Adhesive applied to quartz product as well as preparation method and use method of adhesive

Abstract

The invention provides an adhesive applied to a quartz product as well as a preparation method and a use method of the adhesive. The adhesive comprises the following components in percentage by weight: 5-10% of glass powder; 55%-70% of silica sol; 3%-5% of silicate; the weight fraction of rare earth elements in the rare earth compound in the adhesive is 3%-25%; 10%-20% of a thickening agent; 3%-5% of a dispersant; and 1%-2% of a room temperature curing agent. According to the adhesive, rare earth elements are introduced, the component proportion is reasonable, the adhesive can tolerate a high-temperature environment, the adhesive not only has an extremely low thermal expansion coefficient, but also has better thermal shock resistance, excellent chemical stability and good corrosion resistance, and a more complex network structure is formed in the adhesive through the synergistic effect of all the components, so that the adhesive has a better heat insulation effect. The stability is improved, meanwhile, a certain shape memory function exists, slow self-repairing can be carried out through temperature rise when the quartz product is slightly damaged, and the service life of the quartz product is prolonged.

Description

Technical Field

[0001] The present invention relates to the technical field of bonding materials, and in particular to an adhesive applied to quartz products and a preparation method and a use method thereof. Background Art

[0002] In existing semiconductor processing, quartz boats and quartz boat holders are commonly used to transport silicon wafers. Currently, these boats and quartz boat holders are mostly manufactured by welding, which results in high production costs. Furthermore, due to the brittleness of quartz, they are easily bumped or damaged during processing, which is difficult to repair, further increasing costs.

[0003] Currently, quartz adhesives are available that can operate at high temperatures and have a low coefficient of thermal expansion, meeting the requirements of most quartz products. However, semiconductor processing experiences repeated temperature fluctuations, and the deposition process occurs under low pressure, using a large amount of chemical gases. These can deposit various chemical compounds on the surfaces of the quartz boat and adhesive, potentially corroding the adhesive or causing it to age and lose its adhesive properties, thereby reducing its performance and damaging the quartz product. Summary of the Invention

[0004] The purpose of the present invention is to address the shortcomings of the prior art and to propose an adhesive for quartz products, a preparation method thereof, and a use method thereof. The adhesive is added with rare earth elements and the component ratio is rationally designed, can withstand high temperature environments, not only has an extremely low thermal expansion coefficient, but also has good thermal shock resistance, excellent chemical stability and good corrosion resistance. The addition of rare earth elements can form a more complex network structure inside the adhesive, increase stability and have a certain shape memory function. When suffering minor damage, it can slowly self-repair by increasing the temperature. It can perfectly match the high temperature environment of quartz products in the semiconductor processing process, extend the service life of quartz products, and significantly reduce production costs and maintenance costs.

[0005] To achieve the above object, the present invention adopts the following technical solutions:

[0006] According to a first aspect of the present invention, there is provided an adhesive for use in quartz products, the adhesive comprising the following components in weight fractions:

[0007] Glass powder: 5% to 10%;

[0008] Silica sol: 55% to 70%;

[0009] Silicate: 3% to 5%;

[0010] A rare earth compound, wherein the weight fraction of the rare earth element in the rare earth compound in the adhesive is 3% to 25%;

[0011] Thickener: 10% to 20%;

[0012] Dispersant: 3% to 5%;

[0013] Room temperature curing agent: 1%~2%.

[0014] Preferably, the rare earth compound is one or more compounds containing yttrium, lanthanum, and cerium, and the weight of the yttrium element in the rare earth compound is 0 to 3 times the weight of the lanthanum element, and the weight of the cerium element is 0 to 3 times the weight of the lanthanum element.

[0015] Preferably, the weight fraction of the rare earth element in the rare earth compound in the adhesive may be in the range of 5% to 20%, and more preferably, in the range of 9% to 18%.

[0016] Preferably, the rare earth compound includes one or more of yttrium oxide, lanthanum oxide, and cerium oxide, and the average particle size of the rare earth compound is 1 to 5 μm; or, the rare earth compound includes one or more of yttrium acetate, lanthanum acetate, and cerium acetate.

[0017] Preferably, the rare earth compound includes one or more of yttrium oxide-cerium oxide composite oxide, lanthanum oxide-cerium oxide composite oxide, and yttria-stabilized zirconia.

[0018] Preferably, the glass powder comprises the following components in weight fractions: silicon oxide: 70% to 75%, aluminum oxide: 10% to 15%, zinc oxide: 5% to 10%, tellurium oxide: 3% to 5%, and alkaline earth metal oxide: 7% to 11%.

[0019] Preferably, the silica sol has a solid content of 20-30%, an average particle size of 10-20 nm, and a particle dispersion index of less than 0.2.

[0020] Preferably, the silicate is one or both of sodium silicate and potassium silicate.

[0021] Preferably, the thickener is one or both of carboxymethyl cellulose and sodium carboxymethyl cellulose. The dispersant is sodium polyacrylate. The room temperature curing agent includes one or both of benzoyl peroxide and azobisisobutyronitrile.

[0022] According to a second aspect of the present invention, there is provided a method for preparing the adhesive for use in quartz products as described above, the method comprising the following steps:

[0023] Step S1-1: weighing raw materials in proportion;

[0024] Step S1-2: adding glass powder and silicate to the silica sol, then adding a dispersant to fully dissolve, and stirring for 20 to 30 minutes to prepare a first mixture;

[0025] Step S1-3: adding the rare earth compound to the first mixture and stirring for 20 to 30 minutes to obtain a second mixture;

[0026] Step S1-4: adding a thickener to the second mixture to adjust the viscosity to obtain a third mixture;

[0027] Step S1-5: Add a room temperature curing agent to the third mixture and stir for 60 to 120 minutes to obtain an adhesive.

[0028] According to a third aspect of the present invention, there is provided a method for using the adhesive as described above for use on quartz products, the method comprising the following steps:

[0029] Step S2-1: Apply adhesive to the bonding surfaces of the quartz products to be bonded, align the bonding surfaces, and let them stand for 20 to 40 minutes to allow the adhesive to cure, thus completing the initial bonding;

[0030] Step S2-2: Place the preliminarily bonded quartz product into a high-temperature furnace, heat it to 900-1100°C at a rate of 8-15°C / min, and hold it for 120-240 minutes to allow the adhesive to sinter and bond to the quartz product.

[0031] Step S2-3: Take the quartz product out of the high-temperature furnace and cool it to room temperature.

[0032] Compared with the prior art, the present invention has the following beneficial effects: When the adhesive of the present invention is applied to quartz products, the silica sol undergoes a polycondensation reaction to form a silica-oxygen network, providing high tensile bond strength; the glass powder enhances temperature resistance through the silica-oxygen network, matching the thermal expansion coefficient of the quartz substrate and reducing interfacial thermal stress; the rare earth elements interact with the silica-oxygen bonds on the surface of the quartz substrate, forming a transition layer through chemical bonding, which strengthens the bonding between the adhesive and the quartz substrate. Furthermore, the introduction of the rare earth elements creates a more complex network structure within the adhesive, which increases stability and exhibits a certain shape memory function. The adhesive has an extremely low thermal expansion coefficient, good thermal shock resistance, excellent chemical stability, good corrosion resistance, and a certain self-repairing function. It can match the operating environment of quartz products in semiconductor processing, extend the service life of quartz products, and significantly reduce production and maintenance costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 The present invention is a flow chart of a method for preparing an adhesive for quartz products.

[0034] Figure 2 The present invention is a flowchart of a method for using an adhesive applied to quartz products. DETAILED DESCRIPTION

[0035] In order to make the purpose, technical solutions and advantages of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings of the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the described embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention. It is understood that in the absence of conflict, some technical means of the various embodiments described herein can be replaced or combined with each other.

[0036] In the description of the present invention, the terms "first," "second," etc., if used, are used solely to distinguish the objects being described and do not convey any order or technical meaning. Therefore, a term defined as "first," "second," etc. may explicitly or implicitly include one or more of such objects. Furthermore, "a," "an," and similar terms do not denote a limitation on quantity, but rather indicate the presence of at least one, and "plurality" means at least two.

[0037] In the description of the present invention, reference to "one embodiment" or "some embodiments" means that the particular features, structures, or characteristics described in conjunction with the embodiment are included in one or more embodiments of the present invention. Therefore, the phrases "in one embodiment," "in some embodiments," "in other embodiments," "in further embodiments," etc., appearing in different places in this specification do not necessarily refer to the same embodiment, but rather mean "one or more but not all embodiments," unless otherwise specifically emphasized.

[0038] According to a first aspect of the present invention, there is provided an adhesive for use in quartz products, the adhesive comprising the following components in weight fractions:

[0039] Glass powder: 5% to 10%;

[0040] Silica sol: 55% to 70%;

[0041] Silicate: 3% to 5%;

[0042] Rare earth compound, the weight fraction of the rare earth element in the rare earth compound in the adhesive is 3% to 25%;

[0043] Thickener: 10% to 20%;

[0044] Dispersant: 3% to 5%;

[0045] Room temperature curing agent: 1%~2%.

[0046] The preparation method of the above-mentioned adhesive includes: weighing raw materials in proportion; adding glass powder and silicate to silica sol, then adding a dispersant to fully dissolve, and stirring for 20 to 30 minutes to obtain a first mixture; adding a rare earth compound to the first mixture, stirring for 20 to 30 minutes, to obtain a second mixture; adding a thickener to the second mixture to adjust the viscosity, to obtain a third mixture; adding a room temperature curing agent to the third mixture, stirring for 60 to 120 minutes, to obtain an adhesive.

[0047] When the above adhesive is used in the bonding operation of quartz products, first, the adhesive is applied to the bonding surface of the quartz products to be bonded, the bonding surfaces are placed together, and the products are left to stand for 20 to 40 minutes to allow the adhesive to cure and complete the initial bonding; then, the quartz products after the initial bonding are sent to a high-temperature furnace, heated to 900 to 1100°C at a heating rate of 8 to 15°C / minute, and kept at this temperature for 120 to 240 minutes to allow the adhesive to sinter and form a bond with the quartz products; finally, the quartz products are removed from the high-temperature furnace and cooled to room temperature.

[0048] In this adhesive, the silica components of the silica sol and glass frit chemically bond to the quartz substrate, while rare earth elements strengthen the interface. The dispersant and thickener ensure a homogeneous structure, collectively achieving high bonding strength. Furthermore, the glass frit and rare earth elements regulate the coefficient of thermal expansion (CTE), while the silica sol network provides high-temperature stability and the rare earth elements stabilize the glass phase structure, synergistically resisting stress cracking caused by sudden temperature changes. As a result, this adhesive exhibits an extremely low CTE, along with good thermal shock resistance, excellent chemical stability, and good corrosion resistance. This makes it suitable for the operating environments of quartz products in semiconductor processing, extending their service life while reducing production costs.

[0049] Specifically, silica sol is a colloidal solution of nano-sized silica particles dispersed in water or a solvent. Upon curing, it forms a silica network, providing excellent adhesion and high-temperature resistance. The high silica sol content (55% to 70%) means that the adhesive forms a dense three-dimensional network structure upon curing. Its chemical similarity to the quartz substrate allows the two to be tightly bonded through chemical bonds, ensuring high bonding strength. The high melting point of silica (approximately 1700°C) imparts excellent high-temperature resistance to the adhesive, enabling it to resist structural damage from thermal shock. Furthermore, the high silica sol content ensures that the thermal expansion coefficients of the adhesive and quartz match, reducing thermal mismatch stress.

[0050] Glass powder enhances temperature resistance through a silica-oxygen network, matching the thermal expansion coefficient of the quartz substrate and reducing interfacial thermal stress. Rare earth elements interact with the silica bonds on the surface of the quartz substrate, forming a transition layer through chemical bonding. This strengthens the bond between the adhesive and the quartz substrate, achieving interfacial reinforcement. It also enhances the adhesive's antioxidant properties and chemical stability, making it more resistant to high temperatures and chemical corrosion. Thickeners adjust the adhesive's rheological properties, ensuring uniform application during application and avoiding stress concentrations caused by localized thickness variations. They also inhibit component settling during the curing process, maintaining structural uniformity and reducing weak interfaces caused by component segregation. Dispersants prevent agglomeration of particles such as glass powder and rare earth element additives, ensuring uniform distribution of components and a homogeneous cured structure, avoiding localized weaknesses. They also enhance the adhesive's storage stability, preventing delamination or precipitation that could affect performance. Room-temperature curing agents promote the gelation of the silica sol and the cross-linking reaction of the system, forming a high-density crosslinking network and increasing the stiffness and strength of the adhesive layer.

[0051] After testing, the adhesive was found to provide a shear strength of more than 8 MPa when applied to quartz products, exhibiting good bonding properties. It also performed well in heat shock resistance tests, maintaining a shear strength of more than 5 MPa after 10 rounds of 200°C to 800°C cyclic heat shock tests.

[0052] In some preferred embodiments, the glass frit comprises the following components by weight: silicon oxide (SiO2): 70%-75%, aluminum oxide (Al2O3): 10%-15%, zinc oxide (ZnO): 5%-10%, tellurium oxide: 3%-5%, and alkaline earth metal oxide: 7%-11%. Tellurium oxide is preferably tellurium dioxide (TeO2), whose core function is to adjust the thermal expansion coefficient and high-temperature stability of the glass phase, ensuring compatibility between the adhesive and the quartz substrate under thermal shock. Alkaline earth metal oxides include one or more of barium oxide (BaO), magnesium oxide (MgO), and calcium oxide (CaO).

[0053] Furthermore, in some embodiments, the glass powder includes the following components in weight fractions: silicon oxide (SiO2): 70% to 75%, aluminum oxide (Al2O3): 10% to 15%, zinc oxide (ZnO): 5% to 10%, tellurium dioxide (TeO2): 3% to 5%, barium oxide (BaO): 5% to 8%, magnesium oxide (MgO) + calcium oxide (CaO): 2% to 3%.

[0054] In the above-mentioned glass powder, silicon oxide is the main component, which is chemically compatible with the quartz substrate (SiO2), forming a strong interface bond through silicon-oxygen bonds, thereby improving the bonding strength. Aluminum oxide can increase the hardness and high temperature resistance of the glass phase, enhance the chemical stability and mechanical properties of the adhesive, inhibit high temperature softening, and reduce deformation under thermal stress. Zinc oxide can be used as a flux to lower the melting temperature of the glass powder, promote its fluidity during solidification, and improve wetting on the quartz surface. Barium oxide is used to adjust the thermal expansion coefficient to make it closer to quartz (low CTE, about 0.5×10 -6 / K), reducing interfacial stress caused by temperature fluctuations. Tellurium oxide optimizes the glass network structure, enhances high-temperature stability, and assists in adjusting the CTE. Alkaline earth metal oxides stabilize the glass structure, improve heat resistance, and inhibit phase separation at high temperatures.

[0055] In some preferred embodiments, the solid content of the silica sol (the weight fraction of silicon dioxide in the solution) is 20-30%, the average particle size is 10-20 nm, and the particle dispersion index (PDI) is less than 0.2.

[0056] The reasonable solid content in the silica sol ensures sufficient silica nanoparticle loading to form a dense network, while avoiding the difficulty of coating caused by excessive viscosity of the system. The three-dimensional network structure formed after curing is more complete and the mechanical strength is significantly improved. It can also reduce the volume shrinkage caused by water volatilization during the curing process, reduce interfacial stress, and prevent cracking or debonding of the adhesive layer. The specific surface area of ​​nano-scale particles is about 100 to 300 m 2 / g, fully penetrating the microscopic pores on the quartz substrate surface, creating a mechanical anchoring effect and enhancing interfacial bonding. The high surface activity of the nanoparticles promotes synergistic sintering with glass powder and rare earth elements, forming a uniform "glass-nanoceramic" composite structure in microscopic areas and enhancing thermal shock resistance. Excellent particle monodispersity avoids localized accumulation or defects caused by a wide particle size distribution, ensuring a uniform cured layer structure and stable mechanical properties.

[0057] In some preferred embodiments, the silicate is one or both of sodium silicate and potassium silicate. Silicate has excellent bonding properties, and it can synergize with silica sol to form a denser silica network structure, significantly improving the bonding strength and mechanical properties of the adhesive. The alkaline environment of the silicate can adjust the pH of the system, promote the gelation process of the silica sol, and dissolve some components in the glass powder (such as silicon oxide or metal oxide), releasing active ions to participate in the reaction, thereby enhancing the structural stability after curing. During the curing process, silicate forms water-insoluble silicon-oxygen bonds (Si-O-Si), giving the adhesive good water resistance and chemical corrosion resistance. In addition, after drying or curing, the silicate forms a glassy matrix, filling the pores in the adhesive layer, reducing stress concentration, and thus improving the impact resistance and durability of the adhesive.

[0058] In some preferred embodiments, the rare earth compound is one or more compounds containing yttrium (Y), lanthanum (La), and cerium (Ce), including but not limited to metal oxides, composite metal oxides or organometallic compounds, and the weight of the yttrium element in the rare earth compound is 0 to 3 times the weight of the lanthanum element, and the weight of the cerium element is 0 to 3 times the weight of the lanthanum element.

[0059] Yttrium enables the adhesive to form a more uniform and dense network structure during the curing process, improving its mechanical properties and increasing the contact area and bonding strength with the quartz glass, thereby enhancing the adhesive's bond strength. Yttrium also modulates the adhesive's thermal expansion coefficient to a certain extent, reducing internal stress caused by differential thermal expansion. Lanthanum improves the adhesive's chemical stability, enhancing its corrosion resistance and protecting the bonding interface from erosion. Cerium, with its unique electronic structure, interacts with the silicon-oxygen bonds on the quartz surface, forming a transition layer through chemical bonding, strengthening the adhesive's bond to the quartz glass and enhancing its antioxidant properties, resulting in improved high-temperature resistance. By adjusting the ratio of Y2O3, La2O3, and CeO2, precise matching of the adhesive's thermal expansion coefficient, high-temperature phase stability, multi-mechanism interface strengthening, and cross-scale optimization of thermal shock resistance can be achieved.

[0060] Specifically, La 3+ Larger ionic radius It can significantly reduce the thermal expansion coefficient of the glass phase. It forms [LaO6] polyhedrons with silicon dioxide, which can inhibit the high-temperature expansion of the silicon-oxygen network. 3+ Small ionic radius After introduction, it can form a more compact [YO4] tetrahedron, and cooperate with La2O3 to adjust the thermal expansion coefficient gradient, making the overall thermal expansion coefficient of the adhesive closer to that of quartz. 4+ / Ce 3+The variable valence property locally adjusts the oxygen vacancy concentration, dynamically compensating for thermal expansion fluctuations caused by temperature changes. The three functions synergistically to ensure a dynamic balance in the thermal expansion coefficient.

[0061] Y 3+ and La 3+ The formation of double rare earth ion barrier in the glass phase can inhibit the depolymerization of silicon-oxygen chains at high temperature and increase the softening point of glass from 800℃ to above 950℃. 4+ →Ce 3+ The reduction reaction absorbs oxygen free radicals, preventing the adhesive layer from becoming brittle due to oxidation. The synergistic combination of yttrium oxide, lanthanum oxide, and cerium oxide enables the adhesive to retain >85% of its bond strength after aging at 1000°C for 24 hours, achieving a synergistic enhancement of high-temperature phase stability.

[0062] In terms of strengthening the interface bonding strength, La 3+ It preferentially adsorbs on the defects of the quartz surface and forms La-O-Si bonds with silicon dioxide; Y 3+ CeO2 nanoparticles (especially partially reduced Ce2O3) can fill the nano-scale pores on the quartz surface and form a mechanical interlocking structure. 3+ The excess positive charge neutralizes the Si-O - Groups can reduce interfacial electrostatic repulsion and promote wetting.

[0063] In some embodiments, the rare earth compound includes yttrium oxide (Y2O3), lanthanum oxide (La2O3), and cerium oxide (CeO2), wherein the weight ratio of yttrium, lanthanum, and cerium is (0.5-3):1:(0.5-3). During the adhesive preparation process, in order to obtain the rare earth compound of the desired fineness, it is necessary to first weigh yttrium oxide (Y2O3), lanthanum oxide (La2O3), and cerium oxide (CeO2) in proportion, then add the weighed rare earth compound to deionized water, with the weight ratio of deionized water to rare earth compound being (2-4:1), and then use a ball mill to perform ball milling; after drying, a second ball milling is performed to obtain the rare earth compound of the desired fineness. The average particle size of the obtained rare earth compound is 1-5 μm, which gives the rare earth compound a large specific surface area, can improve the bonding strength of the compound with other components, and enhance the density and impact resistance of the adhesive.

[0064] Preferably, the weight ratio of yttrium: lanthanum: cerium in the rare earth compound is 1:1:1.

[0065] In other embodiments, the rare earth compound includes yttrium acetate (Y(C2H3O2)3), lanthanum acetate (La(CH3COO)3) and cerium acetate (Ce(C2H3O2)3), and the weight ratio of yttrium, lanthanum and cerium is (0.5~3):1:(0.5~3).

[0066] In some other embodiments, the rare earth compound includes yttrium oxide-cerium oxide composite oxide, lanthanum oxide-cerium oxide composite oxide, and yttria-stabilized zirconia (YSZ), wherein the weight ratio of yttrium, lanthanum, and cerium is (0.5-3):1:(0.5-3). Preferably, the mole fraction of Y2O3 in YSZ is 8%. During the adhesive preparation process, to obtain the rare earth compound of the desired fineness, it is necessary to first weigh the yttrium oxide-cerium oxide composite oxide, lanthanum oxide-cerium oxide composite oxide, and yttria-stabilized zirconia in proportion. The weighed rare earth compound is then added to deionized water in a weight ratio of (2-4):1, and ball milled using a ball mill. After drying, the mixture is ball milled again to obtain the rare earth compound of the desired fineness.

[0067] Y from Y2O3 and YSZ 3+ Simultaneously bonding the Si-O-groups on the quartz surface and the Zr-O network in YSZ to form a YO-Si and YO-Zr double-interface bridging structure. La2O3 preferentially migrates to the quartz interface and reacts with SiO2 to form a La2Si2O7 layer, achieving chemical anchoring. YSZ is preferably in the form of rod-shaped or flake-shaped particles (aspect ratio>5), which can be mechanically inserted into the microcracks on the quartz surface to form a "claw" type anchoring, thereby increasing shear strength. The Y2O3 in YSZ stabilizes the high-temperature cubic zirconia (c-ZrO2) to room temperature, and triggers the martensitic phase transformation of t-ZrO2→monoclinic phase (m-ZrO2) under stress (such as thermal stress), accompanied by a 3-5% volume expansion, squeezing the crack tip and inhibiting crack propagation. Doping with La2O3 and CeO2 can adjust the phase transition temperature of YSZ (lowering the critical stress for the t→m phase transition), extending the toughening effect across a wider temperature range (-100°C to 800°C), making it particularly suitable for thermal shock environments in quartz products. The La / Ce-rich transition layer formed around the YSZ particles (through ion diffusion) can gradient CTE differences and reduce interfacial thermal stress concentration.

[0068] By introducing YSZ and adjusting the ratio, the adhesive can better match the thermal expansion coefficient of quartz, extend the high-temperature service life of quartz products, and have high thermal shock resistance and corrosion resistance. It is especially suitable for bonding quartz components in extreme environments such as semiconductor high-temperature reaction chambers.

[0069] In some preferred embodiments, the thickener is one or both of carboxymethyl cellulose and sodium carboxymethyl cellulose. The thickener is used to adjust the rheological properties of the adhesive, ensuring uniform application during application and avoiding stress concentration caused by localized thickness variations. Furthermore, the thickener can inhibit component sedimentation during the curing process, maintaining structural uniformity and reducing weak interfaces caused by component segregation.

[0070] In some preferred embodiments, the dispersant is sodium polyacrylate. Dispersants can prevent agglomeration of particles such as glass powder and rare earth element additives, ensuring even distribution of components and forming a homogeneous cured structure, avoiding localized weaknesses. Dispersants can also improve the storage stability of the adhesive, preventing delamination or precipitation that could affect performance.

[0071] In some preferred embodiments, the room temperature curing agent includes one or both of benzoyl peroxide and azobisisobutyronitrile. The room temperature curing agent is used to promote the gelation of the silica sol and the cross-linking reaction of the system, forming a high cross-linking density network, and improving the rigidity and strength of the adhesive layer.

[0072] According to a second aspect of the present invention, a method for preparing the adhesive for quartz products as described above is provided, referring to Figure 1 , the preparation method comprises the following steps:

[0073] Step S1-1: Weigh the raw materials in proportion; wherein the weight fraction of each component is: glass powder: 5% to 10%; silica sol: 55% to 70%; silicate: 3% to 5%; rare earth compound, the weight fraction of the rare earth element in the rare earth compound in the adhesive is 3% to 25%; thickener: 10% to 20%; dispersant: 3% to 5%; room temperature curing agent: 1% to 2%.

[0074] Step S1-2: adding glass powder and silicate to the silica sol, then adding a dispersant to fully dissolve, and stirring for 20 to 30 minutes to prepare a first mixture;

[0075] Step S1-3: adding the rare earth compound to the first mixture and stirring for 20 to 30 minutes to obtain a second mixture;

[0076] Step S1-4: adding a thickener to the second mixture to adjust the viscosity to obtain a third mixture;

[0077] Step S1-5: Add a room temperature curing agent to the third mixture and stir for 60 to 120 minutes to obtain an adhesive.

[0078] In the above preparation method, the raw materials are mixed in stages and kept warm continuously to ensure that the glass powder is fully dissolved in the silica sol and to avoid gelation of the silica sol caused by high temperature; the dispersant and mechanical stirring work synergistically to significantly improve the dispersion of the glass powder in the silica sol, reduce interface defects, and improve the density and shear strength of the bonding layer.

[0079] The adhesive prepared by the above method is applied to quartz products. The silica sol forms a silicon-oxygen network through a condensation reaction, providing high tensile bonding strength; the glass powder enhances temperature resistance through the silicon-oxygen network, matches the thermal expansion coefficient of the quartz matrix, and reduces interfacial thermal stress; the rare earth elements interact with the silicon-oxygen bonds on the surface of the quartz matrix, forming a transition layer through chemical bonding, thereby enhancing the bonding force between the adhesive and the quartz matrix; the adhesive has an extremely low thermal expansion coefficient, good thermal shock resistance, excellent chemical stability and good corrosion resistance, can match the use environment of quartz products in the semiconductor processing process, and extend the service life of the quartz products.

[0080] According to a third aspect of the present invention, a method for using the adhesive for quartz products as described above is provided, referring to Figure 2 The method for using the adhesive comprises the following steps:

[0081] Step S2-1: Apply adhesive to the bonding surfaces of the quartz products to be bonded, place the surfaces together, and allow the adhesive to cure for 20-40 minutes, completing the initial bonding. This step allows for quick positioning of the quartz products, facilitating operation and temporary fixation.

[0082] Step S2-2: The quartz product after preliminary bonding is sent into a high-temperature furnace, heated to 900-1100°C at a heating rate of 8-15°C / minute, and kept warm for 120-240 minutes to allow the adhesive to sinter and bond with the quartz product. Controlling the heating rate to 8-15°C / minute can balance the release of thermal stress and the sintering efficiency, and prevent the quartz product from breaking due to sudden heat. The sintering temperature is 900-1100°C, and the insulation stage is controlled to 120-240 minutes to ensure that the interface reaction between the adhesive and quartz is fully completed, making the interface structure densified. After high-temperature sintering and curing, the glass phase and the quartz matrix form chemical bonds through diffusion bonding, which significantly improves the final bonding strength. At the same time, the adhesive layer after high-temperature sintering is an inorganic system, which avoids the pollution problem caused by high-temperature decomposition of organic adhesives.

[0083] Step S2-3: Take the quartz product out of the high-temperature furnace and cool it to room temperature.

[0084] The present invention significantly improves the reliability and life of quartz products in extreme environments through an inorganic-rare earth composite system and a step-by-step curing process, reduces production costs, and achieves environmental protection goals, thus having clear industrial application value.

[0085] The following comparative analysis uses four examples of the present invention and two comparative examples to analyze the effects of different adhesive compositions or processes on the performance of quartz products. Table 1 below shows the weight ratios of the adhesive components in the four examples of the present invention (the ratio of the rare earth compound is calculated based on the weight fraction of the rare earth element in the rare earth compound in the adhesive):

[0086] Table 1

[0087]

[0088] The test results of shear strength and service life of the quartz products in four embodiments and two comparative examples are shown in Table 2.

[0089] Table 2

[0090]

[0091] Example 1:

[0092] The adhesive includes the following components in weight fractions: glass powder: 6%, silica sol: 63%, silicate: 4% (including sodium silicate: 2%, potassium silicate 2%), thickener (sodium carboxymethyl cellulose): 11%, dispersant (sodium polyacrylate): 2%, room temperature curing agent (benzoyl peroxide): 2%, rare earth compounds include: yttrium oxide, lanthanum oxide, cerium oxide, and the weight fractions of yttrium, lanthanum, and cerium in the adhesive are 4%, 4%, and 4%, respectively.

[0093] The preparation method of the adhesive is as follows:

[0094] Step S1-1: weighing raw materials in proportion;

[0095] Step S1-2: adding glass powder and silicate to the silica sol, then adding a dispersant to fully dissolve, and stirring for 30 minutes to prepare a first mixture;

[0096] Step S1-3: adding a rare earth compound to deionized water at a weight ratio of 2:1, and ball milling the mixture using a ball mill; after drying, ball milling the mixture a second time to obtain a rare earth compound of a desired fineness; adding the rare earth compound of a desired fineness to the first mixture, and stirring for 30 minutes to obtain a second mixture;

[0097] Step S1-4: adding a thickener to the second mixture to adjust the viscosity to obtain a third mixture;

[0098] Step S1-5: Add a room temperature curing agent to the third mixture and stir for 60 to 120 minutes to obtain an adhesive.

[0099] The use of this adhesive includes:

[0100] Step S2-1: Apply adhesive to the bonding surfaces of the quartz products to be bonded, align the bonding surfaces, and let them stand for 30 minutes to allow the adhesive to cure, thus completing the initial bonding;

[0101] Step S2-2: Place the preliminarily bonded quartz product into a muffle furnace, heat it to 950°C at a rate of 10°C / min, and hold it for 180 minutes to allow the adhesive to sinter and bond to the quartz product;

[0102] Step S2-3: Take the quartz product out of the muffle furnace and cool it to room temperature.

[0103] In adhesive materials, shear strength is commonly used to measure a material's resistance to shear failure. Shear strength refers to the maximum shear stress a material or object can withstand when subjected to a shear force. The shear strength test method used in this article follows the test protocol outlined in national standard GB / T 7124-2008. A tensile force is applied parallel to the bonding surface and in the direction of the principal axis, and the shear stress at the lap joint is measured. Testing has shown that this adhesive provides a shear strength exceeding 8.5 MPa, demonstrating excellent bonding performance. It also performs well in thermal shock resistance tests, maintaining a shear strength of over 7.7 MPa after 10 cycles of thermal shock testing at 200°C to 800°C, demonstrating its adaptability to the working environment. Testing has shown that quartz boats produced using this method have an average service life of 215 days in semiconductor processing, compared to the average service life of quartz boats produced using welding processes, which is generally around 240 days. Therefore, the adhesive of this invention, when used in quartz products in the semiconductor industry, can achieve a lifespan comparable to that of quartz tubes produced using welding processes, while offering lower production costs and easier repair.

[0104] Example 2:

[0105] The adhesive includes the following components in weight fractions: glass powder: 6%, silica sol: 63%, silicate: 4% (including sodium silicate: 2%, potassium silicate 2%), thickener (sodium carboxymethyl cellulose): 11%, dispersant (sodium polyacrylate): 2%, room temperature curing agent (benzoyl peroxide): 2%, rare earth compounds include: yttrium oxide-cerium oxide, lanthanum oxide-cerium oxide, yttrium oxide stabilized zirconia, and the weight fractions of yttrium, lanthanum, and cerium in the adhesive are 4%, 4%, and 4%, respectively.

[0106] The preparation method of the adhesive is as follows:

[0107] Step S1-1: weighing raw materials in proportion;

[0108] Step S1-2: adding glass powder and silicate to the silica sol, then adding a dispersant to fully dissolve, and stirring for 20 minutes to prepare a first mixture;

[0109] Step S1-3: adding a rare earth compound to deionized water at a weight ratio of 3:1, and ball milling the mixture using a ball mill; after drying, ball milling the mixture a second time to obtain a rare earth compound of a desired fineness; adding the rare earth compound of a desired fineness to the first mixture, and stirring for 30 minutes to obtain a second mixture;

[0110] Step S1-4: adding a thickener to the second mixture to adjust the viscosity to obtain a third mixture;

[0111] Step S1-5: Add a room temperature curing agent to the third mixture and stir for 60 to 120 minutes to obtain an adhesive.

[0112] The use of this adhesive includes:

[0113] Step S2-1: Apply adhesive to the bonding surfaces of the quartz products to be bonded, align the bonding surfaces, and let them stand for 30 minutes to allow the adhesive to cure, thus completing the initial bonding;

[0114] Step S2-2: Place the preliminarily bonded quartz product into a muffle furnace, heat it to 950°C at a rate of 10°C / min, and hold it for 180 minutes to allow the adhesive to sinter and bond to the quartz product;

[0115] Step S2-3: Take the quartz product out of the muffle furnace and cool it to room temperature.

[0116] Compared to Example 1, Example 2 adjusted the composition of the rare earth compound. Testing showed that the adhesive in Example 2 provided a shear strength exceeding 9.5 MPa, demonstrating excellent bonding performance. It also performed well in thermal shock resistance tests, maintaining a shear strength exceeding 9.2 MPa after 10 cycles of thermal shock testing at 200°C to 800°C, demonstrating improved performance compared to Example 1. Testing also demonstrated that quartz boats prepared using this solution had a service life of up to 243 days in semiconductor processing.

[0117] Example 3:

[0118] The adhesive includes the following components in weight fractions: glass powder: 6%, silica sol: 63%, silicate: 4% (including sodium silicate: 2%, potassium silicate 2%), thickener (sodium carboxymethyl cellulose): 11%, dispersant (sodium polyacrylate): 2%, room temperature curing agent (benzoyl peroxide): 2%, rare earth compounds include: yttrium acetate, lanthanum acetate, cerium acetate, and the weight fractions of yttrium, lanthanum, and cerium in the adhesive are 4%, 4%, and 4%, respectively.

[0119] The preparation method of the adhesive is as follows:

[0120] Step S1-1: weighing raw materials in proportion;

[0121] Step S1-2: adding glass powder and silicate to the silica sol, then adding a dispersant to fully dissolve, and stirring for 30 minutes to prepare a first mixture;

[0122] Step S1-3: adding a rare earth compound of desired fineness to the first mixture and stirring for 30 minutes to obtain a second mixture;

[0123] Step S1-4: adding a thickener to the second mixture to adjust the viscosity to obtain a third mixture;

[0124] Step S1-5: Add a room temperature curing agent to the third mixture and stir for 60 to 120 minutes to obtain an adhesive.

[0125] The use of this adhesive includes:

[0126] Step S2-1: Apply adhesive to the bonding surfaces of the quartz products to be bonded, align the bonding surfaces, and let them stand for 30 minutes to allow the adhesive to cure, thus completing the initial bonding;

[0127] Step S2-2: Place the preliminarily bonded quartz product into a muffle furnace, heat it to 950°C at a rate of 10°C / min, and hold it for 180 minutes to allow the adhesive to sinter and bond to the quartz product;

[0128] Step S2-3: Take the quartz product out of the muffle furnace and cool it to room temperature.

[0129] After testing, the adhesive can provide a shear strength of more than 7.4MPa, has good bonding properties, and performs well in heat shock resistance tests. After 10 rounds of 200℃~800℃ cyclic heat shock tests, it still maintains a shear strength of more than 6.5MPa. After testing, the quartz boat products prepared using this solution can have a service life of up to 205 days in semiconductor processing technology.

[0130] Example 4:

[0131] The adhesive includes the following components in weight fractions: glass powder: 8%, silica sol: 58%, silicate: 4% (including sodium silicate: 2%, potassium silicate 2%), thickener (sodium carboxymethyl cellulose): 10%, dispersant (sodium polyacrylate): 2%, room temperature curing agent (benzoyl peroxide): 2%, rare earth compounds include: yttrium oxide, lanthanum oxide, cerium oxide, and the weight fractions of yttrium, lanthanum, and cerium in the adhesive are 5%, 4%, and 7%, respectively.

[0132] The preparation method of the adhesive is as follows:

[0133] Step S1-1: weighing raw materials in proportion;

[0134] Step S1-2: adding glass powder and silicate to the silica sol, then adding a dispersant to fully dissolve, and stirring for 30 minutes to prepare a first mixture;

[0135] Step S1-3: adding a rare earth compound to deionized water at a weight ratio of 2:1, and ball milling the mixture using a ball mill; after drying, ball milling the mixture a second time to obtain a rare earth compound of a desired fineness; adding the rare earth compound of a desired fineness to the first mixture, and stirring for 30 minutes to obtain a second mixture;

[0136] Step S1-4: adding a thickener to the second mixture to adjust the viscosity to obtain a third mixture;

[0137] Step S1-5: Add a room temperature curing agent to the third mixture and stir for 60 to 120 minutes to obtain an adhesive.

[0138] The use of this adhesive includes:

[0139] Step S2-1: Apply adhesive to the bonding surfaces of the quartz products to be bonded, align the bonding surfaces, and let them stand for 30 minutes to allow the adhesive to cure, thus completing the initial bonding;

[0140] Step S2-2: Place the preliminarily bonded quartz product into a muffle furnace, heat it to 950°C at a rate of 10°C / min, and hold it for 180 minutes to allow the adhesive to sinter and bond to the quartz product;

[0141] Step S2-3: Take the quartz product out of the muffle furnace and cool it to room temperature.

[0142] After testing, the adhesive can provide a shear strength of more than 7.1MPa, has good bonding performance, and performs well in the heat shock test. After 10 rounds of 200℃~1100℃ cyclic heat shock tests, it still maintains a shear strength of more than 6.3MPa, which can be used in processing techniques that require higher temperatures. After testing, the quartz boat products prepared using this solution can have a service life of up to 201 days in semiconductor processing technology. The adhesive in Example 4 can withstand high temperatures exceeding 1080℃, so it can be used in more harsh high-temperature environments and can perform better in processing techniques that require higher temperatures.

[0143] Comparative Example 1: A quartz product was produced using a direct welding process. Testing showed that the quartz product had a shear strength of 10.0 MPa and maintained this shear strength after 10 cycles of 200°C to 1100°C thermal shock testing. The quartz product had a service life of 240 days in semiconductor processing.

[0144] Comparative Example 2: A quartz product was bonded using a conventional adhesive. Testing revealed that the adhesive, while providing a shear strength of 4.3 MPa, retained only 2.7 MPa after 10 cycles of thermal shock testing at 200°C to 1100°C. The quartz product's service life in semiconductor processing was only 50 days.

[0145] From the above data comparison, it can be seen that compared with the adhesive products in the prior art, the adhesives in the four embodiments of the present invention have good use effects and can effectively extend the service life of quartz products. The service life of the quartz product in Example 2 is longer than that of the quartz product prepared by welding in Comparative Example 1. It can also reduce production costs and facilitate the self-repair of quartz products.

[0146] The adhesive of the present invention is applied to quartz products. Silica sol forms a silicon-oxygen network through a polycondensation reaction, providing high tensile bond strength. Glass powder enhances temperature resistance through the silicon-oxygen network, matches the thermal expansion coefficient of the quartz substrate, and reduces interfacial thermal stress. Rare earth elements interact with silicon-oxygen bonds on the surface of the quartz substrate, forming a transition layer through chemical bonding, which strengthens the bonding between the adhesive and the quartz substrate. The introduction of rare earth elements also creates a more complex network structure within the adhesive, which can increase stability and provide a certain shape memory function. The adhesive has an extremely low thermal expansion coefficient, good thermal shock resistance, excellent chemical stability, good corrosion resistance, and a certain self-repairing function. It can match the use environment of quartz products in semiconductor processing processes, extend the service life of quartz products, and significantly reduce production and maintenance costs.

[0147] The present invention has been described with reference to the above embodiments. However, the above embodiments are merely exemplary embodiments of the present invention. It should be noted that the disclosed embodiments do not limit the scope of the present invention. On the contrary, modifications and improvements that do not depart from the spirit and scope of the present invention are intended to be protected by the present invention.

Claims

1. An adhesive for quartz products, characterized by: The adhesive comprises the following components by weight: Glass powder: 5% to 10%; Silica sol: 55% to 70%; Silicate: 3% to 5%; A rare earth compound, wherein the weight fraction of the rare earth element in the rare earth compound in the adhesive is 3% to 25%; Thickener: 10% to 20%; Dispersant: 3% to 5%; Room temperature curing agent: 1%~2%.

2. The adhesive for quartz products according to claim 1, wherein: The rare earth compound is one or more compounds containing yttrium, lanthanum, and cerium, and the weight of the yttrium element in the rare earth compound is 0 to 3 times the weight of the lanthanum element, and the weight of the cerium element is 0 to 3 times the weight of the lanthanum element.

3. The adhesive for quartz products according to claim 2, wherein: The rare earth compound includes one or more of yttrium oxide, lanthanum oxide, and cerium oxide, and the average particle size of the rare earth compound is 1 to 5 μm; or, the rare earth compound includes one or more of yttrium acetate, lanthanum acetate, and cerium acetate.

4. The adhesive for quartz products according to claim 2, wherein: The rare earth compound includes one or more of yttrium oxide-cerium oxide composite oxide, lanthanum oxide-cerium oxide composite oxide, and yttria-stabilized zirconia.

5. The adhesive for quartz products according to claim 1, wherein: The glass powder includes the following components in weight fractions: silicon oxide: 70% to 75%, aluminum oxide: 10% to 15%, zinc oxide: 5% to 10%, tellurium oxide: 3% to 5%, and alkaline earth metal oxide: 7% to 11%.

6. The adhesive for quartz products according to claim 1, wherein: The solid content of the silica sol is 20-30%, the average particle size is 10-20 nm, and the particle dispersion index is less than 0.

2.

7. The adhesive for quartz products according to claim 1, wherein: The silicate is one or both of sodium silicate and potassium silicate.

8. The adhesive for quartz products according to claim 1, wherein: The thickener is one or both of carboxymethyl cellulose and sodium carboxymethyl cellulose; the dispersant is sodium polyacrylate; and the room temperature curing agent includes one or both of benzoyl peroxide and azobisisobutyronitrile.

9. A method for preparing an adhesive for quartz products according to any one of claims 1 to 8, characterized in that: The preparation method comprises the following steps: Step S1-1: weighing raw materials in proportion; Step S1-2: adding glass powder and silicate to the silica sol, then adding a dispersant to fully dissolve, and stirring for 20 to 30 minutes to prepare a first mixture; Step S1-3: adding the rare earth compound to the first mixture and stirring for 20 to 30 minutes to obtain a second mixture; Step S1-4: adding a thickener to the second mixture to adjust the viscosity to obtain a third mixture; Step S1-5: Add a room temperature curing agent to the third mixture and stir for 60 to 120 minutes to obtain an adhesive.

10. A method for using the adhesive for quartz products according to any one of claims 1 to 8, characterized in that: The method of use comprises the following steps: Step S2-1: Apply adhesive to the bonding surfaces of the quartz products to be bonded, align the bonding surfaces, and let them stand for 20 to 40 minutes to allow the adhesive to cure, thus completing the initial bonding; Step S2-2: Place the preliminarily bonded quartz product into a high-temperature furnace, heat it to 900-1100°C at a rate of 8-15°C / min, and hold it for 120-240 minutes to allow the adhesive to sinter and bond to the quartz product. Step S2-3: Take the quartz product out of the high-temperature furnace and cool it to room temperature.

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