A ceramic substrate green body powder application sintering process

Abstract

The present application relates to the technical field of ceramic substrate, and particularly relates to a ceramic substrate green body powder coating sintering process. The process comprises the following steps: step 1: uniformly stirring boron nitride powder, terpineol, ethyl cellulose, butyl benzyl phthalate and phosphate ester, and grinding to obtain a powder coating; step 2: using a silk screen printing technology to print the powder coating on the surface of a green body to form a powder coating pattern; obtaining a powder coating green body; step 3: stacking N powder coating green bodies to obtain a laminated green body; step 4: sequentially arranging the laminated green body to perform glue removal sintering and sand blasting; and obtaining a ceramic substrate.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of ceramic substrate, and particularly relates to a ceramic substrate green body powder coating sintering process. BACKGROUND

[0002] The powder coating of the super-large and super-thin green body is a special powder application technology, which is mainly applied to the surface of the ceramic substrate or other large and super-thin green bodies to realize uniform coating. This technology has important applications in the fields of super-high thermal conductivity, functional ceramic substrate, electronic components and the like.

[0003] The ceramic substrate is an electronic substrate made of ceramic material and belongs to inorganic material. The ceramic substrate is mainly composed of alumina (Al2O3), aluminum nitride (AlN) and silicon nitride (Si3N4) and the like. The ceramic substrate has good thermal conductivity, high frequency and high temperature stability and the like, and is widely applied to electronic equipment in harsh environments such as high power, high frequency and high temperature.

[0004] As a strong covalent compound, the silicon nitride has a very low diffusion coefficient, and therefore, the pure silicon nitride cannot be sintered to be dense. Therefore, a sintering aid must be added to form a liquid phase to help the densification during sintering. During the sintering process, the sintering aid is very easy to volatilize, which causes the ceramic sheet to be prone to sticking and cracking. The thinner and larger the green body is, the more serious the problem is.

[0005] In view of the above, it is of great significance to develop a ceramic substrate green body powder coating sintering process to solve the problem of sintering sticking and cracking. SUMMARY

[0006] The present application aims to provide a ceramic substrate green body powder coating sintering process to solve the problems in the prior art.

[0007] To achieve the above-mentioned purpose, the present application provides the following technical scheme:

[0008] A ceramic substrate green body powder coating sintering process comprises the following steps:

[0009] Step 1: uniformly stir, grind and obtain a powder coating by using boron nitride powder, terpineol, ethyl cellulose, butyl benzyl phthalate and phosphate ester;

[0010] Step 2: print the powder coating on the surface of the green body by using a silk screen printing technology to form a powder coating pattern, and obtain a powder coating green body;

[0011] Step 3: stack N powder coating green bodies to obtain a laminated green body;

[0012] Step 4: sequentially perform a glue removal sintering and sand blasting on the laminated green body to obtain a ceramic substrate.

[0013] More preferably, in step 1, the raw material for the powder coating contains, by mass fraction: 25-40 parts of boron nitride powder, 25-50 parts of terpineol, 2-8 parts of ethyl cellulose, 0.2-5 parts of butyl benzyl phthalate, and 0.2-5 parts of phosphate ester.

[0014] More preferably, in step 2, the powder coating pattern includes one of a dot array and a full plate; and the powder coating printing has a thickness of 3-30 um. The pattern size can be designed, and the dot array pattern includes a circle or a rhombus, the dot array pattern has a diameter of 30-300 um, a pitch of 30-500 um, and a powder coating thickness of 3-30 um.

[0015] More preferably, in step 3, N≥8; and the stacking mode includes one of a sandwich stacking and a non-sandwich stacking. The non-sandwich stacking is a direct stacking of a powder coating green body (0.10-0.14 mm in thickness); and the sandwich stacking is a stacking of a double-sided powder coating thick green body (0.44-0.46 mm in thickness) and an uncoated thin sheet (0.10-0.14 mm in thickness) in the order of thick sheet-thin sheet-thick sheet.

[0016] More preferably, in step 4, the process parameters for the glue removal and sintering are as follows: a glue removal temperature of 500-700℃, a holding time of 2-8 h; a sintering temperature of 1750-1900℃, a holding time of 2-8 h, and a nitrogen pressure of 0.5-2 Mpa.

[0017] The process parameters for the sand blasting are as follows: a transmission speed of 200-1500 mm / min and a sand blasting pressure of 1.0-3.0 kgf / cm².

[0018] More preferably, the raw material for the powder coating further contains modified short basalt fibers, which account for 6-8% of the amount of boron nitride powder.

[0019] More preferably, the preparation method of the modified short basalt fibers is as follows:

[0020] S1-1: short basalt fibers are added to a solvent, a dispersant is added and ultrasonic dispersion is performed for 20-40 min to obtain a short basalt fiber suspension; tetrabutyl titanate is slowly added to anhydrous ethanol, and stirring is performed to obtain a 0.1-0.5 mol / L tetrabutyl titanate solution; aluminum nitrate is dissolved in deionized water, and stirring is performed to obtain a 0.1-0.3 mol / L aluminum nitrate solution;

[0021] S1-2: The chopped basalt fiber suspension is heated to 45~55℃ under stirring, and 0.1~0.5 mol / L tetrabutyl titanate solution, 0.1~0.3 mol / L aluminum nitrate solution and 25wt%~28wt% ammonia water are added at a speed of 1~3ml / min, the pH is adjusted to 8.8~9.2, the reaction is carried out for 3~5 hours, and then centrifugal separation, precipitation and drying are carried out to obtain the modified chopped basalt fiber.

[0022] More preferably, in the raw materials of the modified chopped basalt fiber, the mass ratio of the chopped basalt fiber suspension, 0.1~0.5 mol / L tetrabutyl titanate solution, 0.1~0.3 mol / L aluminum nitrate solution and 25wt%~28wt% ammonia water is 10:1~3:0.5~2:1~2.

[0023] In the raw materials of the chopped basalt fiber suspension, the chopped basalt fiber accounts for 5wt%~15wt% of the chopped basalt fiber suspension.

[0024] More preferably, the dispersant includes one of polyethylene glycol, polyacrylic acid and sodium hexametaphosphate; and the solvent includes one of deionized water and anhydrous ethanol.

[0025] Compared with the prior art, the present application has the following beneficial effects:

[0026] (1) The present application can control the size of the powder coating particle size by the dot array powder coating method, thereby avoiding the problem of density reduction caused by uneven shrinkage;

[0027] (2) The present application coats powder on the thick sheet and does not coat powder on the thin sheet, thereby reducing the influence of the insulating powder on the shrinkage rate of the thin green body;

[0028] (3) The present application adopts the thick sheet after powder coating and the thin sheet without powder coating to stack and remove glue and sinter, thereby reducing the problem of edge deformation during sintering of the thin sheet;

[0029] (4) The thickness of the powder coating of the present application can be freely controlled, and the appropriate powder coating thickness is controlled for green bodies of different sizes, and the sintered ceramic sheet is uniformly shrunk without cracking and other problems;

[0030] (5) The present application introduces modified chopped basalt fiber, specifically nano-titanium dioxide and nano-alumina loaded chopped basalt fiber. In terms of improving the purity of the ceramic substrate, the photocatalytic activity of nano-titanium dioxide can decompose organic impurities on the surface of the green body before sintering, effectively reducing the problem of incomplete glue removal, thereby improving the purity of the ceramic substrate. In terms of enhancing wear resistance and prolonging service life, nano-alumina significantly enhances the hardness and wear resistance of the loaded layer, making the sintered ceramic substrate more wear-resistant during use, and greatly improving its service life.

[0031] The addition of the chopped basalt fiber can adjust the rheological properties of the powder coating on one hand, so that the powder coating process is more easily controlled, and the uniformity and precision of the powder coating are effectively improved; on the other hand, the chopped basalt fiber BS16-6-76 is used as raw material, and the fiber forms crystalline inclusions during the cooling process after sintering, so as to fill in the voids, improve the compactness and buffer stress, and promote the performance improvement.

[0032] In addition, the nanoparticle loading layer increases the compatibility of the powder with other components of the powder coating, so that the powder coating system is more stable, and the agglomeration phenomenon is reduced. The nano-titanium dioxide, nano-aluminum oxide and chopped basalt fiber synergistically improve the overall performance of the ceramic substrate.

[0033] Through the above process, a ceramic sheet with a size of 10 inches and a thickness of 0.1-0.15 mm can be prepared. BRIEF DESCRIPTION OF DRAWINGS

[0034] The accompanying drawings are included to provide a further understanding of the present application, and constitute a part of the specification, illustrate the present application and explain the technical scheme of the present application, and do not constitute a limitation on the present application. In the drawings:

[0035] Figure 1 It is a sintering out of the furnace photo of the ceramic substrate of Example 4;

[0036] Figure 2 It is a sintering out of the furnace photo of the ceramic substrate of Comparative Example 1;

[0037] Figure 3 It is a graph showing the effect of the thickness of different powder coating printing on the sintering shrinkage rate of the green body of Example 4. DETAILED DESCRIPTION

[0038] The technical scheme in the embodiments of the present application will be described clearly and completely below in combination with the drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, but not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application.

[0039] It should be noted that there is no special limitation on the manufacturers of all raw materials involved in the present application, which exemplarily includes the following: in the embodiments below, the model of the chopped basalt fiber is BS16-6-76.

[0040] Example 1: A ceramic substrate green body powder coating sintering process, comprising the following steps:

[0041] Step 1: 30g boron nitride powder, 40g terpineol, 5g ethyl cellulose, 1g butyl benzyl phthalate, 0.5g phosphate ester are stirred uniformly, and three-roll grinding is used to obtain a powder;

[0042] Step 2: The powder is printed on the surface of the green body using a screen printing technique to form a full-plate powder pattern, and the thickness of the powder printing is 10um, to obtain a powder green body;

[0043] Step 3: 15 pieces of powder green body are taken for non-interlayer stacking (each green body is 0.12mm thick), to obtain a laminated green body;

[0044] Step 4: The laminated green body is degassed at 650℃ for 4 hours, and sintered at 1850℃ for 2 hours under a nitrogen pressure of 1.5Mpa, to obtain a ceramic sheet; then the ceramic sheet transmission speed is set to 500mm / min, and the surface is sandblasted using a sandblasting machine under a sandblasting pressure of 2.5kgf / cm² to remove the surface boron nitride powder, to obtain a ceramic substrate.

[0045] Example 2: A ceramic substrate green body powder sintering process, comprising the following steps:

[0046] Step 1: 30g boron nitride powder, 40g terpineol, 5g ethyl cellulose, 1g butyl benzyl phthalate, 0.5g phosphate ester are stirred uniformly, and three-roll grinding is used to obtain a powder;

[0047] Step 2: The powder is printed on the surface of the green body using a screen printing technique to form a full-plate powder pattern, and the thickness of the powder printing is 10um, to obtain a powder green body;

[0048] Step 3: 15 pieces of powder green body are taken for non-interlayer stacking (each green body is 0.12mm thick), to obtain a laminated green body;

[0049] Step 4: The laminated green body is degassed at 650℃ for 4 hours, and sintered at 1850℃ for 2 hours under a nitrogen pressure of 1.5Mpa, to obtain a ceramic sheet; then the ceramic sheet transmission speed is set to 500mm / min, and the surface is sandblasted using a sandblasting machine under a sandblasting pressure of 2.5kgf / cm² to remove the surface boron nitride powder, to obtain a ceramic substrate.

[0050] Example 3: A ceramic substrate green body powder sintering process, comprising the following steps:

[0051] Step 1: 30g boron nitride powder, 40g terpineol, 5g ethyl cellulose, 1g butyl benzyl phthalate, 0.5g phosphate ester are stirred uniformly, and three-roll grinding is used to obtain a powder;

[0052] Step 2: Print the powder on the surface of the green body by using the screen printing technology to form a dot-matrix powder pattern with a diameter of 150 um and a pitch of 265 um, and the thickness of the powder printing is 10 um, to obtain the powder-coated green body;

[0053] Step 3: Take 15 pieces of powder-coated green bodies to perform non-interlayer stacking (the thickness of each green body is 0.12 mm) to obtain the laminated green body;

[0054] Step 4: Perform the glue removal of the laminated green body at 650°C for 4 hours, and then perform the sintering at 1850°C for 2 hours under the nitrogen pressure of 1.5 Mpa to obtain the ceramic sheet; then set the transmission speed of the ceramic sheet to 500 mm / min, and use the sand blasting machine to perform the sand blasting on the surface of the ceramic sheet under the sand blasting pressure of 2.5 kgf / cm² to remove the boron nitride powder on the surface, to obtain the ceramic substrate.

[0055] Example 4: A powder-coated sintering process for a ceramic substrate green body, comprising the following steps:

[0056] Step 1: Stir 30 g of boron nitride powder, 40 g of terpineol, 5 g of ethyl cellulose, 1 g of butyl benzyl phthalate, and 0.5 g of phosphate to obtain the powder, and then use the three-roll mill to obtain the powder;

[0057] Step 2: Print the powder on the surface of the green body by using the screen printing technology to form a dot-matrix powder pattern with a diameter of 150 um and a pitch of 265 um, and the thickness of the powder printing is 10 um, to obtain the powder-coated green body;

[0058] Step 3: Take 15 pieces of powder-coated green bodies to perform interlayer stacking (the thick green body with powder (the thickness is 0.45 mm) and the thin sheet without powder (the thickness is 0.12 mm) are stacked in the order of thick sheet-thin sheet-thick sheet), to obtain the laminated green body;

[0059] Step 4: Perform the glue removal of the laminated green body at 650°C for 4 hours, and then perform the sintering at 1850°C for 2 hours under the nitrogen pressure of 1.5 Mpa to obtain the ceramic sheet; then set the transmission speed of the ceramic sheet to 500 mm / min, and use the sand blasting machine to perform the sand blasting on the surface of the ceramic sheet under the sand blasting pressure of 2.5 kgf / cm² to remove the boron nitride powder on the surface, to obtain the ceramic substrate; as Figure 1 shown.

[0060] Example 5: A powder-coated sintering process for a ceramic substrate green body, comprising the following steps:

[0061] Step 1: S1: Cut basalt fibers were added to deionized water, the cut basalt fibers accounted for 10wt% of the cut basalt fiber suspension, polyethylene glycol was added and ultrasonic dispersion was performed for 30min to obtain a cut basalt fiber suspension; tetrabutyl titanate was slowly added to anhydrous ethanol, stirring to obtain a 0.3mol / L tetrabutyl titanate solution; aluminum nitrate was dissolved in deionized water, stirring to obtain a 0.2mol / L aluminum nitrate solution; S2: under stirring conditions, the cut basalt fiber suspension was heated to 50℃, while 0.3mol / L tetrabutyl titanate solution, 0.2mol / L aluminum nitrate solution, 26wt% ammonia water were added at a speed of 2ml / min, the pH was adjusted to 9.0, and the reaction was performed for 4 hours, centrifugal separation, precipitation, drying to obtain modified cut basalt fibers;

[0062] Step 2: 30g boron nitride powder, 40g terpineol, 5g ethyl cellulose, 1g butyl benzyl phthalate, 0.5g phosphate ester, 2.1g modified cut basalt fibers were stirred uniformly, and three-roll grinding was used to obtain a powder;

[0063] Step 3: The powder was printed on the green body by using a screen printing technology to form a powder pattern of a dot matrix, and the thin sheet was not coated with powder, the diameter was 150um, the pitch was 265um, and the powder thickness was 10um, to obtain a powder green body;

[0064] Step 4: 15 pieces of powder green bodies were stacked in a sandwich manner (the thick green body with powder (thickness 0.45mm) and the thin sheet without powder (thickness 0.12mm) were stacked in turn, i.e. thick sheet-thin sheet-thick sheet), to obtain a laminated green body;

[0065] Step 5: The laminated green body was degreased at 650℃ for 4 hours, and sintered at 1850℃ for 2 hours under a nitrogen pressure of 1.5Mpa, to obtain a ceramic sheet; then the ceramic sheet transmission speed was set to 500mm / min, and the surface was sandblasted by using a sandblasting machine under a sandblasting pressure of 2.5kgf / cm² to remove the surface boron nitride powder, to obtain a ceramic substrate.

[0066] Comparative Example 1: Based on Example 1, the green body was not coated with powder, and the rest of the process was unchanged, specifically:

[0067] Step 1: 15 pieces of green bodies were stacked in a non-interlayer manner (each green body had a thickness of 0.12mm), to obtain a laminated green body;

[0068] Step 2: The laminated green body is degassed at 650°C for 4 hours, and sintered at 1850°C for 2 hours under a nitrogen pressure of 1.5 MPa to obtain the ceramic sheet; then the ceramic sheet is transferred at a speed of 500 mm / min, and the surface is sandblasted at a sandblasting pressure of 2.5 kgf / cm² using a sandblasting machine to remove the boron nitride powder on the surface, thereby obtaining the ceramic substrate. Figure 2

[0069] Comparative Example 2: Based on Example 1, no phosphoric acid ester is added, and the rest of the process remains unchanged, specifically:

[0070] Step 1: 30 g of boron nitride powder, 40 g of terpineol, 5 g of ethyl cellulose, and 1 g of butyl benzyl phthalate are stirred uniformly, and three-roll grinding is used to obtain the powder coating;

[0071] Step 2: The powder coating is printed on the surface of the green body using a screen printing technique to form a full-plate powder coating pattern, and the thickness of the powder coating printing is 10 um, thereby obtaining the powder-coated green body;

[0072] Step 3: 15 pieces of the powder-coated green body are stacked without interlayers (each green body has a thickness of 0.12 mm) to obtain the laminated green body;

[0073] Step 4: The laminated green body is degassed at 650°C for 4 hours, and sintered at 1850°C for 2 hours under a nitrogen pressure of 1.5 MPa to obtain the ceramic sheet; then the ceramic sheet is transferred at a speed of 500 mm / min, and the surface is sandblasted at a sandblasting pressure of 2.5 kgf / cm² using a sandblasting machine to remove the boron nitride powder on the surface, thereby obtaining the ceramic substrate.

[0074] Comparative Example 3: Based on Example 5, only unloaded short basalt fibers are added, and the rest of the process remains unchanged, specifically:

[0075] Step 1: 30 g of boron nitride powder, 40 g of terpineol, 5 g of ethyl cellulose, 1 g of butyl benzyl phthalate, 0.5 g of phosphoric acid ester, and 2.1 g of short basalt fibers are stirred uniformly, and three-roll grinding is used to obtain the powder coating;

[0076] Step 2: The powder coating is printed on both sides of the green body using a screen printing technique to form a dot matrix powder coating pattern, and the thin sheets are not coated with powder, with a diameter of 150 um and a pitch of 265 um, and the powder coating thickness is 10 um, thereby obtaining the powder-coated green body;

[0077] Step 3: 15 pieces of the powder-coated green body are stacked with interlayers (the double-sided powder-coated thick green body (thickness 0.45 mm) and the uncoated thin sheets (thickness 0.12 mm) are stacked in the order of thick sheet-thin sheet-thick sheet), thereby obtaining the laminated green body;

[0078] ​Step 4: The laminated green body is degassed at 650℃ for 4 hours, and sintered at 1850℃ for 2 hours under a nitrogen pressure of 1.5Mpa, to obtain the ceramic sheet; then the ceramic sheet transmission speed is set to 500mm / min, and the surface is sandblasted by a sandblasting machine under a sandblasting pressure of 2.5kgf / cm² to remove the surface boron nitride powder, to obtain the ceramic substrate.

[0079] Comparative Example 4, based on Example 5, only short basalt fibers loaded with nano titanium dioxide are added, and the rest of the process remains unchanged, specifically:

[0080] Step 1: S1: Add short basalt fibers to deionized water, the short basalt fibers account for 10wt% of the short basalt fiber suspension, add polyethylene glycol and ultrasonic dispersion for 30min to obtain a short basalt fiber suspension; slowly add tetrabutyl titanate to anhydrous ethanol, stir to obtain a 0.3mol / L tetrabutyl titanate solution; S2: under stirring conditions, add the short basalt fiber suspension to 50℃, while adding 0.3mol / L tetrabutyl titanate solution and 26wt% ammonia water at a speed of 2ml / min, adjust the pH to 9.0, react for 4 hours, centrifugal separation, precipitation, drying, to obtain modified short basalt fibers;

[0081] Step 2: Stir 30g boron nitride powder, 40g terpineol, 5g ethyl cellulose, 1g butyl benzyl phthalate, 0.5g phosphate, and 2.1g modified short basalt fibers uniformly, and use a three-roll mill to obtain a powder;

[0082] Step 3: Use screen printing technology to print the powder on both sides of the green body to form a dot matrix powder pattern, and the thin sheet is not coated with powder, the diameter is 150um, the pitch is 265um, and the powder thickness is 10um, to obtain a powder-coated green body;

[0083] Step 4: Take 15 pieces of powder-coated green body for sandwich stacking (double-sided powder-coated thick green body (thickness 0.45mm) and uncoated thin sheet (thickness 0.12mm) are stacked in turn, i.e. thick sheet-thin sheet-thick sheet), to obtain a laminated green body;

[0084] Step 5: The laminated green body is degassed at 650℃ for 4 hours, and sintered at 1850℃ for 2 hours under a nitrogen pressure of 1.5Mpa, to obtain the ceramic sheet; then the ceramic sheet transmission speed is set to 500mm / min, and the surface is sandblasted by a sandblasting machine under a sandblasting pressure of 2.5kgf / cm² to remove the surface boron nitride powder, to obtain the ceramic substrate.

[0085] Comparative Example 5, based on Example 5, the amount of modified short basalt fibers is increased, and the rest of the process remains unchanged, specifically:

[0086] Step 1: S1: Cut basalt fibers were added to deionized water, the cut basalt fibers accounted for 10wt% of the cut basalt fiber suspension, polyethylene glycol was added and ultrasonic dispersion was performed for 30min to obtain a cut basalt fiber suspension; tetrabutyl titanate was slowly added to anhydrous ethanol, stirring to obtain a 0.3mol / L tetrabutyl titanate solution; aluminum nitrate was dissolved in deionized water, stirring to obtain a 0.2mol / L aluminum nitrate solution; S2: under stirring conditions, the cut basalt fiber suspension was heated to 50°C, and at the same time, 0.3mol / L tetrabutyl titanate solution, 0.2mol / L aluminum nitrate solution, 26wt% ammonia water were added at a speed of 2ml / min, the pH was adjusted to 9.0, the reaction was carried out for 4 hours, centrifugal separation, precipitation, drying to obtain modified cut basalt fibers;

[0087] Step 2: 30g boron nitride powder, 40g terpineol, 5g ethyl cellulose, 1g butyl benzyl phthalate, 0.5g phosphate, 8g modified cut basalt fibers were stirred uniformly, and three-roll grinding was used to obtain a powder;

[0088] Step 3: The powder was printed on the green body by screen printing technology to form a powder pattern of dot matrix, and the thin sheet was not coated with powder, the diameter was 150um, the pitch was 265um, and the powder thickness was 10um, to obtain a powder green body;

[0089] Step 4: 15 pieces of powder green body were stacked in layers (double-sided powder coated thick green body (thickness 0.45mm) and uncoated thin sheet (thickness 0.12mm) were stacked in turn, i.e. thick sheet-thin sheet-thick sheet), to obtain a laminated green body;

[0090] Step 5: The laminated green body was degreased at 650°C for 4 hours, and sintered at 1850°C for 2 hours under a nitrogen pressure of 1.5Mpa, to obtain a ceramic sheet; then the ceramic sheet transmission speed was set to 500mm / min, and the surface was sandblasted by a sandblasting machine under a sandblasting pressure of 2.5kgf / cm² to remove the surface boron nitride powder, to obtain a ceramic substrate.

[0091] Detection experiment 1: The thickness of the powder printed on the ceramic substrate prepared by the ceramic substrate powder sintering process of Example 4 was controlled: the powder thickness was 5μm, 10μm, 15μm, 20μm, 25μm and 30μm, respectively, and the ceramic sheet density was detected, as shown in Figure 3

[0092] Conclusion: From Figure 3 ​It can be seen that the powder coating pattern in Example 4 adopts a dot array, the stacking mode uses a thick-thin sheet sandwich stacking mode, the sintered ceramic sheet has no adhesive sheet, the edge is flat, and the shrinkage rate and density are relatively large.

[0093] Detection Experiment 2: The ceramic substrates prepared by Examples 1-5 and Comparative Examples 1 were detected for performance, such as whether the substrate was adhered, flatness, shrinkage rate, and density, and the powder coating, stacking mode, and performance were compared, as shown in Table 1 below.

[0094]

[0095] Result Analysis: According to the data analysis in Table 1, it can be seen that the ceramic substrate prepared by the specific process of the present scheme has a size of 10 inches, which is increased from the original 6 inches, and a green body thickness of 0.12 mm, which is reduced from the original 0.45 mm. The green body of the powder coating can realize 8-20 green body stacking and glue sintering, and can avoid problems such as green body sintering, adhesion, and uneven shrinkage, thereby improving the yield and capacity of the ceramic sheet.

[0096] Detection Experiment 3: The ceramic substrates prepared by Examples 4-5 and Comparative Examples 1-5 were tested for impact resistance, and the test results are shown in Table 2.

[0097]

[0098] Result Analysis: According to the data analysis in Table 2, it can be seen from the data of Example 5 that the modified fiber can improve the compactness, stress buffering, wear resistance, and overall impact resistance. From the data of Example 4, it can be seen that without adding modified short basalt fiber, the impact resistance is lower than that of Example 5. The modified short basalt fiber can enhance the toughness of the ceramic substrate and improve the impact resistance of the material. From the data of Comparative Example 1, it can be seen that the powder coating can improve the surface performance and uniformity of the internal structure of the substrate, and the sandwich stacking can enhance the overall strength and impact resistance of the substrate. From the data of Comparative Example 2, it can be seen that without adding phosphate ester powder coating, the uniformity decreases, the overall performance of the substrate decreases, and the impact resistance is affected. From the data of Comparative Example 3, it can be seen that the modified short basalt fiber is better combined with the ceramic matrix, and can more effectively play the role of reinforcement and toughening. The unmodified fiber has relatively poor reinforcement effect. From the data of Comparative Example 4, it can be seen that compared with the fiber loaded with titanium dioxide and aluminum oxide in Example 5, the effect is weaker, and the improvement of the impact resistance of the ceramic substrate is limited. From the data of Comparative Example 5, it can be seen that too much fiber will cause uneven dispersion of the fiber, forming agglomeration, and thus reducing the performance of the material.

[0099] It will be apparent to those skilled in the art that the application is not limited to the details of the above-exemplified embodiments and that the present application can be implemented in other particular forms without departing from the spirit or essential characteristics of the present application. The embodiments should therefore be considered in all respects as illustrative and not restrictive, the scope of the application being indicated by the appended claims rather than by the above description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. No reference signs in the claims should be considered as limiting the scope of the claims with respect to the figures of the patent document.

Claims

1. A ceramic substrate green body dusting sintering process characterized by: The method comprises the following steps: Step 1: uniformly stir boron nitride powder, terpineol, ethyl cellulose, butyl benzyl phthalate and phosphate, grind, and obtain a powder; Step 2: print the powder on the surface of a green body by using a silk screen printing technology to form a powder pattern, and obtain a powder green body; Step 3: stack N powder green bodies to obtain a laminated green body; Step 4: sequentially perform glue removal sintering and sand blasting on the laminated green body to obtain a ceramic substrate; The raw material of the powder further comprises modified short basalt fibers, and the modified short basalt fibers account for 6-8% of the amount of boron nitride powder. The preparation method of the modified short basalt fibers is as follows: S1-1: add short basalt fibers to a solvent, add a dispersant and ultrasonically disperse for 20-40 minutes to obtain a short basalt fiber suspension; slowly add tetrabutyl titanate to anhydrous ethanol, and stir to obtain a 0.1-0.5 mol / L tetrabutyl titanate solution; Dissolve aluminum nitrate in deionized water, and stir to obtain a 0.1-0.3 mol / L aluminum nitrate solution; S1-2: under stirring, heat the short basalt fiber suspension to 45-55 DEG C, and simultaneously add the 0.1-0.5 mol / L tetrabutyl titanate solution, the 0.1-0.3 mol / L aluminum nitrate solution and 25 wt%-28 wt% ammonia water at a speed of 1-3 ml / min, adjust the pH to 8.8-9.2, react for 3-5 hours, centrifugally separate, precipitate and dry to obtain modified short basalt fibers; In step 4, the process parameters of the glue removal sintering are as follows: the glue removal temperature is 500-700 DEG C, the holding time is 2-8 hours, the sintering temperature is 1750-1900 DEG C, the holding time is 2-8 hours, and the nitrogen pressure is 0.5-2 MPa; The process parameters of the sand blasting are as follows: the transmission speed is 200-1500 mm / min, and the sand blasting pressure is 1.0-3.0 kgf / cm².

2. A process for dusting and sintering of a ceramic substrate green body as claimed in claim 1, wherein: In step 1, in the raw material of the powder, by mass fraction: 25-40 parts of boron nitride powder, 25-50 parts of terpineol, 2-8 parts of ethyl cellulose, 0.2-5 parts of butyl benzyl phthalate and 0.2-5 parts of phosphate.

3. A process for powder application and sintering of a ceramic substrate green body as claimed in claim 1, wherein: In step 2, the powder pattern comprises one of a dot array and a full plate; and the thickness of the powder printing is 3-30 um.

4. The process for powder application and sintering of a ceramic substrate green body according to claim 1, characterized in that: In step 3, N is greater than or equal to 8; and the stacking mode comprises one of a sandwich stacking mode and a non-sandwich stacking mode.

5. The process for dusting and sintering of a ceramic substrate green body as claimed in claim 1, wherein: In the raw material of the modified short basalt fibers, the mass ratio of the short basalt fiber suspension, the 0.1-0.5 mol / L tetrabutyl titanate solution, the 0.1-0.3 mol / L aluminum nitrate solution and the 25 wt%-28 wt% ammonia water is 10:1-3:0.5-2:1-2; In the raw material of the short basalt fiber suspension, the short basalt fibers account for 5 wt%-15 wt% of the short basalt fiber suspension.

6. A process for powder application and sintering of a ceramic substrate green body as claimed in claim 1, wherein: The dispersant comprises one of polyethylene glycol, polyacrylic acid and sodium hexametaphosphate; and the solvent comprises one of deionized water and anhydrous ethanol.

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