Method for preparing yttrium-stabilized zirconia coating on surface of quartz part

Abstract

The invention relates to the technical field of ceramic material surface treatment, in particular to a method for preparing an yttrium-stabilized zirconia coating on the surface of a quartz part. The preparation method comprises the following steps: firstly, uniformly mixing a dispersing agent, a binding agent, a defoaming agent, a flatting agent and yttrium-stabilized zirconium oxide slurry to obtain yttrium-stabilized zirconium oxide composite slurry; then pretreating the surface of the quartz part, coating and / or impregnating the yttrium-stabilized zirconia composite slurry on the surface of the quartz part after post-treatment, drying in the shade, and then drying; and finally, sintering treatment is conducted, cooling treatment is conducted after sintering is completed, and preparation of the yttrium-stabilized zirconia coating on the surface of the quartz part is completed. The method provided by the invention is simple in process flow, low in cost, high in efficiency and wide in applicability.

Description

Technical Field

[0001] The present invention relates to the technical field of ceramic material surface treatment, and in particular to a method for preparing a yttrium-stabilized zirconia coating on the surface of a quartz part. Background Art

[0002] The metallic uranium-zirconium alloy fuel is the main fuel type for the next-generation Sodium cooled Fast Reactors (SFR). The fuel rod is in the form of an annular fuel, with an inner diameter of 3.25 mm, an outer diameter of 4.86 mm, and a total length of 38 mm, and the composition is U-10Zr (wt.%). Currently, this fuel rod alloy is melted by uranium and zirconium metals in an arc melting furnace. After multiple melt homogenizations, it is injected into a quartz mold with an inner quartz core. After injection casting, the internal quartz core is drilled out, the external quartz is broken, the uranium-zirconium alloy fuel rod is taken out, and cut into the required length for irradiation. The silicon content in the uranium-zirconium alloy fuel rod directly cast using a quartz mold is usually >500 ppm. Silicon has a certain neutron absorption cross-section and will absorb some neutrons, thus reducing the number of neutrons available for initiating fission reactions, which may lead to a decrease in the rate of fission reactions. Moreover, silicon will scatter neutrons, changing the energy and movement direction of neutrons, which will affect the probability and energy distribution of neutrons reaching the fissile nuclides in the fuel pellets, and thus have an indirect impact on the fission reaction.

[0003] Casting uranium-zirconium alloy in a quartz mold will inevitably introduce silicon elements into the fuel rod. The introduction of silicon may change the melting point and boiling point of the metallic fuel, thus affecting its state and performance at different temperatures, and will also have an impact on the thermal conductivity of the metallic fuel, and thus affect the heat transfer and distribution in the reactor. Preparing a coating on the inner wall of a quartz tube by the slurry coating and sintering method has a simple process and low cost. When the structure of the quartz component is complex, the slurry brushing can be replaced by impregnation. This process is applicable to quartz parts with different shapes and complex or narrow inner cavity structures. However, the quality of the coating prepared by the slurry coating and sintering method is greatly affected by the solid content in the slurry and the sintering process parameters. The flatness of the coating surface has a great impact on the surface roughness of the injected metal.

[0004] Therefore, preparing a coating with good compactness on the surface of a quartz part has always been the goal pursued by those skilled in the art. Summary of the Invention

[0005] To solve the above problems, the object of the present invention is to provide a method for preparing a yttria-stabilized zirconia coating on the surface of a quartz part. In the casting of uranium-zirconium alloy fuel rods, the concentration of silicon should be lower than 500 ppm. To prevent the introduction of excessive silicon elements into the metal fuel rods due to the interaction between the alloy melt and the quartz mold during the casting process, a quartz mold coated with yttria-stabilized zirconia (YSZ) slurry is used to cast uranium-zirconium alloy fuel rods. Currently, the most widely used thermal barrier coating material is 8YSZ (6% - 8% Y2O3 partially stabilized ZrO2). Due to the difference in the thermal expansion coefficients of silica (0.5×10 -6 / K) and zirconia (1.08×10 -5 / K), it is very difficult to prepare a YSZ coating on the surface of silica. Therefore, the present invention proposes a method for preparing a YSZ coating on the surface of silica and the inner cavity of a silica complex structure mold through a slurry coating and sintering process to achieve the introduction of silicon elements into the metal melted by quartz parts; this method has a simple process flow, low cost, high efficiency, and wide applicability.

[0006] The object of the present invention can be achieved by the following technical solutions:

[0007] The first object of the present invention is to provide a method for preparing a yttria-stabilized zirconia coating on the surface of a quartz part, including the following steps:

[0008] (S1) Mix a dispersant, a binder, an antifoaming agent, a leveling agent with yttria-stabilized zirconia slurry (the dispersant, the binder, the antifoaming agent, and the leveling agent are used to improve the flatness of the coating during the coating or impregnation process and its bonding strength with the substrate, and mixing is to avoid uneven slurry composition caused by sedimentation), to obtain a yttria-stabilized zirconia composite slurry;

[0009] (S2) Pretreat the surface of the quartz part, and after post-treatment, coat and / or impregnate the yttria-stabilized zirconia composite slurry prepared in step (S1) on the surface of the quartz part, and perform drying treatment after air-drying;

[0010] (S3) After step (S2) is completed, perform sintering treatment on it, and perform cooling treatment after sintering is completed.

[0011] In an embodiment of the present invention, in step (S1), the dispersant is selected from one or more of modified ammonium polycarboxylate, sodium polyacrylate, or sodium lignosulfonate;

[0012] The binder is selected from one or more of polyethylene glycol, polyvinyl alcohol, or sodium carboxymethyl cellulose;

[0013] The antifoaming agent is selected from one or more of polyether-modified silicone solution, silicone antifoaming agent, or mineral oil antifoaming agent;

[0014] The leveling agent is selected from one or more of acrylate leveling agents, silicone leveling agents or fluorocarbon leveling agents;

[0015] The yttria-stabilized zirconia is selected from one of 0YSZ, 3YSZ, 5YSZ or 8YSZ;

[0016] The yttria-stabilized zirconia slurry is a mixture of yttria-stabilized zirconia and absolute ethanol, and the mass ratio of yttria-stabilized zirconia to absolute ethanol is 2-2.6:5. The particle size of the yttria-stabilized zirconia is 500 nm.

[0017] In an embodiment of the present invention, the mass ratio of the dispersant, binder, defoamer, leveling agent to the yttria-stabilized zirconia slurry is 0.025-0.04:0.025-0.04:0.025-0.04:0.025-0.04:1.

[0018] In an embodiment of the present invention, in step (S1), it is mixed evenly by magnetic stirring. During the stirring process, the rotation speed is 100-300 r / min.

[0019] In an embodiment of the present invention, in step (S2), the pretreatment is sandblasting;

[0020] The post-treatment is to wash with deionized water and absolute ethanol in sequence (ultrasonic cleaning for 5-10 min) to remove the residue on the sandblasted surface.

[0021] In an embodiment of the present invention, in step (S2), the drying process is carried out under vacuum conditions, the temperature is 50-70 °C, and the time is 4-12 h.

[0022] In an embodiment of the present invention, if the structure of the quartz part is complex or the inner cavity is extremely narrow and sandblasting cannot be carried out, sandblasting is not necessary;

[0023] The quartz part that has been ultrasonically cleaned is rinsed with deionized water, placed in absolute ethanol, the beaker is sealed with plastic wrap, and stored in ethanol for later use; if the quartz part is large in size, after the ultrasonic cleaning is completed, the quartz part in alcohol is taken out and dried for later use;

[0024] For quartz parts with complex structures or extremely narrow inner cavities where slurry coating cannot be carried out, the quartz parts with complex structures are immersed in the yttria-stabilized zirconia composite slurry, or the yttria-stabilized zirconia composite slurry is injected into the narrow inner cavities of the quartz parts. After the slurry completely covers the surface of the substrate, the parts are taken out. After the excess slurry separates from the surface of the parts, it is heated and cured to realize the preliminary connection between the quartz parts and the yttria-stabilized zirconia coating.

[0025] In an embodiment of the present invention, in step (S3), the sintering treatment is a stepped heating sintering treatment (performed in a resistance furnace or a tube furnace), including a first sintering treatment and a second sintering treatment.

[0026] In an embodiment of the present invention, during the first sintering treatment, the heating rate is 1 - 2 °C / min (uniformly releasing volatile components in the coating to prevent the generation of bubbles or cracks; reducing stress concentration caused by thermal gradients and avoiding the fragmentation of the quartz matrix due to too fast a heating rate), the temperature is 300 - 500 °C (promoting the preliminary sintering of low-melting components in the coating), and the holding time is 1 - 2 h (fully completing the thermal decomposition of organic substances; initially homogenizing the grains);

[0027] During the second sintering treatment, the heating rate is 1 - 2 °C / min (preventing cracking caused by rapid phase transformation; ensuring a uniform temperature field), the temperature is 1120 - 1140 °C (achieving densification sintering and promoting the crystallization of high-melting phases), and the holding time is 15 - 45 min (completing densification but avoiding excessive grain growth).

[0028] In an embodiment of the present invention, during the first sintering treatment, the heating rate is 2 °C / min, the temperature is 300 °C, and the holding time is 1 h;

[0029] During the second sintering treatment, the heating rate is 1 °C / min, the temperature is 1140 °C, and the holding time is 15 min.

[0030] In an embodiment of the present invention, during the cooling treatment, the cooling rate is 1 - 2 °C / min.

[0031] Compared with the prior art, the present invention has the following beneficial effects:

[0032] (1) The present invention controls the formation of the ZrSiO4 transition layer of matrix SiO2 and coating ZrO2 through temperature and holding time, alleviates the significant difference in thermal expansion coefficients between SiO2 and ZrO2, and prepares a dense and high-bonding-strength yttrium-stabilized zirconia coating on the surface of the SiO2 matrix.

[0033] (2) The method for preparing a yttrium-stabilized zirconia coating on the surface of a quartz part by the slurry coating / impregnation-sintering process proposed by the present invention has the advantages of simple slurry preparation, simple coating preparation process flow, low cost, high efficiency, and wide applicability. Description of the Drawings

[0034] Figure 1 SEM image of the coating on the surface of the quartz part in Example 1;

[0035] Figure 2 SEM image of the coating on the surface of the quartz part in Comparative Example 1;

[0036] Figure 3 SEM image of the surface coating of the quartz part in Example 2;

[0037] Figure 4 SEM image of the surface coating of the quartz part in Comparative Example 2;

[0038] Figure 5 SEM image of the surface coating of the quartz part in Example 3;

[0039] Figure 6 SEM image of the surface coating of the quartz part in Comparative Example 3. Detailed implementation mode

[0040] The present invention will be described in detail below in conjunction with specific embodiments.

[0041] In the following embodiments, the modified ammonium polycarboxylate is purchased from San Nopco (Shanghai) Trading Co., Ltd., with the product number SN-DISPERSANT5029, and belongs to the ammonium polycarboxylate type dispersant;

[0042] The polyether-modified silicone solution is purchased from Guangzhou Kerna New Materials Co., Ltd., and its composition contains polyether-modified silicone, with the product number JQ-331;

[0043] The acrylate leveling agent is a polyether silicone copolymer of type WSS-308, purchased from Shanghai Rundao Trading Co., Ltd., with the product number 20200408;

[0044] The fluorocarbon leveling agent is a fluorocarbon-modified polymer of type LS3024, purchased from Kunshan Luolis Polymer Materials Co., Ltd., with the product number 736A;

[0045] The 3YSZ is purchased from Guangzhou Hongwu Material Technology Co., Ltd., with the product number 3Y;

[0046] The 8YSZ is purchased from Guangzhou Hongwu Material Technology Co., Ltd., with the product number 8Y;

[0047] Unless otherwise specified, all reagents used are commercially available reagents, and all detection means and methods used are conventional detection means and methods in the art.

[0048] Example 1

[0049] This example provides a method for preparing a yttria-stabilized zirconia coating on the surface of a quartz part, including the following steps:

[0050] (S1) Weigh anhydrous ethanol and 3YSZ according to a mass ratio of 10:4.5, and mix them evenly to obtain a pure 3YSZ slurry;

[0051] Among them, the particle size of the 3YSZ powder is 500 nm;

[0052] (S2) Using a modified ammonium polycarboxylate as a dispersant (the mass ratio of the dispersant to the pure 3YSZ slurry is 1:25), polyethylene glycol as a binder (the mass ratio of the binder to the pure 3YSZ slurry is 1:25), a polyether-modified silicone solution as an antifoaming agent (the mass ratio of the antifoaming agent to the pure 3YSZ slurry is 1:30), and Tofogood-3358 acrylate leveling agent as a leveling agent (the mass ratio of the leveling agent to the pure 3YSZ slurry is 1:30), and sequentially adding them into the pure 3YSZ slurry prepared in step (S1). After mixing and stirring evenly, a 3YSZ composite slurry is prepared. The 3YSZ composite slurry is placed in a magnetic stirring device and continuously stirred, and the magnetic stirring speed is 150 r / min;

[0053] (S3) Pretreatment of the quartz substrate: Sandblast one side (or one side) of the quartz part where the coating needs to be prepared. After sandblasting, clean the quartz part with deionized water and then put it into absolute ethanol for ultrasonic cleaning for 10 min to remove the sandblasting residue on the surface;

[0054] (S4) Coating application: Take out the quartz part in ethanol, dry it, and evenly apply the 3YSZ coating slurry on the surface of the quartz part substrate with a brush. After air-drying for 12 h, heat and cure it at 65 °C for 5 h to achieve the preliminary connection between the quartz substrate and the 3YSZ coating.

[0055] (S5) Drying of the coating: Place the coated quartz part under vacuum conditions at 60 °C and dry the coating for 6 h.

[0056] (S6) Sintering of the coating: Heat it to 500 °C at a heating rate of 2 °C / min in a tube furnace and hold for 1 h, then heat it to 1130 °C at a heating rate of 2 °C / min and hold for 30 min, and then cool it to room temperature and take it out of the furnace. The cooling rate is 1 °C / min; Complete the preparation of the yttria-stabilized zirconia coating on the surface of the quartz part ( Figure 1 ).

[0057] Through Figure 1 It can be found that the surface particle distribution of the yttria-stabilized zirconia coating prepared in this example is uniform, there is no agglomeration phenomenon, there are few pores, and the density is high.

[0058] The yttria-stabilized zirconia coating prepared in this example has a high bonding degree with the quartz part and is not easily peeled off or damaged.

[0059] Comparative Example 1

[0060] This comparative example provides a method for preparing a coating on the surface of a quartz part, including the following steps:

[0061] (S1) Weigh anhydrous ethanol and 3YSZ according to a mass ratio of 10:4.5, and mix them evenly to obtain a pure 3YSZ slurry;

[0062] Among them, the particle size of the 3YSZ powder is 500 nm;

[0063] (S2) Use modified ammonium polycarboxylate as a dispersant (the mass ratio of the dispersant to the pure 3YSZ slurry is 1:50), polyethylene glycol as a binder (the mass ratio of the binder to the pure 3YSZ slurry is 1:50), polyether-modified silicone solution as an antifoaming agent (the mass ratio of the antifoaming agent to the pure 3YSZ slurry is 1:60), and Tofogood-3358 acrylate leveling agent as a leveling agent (the mass ratio of the leveling agent to the pure 3YSZ slurry is 1:60). Add them successively to the pure 3YSZ slurry prepared in step (S1), mix and stir evenly to prepare a 3YSZ composite slurry, place the 3YSZ composite slurry in a magnetic stirring device and stir continuously, and the magnetic stirring speed is 150 r / min;

[0064] (S3) Pretreatment of the quartz substrate: Sandblast one side (or one side) of the quartz part that needs to be coated, clean the sandblasted quartz part with deionized water, then put it into anhydrous alcohol, and ultrasonically clean it for 10 min to remove the sandblasting residue on the surface;

[0065] (S4) Coating application: Take out the quartz part in ethanol, dry it, and evenly apply the 3YSZ coating slurry on the surface of the quartz part substrate with a brush. After air-drying for 12 h, heat and cure it at 65 °C for 5 h to achieve the preliminary connection between the quartz substrate and the 3YSZ coating.

[0066] (S5) Drying of the coating: Place the coated quartz part under vacuum at 60 °C and dry the coating for 6 h.

[0067] (S6) Sintering of the coating: Heat it in a tubular furnace to 500 °C at a heating rate of 2 °C / min and hold for 1 h, then heat it to 1130 °C at a heating rate of 2 °C / min and hold for 30 min, and then cool it to room temperature and take it out of the furnace, and the cooling rate is 1 °C / min; complete the preparation of the coating on the surface of the quartz part ( Figure 2 ).

[0068] Compared with Example 1, in Comparative Example 1, due to the lower dosages of the dispersant, binder, antifoaming agent, and leveling agent, it may cause uneven dispersion of the slurry during the coating process, the flatness of the coating becomes worse, and the bonding strength with the substrate decreases.

[0069] More particle agglomeration phenomena were found on the surface of the coating in Example 1, and the coating was more likely to fall off from the substrate surface.

[0070] Example 2

[0071] This embodiment provides a method for preparing a yttria-stabilized zirconia coating on the surface of a quartz part, comprising the following steps:

[0072] (S1) Weigh anhydrous ethanol and 8YSZ according to a mass ratio of 10:4.5, and mix them evenly to obtain a pure 8YSZ slurry;

[0073] Among them, the particle size of the 8YSZ powder is 500 nm;

[0074] (S2) Use a modified ammonium polycarboxylate as a dispersant (the mass ratio of the dispersant to the pure 8YSZ slurry is 1:30), polyethylene glycol as a binder (the mass ratio of the binder to the pure 8YSZ slurry is 1:30), a polyether-modified silicone solution as an antifoaming agent (the mass ratio of the antifoaming agent to the pure 8YSZ slurry is 1:40), and a fluorocarbon leveling agent as a leveling agent (the mass ratio of the leveling agent to the pure 8YSZ slurry is 1:40). Add them to the pure 8YSZ slurry prepared in step (S1) in sequence. After mixing and stirring evenly, prepare an 8YSZ composite slurry. Place the 8YSZ composite slurry in a magnetic stirring device and continuously stir at a magnetic stirring speed of 150 r / min;

[0075] (S3) Pretreatment of the quartz substrate: Sandblast one side (or one side) of the quartz part that needs to be coated. After cleaning the sandblasted quartz part with deionized water, put it into anhydrous ethanol and ultrasonically clean it for 10 min to remove the sandblasting residue on the surface;

[0076] (S4) Coating application: Take out the quartz part in ethanol, dry it, and evenly apply the 8YSZ coating slurry on the surface of the quartz part substrate with a brush. After air-drying for 12 h, heat and cure it at 65 °C for 5 h to achieve the preliminary connection between the quartz substrate and the 8YSZ coating.

[0077] (S5) Drying of the coating: Place the coated quartz part under vacuum at 60 °C and dry the coating for 6 h.

[0078] (S6) Sintering of the coating: Heat it to 500 °C at a heating rate of 1 °C / min in a tubular furnace and hold for 1 h, then heat it to 1120 °C at a heating rate of 1 °C / min and hold for 45 min, and then cool it to room temperature and take it out of the furnace. The cooling rate is 2 °C / min; complete the preparation of the yttria-stabilized zirconia coating on the surface of the quartz part( Figure 3 ).

[0079] Through Figure 3 It can be found that the surface particles of the yttria-stabilized zirconia coating prepared in this embodiment are evenly distributed, there is no agglomeration phenomenon, there are few pores, and the density is high.

[0080] The yttria-stabilized zirconia coating prepared in this embodiment has a high bonding degree with the quartz part and is not easy to peel off or damage.

[0081] Comparative Example 2

[0082] This comparative example provides a method for preparing a coating on the surface of a quartz part, including the following steps:

[0083] (S1) Weigh anhydrous ethanol and 8YSZ according to a mass ratio of 10:4.5, and mix them evenly to obtain a pure 8YSZ slurry;

[0084] Among them, the particle size of the 8YSZ powder is 500 nm;

[0085] (S2) Using modified ammonium polycarboxylate as a dispersant (the mass ratio of the dispersant to the pure 8YSZ slurry is 1:30), polyethylene glycol as a binder (the mass ratio of the binder to the pure 8YSZ slurry is 1:30), polyether-modified silicone solution as an antifoaming agent (the mass ratio of the antifoaming agent to the pure 8YSZ slurry is 1:40), and fluorocarbon leveling agent as a leveling agent (the mass ratio of the leveling agent to the pure 8YSZ slurry is 1:40), add them to the pure 8YSZ slurry prepared in step (S1) in sequence. After mixing and stirring evenly, prepare an 8YSZ composite slurry. Place the 8YSZ composite slurry in a magnetic stirring device and continuously stir. The magnetic stirring speed is 150 r / min;

[0086] (S3) Pretreatment of the quartz substrate: Sandblast one side (or one side) of the quartz part that needs to be coated. After sandblasting, wash the quartz part with deionized water, then put it into anhydrous ethanol and ultrasonically clean it for 10 min to remove the sandblasting residue on the surface;

[0087] (S4) Coating application: Take out the quartz part in ethanol, dry it, and evenly apply the 8YSZ coating slurry on the surface of the quartz part substrate with a brush. After air-drying for 12 h, heat and cure it at 65 °C for 5 h to achieve the preliminary connection between the quartz substrate and the 8YSZ coating.

[0088] (S5) Drying of the coating: Place the coated quartz part under vacuum at 60 °C and dry the coating for 6 h.

[0089] (S6) Sintering of the coating: Heat it to 1130 °C in a tube furnace at a heating rate of 5 °C / min, hold it for 30 min, then cool it to room temperature and take it out of the furnace. The cooling rate is 1 °C / min; complete the preparation of the coating on the surface of the quartz part( Figure 4 ).

[0090] Compared with Example 2, in this comparative example, rapid heating and skipping the first sintering treatment may cause stress concentration inside the coating, and it is impossible to effectively form a ZrSiO4 transition layer to relieve the difference in thermal expansion coefficient. When detecting the coating, it is found that there are more cracks in the coating, the denseness becomes worse, which affects its protective effect on the quartz part and the bonding strength with the quartz substrate.

[0091] Example 3

[0092] This example provides a method for preparing a yttria-stabilized zirconia coating on the surface of a quartz part, including the following steps:

[0093] (S1) Weigh anhydrous ethanol and 8YSZ according to a mass ratio of 10:5.2, and mix them evenly to obtain a pure 8YSZ slurry;

[0094] Among them, the particle size of the 8YSZ powder is 500 nm;

[0095] (S2) Use modified ammonium polycarboxylate as a dispersant (the mass ratio of the dispersant to the pure 8YSZ slurry is 1:30), polyethylene glycol as a binder (the mass ratio of the binder to the pure 8YSZ slurry is 1:30), polyether-modified silicone solution as an antifoaming agent (the mass ratio of the antifoaming agent to the pure 8YSZ slurry is 1:45), and organosilicon leveling agent as a leveling agent (the mass ratio of the leveling agent to the pure 8YSZ slurry is 1:45). Add them to the pure 8YSZ slurry prepared in step (S1) in sequence. After mixing and stirring evenly, prepare an 8YSZ composite slurry. Place the 8YSZ composite slurry in a magnetic stirring device and continuously stir. The magnetic stirring speed is 300 r / min;

[0096] (S3) Pretreatment of the quartz substrate: Sandblast one side (or one side) of the quartz part that needs to be coated. After sandblasting, clean the quartz part with deionized water, then put it into anhydrous ethanol and ultrasonically clean it for 10 min to remove the sandblasting residue on the surface;

[0097] (S4) Coating application: Take out the quartz part in ethanol, dry it, and evenly apply the 8YSZ coating slurry on the surface of the quartz part substrate with a brush and air-dry it for 12 h, then heat and cure it at 60 °C for 5 h to achieve the preliminary connection between the quartz substrate and the 8YSZ coating.

[0098] (S5) Drying of the coating: Place the coated quartz part in a vacuum at 60 °C and dry the coating for 12 h.

[0099] (S6) Sintering of the coating: Heat it to 300 °C at a heating rate of 2 °C / min in a tube furnace and hold for 1 h, then heat it to 1140 °C at a heating rate of 2 °C / min and hold for 15 min, and then cool it to room temperature and take it out of the furnace. The cooling rate is 1 °C / min; complete the preparation of the yttria-stabilized zirconia coating on the surface of the quartz part( Figure 5 ).

[0100] Through Figure 5 It can be found that the surface particle distribution of the yttria-stabilized zirconia coating prepared in this example is uniform, there is no agglomeration phenomenon, there are few pores, and the density is high.

[0101] The yttrium-stabilized zirconia coating prepared in this example has a high bonding degree with the quartz part and is not easily peeled off or damaged.

[0102] Comparative Example 3

[0103] This comparative example provides a method for preparing a coating on the surface of a quartz part, including the following steps:

[0104] (S1) Weigh anhydrous ethanol and 8YSZ according to a mass ratio of 10:5.2, mix them evenly to obtain a pure 8YSZ slurry;

[0105] Among them, the particle size of the 8YSZ powder is 500 nm;

[0106] (S2) Use modified ammonium polycarboxylate as a dispersant (the mass ratio of the dispersant to the pure 8YSZ slurry is 1:30), polyethylene glycol as a binder (the mass ratio of the binder to the pure 8YSZ slurry is 1:30), polyether-modified silicone solution as an antifoaming agent (the mass ratio of the antifoaming agent to the pure 8YSZ slurry is 1:45), and organosilicon leveling agent as a leveling agent (the mass ratio of the leveling agent to the pure 8YSZ slurry is 1:45). Add them to the pure 8YSZ slurry prepared in step (S1) in sequence. After mixing and stirring evenly, prepare an 8YSZ composite slurry. Place the 8YSZ composite slurry in a magnetic stirring device and continuously stir. The magnetic stirring speed is 300 r / min;

[0107] (S3) Pretreatment of the quartz substrate: Sandblast one side (or one side) of the quartz part that needs to be coated;

[0108] (S4) Coating application: After taking out the sandblasted quartz substrate from the sandblasting equipment in step (S2), use a brush to evenly apply the 3YSZ coating slurry on the surface of the quartz part substrate. After air-drying for 12 h, heat and cure at 65 °C for 5 h to achieve the preliminary connection between the quartz substrate and the 3YSZ coating.

[0109] (S5) Drying of the coating: Place the coated quartz part in a vacuum at 60 °C and dry the coating for 12 h.

[0110] (S6) Sintering of the coating: Heat in a tube furnace at a heating rate of 2 °C / min to 300 °C and hold for 1 h, then heat at a heating rate of 2 °C / min to 1140 °C and hold for 15 min, and then cool to room temperature and take out of the furnace. The cooling rate is 1 °C / min; complete the preparation of the coating on the surface of the quartz part ( Figure 6 ).

[0111] Compared with Example 3, in Comparative Example 3, the surface of the quartz part after sandblasting was not cleaned thoroughly, which would affect the bonding between the coating and the substrate, resulting in a decrease in the bonding strength. When testing the adhesion of the coating, it was found that the adhesion of the coating was significantly lower than that of Example 1, and due to the presence of residual impurities, the uniformity and density of the coating might be affected, making the performance of the coating unable to achieve the expected effect.

[0112] Example 4

[0113] This example provides a method for preparing a yttria-stabilized zirconia coating on the surface of a quartz part, including the following steps:

[0114] (S1) Weigh anhydrous ethanol and 8YSZ according to a mass ratio of 10:5.2, and mix them evenly to obtain a pure 8YSZ slurry; among them, the particle size of the 8YSZ powder is 500 nm;

[0115] (S2) Using modified ammonium polycarboxylate as a dispersant (the mass ratio of the dispersant to the pure 8YSZ slurry is 1:30), polyethylene glycol as a binder (the mass ratio of the binder to the pure 8YSZ slurry is 1:30), polyether-modified silicone solution as an antifoaming agent (the mass ratio of the antifoaming agent to the pure 8YSZ slurry is 1:45), and organosilicon leveling agent as a leveling agent (the mass ratio of the leveling agent to the pure 8YSZ slurry is 1:45), add them to the pure 8YSZ slurry prepared in step (S1) in sequence, mix and stir evenly to prepare an 8YSZ composite slurry, and place the 8YSZ composite slurry in a magnetic stirring device for continuous stirring, and the magnetic stirring speed is 300 r / min;

[0116] (S3) Pretreatment of the quartz substrate: Sandblast one side (or one side) of the quartz part that needs to be coated, clean the sandblasted quartz part with deionized water, and then put it into anhydrous alcohol and ultrasonically clean it for 10 min to remove the sandblasting residue on the surface;

[0117] (S4) Coating application: Take out the quartz part in ethanol, dry it, and evenly apply the 8YSZ coating slurry on the surface of the quartz part substrate with a brush and air-dry it for 12 h, and heat and cure it at 60 °C for 5 h to achieve the preliminary connection between the quartz substrate and the 8YSZ coating.

[0118] (S5) Drying of the coating: Place the coated quartz part under vacuum at 60 °C and dry the coating for 12 h.

[0119] (S6) Sintering of the coating: Heat it to 400 °C at a heating rate of 2 °C / min in a tubular furnace and hold for 2 h, then heat it to 1120 °C at a heating rate of 2 °C / min and hold for 45 min, and then cool it to room temperature and take it out of the furnace, and the cooling rate is 1 °C / min; complete the preparation of the yttria-stabilized zirconia coating on the surface of the quartz part.

[0120] Example 5

[0121] This example provides a method for preparing a yttria-stabilized zirconia coating on the surface of a quartz part, including the following steps:

[0122] (S1) Weigh anhydrous ethanol and 8YSZ according to a mass ratio of 10:5.2, and mix them evenly to obtain a pure 8YSZ slurry; among them, the particle size of the 8YSZ powder is 500 nm;

[0123] (S2) Use modified ammonium polycarboxylate as a dispersant (the mass ratio of the dispersant to the pure 8YSZ slurry is 1:30), polyethylene glycol as a binder (the mass ratio of the binder to the pure 8YSZ slurry is 1:30), polyether-modified silicone solution as an antifoaming agent (the mass ratio of the antifoaming agent to the pure 8YSZ slurry is 1:45), and organosilicon leveling agent as a leveling agent (the mass ratio of the leveling agent to the pure 8YSZ slurry is 1:45). Add them to the pure 8YSZ slurry prepared in step (S1) in sequence. After mixing and stirring evenly, prepare an 8YSZ composite slurry. Place the 8YSZ composite slurry in a magnetic stirring device and continuously stir at a magnetic stirring speed of 300 r / min;

[0124] (S3) Pretreatment of the quartz substrate: Sandblast one side (or one side) of the quartz part that needs to be coated. After sandblasting, clean the quartz part with deionized water and then put it into anhydrous alcohol, and ultrasonically clean it for 10 min to remove the sandblasting residue on the surface;

[0125] (S4) Coating application: Take out the quartz part in ethanol, dry it, and evenly apply the 8YSZ coating slurry on the surface of the quartz part substrate with a brush and air-dry it for 12 h, and heat and cure it at 60 °C for 5 h to achieve the preliminary connection between the quartz substrate and the 8YSZ coating.

[0126] (S5) Drying of the coating: Place the coated quartz part in a vacuum at 60 °C and dry the coating for 12 h.

[0127] (S6) Sintering of the coating: Heat it to 500 °C at a heating rate of 1 °C / min in a tube furnace and hold for 1 h, then heat it to 1130 °C at a heating rate of 1 °C / min and hold for 30 min, and then cool it to room temperature and take it out of the furnace, and the cooling rate is 1 °C / min; complete the preparation of the yttria-stabilized zirconia coating on the surface of the quartz part.

[0128] Example 6

[0129] This example provides a method for preparing a yttria-stabilized zirconia coating on the surface of a quartz part, including the following steps:

[0130] (S1) Weigh anhydrous ethanol and 8YSZ according to a mass ratio of 10:5.2, and mix them evenly to obtain a pure 8YSZ slurry; among them, the particle size of the 8YSZ powder is 500 nm;

[0131] (S2) Use modified ammonium polycarboxylate as a dispersant (the mass ratio of the dispersant to the pure 8YSZ slurry is 1:30), polyethylene glycol as a binder (the mass ratio of the binder to the pure 8YSZ slurry is 1:30), polyether-modified silicone solution as an antifoaming agent (the mass ratio of the antifoaming agent to the pure 8YSZ slurry is 1:45), and organosilicon leveling agent as a leveling agent (the mass ratio of the leveling agent to the pure 8YSZ slurry is 1:45). Add them to the pure 8YSZ slurry prepared in step (S1) in sequence. After mixing and stirring evenly, prepare an 8YSZ composite slurry. Place the 8YSZ composite slurry in a magnetic stirring device and stir continuously. The magnetic stirring speed is 300 r / min;

[0132] (S3) Pretreatment of the quartz substrate: Sandblast one side (or one side) of the quartz part that needs to be coated. After sandblasting, clean the quartz part with deionized water and then put it into anhydrous alcohol, and ultrasonically clean it for 10 min to remove the sandblasting residue on the surface;

[0133] (S4) Coating application: Take out the quartz part in ethanol, dry it, and evenly apply the 8YSZ coating slurry on the surface of the quartz part substrate with a brush and air-dry it for 12 h, and heat and cure it at 60 °C for 5 h to achieve the preliminary connection between the quartz substrate and the 8YSZ coating.

[0134] (S5) Coating drying: Place the coated quartz part under vacuum at 60 °C and dry the coating for 12 h.

[0135] (S6) Coating sintering: Heat in a tubular furnace at a heating rate of 1 °C / min to 400 °C and hold for 1 h, then heat at a heating rate of 2 °C / min to 1140 °C and hold for 30 min, and then cool to room temperature and take out of the furnace. The cooling rate is 1 °C / min; complete the preparation of the yttrium-stabilized zirconia coating on the surface of the quartz part.

[0136] The properties of the yttrium-stabilized zirconia coatings on the surfaces of the quartz parts prepared in Examples 4 to 6 are roughly the same as those of the yttrium-stabilized zirconia coatings on the surfaces of the quartz parts prepared in Example 3.

[0137] Comparative Example 4 (During the first sintering treatment process, the temperature rises and the holding time is shortened)

[0138] This comparative example provides a method for preparing a coating on the surface of a quartz part, including the following steps:

[0139] (S1) Weigh anhydrous ethanol and 8YSZ according to a mass ratio of 10:5.2, and mix them evenly to obtain a pure 8YSZ slurry; among them, the particle size of the 8YSZ powder is 500 nm;

[0140] (S2) Use modified ammonium polycarboxylate as a dispersant (the mass ratio of the dispersant to the pure 8YSZ slurry is 1:30), polyethylene glycol as a binder (the mass ratio of the binder to the pure 8YSZ slurry is 1:30), polyether-modified silicone solution as an antifoaming agent (the mass ratio of the antifoaming agent to the pure 8YSZ slurry is 1:45), and organosilicon leveling agent as a leveling agent (the mass ratio of the leveling agent to the pure 8YSZ slurry is 1:45). Add them to the pure 8YSZ slurry prepared in step (S1) in sequence. After mixing and stirring evenly, prepare an 8YSZ composite slurry. Place the 8YSZ composite slurry in a magnetic stirring device and continuously stir at a magnetic stirring speed of 300 r / min;

[0141] (S3) Pretreatment of the quartz substrate: Sandblast one side (or one side) of the quartz part that needs to be coated. After sandblasting, clean the quartz part with deionized water and then put it into anhydrous alcohol, and ultrasonically clean it for 10 min to remove the sandblasting residue on the surface;

[0142] (S4) Coating application: Take out the quartz part in ethanol, dry it, and evenly apply the 8YSZ coating slurry on the surface of the quartz part substrate with a brush and air-dry it for 12 h, and heat and cure it at 60 °C for 5 h to achieve the preliminary connection between the quartz substrate and the 8YSZ coating.

[0143] (S5) Drying of the coating: Place the coated quartz part under vacuum at 60 °C and dry the coating for 12 h.

[0144] (S6) Sintering of the coating: Heat it to 600 °C at a heating rate of 1 °C / min in a tubular furnace and hold for 1 h, then heat it to 1140 °C and hold for 15 min, and then cool it to room temperature and take it out of the furnace, and the cooling rate is 1 °C / min; complete the preparation of the coating on the surface of the quartz part.

[0145] Comparative Example 5 (During the first sintering treatment process, the temperature is reduced and the holding time is extended)

[0146] This comparative example provides a method for preparing a coating on the surface of a quartz part, including the following steps:

[0147] (S1) Weigh anhydrous ethanol and 8YSZ according to a mass ratio of 10:5.2, and mix them evenly to obtain a pure 8YSZ slurry; among them, the particle size of the 8YSZ powder is 500 nm;

[0148] (S2) Using modified ammonium polycarboxylate as a dispersant (the mass ratio of the dispersant to the pure 8YSZ slurry is 1:30), polyethylene glycol as a binder (the mass ratio of the binder to the pure 8YSZ slurry is 1:30), polyether-modified silicone solution as an antifoaming agent (the mass ratio of the antifoaming agent to the pure 8YSZ slurry is 1:45), and organosilicon leveling agent as a leveling agent (the mass ratio of the leveling agent to the pure 8YSZ slurry is 1:45), add them successively to the pure 8YSZ slurry prepared in step (S1), mix and stir evenly to prepare an 8YSZ composite slurry, place the 8YSZ composite slurry in a magnetic stirring device and stir continuously, and the magnetic stirring speed is 300 r / min;

[0149] (S3) Pretreatment of the quartz substrate: Sandblast one side (or one side) of the quartz part that needs to be coated, clean the sandblasted quartz part with deionized water, then put it into anhydrous alcohol, and ultrasonically clean it for 10 min to remove the sandblasting residue on the surface;

[0150] (S4) Coating application: Take out the quartz part in ethanol, dry it with a blower, and evenly apply the 8YSZ coating slurry on the surface of the quartz part substrate with a brush and air-dry it for 12 h, and heat and cure it at 60 °C for 5 h to achieve the preliminary connection between the quartz substrate and the 8YSZ coating.

[0151] (S5) Drying of the coating: Place the coated quartz part under vacuum at 60 °C and dry the coating for 12 h.

[0152] (S6) Sintering of the coating: Heat it to 200 °C at a heating rate of 3 °C / min in a tube furnace and hold for 3 h, then raise the temperature to 1140 °C at a heating rate of 2 °C / min and hold for 15 min, and then cool it to room temperature and take it out of the furnace, and the cooling rate is 1 °C / min; complete the preparation of the coating on the surface of the quartz part.

[0153] Comparative Example 6 (The temperature is reduced and the holding time is extended during the second sintering process)

[0154] This comparative example provides a method for preparing a coating on the surface of a quartz part, including the following steps:

[0155] (S1) Weigh anhydrous ethanol and 8YSZ according to a mass ratio of 10:5.2, and mix them evenly to obtain a pure 8YSZ slurry; among them, the particle size of the 8YSZ powder is 500 nm;

[0156] (S2) Using modified ammonium polycarboxylate as a dispersant (the mass ratio of the dispersant to the pure 8YSZ slurry is 1:30), polyethylene glycol as a binder (the mass ratio of the binder to the pure 8YSZ slurry is 1:30), polyether-modified silicone solution as an antifoaming agent (the mass ratio of the antifoaming agent to the pure 8YSZ slurry is 1:45), and organosilicon leveling agent as a leveling agent (the mass ratio of the leveling agent to the pure 8YSZ slurry is 1:45), add them successively to the pure 8YSZ slurry prepared in step (S1). After mixing and stirring evenly, an 8YSZ composite slurry is prepared. Place the 8YSZ composite slurry in a magnetic stirring device and continuously stir at a magnetic stirring speed of 300 r / min;

[0157] (S3) Pretreatment of the quartz substrate: Sandblast one side (or one side) of the quartz part that needs to be coated. After sandblasting, clean the quartz part with deionized water and then put it into absolute ethanol for ultrasonic cleaning for 10 min to remove the sandblasting residue on the surface;

[0158] (S4) Coating application: Take out the quartz part in ethanol, dry it, and evenly apply the 8YSZ coating slurry on the surface of the quartz part substrate with a brush and air-dry it for 12 h, and heat and cure it at 60 °C for 5 h to achieve the preliminary connection between the quartz substrate and the 8YSZ coating.

[0159] (S5) Drying of the coating: Place the coated quartz part under vacuum at 60 °C and dry the coating for 12 h.

[0160] (S6) Sintering of the coating: Heat it to 300 °C at a heating rate of 2 °C / min in a tube furnace and hold for 1 h, then heat it to 1000 °C at a heating rate of 2 °C / min and hold for 1 h, and then cool it to room temperature and take it out of the furnace, and the cooling rate is 1 °C / min; complete the preparation of the coating on the surface of the quartz part.

[0161] Comparative Example 7 (During the second sintering treatment process, the temperature increases and the holding time is shortened)

[0162] This comparative example provides a method for preparing a coating on the surface of a quartz part, including the following steps:

[0163] (S1) Weigh anhydrous ethanol and 8YSZ according to a mass ratio of 10:5.2 and mix them evenly to obtain a pure 8YSZ slurry; among them, the particle size of the 8YSZ powder is 500 nm;

[0164] (S2) Using modified ammonium polycarboxylate as a dispersant (the mass ratio of the dispersant to the pure 8YSZ slurry is 1:30), polyethylene glycol as a binder (the mass ratio of the binder to the pure 8YSZ slurry is 1:30), polyether-modified silicone solution as an antifoaming agent (the mass ratio of the antifoaming agent to the pure 8YSZ slurry is 1:45), and organosilicon leveling agent as a leveling agent (the mass ratio of the leveling agent to the pure 8YSZ slurry is 1:45), add them successively to the pure 8YSZ slurry prepared in step (S1), mix and stir evenly to prepare an 8YSZ composite slurry, place the 8YSZ composite slurry in a magnetic stirring device and stir continuously, and the magnetic stirring speed is 300 r / min;

[0165] (S3) Pretreatment of the quartz substrate: Sandblast one side (or one side) of the quartz part that needs to be coated, clean the sandblasted quartz part with deionized water, then put it into absolute ethanol, and ultrasonically clean it for 10 min to remove the sandblasting residue on the surface;

[0166] (S4) Coating application: Take out the quartz part in ethanol, dry it, and evenly apply the 8YSZ coating slurry on the surface of the quartz part substrate with a brush and air-dry it for 12 h, and heat and cure it at 60 °C for 5 h to achieve the preliminary connection between the quartz substrate and the 8YSZ coating.

[0167] (S5) Drying of the coating: Place the coated quartz part under vacuum at 60 °C and dry the coating for 12 h.

[0168] (S6) Sintering of the coating: Heat it to 300 °C at a heating rate of 2 °C / min in a tube furnace and hold for 1 h, then heat it to 1200 °C at a heating rate of 1 °C / min and hold for 10 min, and then cool it to room temperature and take it out of the furnace, and the cooling rate is 1 °C / min; complete the preparation of the coating on the surface of the quartz part.

[0169] It was found that the coatings prepared in Comparative Examples 4 to 7 had the following disadvantages:

[0170] Comparative Example 4: The bonding strength between the coating and the substrate is low, and the brittleness of the coating increases;

[0171] Comparative Example 5: The bonding strength between the coating and the substrate is low, the porosity of the coating increases, and the density difference is poor;

[0172] Comparative Example 6: The bonding strength between the coating and the substrate is low, and the density of the coating is poor;

[0173] Comparative Example 7: The bonding strength between the coating and the substrate is low, the porosity of the coating increases, and the brittleness of the coating increases.

[0174] The above description of the embodiments is to enable those of ordinary skill in the art to understand and use the invention. It is obvious that those skilled in the art can easily make various modifications to these embodiments and apply the general principles described herein to other embodiments without creative efforts. Therefore, the present invention is not limited to the above embodiments, and all improvements and modifications made by those skilled in the art without departing from the scope of the present invention according to the interpretation of the present invention should be within the protection scope of the present invention.

Claims

1. A method for preparing a yttrium-stabilized zirconia coating on the surface of a quartz part, characterized in that, It includes the following steps: (S1) Mix a dispersant, a binder, an antifoaming agent, a leveling agent with a yttria-stabilized zirconia slurry to obtain a yttria-stabilized zirconia composite slurry; (S2) Pretreat the surface of the quartz part. After post-treatment, coat and / or impregnate the yttria-stabilized zirconia composite slurry prepared in step (S1) on the surface of the quartz part, and perform drying treatment after air-drying; (S3) After step (S2) ends, perform sintering treatment on it, and perform cooling treatment after sintering ends.

2. The method for preparing a yttrium-stabilized zirconia coating on the surface of a quartz part according to claim 1, characterized in that, In step (S1), the dispersant is selected from one or more of modified ammonium polycarboxylate, sodium polyacrylate or sodium lignosulfonate; The binder is selected from one or more of polyethylene glycol, polyvinyl alcohol or sodium carboxymethyl cellulose; The antifoaming agent is selected from one or more of polyether-modified silicone solution, silicone antifoaming agent or mineral oil antifoaming agent; The leveling agent is selected from one or more of acrylate leveling agent, silicone leveling agent or fluorocarbon leveling agent; The yttria-stabilized zirconia is selected from one of 0YSZ, 3YSZ, 5YSZ or 8YSZ; The yttria-stabilized zirconia slurry is a mixture of yttria-stabilized zirconia and absolute ethanol, and the mass ratio of yttria-stabilized zirconia to absolute ethanol is 2-2.6:

5.

3. A method for preparing a yttria-stabilized zirconia coating on the surface of a quartz part according to claim 2, characterized in that, The mass ratio of the dispersant, the binder, the antifoaming agent, the leveling agent to the yttria-stabilized zirconia slurry is 0.025-0.04:0.025-0.04:0.025-0.04:0.025-0.04:

1.

4. A method for preparing a yttrium-stabilized zirconia coating on the surface of a quartz part according to claim 1, characterized in that, In step (S1), mix evenly by magnetic stirring. During the stirring process, the rotation speed is 100-300 r / min.

5. A method for preparing a yttrium-stabilized zirconia coating on the surface of a quartz part according to claim 1, characterized in that, In step (S2), the post-treatment is to wash with deionized water and absolute ethanol in sequence.

6. A method for preparing a yttrium-stabilized zirconia coating on the surface of a quartz part according to claim 1, characterized in that, In step (S2), the drying process is in a vacuum state, the temperature is 50-70 °C, and the time is 4-12 h.

7. A method for preparing a yttrium-stabilized zirconia coating on the surface of a quartz part according to claim 1, characterized in that, In step (S3), the sintering treatment is a stepwise heating sintering treatment, including a first sintering treatment and a second sintering treatment.

8. A method for preparing a yttrium-stabilized zirconia coating on the surface of a quartz part according to claim 7, characterized in that, During the first sintering treatment, the heating rate is 1-2 °C / min, the temperature is 300-500 °C, and the holding time is 1-2 h; During the second sintering treatment, the heating rate is 1-2 °C / min, the temperature is 1120-1140 °C, and the holding time is 15-45 min.

9. A method for preparing a yttrium-stabilized zirconia coating on the surface of a quartz part according to claim 8, characterized in that, During the first sintering treatment, the heating rate is 2 °C / min, the temperature is 300 °C, and the holding time is 1 h; During the second sintering treatment, the heating rate is 1 °C / min, the temperature is 1140 °C, and the holding time is 15 min.

10. A method for preparing a yttrium-stabilized zirconia coating on the surface of a quartz part according to claim 1, characterized in that, During the cooling treatment, the cooling rate is 1-2 °C / min.

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