CN115321954B - Preparation method of ceramic substrate and low-temperature co-fired ceramic substrate - Google Patents
Preparation method of ceramic substrate and low-temperature co-fired ceramic substrate Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 191
- 239000000758 substrate Substances 0.000 title claims abstract description 98
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 238000003825 pressing Methods 0.000 claims abstract description 76
- 238000000926 separation method Methods 0.000 claims abstract description 72
- 238000005245 sintering Methods 0.000 claims abstract description 65
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 61
- 238000000462 isostatic pressing Methods 0.000 claims abstract description 54
- 238000007789 sealing Methods 0.000 claims abstract description 16
- 239000010410 layer Substances 0.000 claims description 131
- 239000011241 protective layer Substances 0.000 claims description 36
- 239000000463 material Substances 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 20
- 238000007599 discharging Methods 0.000 claims description 18
- 239000003292 glue Substances 0.000 claims description 18
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 14
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 229910052863 mullite Inorganic materials 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 48
- 238000005520 cutting process Methods 0.000 description 16
- 229910000831 Steel Inorganic materials 0.000 description 15
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 9
- 229910052782 aluminium Inorganic materials 0.000 description 9
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- 238000010030 laminating Methods 0.000 description 8
- 238000004080 punching Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 238000003475 lamination Methods 0.000 description 7
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- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007729 constrained sintering Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
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- 230000001419 dependent effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract
The application relates to the technical field of electronic ceramic technology, in particular to a preparation method of a ceramic substrate and a low-temperature co-fired ceramic substrate. The preparation method of the ceramic substrate provided by the application comprises the following steps: making the raw porcelain band into raw porcelain blocks; respectively attaching a first separation layer and a second separation layer to the two surfaces of the raw porcelain bar block, respectively attaching a first protection layer and a second protection layer, and sequentially stacking the second protection layer, the second separation layer, the raw porcelain bar block, the first separation layer and the first protection layer to form a to-be-sintered object block; sealing the object to be sintered, performing isostatic pressing treatment, and respectively attaching a first pressing plate and a second pressing plate to the two surfaces of the object to be sintered; and sintering the to-be-sintered object blocks attached with the first pressing plate and the second pressing plate to sinter the raw porcelain blocks into the ceramic substrate. The preparation method can well control the shrinkage rate of the ceramic substrate, and the obtained ceramic substrate has smooth surface and good flatness and can remarkably improve sintering efficiency.
Description
Technical Field
The application belongs to the technical field of electronic ceramic technology, and particularly relates to a preparation method of a ceramic substrate and a low-temperature co-fired ceramic substrate.
Background
The low temperature co-fired Ceramic (LTCC) technology is a remarkable integrated component technology developed in the eighties of the 20 th century, is a passive integrated and mixed circuit packaging technology widely used at present, integrates elements such as capacitance, resistance, inductance and the like into a multi-layer substrate, can be directly used as a packaging substrate of an integrated circuit (Integrated Circuit, IC), has the outstanding advantages of high reliability, high integration level and high performance, and provides a good solution for the high-speed development of radio frequency and microwave systems. However, as the performance requirements of the products are higher and higher, the existing low-temperature co-fired ceramic substrate is more and more difficult to meet the requirements of the current products, and the shrinkage of the low-temperature co-fired ceramic substrate after sintering is uneven, for example, the shrinkage rate of the low-temperature co-fired ceramic substrate in the same direction of an X/Y axis is different, the difference is up to +/-0.8%, and the flatness is also greatly different, so that the consistency of the low-temperature co-fired ceramic substrates sintered in the same batch is poor. Therefore, how to control the uniformity of shrinkage and flatness becomes an important direction of low-temperature co-fired ceramic substrates.
Currently, the process methods for controlling shrinkage and flatness are mainly controlled in sintering processes, including pressure-assisted sintering, pressureless assisted sintering, self-constrained sintering and composite co-sintering. By controlling the shrinkage and flatness of the low temperature co-fired ceramic substrate during the sintering process, the equipment requirements are generally very high, the material cost is high, the shrinkage control precision is poor, and cracking and other phenomena are easily caused for thinner products, so that the production efficiency is reduced.
Disclosure of Invention
The purpose of the application is to provide a preparation method of a ceramic substrate and a low-temperature co-fired ceramic substrate, and aims to solve the technical problem of how to more effectively control the shrinkage rate of a ceramic substrate product.
In order to achieve the purposes of the application, the technical scheme adopted by the application is as follows:
in a first aspect, the present application provides a method for preparing a ceramic substrate, including the steps of:
making the raw porcelain band into raw porcelain blocks;
respectively attaching a first separation layer and a second separation layer to the two surfaces of the raw porcelain bar block, respectively attaching a first protection layer and a second protection layer, and sequentially stacking the second protection layer, the second separation layer, the raw porcelain bar block, the first separation layer and the first protection layer to form a to-be-sintered object block;
sealing the object to be sintered, performing isostatic pressing treatment, and respectively attaching a first pressing plate and a second pressing plate to the two surfaces of the object to be sintered;
and sintering the to-be-sintered object blocks attached with the first pressing plate and the second pressing plate to sinter the raw porcelain blocks into the ceramic substrate.
In a second aspect, the present application provides a low temperature co-fired ceramic substrate, the low temperature co-fired ceramic substrate being prepared by the preparation method of the present application.
According to the preparation method of the ceramic substrate, firstly, the two surfaces of the raw porcelain bar block are respectively attached to the separating layer and the protecting layer for isostatic pressing treatment, then the pressing plate is attached to the separating layer for sintering, the protecting layer can protect the raw porcelain bar block in the process, the shrinkage rate is controlled to prevent cracking of a sintered product, the separating layer separates the raw porcelain bar block from the protecting layer, the raw porcelain bar block and the protecting layer are prevented from being fused together in the sintering process, so that the ceramic substrate obtained in the later stage is better separated from the protecting layer, and the pressing plate can further control the shrinkage rate of the raw porcelain bar block after being sintered into the ceramic substrate. Therefore, the preparation method can be used for controlling the shrinkage rate of the ceramic substrate well, the obtained ceramic substrate product has smooth surface and good flatness, meanwhile, the preparation method can be used for improving the consistency of the ceramic substrate product, remarkably improving the sintering efficiency and has good application prospect in the field of ceramic substrate preparation.
The low-temperature co-fired ceramic substrate provided by the second aspect of the application is prepared by the special preparation method, so that the shrinkage rate of the low-temperature co-fired ceramic substrate can be well controlled, and the product has smooth surface, good flatness and good consistency.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a separation layer and a separation layer attached to two surfaces of a raw porcelain bar block in a preparation method of a ceramic substrate provided by an embodiment of the application;
fig. 2 is a schematic diagram of a separation layer, a separation layer and a pressing plate attached to two surfaces of a raw ceramic bar block in the preparation method of a ceramic substrate provided in the embodiment of the application;
wherein, each reference sign in the figure:
10-raw porcelain bar block, 21-first separating layer, 22-second separating layer, 31-first protective layer, 32-second protective layer, 41-first pressing plate, 42-second pressing plate.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved by the present application more clear, the present application is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the present application.
In this application, the term "and/or" describes an association relationship of an association object, which means that there may be three relationships, for example, a and/or B may mean: a alone, a and B together, and B alone. Wherein A, B may be singular or plural. The character "/" generally indicates that the context-dependent object is an "or" relationship.
In the present application, "at least one" means one or more, and "a plurality" means two or more. "at least one of" or the like means any combination of these items, including any combination of single item(s) or plural items(s).
It should be understood that, in various embodiments of the present application, the sequence number of each process does not mean that the sequence of execution is sequential, and some or all of the steps may be executed in parallel or sequentially, where the execution sequence of each process should be determined by its functions and internal logic, and should not constitute any limitation on the implementation process of the embodiments of the present application.
The terminology used in the embodiments of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in this application and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated for distinguishing between objects such as substances from each other. For example, a first XX may also be referred to as a second XX, and similarly, a second XX may also be referred to as a first XX, without departing from the scope of embodiments of the present application. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature.
An embodiment of the present application provides a method for preparing a ceramic substrate, including the following steps:
s01: making the raw porcelain band into raw porcelain blocks;
s02: respectively attaching a first separation layer and a second separation layer to the two surfaces of the raw porcelain bar block, respectively attaching a first protection layer and a second protection layer, and sequentially stacking the second protection layer, the second separation layer, the raw porcelain bar block, the first separation layer and the first protection layer to form a to-be-sintered object block;
s03: sealing the object to be sintered, performing isostatic pressing treatment, and respectively attaching a first pressing plate and a second pressing plate to the two surfaces of the object to be sintered;
s04: and sintering the to-be-sintered object blocks attached with the first pressing plate and the second pressing plate to sinter the raw porcelain blocks into the ceramic substrate.
According to the preparation method of the ceramic substrate, auxiliary materials such as the separating layer, the protecting layer and the pressing plate are comprehensively utilized, shrinkage rate of the raw ceramic bar block during sintering into the ceramic substrate can be effectively controlled, specifically, the separating layer and the protecting layer are attached to two surfaces of the raw ceramic bar block firstly, isostatic pressing treatment is carried out after sealing, then the pressing plate is attached to two surfaces of the raw ceramic bar block for sintering, the protecting layer can protect the raw ceramic bar block during sintering, shrinkage rate is controlled to prevent cracking of a product after sintering, the separating layer separates the raw ceramic bar block from the protecting layer, the raw ceramic bar block and the protecting layer are prevented from being fused together during sintering, and accordingly the ceramic substrate obtained in the later period is better separated from the protecting layer, and the shrinkage rate of the raw ceramic bar block after sintering into the ceramic substrate can be further controlled by the pressing plate. Therefore, the preparation method of the embodiment of the application can finally well control the shrinkage rate of the ceramic substrate, the obtained ceramic substrate product has smooth surface and good flatness, meanwhile, the preparation method can improve the consistency of the ceramic substrate product, remarkably improve the sintering efficiency and has good application prospect in the field of ceramic substrate preparation.
Step S01 is a preparation step for a ceramic block.
In an embodiment, the ceramic substrate obtained by the preparation method of the present application may be an LTCC ceramic substrate, and the LTCC ceramic substrate is obtained by providing a green ceramic tape selected from LTCC green ceramic tapes, and preparing the LTCC green ceramic tape into a green ceramic tile and then performing the preparation method of the present application. Specifically, the step of making the green tape into a green porcelain bar block may include: LTCC green tapes (commercially available) are punched, laminated to give green porcelain blocks of the desired thickness, and then cut for subsequent step flow.
In one embodiment, the thickness of the raw porcelain bar block is 0.8-1.2 mm, and specifically, can be 0.8mm, 1.0mm, 1.2mm, etc.; sintering the raw porcelain blocks with the thickness to obtain the ceramic substrate with the corresponding thickness.
Step S02 is a step of attaching the isolation layer and the protection layer.
As shown in fig. 1, the first separation layer 21 and the second separation layer 22 are attached to two surfaces of the raw porcelain bar block 10, and then the first protection layer 31 and the second protection layer 32 are attached to the two surfaces of the raw porcelain bar block 10, so that the second protection layer 32, the second separation layer 22, the raw porcelain bar block 10, the first separation layer 21 and the first protection layer 31 are sequentially stacked to form a block to be sintered.
In an embodiment, the first separation layer and the second separation layer may be separation layers of the same thickness and the same material, specifically, the thickness of each of the first separation layer and the second separation layer is 0.08 to 0.12mm, for example, 0.08mm, 0.10mm, 0.12mm, etc.; the materials of the first separation layer and the second separation layer are both selected from carbon-based sacrificial materials, such as carbon tapes and carbon black paste, the low-temperature co-fired ceramic sintering generally has detail shrinkage at 850 ℃ and above 600 ℃, and the carbon-based sacrificial materials are generally burnt out at 880 ℃, so that the separation layer has good separation effect between the raw porcelain bars and the protective layer. The first separation layer and the second separation layer with the same thickness and material can uniformly separate the two surfaces of the raw porcelain bar block from the protective layer. The separation layer is arranged between the protection layer and the raw porcelain bar block and is mainly used for separating the protection layer from a final product, the protection layer and the raw porcelain bar block are prevented from being bonded together in the sintering process, the later protection layer and the ceramic substrate product are also convenient to separate, and the separation process of the protection layer and the ceramic substrate product is simplified.
In an embodiment, the first protective layer and the second protective layer may be protective layers with the same thickness and the same material, specifically, the thickness of the first protective layer and the second protective layer is 0.12-0.30 mm, for example, 0.12mm, 0.16mm, 0.18mm, 0.20mm, 0.25mm, etc.; the material of the first protective layer and the second protective layer is selected from at least one of alumina ceramic, zirconia ceramic and aluminum nitride ceramic. High-temperature ceramics such as alumina, zirconia, aluminum nitride and the like have the temperature resistance of more than 1200 ℃ and the flatness of less than 0.1%, can well protect ceramic substrate products, prevent the products from cracking and control the shrinkage rate.
Step S03 is an isostatic pressing treatment and pressing plate attaching step.
Specifically, the isostatic pressing treatment may be a warm isostatic pressing treatment, in which the to-be-sintered object block composed of the second protective layer, the second separation layer, the raw porcelain bar block, the first separation layer and the first protective layer which are sequentially stacked is placed in an aluminum foil bag for vacuum sealing, and then placed in a warm water isostatic press for isostatic pressing, and the isostatic pressing curve can be changed according to different shrinkage rates.
In one embodiment, the step of isostatic pressing after sealing the block to be sintered comprises: starting pressurizing the sealed block to be sintered at 70-80 ℃ and 0-0.5 MPa: pressurizing for 8-12 min to 5-10 MPa, maintaining the pressure for 8-12 min, continuously pressurizing for 10-20 min to 14-16 MPa, maintaining the pressure for 18-22 min, and finally pressurizing for 8-12 min to 19-21 MPa, maintaining the pressure for 1.5-2.5 hours. Specifically, the pressure is increased from 0MPa for 10 minutes to 10MPa, and the pressure is maintained for 10 minutes; pressurizing at 10MPa for 20 minutes to 15MPa, and maintaining the pressure for 20 minutes; pressurizing for 10 minutes to 20MPa, maintaining the pressure for 2 hours, and ending the isostatic pressing. The raw porcelain bar block, the separating layer and the protective layer are combined together in a lamination and isostatic pressing mode, so that a firm raw porcelain blank body can be obtained, and the density and hardness of a final ceramic substrate product can be improved.
As shown in fig. 2, the two surfaces of the isostatically processed block to be sintered (the second protective layer 32, the second separation layer 22, the raw porcelain block 10, the first separation layer 21, and the first protective layer 32, which are laminated in this order) are respectively bonded to the first platen 41 and the second platen 42, thereby forming the laminated second platen 42, second protective layer 32, second separation layer 22, raw porcelain block 10, first separation layer 21, first protective layer 32, and first platen 41. The green ceramic tile 10 can be sintered to produce a ceramic substrate having a controllable shrinkage factor, a high hardness, and a good uniformity by performing the sintering process under the conditions of the bonded first and second separation layers 21 and 22, first and second protective layers 31 and 32, and first and second pressing plates 41 and 42.
In one embodiment, the first pressing plate and the second pressing plate can be the same pressing plate, the weight is 2-6 kg, and the pressing plates with different weights are selected according to different required shrinkage rates; the material can be selected from alumina, zirconia, corundum mullite and other materials, the temperature resistance is higher than 1300 ℃, the porosity of the first pressing plate and the second pressing plate is 20-30%, the roughness is less than 0.5 mu m, and the flatness is less than 0.1%. Placing the object to be sintered after isostatic pressing in the middle of the first pressing plate and the second pressing plate with the parameters, and then placing the object to be sintered in a sintering furnace for sintering, wherein the pressing plates can effectively control the shrinkage rate and the flatness, and the LTCC substrate suitable for various thicknesses is prepared.
Step S04 is a sintering step.
In one embodiment, the step of sintering includes: firstly, glue discharging treatment is carried out at 450-480 ℃, and then the temperature is raised to 800-900 ℃ for sintering. Specifically, the temperature of the adhesive discharge can be 450 ℃, 460 ℃, 480 ℃ and the like, the heating rate of the adhesive discharge to 800-900 ℃ can be 5-7 ℃/min, and the sintering time at 800-900 ℃ can be 10-15 minutes. Such a sintering process may sinter the LTCC green ceramic tile into an LTCC ceramic substrate.
In one embodiment, a method for preparing an LTCC ceramic substrate includes the steps of:
step one：And punching the LTCC green ceramic tape, laminating to obtain LTCC green ceramic blocks with required thickness, and cutting into green ceramic blocks to be processed.
Step two:and respectively placing a layer of carbon-based sacrificial material film with the same thickness on the upper surface and the lower surface of the obtained raw porcelain bar block as a separating layer for lamination, and then respectively placing a layer of high-temperature porcelain bar block with the same thickness on the upper surface and the lower surface as a protecting layer for lamination to obtain a new to-be-sintered object block.
Step three:and placing steel sheets on the upper and lower surfaces of the obtained to-be-sintered object, placing the to-be-sintered object in an aluminum foil bag for vacuumizing and sealing, and then placing the to-be-sintered object in a warm water isostatic press for isostatic pressing treatment, wherein an isostatic pressing curve is changed according to control of different shrinkage rates.
Step four:respectively placing a pressing plate on the upper surface and the lower surface of the to-be-sintered object block obtained after isostatic pressing treatment, matching the weights according to different shrinkage rates, and then placing the to-be-sintered object block in a sintering furnace for sintering: raising the temperature from room temperature (25-27 ℃) to 450-480 ℃, preserving heat, discharging glue, continuing raising the temperature to 800-900 ℃ after the glue discharging is completed, preserving heat and sintering; and (3) naturally cooling after sintering, removing the pressing plate, the protective layer and the isolation layer, and cleaning the surface of the product to obtain the LTCC ceramic substrate with the required shrinkage rate.
The preparation method of the embodiment of the application can effectively control the shrinkage and flatness of the LTCC ceramic substrate product, the surface of the sintered product is smooth, the flatness of the sintered product is less than 0.2% of the side length of the product, and the tolerance range of the linear shrinkage on the X/Y axis is less than +/-0.3%; and the consistency, density and hardness of the product are improved, the porosity is reduced, and the sintering efficiency is remarkably improved.
The second aspect of the embodiment of the present application provides a low-temperature co-fired ceramic substrate, which is prepared by the specific preparation method described in the embodiments of the present application.
The low-temperature co-fired ceramic substrate provided by the embodiment of the application is prepared by the specific preparation method, so that the shrinkage rate of the low-temperature co-fired ceramic substrate can be well controlled, and the product has smooth surface, good flatness and good consistency.
The following description is made with reference to specific embodiments.
Example 1
A preparation method of an LTCC ceramic substrate comprises the following steps:
s11: preparing an LTCC green ceramic tape (MG 60 of Shanghai crystal material new material Co., ltd.), punching and laminating the green ceramic tape to obtain an LTCC green ceramic bar block with the thickness of 0.8mm, cutting the LTCC green ceramic bar block with the thickness of 0.8mm into small green ceramic bar blocks with the thickness of 50mm and 50mm, and taking 7 small green ceramic bar blocks for sintering;
s12: preparing two carbon strips of carbon-based material with the thickness of 0.1mm, and cutting the carbon strips into 50mm small pieces serving as a first separation layer and a second separation layer; preparing two aluminum nitride ceramic green ceramic tapes with the thickness of 0.15mm, and cutting the aluminum nitride ceramic green ceramic tapes into 50mm small blocks serving as a first protective layer and a second protective layer;
and respectively attaching a first separation layer and a second separation layer to the two surfaces of the obtained small raw porcelain bar block, respectively attaching a first protection layer and a second protection layer, and sequentially stacking the second protection layer, the second separation layer, the raw porcelain bar block, the first separation layer and the first protection layer to form a to-be-sintered object block.
S13: placing steel sheets up and down on a to-be-sintered object block, placing the steel sheets in an aluminum foil bag, vacuumizing and sealing; opening a warm water isostatic pressing machine, preheating to 75 ℃, then placing a sealed object to be sintered, carrying out isostatic pressing treatment according to an isostatic pressing curve, and obtaining a new green ceramic blank after finishing; the isostatic pressure curve is: pressurizing at 0MPa for 10 minutes to 10MPa, and maintaining the pressure for 10 minutes; pressurizing at 10MPa for 20 minutes to 15MPa, and maintaining the pressure for 20 minutes; pressurizing for 10 minutes to 20MPa, maintaining the pressure for 2 hours, and ending the isostatic pressing.
Two alumina pressing plates weighing 6kg are prepared as a first pressing plate and a second pressing plate, and a green ceramic body obtained through isostatic pressing treatment is placed between the first pressing plate and the second pressing plate for lamination.
S14: placing a green ceramic green body formed by combining a first pressing plate and a second pressing plate in a sintering furnace for sintering: starting to rise to 450 ℃ from room temperature at 1 ℃/min, preserving heat for 2 hours to perform glue discharging, and continuously rising to 850 ℃ at 6 ℃/min after the glue discharging is completed, preserving heat for 10 minutes, and sintering into porcelain; and (3) naturally cooling after sintering, removing the pressing plate and the protective layer, and then cleaning the surface to obtain the LTCC ceramic substrate product.
The LTCC ceramic substrate product was measured and the shrinkage repeatability was + -0.05% over multiple repeated experiments. The surface of the LTCC ceramic substrate product is smooth by visual inspection, the flatness of the product is 0.03mm, the repeatability of the flatness is +/-0.05%, and the flatness is good by testing through a step meter. Test data are shown in table 1 below.
TABLE 1
Example 2
A preparation method of an LTCC ceramic substrate comprises the following steps:
s21: preparing a crystal material LTCC green ceramic tape (MG 60 of Shanghai crystal material new material science and technology Co., ltd.), punching and laminating the green ceramic tape to obtain an LTCC green ceramic bar block with the thickness of 1mm, and cutting the LTCC green ceramic bar block with the thickness of 1mm into small green ceramic bar blocks with the thickness of 50mm and 50 mm;
s22: preparing two carbon strips of carbon-based material with the thickness of 0.1mm, and cutting the carbon strips into 50mm small pieces serving as a first separation layer and a second separation layer; preparing two aluminum nitride ceramic green ceramic tapes with the thickness of 0.2mm, and cutting the aluminum nitride ceramic green ceramic tapes into 50mm small blocks serving as a first protective layer and a second protective layer;
and respectively attaching a first separation layer and a second separation layer to the two surfaces of the obtained small raw porcelain bar block, respectively attaching a first protection layer and a second protection layer, and sequentially stacking the second protection layer, the second separation layer, the raw porcelain bar block, the first separation layer and the first protection layer to form a to-be-sintered object block.
S23: placing steel sheets up and down on a to-be-sintered object block, placing the steel sheets in an aluminum foil bag, vacuumizing and sealing; opening a warm water isostatic pressing machine, preheating to 75 ℃, then placing a sealed object to be sintered, carrying out isostatic pressing treatment according to an isostatic pressing curve, and obtaining a new green ceramic blank after finishing; the isostatic pressure curve is: pressurizing at 0MPa for 10 minutes to 10MPa, and maintaining the pressure for 10 minutes; pressurizing at 10MPa for 20 minutes to 15MPa, and maintaining the pressure for 20 minutes; pressurizing for 10 minutes to 20MPa, maintaining the pressure for 2 hours, and ending the isostatic pressing.
Two alumina pressing plates weighing 6kg are prepared as a first pressing plate and a second pressing plate, and a green ceramic body obtained through isostatic pressing treatment is placed between the first pressing plate and the second pressing plate for lamination.
S24: placing a green ceramic green body formed by combining a first pressing plate and a second pressing plate in a sintering furnace for sintering: starting to rise to 450 ℃ from room temperature at 1 ℃/min, preserving heat for 2 hours to perform glue discharging, and continuously rising to 850 ℃ at 6 ℃/min after the glue discharging is completed, preserving heat for 10 minutes, and sintering into porcelain; and (3) naturally cooling after sintering, removing the pressing plate and the protective layer, and then cleaning the surface to obtain the LTCC ceramic substrate product.
The LTCC ceramic substrate product was measured and the shrinkage repeatability was + -0.05% over multiple repeated experiments. The surface of the LTCC ceramic substrate product is smooth by visual inspection, the flatness of the product is 0.02mm, the repeatability of the flatness is +/-0.05%, and the flatness is good by testing through a step meter. Test data are shown in table 2 below.
TABLE 2
Example 3
A preparation method of an LTCC ceramic substrate comprises the following steps:
s31: preparing an LTCC green ceramic tape (A6 of the American ferro company), punching and laminating the green ceramic tape to obtain an LTCC green ceramic bar block with the thickness of 1mm, and cutting the LTCC green ceramic bar block with the thickness of 1mm into small green ceramic bar blocks with the thickness of 50 mm;
s32: preparing two carbon strips of carbon-based material with the thickness of 0.1mm, and cutting the carbon strips into 50mm small pieces serving as a first separation layer and a second separation layer; preparing two aluminum nitride ceramic green ceramic tapes with the thickness of 0.15mm, and cutting the aluminum nitride ceramic green ceramic tapes into 50mm small blocks serving as a first protective layer and a second protective layer;
and respectively attaching a first separation layer and a second separation layer to the two surfaces of the obtained small raw porcelain bar block, respectively attaching a first protection layer and a second protection layer, and sequentially stacking the second protection layer, the second separation layer, the raw porcelain bar block, the first separation layer and the first protection layer to form a to-be-sintered object block.
S33: placing steel sheets up and down on a to-be-sintered object block, placing the steel sheets in an aluminum foil bag, vacuumizing and sealing; opening a warm water isostatic pressing machine, preheating to 75 ℃, then placing a sealed object to be sintered, carrying out isostatic pressing treatment according to an isostatic pressing curve, and obtaining a new green ceramic blank after finishing; the isostatic pressure curve is: pressurizing at 0MPa for 10 minutes to 5MPa, and maintaining the pressure for 10 minutes; pressurizing at 10MPa for 10 minutes to 15MPa, and maintaining the pressure for 20 minutes; pressurizing for 10 minutes to 20MPa, maintaining the pressure for 2 hours, and ending the isostatic pressing.
Two zirconia pressing plates weighing 4kg are prepared as a first pressing plate and a second pressing plate, and the green ceramic body obtained by isostatic pressing treatment is placed between the first pressing plate and the second pressing plate for lamination.
S34: placing a green ceramic green body formed by combining a first pressing plate and a second pressing plate in a sintering furnace for sintering: starting to rise to 450 ℃ from room temperature at 0.8 ℃/min, preserving heat for 2 hours, discharging glue, continuously rising to 850 ℃ at 5 ℃/min after the glue discharging is completed, preserving heat for 10 minutes, and sintering into porcelain; and (3) naturally cooling after sintering, removing the pressing plate and the protective layer, and then cleaning the surface to obtain the LTCC ceramic substrate product.
The LTCC ceramic substrate product was measured and the shrinkage repeatability was + -0.05% over multiple repeated experiments. The surface of the LTCC ceramic substrate product is smooth by visual inspection, the flatness of the product is 0.04mm, the repeatability of the flatness is +/-0.05%, and the flatness is good by testing through a step meter. Test data are shown in table 3 below.
TABLE 3 Table 3
Example 4
A preparation method of an LTCC ceramic substrate comprises the following steps:
s41: preparing an LTCC green ceramic tape (951C 2 of DuPont company in U.S.) and punching and laminating the green ceramic tape to obtain an LTCC green ceramic bar block with the thickness of 1mm, and cutting the 1mm LTCC green ceramic bar block into small green ceramic bar blocks with the thickness of 50 mm;
s42: preparing two carbon strips of carbon-based material with the thickness of 0.1mm, and cutting the carbon strips into 50mm small pieces serving as a first separation layer and a second separation layer; preparing two aluminum nitride ceramic green ceramic tapes with the thickness of 0.3mm, and cutting the aluminum nitride ceramic green ceramic tapes into 50mm small blocks serving as a first protective layer and a second protective layer;
and respectively attaching a first separation layer and a second separation layer to the two surfaces of the obtained small raw porcelain bar block, respectively attaching a first protection layer and a second protection layer, and sequentially stacking the second protection layer, the second separation layer, the raw porcelain bar block, the first separation layer and the first protection layer to form a to-be-sintered object block.
S43: placing steel sheets up and down on a to-be-sintered object block, placing the steel sheets in an aluminum foil bag, vacuumizing and sealing; opening a warm water isostatic pressing machine, preheating to 75 ℃, then placing a sealed object to be sintered, carrying out isostatic pressing treatment according to an isostatic pressing curve, and obtaining a new green ceramic blank after finishing; the isostatic pressure curve is: pressurizing at 0MPa for 10 minutes to 10MPa, and maintaining the pressure for 10 minutes; pressurizing at 10MPa for 10 minutes to 15MPa, and maintaining the pressure for 20 minutes; pressurizing for 10 minutes to 20MPa, maintaining the pressure for 2 hours, and ending the isostatic pressing.
Two oxidizing pick pressing plates weighing 4kg are prepared as a first pressing plate and a second pressing plate, and a green ceramic blank obtained through isostatic pressing treatment is placed between the first pressing plate and the second pressing plate for lamination.
S44: placing a green ceramic green body formed by combining a first pressing plate and a second pressing plate in a sintering furnace for sintering: starting to rise to 450 ℃ from room temperature at 1.2 ℃/min, preserving heat for 2 hours to perform glue discharging, and continuously rising to 850 ℃ at 7 ℃/min after the glue discharging is completed, preserving heat for 15 minutes, and sintering into porcelain; and (3) naturally cooling after sintering, removing the pressing plate and the protective layer, and then cleaning the surface to obtain the LTCC ceramic substrate product.
The LTCC ceramic substrate product was measured and the shrinkage repeatability was + -0.05% over multiple repeated experiments. The surface of the LTCC ceramic substrate product is smooth by visual inspection, the flatness of the product is 0.05mm, the repeatability of the flatness is +/-0.05%, and the flatness is good by testing through a step meter. Test data are shown in table 4 below.
TABLE 4 Table 4
Comparative example 1
A preparation method of an LTCC ceramic substrate comprises the following steps:
s51: preparing an LTCC green ceramic tape (MG 60 of Shanghai crystal material new material science and technology Co., ltd.), punching, laminating to obtain an LTCC green ceramic bar block with the thickness of 0.8mm, and cutting the LTCC green ceramic bar block with the thickness of 0.8mm into small green ceramic bar blocks with the thickness of 50mm and 50 mm;
s52: placing steel sheets up and down on the small raw porcelain bars, placing the steel sheets on an aluminum foil, vacuumizing and sealing; opening a warm water isostatic pressing machine, preheating to 75 ℃, placing a sealed to-be-sintered object block, and carrying out isostatic pressing according to an isostatic pressing curve to obtain a new green ceramic blank after finishing; the isostatic pressure curve is: pressurizing at 0MPa for 10 minutes to 10MPa, and maintaining the pressure for 10 minutes; pressurizing at 10MPa for 20 minutes to 15MPa, and maintaining the pressure for 20 minutes; pressurizing for 10 minutes to 20MPa, maintaining the pressure for 2 hours, and ending the isostatic pressing.
Placing the green ceramic blank obtained after the isostatic pressing is finished in a sintering furnace for sintering: and (3) starting to rise to 450 ℃ from room temperature at 1 ℃/min, preserving heat for 2 hours, discharging glue, continuously rising to 850 ℃ at 6 ℃/min after the glue discharging is completed, preserving heat for 10 minutes, and sintering to obtain the LTCC ceramic substrate product.
The shrinkage on both X/Y sides was measured to be 16.3% for the sintered LTCC ceramic substrate product.
As can be seen from the comparison, the low-temperature co-fired ceramic substrate obtained by the preparation method provided by the embodiment of the application can well control the shrinkage rate by controlling the weight of the pressing plate, the technological parameters and the like, and the product has smooth surface, good flatness and good consistency.
Comparative example 2
A preparation method of an LTCC ceramic substrate comprises the following steps:
s61: preparing an LTCC green ceramic tape (A6 of Ferro company in the United states), punching, laminating to obtain an LTCC green ceramic bar block with the thickness of 0.8mm, and cutting the LTCC green ceramic bar block with the thickness of 0.8mm into small green ceramic bar blocks with the thickness of 50 mm;
s62: placing steel sheets up and down on the small raw porcelain bars, placing the steel sheets on an aluminum foil, vacuumizing and sealing; opening a warm water isostatic pressing machine, preheating to 75 ℃, placing a sealed to-be-sintered object block, and carrying out isostatic pressing according to an isostatic pressing curve to obtain a new green ceramic blank after finishing; the isostatic pressure curve is: pressurizing at 0MPa for 10 minutes to 10MPa, and maintaining the pressure for 10 minutes; pressurizing at 10MPa for 20 minutes to 15MPa, and maintaining the pressure for 20 minutes; pressurizing for 10 minutes to 20MPa, maintaining the pressure for 2 hours, and ending the isostatic pressing.
Placing the green ceramic blank obtained after the isostatic pressing is finished in a sintering furnace for sintering: and (3) starting to rise to 450 ℃ from room temperature at 1 ℃/min, preserving heat for 2 hours, discharging glue, continuously rising to 850 ℃ at 6 ℃/min after the glue discharging is completed, preserving heat for 10 minutes, and sintering to obtain the LTCC ceramic substrate product.
The shrinkage on both X/Y sides was measured for the sintered LTCC ceramic substrate product at 16%.
As can be seen from the comparison, the low-temperature co-fired ceramic substrate obtained by the preparation method provided by the embodiment of the application can well control the shrinkage rate by controlling the weight of the pressing plate, the technological parameters and the like, and the product has smooth surface, good flatness and good consistency.
Comparative example 3
A preparation method of an LTCC ceramic substrate comprises the following steps:
s71: preparing an LTCC green ceramic tape (951C 2 of DuPont company of U.S.), punching, laminating to obtain an LTCC green ceramic bar block with the thickness of 0.8mm, and cutting the LTCC green ceramic bar block with the thickness of 0.8mm into small green ceramic bar blocks with the thickness of 50 mm;
s72: placing steel sheets up and down on the small raw porcelain bars, placing the steel sheets on an aluminum foil, vacuumizing and sealing; opening a warm water isostatic pressing machine, preheating to 75 ℃, placing a sealed to-be-sintered object block, and carrying out isostatic pressing according to an isostatic pressing curve to obtain a new green ceramic blank after finishing; the isostatic pressure curve is: pressurizing at 0MPa for 10 minutes to 10MPa, and maintaining the pressure for 10 minutes; pressurizing at 10MPa for 20 minutes to 15MPa, and maintaining the pressure for 20 minutes; pressurizing for 10 minutes to 20MPa, maintaining the pressure for 2 hours, and ending the isostatic pressing.
Placing the green ceramic blank obtained after the isostatic pressing is finished in a sintering furnace for sintering: and (3) starting to rise to 450 ℃ from room temperature at 1 ℃/min, preserving heat for 2 hours, discharging glue, continuously rising to 850 ℃ at 6 ℃/min after the glue discharging is completed, preserving heat for 10 minutes, and sintering to obtain the LTCC ceramic substrate product.
The shrinkage on both X/Y sides was measured for the sintered LTCC ceramic substrate product at 15%.
As can be seen from the comparison, the low-temperature co-fired ceramic substrate obtained by the preparation method provided by the embodiment of the application can well control the shrinkage rate by controlling the weight of the pressing plate, the technological parameters and the like, and the product has smooth surface, good flatness and good consistency.
The foregoing description of the preferred embodiments of the present application is not intended to be limiting, but is intended to cover any and all modifications, equivalents, and alternatives falling within the spirit and principles of the present application.
Claims (6)
1. The preparation method of the ceramic substrate is characterized by comprising the following steps of:
making the raw porcelain band into raw porcelain blocks;
a first separation layer and a second separation layer are respectively attached to the two surfaces of the raw porcelain bar block, then a first protection layer and a second protection layer are respectively attached, and the second protection layer, the second separation layer, the raw porcelain bar block, the first separation layer and the first protection layer which are sequentially stacked form a block to be sintered;
sealing the object to be sintered, performing isostatic pressing treatment, and respectively attaching a first pressing plate and a second pressing plate on two surfaces of the object to be sintered;
sintering the to-be-sintered object blocks attached with the first pressing plate and the second pressing plate to sinter the raw porcelain blocks into a ceramic substrate;
wherein,,
the material of the first protective layer is at least one of alumina ceramic, zirconia ceramic and aluminum nitride ceramic, and the material of the second protective layer is at least one of alumina ceramic, zirconia ceramic and aluminum nitride ceramic;
the material of the first pressing plate is at least one of alumina, zirconia and corundum-mullite, and the material of the second pressing plate is at least one of alumina, zirconia and corundum-mullite;
the material of the first separation layer is selected from carbon-based sacrificial materials, the material of the second separation layer is selected from carbon-based sacrificial materials, the thickness of the first separation layer is 0.08-0.12 mm, and the thickness of the second separation layer is 0.08-0.12 mm;
the step of sintering treatment comprises the following steps: firstly, glue discharging treatment is carried out at 450-480 ℃, and then the temperature is raised to 800-850 ℃ for sintering.
2. The method of claim 1, wherein the green tape is selected from LTCC green tapes, and the resulting ceramic substrate is an LTCC ceramic substrate.
3. The method according to claim 1, wherein the thickness of the raw porcelain bar is 0.8-1.2 mm; and/or the number of the groups of groups,
the thickness of the first protective layer and the second protective layer is 0.12-0.30 mm.
4. The method of claim 1, wherein the weight of the first platen and the second platen is 2 to 6kg; and/or the number of the groups of groups,
the porosity of the first pressing plate and the second pressing plate is 20-30%, the roughness is less than 0.5 mu m, and the flatness is less than 0.1%.
5. The method according to any one of claims 1 to 4, wherein the step of sealing the block to be sintered and then performing an isostatic pressing process comprises: starting pressurizing the sealed to-be-sintered object block under the conditions of 70-80 ℃ and 0-0.5 MPa: pressurizing for 8-12 min to 5-10 MPa, maintaining the pressure for 8-12 min, continuously pressurizing for 10-20 min to 14-16 MPa, maintaining the pressure for 18-22 min, and finally pressurizing for 8-12 min to 19-21 MPa, maintaining the pressure for 1.5-2.5 hours.
6. A low temperature co-fired ceramic substrate, characterized in that it is prepared by the preparation method according to any one of claims 1 to 5.
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