum hydroxide and 7.2g of phosphoric acid are heated to react and produce a transparent, viscous liquid of aluminum dihydrogen phosphate;

[0067] 2) Mix 49g of ultrafine quartz powder and 24g of kaolin evenly, and slowly pour the mixture into the liquid in step 1) while stirring. Then slowly add an appropriate amount of sodium hydroxide to adjust the pH of the system to between 6.5 and 7.5. Then add 19g of water and 2.8g of naphthalene-based water-reducing agent, and gradually stir until it becomes a thick paste. Knead the paste repeatedly to obtain the quartz crucible repair material.

[0068] The method of using the above-mentioned quartz crucible repair material includes the following steps:

[0069] 1) Apply the quartz crucible repair material to the area of ​​the quartz crucible that needs repair, put it in an oven and dry it at 80°C for 720 minutes, then take it out to obtain an incompletely repaired quartz crucible;

[0070] 2) Place the partially repaired quartz crucible into a heating furnace and heat it to 1500℃ for sintering for 30 minutes. Then cool it down to room temperature and remove it to obtain a fully repaired quartz crucible. Example 7

[0071] A quartz crucible repair material is made from the following raw materials in parts by weight: 50g of ultrafine quartz powder, 27g of kaolin, 1.7g of aluminum hydroxide, 6g of phosphoric acid, 2g of naphthalene-based water-reducing agent, and 16.5g of water.

[0072] The preparation method of the above-mentioned quartz crucible repair material includes the following steps:

[0073] 1) 1.7g of aluminum hydroxide and 6g of phosphoric acid are heated to react and produce a transparent, viscous liquid of aluminum dihydrogen phosphate;

[0074] 2) Mix 50g of ultrafine quartz powder and 27g of kaolin evenly, and slowly pour the mixture into the liquid in step 1) while stirring. Then slowly add an appropriate amount of sodium hydroxide to adjust the pH of the system to between 6.5 and 7.5. Then add 16.5g of water and 2g of naphthalene-based water-reducing agent, and gradually stir until it becomes a thick paste. Knead the paste repeatedly to obtain the quartz crucible repair material.

[0075] The method of using the above-mentioned quartz crucible repair material includes the following steps:

[0076] 1) Apply the quartz crucible repair material to the area of ​​the quartz crucible that needs repair, put it in an oven and dry it at 80°C for 720 minutes, then take it out to obtain an incompletely repaired quartz crucible;

[0077] 2) Place the partially repaired quartz crucible into a heating furnace and heat it to 1500℃ for sintering for 30 minutes. Then cool it down to room temperature and remove it to obtain a fully repaired quartz crucible. Example 8

[0078] A quartz crucible repair material is made from the following raw materials in parts by weight: 46g of ultrafine quartz powder, 22g of kaolin, 1.9g of aluminum hydroxide, 7.3g of phosphoric acid, 2.2g of naphthalene-based water-reducing agent, and 16g of water.

[0079] The preparation method of the above-mentioned quartz crucible repair material includes the following steps:

[0080] 1) 1.9g of aluminum hydroxide and 7.3g of phosphoric acid are heated to react and produce a transparent, viscous liquid of aluminum dihydrogen phosphate;

[0081] 2) Mix 46g of ultrafine quartz powder and 22g of kaolin evenly, and slowly pour the mixture into the liquid in step 1) while stirring. Then slowly add an appropriate amount of sodium hydroxide to adjust the pH of the system to between 6.5 and 7.5. Then add 16g of water and 2.2g of naphthalene-based water-reducing agent, and gradually stir until it becomes a thick paste. Knead the paste repeatedly to obtain the quartz crucible repair material.

[0082] The method of using the above-mentioned quartz crucible repair material includes the following steps:

[0083] 1) Apply the quartz crucible repair material to the area of ​​the quartz crucible that needs repair, put it in an oven and dry it at 80°C for 720 minutes, then take it out to obtain an incompletely repaired quartz crucible;

[0084] 2) Place the partially repaired quartz crucible into a heating furnace and heat it to 1500℃ for sintering for 20 minutes. Then cool it down to room temperature and remove it to obtain a fully repaired quartz crucible.

[0085] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention, and they should all be covered within the scope of the claims and specification of the present invention.

Claims

1. A quartz crucible repair material, characterized in that, It is made from the following raw materials in parts by weight: 40-50 parts ultrafine quartz powder, 20-30 parts kaolin, 1.5-2.0 parts aluminum hydroxide, 5-7.5 parts phosphoric acid, 2-3 parts naphthalene-based water-reducing agent, and 16-20 parts water; The preparation method of the above-mentioned quartz crucible repair material includes the following steps: 1) Heating aluminum hydroxide and phosphoric acid produces a transparent, viscous liquid, aluminum dihydrogen phosphate; 2) After mixing the ultrafine quartz powder and kaolin evenly, slowly pour the mixture into the liquid obtained in step 1) while stirring; then slowly add an appropriate amount of sodium hydroxide to adjust the pH value of the system to between 6.5 and 7.5; then add naphthalene-based water-reducing agent and water, and gradually stir until it becomes a thick paste. Knead the paste repeatedly to obtain the quartz crucible repair material.

2. The method of using the quartz crucible repair material as described in claim 1, characterized in that, Includes the following steps: 1) Apply the quartz crucible repair material to the area of ​​the crucible that needs repair, and then put it in an oven to dry at 80°C for 720 minutes. After taking it out, you will get an incompletely repaired crucible. 2) Place the partially repaired crucible into a heating furnace and heat it to sinter. The furnace temperature is raised to 1500℃ and sintered for 20-30 minutes. Then, it is cooled down and removed to obtain a fully repaired crucible. The cooling process involves first mechanically cooling the crucible to 300℃ and then allowing it to cool naturally.

3. The method of using the quartz crucible repair material according to claim 2, characterized in that: Let it cool naturally to room temperature.