CN115321954A - 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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Abstract
The application relates to the technical field of electronic ceramic processes, 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 comprises the following steps: preparing the raw porcelain strips into raw porcelain blocks; firstly respectively attaching a first separation layer and a second separation layer to two surfaces of the raw porcelain bar block, then respectively attaching a first protective layer and a second protective layer, and forming a to-be-sintered block by the sequentially stacked second protective layer, second separation layer, raw porcelain bar block, first separation layer and first protective layer; sealing the object to be sintered, performing isostatic pressing treatment, and then 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 block 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 the sintering efficiency.
Description
Technical Field
The application belongs to the technical field of electronic ceramic processes, 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 integration and hybrid Circuit packaging technology widely used at present, integrates elements such as a capacitor, a resistor, an inductor and the like into a multilayer substrate, can be directly used as a packaging substrate of an Integrated Circuit (IC), has the outstanding advantages of high reliability, high integration 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 products are higher and higher, the existing low-temperature co-fired ceramic substrates are more and more difficult to meet the requirements of current products, and the sizes of the sintered low-temperature co-fired ceramic substrates are not uniform, for example, the shrinkage rates of the sintered low-temperature co-fired ceramic substrates in the same direction of the X/Y axis are different, the difference is up to +/-0.8%, and the flatness is also greatly different, so that the consistency of the sintered low-temperature co-fired ceramic substrates in the same batch is poor. Therefore, how to control the shrinkage and the uniformity of flatness becomes a key direction of the low temperature co-fired ceramic substrate.
At present, the process methods for controlling shrinkage and flatness are mainly controlled in the sintering process, and include a pressure-assisted sintering method, a pressureless assisted sintering method, a self-constrained sintering method and a composite co-sintering method. The shrinkage rate and the flatness of the low-temperature co-fired ceramic substrate are controlled in the sintering process, so that the requirements on equipment are generally high, the material cost is high, the shrinkage rate control precision is poor, and the phenomena of cracking and the like are easily caused on thin products, so that the production efficiency is reduced.
Disclosure of Invention
The application aims 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 purpose 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, comprising the steps of:
preparing the raw porcelain strips into raw porcelain blocks;
the method comprises the following steps of firstly respectively attaching a first separation layer and a second separation layer to two surfaces of a raw porcelain bar block, then respectively attaching a first protective layer and a second protective layer, and forming a to-be-sintered object block by the sequentially stacked second protective layer, second separation layer, raw porcelain bar block, first separation layer and first protective layer;
sealing the object to be sintered, carrying out isostatic pressing treatment, and then 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 block 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, which is prepared by the preparation method of the present application.
The utility model provides a ceramic substrate's preparation method, all laminate separation layer and protective layer with the two surfaces of porcelain ba bloc earlier and carry out isostatic pressing and handle, then laminate the clamp plate and carry out the sintering, this in-process protective layer can protect the sintering of porcelain ba bloc, the control shrinkage factor is in order to prevent the product fracture after the sintering, the separation layer separates porcelain ba bloc and protective layer, prevent that in sintering process porcelain ba bloc and protective layer fuse together, thereby make the ceramic substrate that the later stage obtained separate better with the protective layer, and the clamp plate can further control the shrinkage factor after the porcelain ba bloc sinters into ceramic substrate. Therefore, the preparation method can control the shrinkage rate of the ceramic substrate well finally, the obtained ceramic substrate product is smooth in surface and good in flatness, meanwhile, the preparation method can improve the consistency of the ceramic substrate product, remarkably improves 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 specific preparation method of the application, so that the low-temperature co-fired ceramic substrate can well control the shrinkage rate, and the product has a smooth surface, good flatness and good consistency.
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In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic diagram of a green ceramic block with a separation layer attached to two surfaces thereof and a separation layer in a method for manufacturing a ceramic substrate according to an embodiment of the present disclosure;
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 block in a method for manufacturing a ceramic substrate according to an embodiment of the present application;
wherein, in the figures, the various reference numbers:
10-green ceramic bar block, 21-first separation layer, 22-second separation layer, 31-first protective layer, 32-second protective layer, 41-first press plate, 42-second press plate.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present application more clearly apparent, 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 merely illustrative of the present application and are not intended to limit the present application.
In this application, the term "and/or" describes an association relationship of associated objects, meaning that there may be three relationships, e.g., a and/or B, which may mean: a is present alone, A and B are present simultaneously, and B is present alone. Wherein A and B can be singular or plural. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
In the present application, "at least one" means one or more, "plural" means two or more. "at least one of the following" or similar expressions refer to any combination of these items, including any combination of the singular or plural items.
It should be understood that, in various embodiments of the present application, the sequence numbers of the foregoing processes do not imply an execution sequence, some or all of the steps may be executed in parallel or executed sequentially, and the execution sequence of each process should be determined by its function and inherent logic, and should not limit the implementation process of the embodiments of the present application.
The terminology used in the embodiments of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in the examples of 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 used for distinguishing purposes such as substances from one another, and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. 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 defined as "first" or "second" may explicitly or implicitly include one or more of that feature.
A first aspect of an embodiment of the present application provides a method for manufacturing a ceramic substrate, including:
s01: preparing the raw porcelain strips into raw porcelain blocks;
s02: the method comprises the following steps of firstly respectively attaching a first separation layer and a second separation layer to two surfaces of a raw porcelain bar block, then respectively attaching a first protective layer and a second protective layer, and forming a to-be-sintered object block by the sequentially stacked second protective layer, second separation layer, raw porcelain bar block, first separation layer and first protective layer;
s03: sealing the object to be sintered, carrying out isostatic pressing treatment, and then 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 block attached with the first pressing plate and the second pressing plate to sinter the raw porcelain blocks into the ceramic substrate.
The ceramic substrate preparation method provided by the embodiment of the application, the separation layer has been used multipurposely, auxiliary material such as protective layer and clamp plate, shrinkage factor obtains effective control when can making the raw porcelain ba piece sinter into ceramic substrate, specifically, at first, separation layer and protective layer are all laminated on raw porcelain ba piece both surfaces, carry out isostatic pressing after the sealing and handle, then two surface laminating clamp plates sinter, the sintering of raw porcelain ba piece can be protected to the protective layer in this process, the control shrinkage factor is in order to prevent the product fracture after the sintering, the separation layer separates raw porcelain ba piece and protective layer, prevent in sintering process raw porcelain ba piece and protective layer fuse together, thereby make the ceramic substrate that the later stage obtained separate better with the protective layer, and the clamp plate can further control the shrinkage factor after the raw porcelain ba piece sinters into ceramic substrate. Therefore, the preparation method of the embodiment of the application can well control the shrinkage rate of the ceramic substrate finally, the obtained ceramic substrate product has a smooth surface and good flatness, and meanwhile, the preparation method can improve the consistency of the ceramic substrate product, remarkably improve the sintering efficiency and has good application prospects in the field of ceramic substrate preparation.
Step S01 is a raw porcelain nugget preparation step.
In an embodiment, the ceramic substrate obtained by the preparation method of the present application may be an LTCC ceramic substrate, the provided green tape is selected from an LTCC green tape, and the LTCC green tape is made into a green ceramic block and then subjected to the process of the preparation method of the present application, so as to obtain the LTCC ceramic substrate. Specifically, the step of making the green ceramic tape into a green ceramic block may include: LTCC green tape (commercially available) is punched, laminated to give green blocks of desired thickness, and then cut for subsequent processing.
In one embodiment, the thickness of the green ceramic bar block is 0.8-1.2 mm, specifically, 0.8mm, 1.0mm, 1.2mm, etc.; and sintering the raw ceramic blocks with the thicknesses to obtain the ceramic substrate with the corresponding thickness.
Step S02 is a bonding step of the isolation layer and the protective layer.
As shown in fig. 1, the first and second separation layers 21 and 22 are respectively attached to both surfaces of the raw porcelain bar block 10, and then the first and second protective layers 31 and 32 are respectively attached to both surfaces of the raw porcelain bar block, so that the second protective layer 32, the second separation layer 22, the raw porcelain bar block 10, the first separation layer 21, and the first protective layer 31, which are sequentially stacked, constitute a block to be sintered.
In one embodiment, the first separation layer and the second separation layer may be separation layers with the same thickness and the same material, and specifically, the thickness of each of the first separation layer and the second separation layer is 0.08 to 0.12mm, such as 0.08mm, 0.10mm, 0.12mm, and the like; the materials of the first separation layer and the second separation layer are selected from carbon-based sacrificial materials, such as carbon ribbons and carbon black paste, the low-temperature co-fired ceramic sintering generally has fine 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 ceramic blocks and the protective layer. Through the first separation layer and the second separation layer which are made of the same thickness and material, the two surfaces of the raw porcelain blocks can be uniformly separated from the protective layer. The separation layer is arranged between the protective layer and the raw porcelain bar block and is mainly used for separating the protective layer from a final product, so that the protective layer and the raw porcelain bar block are prevented from being bonded together in a sintering process, the protective layer and a ceramic substrate product can be conveniently separated in a later period, and the separation process of the protective layer and the ceramic substrate product is simplified.
In an embodiment, the first protection layer and the second protection layer may be protection layers with the same thickness and the same material, and specifically, the thickness of each of the first protection layer and the second protection layer is 0.12 to 0.30mm, such as 0.12mm, 0.16mm, 0.18mm, 0.20mm, 0.25mm, and the like; the material of the first protective layer and the second protective layer is selected from at least one of alumina ceramics, zirconia ceramics and aluminum nitride ceramics. The high-temperature ceramics such as alumina, zirconia, aluminum nitride and the like can resist the temperature of more than 1200 ℃ and the flatness of less than 0.1 percent, can well protect ceramic substrate products, prevent the products from cracking and control the shrinkage rate.
Step S03 is an isostatic pressing process and a platen bonding process.
Specifically, the isostatic pressing treatment may be warm isostatic pressing treatment, 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 to be vacuumized and sealed, and then is placed in a warm water isostatic pressing machine to be subjected to isostatic pressing, and an isostatic pressing curve may be changed according to control of different shrinkage rates.
In one embodiment, the step of sealing the to-be-sintered block and then performing isostatic pressing comprises: pressurizing the sealed to-be-sintered block at 70-80 ℃ under the pressure of 0-0.5 MPa: pressurizing for 8-12 minutes to 5-10 MPa, maintaining the pressure for 8-12 minutes, then continuously pressurizing for 10-20 minutes to 14-16 MPa, maintaining the pressure for 18-22 minutes, and finally pressurizing for 8-12 minutes to 19-21 MPa for 1.5-2.5 hours. Specifically, pressurizing at 0MPa for 10min to 10MPa, and maintaining the pressure for 10 min; pressurizing at 10MPa for 20 min to 15MPa, and maintaining the pressure for 20 min; pressurizing for 10 minutes to 20MPa, maintaining the pressure for 2 hours, and finishing isostatic pressing. The green ceramic blocks, the separation layer and the protective layer are combined together in a laminating and isostatic pressing mode, so that a solid green ceramic blank can be obtained, and the density and hardness of a final ceramic substrate product can be improved.
As shown in fig. 2, both surfaces of the isostatic-pressed to-be-sintered object block (the second protective layer 32, the second separation layer 22, the raw porcelain nugget 10, the first separation layer 21, and the first protective layer 32 stacked in this order) are respectively bonded to a first pressing plate 41 and a second pressing plate 42, thereby forming a stacked second pressing plate 42, second protective layer 32, second separation layer 22, raw porcelain nugget 10, first separation layer 21, first protective layer 32, and first pressing plate 41. Sintering treatment is performed under the conditions of the attached first separation layer 21 and second separation layer 22, the first protection layer 31 and second protection layer 32, and the first pressing plate 41 and second pressing plate 42, so that the raw porcelain blocks 10 can be sintered to generate ceramic substrates with controllable shrinkage rate, high hardness and good consistency.
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 materials such as aluminum oxide, zirconium oxide, corundum mullite and the like, 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%. And placing the to-be-sintered block subjected to isostatic pressing treatment between the first pressing plate and the second pressing plate with the parameters, and then placing the to-be-sintered block into a sintering furnace for sintering, wherein the shrinkage rate and the flatness of the pressing plate can be effectively controlled, so that the LTCC substrate suitable for various thicknesses can be prepared.
Step S04 is a sintering step.
In one embodiment, the step of sintering comprises: firstly, the binder removal treatment is carried out at the temperature of 450-480 ℃, and then the temperature is raised to 800-900 ℃ for sintering. Specifically, the temperature of the binder removal can be 450 ℃, 460 ℃, 480 ℃ and the like, the heating rate of the temperature rise to 800-900 ℃ can be 5-7 ℃/min, and the sintering time of 800-900 ℃ can be 10-15 minutes. Such a sintering process can sinter green LTCC ceramic blocks into LTCC ceramic substrates.
In one embodiment, a method for preparing an LTCC ceramic substrate includes the steps of:
the method comprises the following steps:and punching the LTCC green ceramic tape, laminating to obtain an LTCC green ceramic block with required thickness, and cutting into a green ceramic block to be processed.
Step two:and (3) 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 ceramic block as a separation layer for lamination, and then respectively placing a layer of high-temperature ceramic block with the same thickness on the upper surface and the lower surface as a protection layer for lamination to obtain a new block to be sintered.
Step three:and placing steel sheets on the upper and lower surfaces of the obtained to-be-sintered block, then placing the to-be-sintered block in an aluminum foil bag, vacuumizing and sealing the to-be-sintered block, and then placing the to-be-sintered block into 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 object to be sintered after isostatic pressing treatment, matching the weights according to different shrinkage rates, and then placing the objects in a sintering furnace for sintering: raising the temperature from room temperature (25-27 ℃) to 450-480 ℃, preserving heat and discharging glue, continuing raising the temperature to 800-900 ℃ after the glue discharging is finished, preserving heat and sintering; and after sintering, naturally cooling, removing the pressing plate, the protective layer and the isolating 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 rate and the 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 rate on an 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 obviously improved.
In a second aspect of the embodiments of the present application, a low-temperature co-fired ceramic substrate is provided, which is prepared by the above-mentioned specific preparation method of 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 of the embodiment of the application, so that the shrinkage rate of the low-temperature co-fired ceramic substrate can be well controlled, and the product has a smooth surface, good flatness and good consistency.
The following description will be given with reference to specific examples.
Example 1
A preparation method of an LTCC ceramic substrate comprises the following steps:
s11: preparing an LTCC green porcelain tape (MG 60 of Shanghai crystal new material science and technology Co., ltd.), punching and laminating the green porcelain tape to obtain an LTCC green porcelain block with the thickness of 0.8mm, cutting the LTCC green porcelain block with the thickness of 0.8mm into small green porcelain blocks with the thickness of 50mm x 50mm, and sintering 7 small green porcelain blocks;
s12: preparing two carbon belts of carbon-based material with the thickness of 0.1mm, and cutting the carbon belts into small pieces of 50mm as a first separation layer and a second separation layer; preparing two aluminum nitride ceramic green ceramic strips with the thickness of 0.15mm, and cutting the aluminum nitride ceramic green ceramic strips into small blocks with the thickness of 50mm × 50mm to serve as a first protective layer and a second protective layer;
the first separation layer and the second separation layer are respectively attached to two surfaces of the obtained small raw porcelain blocks, then the first protection layer and the second protection layer are respectively attached to the two surfaces of the obtained small raw porcelain blocks, and the second protection layer, the second separation layer, the raw porcelain blocks, the first separation layer and the first protection layer which are sequentially stacked form a to-be-sintered block.
S13: placing steel sheets on the upper part and the lower part of the block to be sintered, placing the block in an aluminum foil bag, and vacuumizing and sealing the block; opening a warm water isostatic pressing machine, preheating to 75 ℃, putting the sealed object to be sintered, carrying out isostatic pressing treatment according to an isostatic pressing curve, and obtaining a new green porcelain blank after finishing the treatment; the isostatic pressure curve is: pressurizing at 0MPa for 10min to 10MPa, and maintaining the pressure for 10 min; pressurizing at 10MPa for 20 min to 15MPa, and maintaining the pressure for 20 min; pressurizing for 10 minutes to 20MPa, maintaining the pressure for 2 hours, and finishing isostatic pressing.
Two alumina press plates weighing 6kg were prepared as a first press plate and a second press plate, and a green porcelain blank obtained by isostatic pressing was placed between the first press plate and the second press plate to be laminated.
S14: placing the green porcelain blank body with the first pressing plate and the second pressing plate combined in a lamination manner in a sintering furnace for sintering: starting to rise from room temperature to 450 ℃ at a speed of 1 ℃/min, preserving heat for 2 hours for glue removal, continuing to rise to 850 ℃ at a speed of 6 ℃/min after the glue removal is finished, preserving heat for 10 minutes, and sintering into porcelain; and after sintering, naturally cooling, 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 is measured, and the experiment is repeated for many times, so that the shrinkage repeatability is +/-0.05%. The visual measurement LTCC ceramic substrate product has a smooth surface, the flatness of the product is 0.03mm through the test of a step profiler, the repeatability of the flatness is +/-0.05%, and the flatness is good. The 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 porcelain tape (MG 60 of Shanghai crystal material New materials science and technology Co., ltd.), punching and laminating the green porcelain tape to obtain an LTCC green porcelain block with the thickness of 1mm, and cutting the LTCC green porcelain block with the thickness of 1mm into small green porcelain blocks with the thickness of 50mm x 50mm;
s22: preparing two carbon belts of carbon-based material with the thickness of 0.1mm, and cutting the carbon belts into small blocks of 50mm as a first separation layer and a second separation layer; preparing two aluminum nitride ceramic green porcelain strips with the thickness of 0.2mm, and cutting the aluminum nitride ceramic green porcelain strips into small blocks with the thickness of 50mm x 50mm to be used as a first protective layer and a second protective layer;
the first separation layer and the second separation layer are respectively attached to two surfaces of the obtained small raw porcelain blocks, then the first protection layer and the second protection layer are respectively attached to the two surfaces of the obtained small raw porcelain blocks, and the second protection layer, the second separation layer, the raw porcelain blocks, the first separation layer and the first protection layer which are sequentially stacked form a to-be-sintered block.
S23: placing steel sheets on the upper part and the lower part of the block to be sintered, placing the block in an aluminum foil bag, and vacuumizing and sealing the block; opening a warm water isostatic pressing machine, preheating to 75 ℃, putting the sealed object to be sintered, carrying out isostatic pressing treatment according to an isostatic pressing curve, and obtaining a new green porcelain blank after finishing the treatment; the isostatic pressure curve is: pressurizing at 0MPa for 10min to 10MPa, and maintaining the pressure for 10 min; pressurizing at 10MPa for 20 min to 15MPa, and maintaining the pressure for 20 min; pressurizing for 10 minutes to 20MPa, maintaining the pressure for 2 hours, and finishing isostatic pressing.
Two alumina press plates weighing 6kg were prepared as a first press plate and a second press plate, and a green porcelain blank obtained by isostatic pressing was placed between the first press plate and the second press plate to be laminated.
S24: placing the green porcelain blank body with the first pressing plate and the second pressing plate combined in a lamination manner in a sintering furnace for sintering: starting to rise from room temperature to 450 ℃ at a speed of 1 ℃/min, preserving heat for 2 hours for glue removal, continuing to rise to 850 ℃ at a speed of 6 ℃/min after the glue removal is finished, preserving heat for 10 minutes, and sintering into porcelain; and after sintering, naturally cooling, 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 is measured, and the experiment is repeated for a plurality of times, so that the shrinkage repeatability is +/-0.05%. The visual measurement LTCC ceramic substrate product has the advantages that the surface is smooth, the flatness of the product is 0.02mm through the test of a step profiler, the repeatability of the flatness is +/-0.05%, and the flatness is good. The 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 tape (A6 of Fero corporation, USA), punching and laminating the green tape to obtain an LTCC green block with the thickness of 1mm, and cutting the LTCC green block with the thickness of 1mm into small green blocks with the thickness of 50mm per 50mm;
s32: preparing two carbon belts of carbon-based material with the thickness of 0.1mm, and cutting the carbon belts into small pieces of 50mm as a first separation layer and a second separation layer; preparing two aluminum nitride ceramic green porcelain strips with the thickness of 0.15mm, and cutting the aluminum nitride ceramic green porcelain strips into small blocks with the thickness of 50mm x 50mm to be used as a first protective layer and a second protective layer;
the first separation layer and the second separation layer are respectively attached to two surfaces of the obtained small raw porcelain blocks, then the first protection layer and the second protection layer are respectively attached to the two surfaces of the obtained small raw porcelain blocks, and the second protection layer, the second separation layer, the raw porcelain blocks, the first separation layer and the first protection layer which are sequentially stacked form a to-be-sintered block.
S33: placing steel sheets on the upper part and the lower part of the block to be sintered, placing the block in an aluminum foil bag, and vacuumizing and sealing the block; opening a warm water isostatic pressing machine, preheating to 75 ℃, putting the sealed object to be sintered, carrying out isostatic pressing treatment according to an isostatic pressing curve, and obtaining a new green porcelain blank after finishing the treatment; the isostatic pressure curve is: pressurizing at 0MPa for 10min to 5MPa, and maintaining the pressure for 10 min; pressurizing at 10MPa for 10min to 15MPa, and maintaining the pressure for 20 min; pressurizing for 10 minutes to 20MPa, maintaining the pressure for 2 hours, and ending isostatic pressing.
Two zirconia press plates weighing 4kg were prepared as a first press plate and a second press plate, and the green porcelain body obtained by the isostatic pressing treatment was placed between the first press plate and the second press plate for lamination.
S34: placing the green porcelain blank body with the first pressing plate and the second pressing plate combined in a lamination manner in a sintering furnace for sintering: starting to rise from room temperature to 450 ℃ at a speed of 0.8 ℃/min, preserving heat for 2 hours for glue removal, continuing to rise to 850 ℃ at a speed of 5 ℃/min after the glue removal is finished, preserving heat for 10 minutes, and sintering into porcelain; and after sintering, naturally cooling, 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 is measured, and the experiment is repeated for a plurality of times, so that the shrinkage repeatability is +/-0.05%. The visual measurement LTCC ceramic substrate product has a smooth surface, the flatness of the product is 0.04mm through the test of a step profiler, the repeatability of the flatness is +/-0.05%, and the flatness is good. The test data are shown in table 3 below.
TABLE 3
Example 4
A preparation method of an LTCC ceramic substrate comprises the following steps:
s41: preparing an LTCC green tape (951C 2 of Dupont, USA), punching and laminating the green tape to obtain an LTCC green block with the thickness of 1mm, and cutting the LTCC green block with the thickness of 1mm into small green blocks with the thickness of 50mm x 50mm;
s42: preparing two carbon belts of carbon-based material with the thickness of 0.1mm, and cutting the carbon belts into small pieces of 50mm as a first separation layer and a second separation layer; preparing two aluminum nitride ceramic green ceramic strips with the thickness of 0.3mm, and cutting the aluminum nitride ceramic green ceramic strips into small blocks with the thickness of 50mm × 50mm to serve as a first protective layer and a second protective layer;
the first separation layer and the second separation layer are respectively attached to two surfaces of the obtained small raw porcelain blocks, then the first protection layer and the second protection layer are respectively attached to the two surfaces of the obtained small raw porcelain blocks, and the second protection layer, the second separation layer, the raw porcelain blocks, the first separation layer and the first protection layer which are sequentially stacked form a to-be-sintered block.
S43: placing steel sheets on the upper part and the lower part of the block to be sintered, placing the block in an aluminum foil bag, and vacuumizing and sealing the block; opening a warm water isostatic pressing machine, preheating to 75 ℃, putting a sealed object to be sintered, performing isostatic pressing treatment according to an isostatic pressing curve, and obtaining a new green porcelain blank after the completion; the isostatic pressure curve is: pressurizing at 0MPa for 10min to 10MPa, and maintaining the pressure for 10 min; pressurizing at 10MPa for 10min to 15MPa, and maintaining the pressure for 20 min; pressurizing for 10 minutes to 20MPa, maintaining the pressure for 2 hours, and finishing isostatic pressing.
Preparing two oxidation pickaxe pressing plates with the weight of 4kg as a first pressing plate and a second pressing plate, and placing a raw porcelain blank obtained by isostatic pressing between the first pressing plate and the second pressing plate for lamination.
S44: placing the green porcelain blank body with the first pressing plate and the second pressing plate combined in a lamination manner in a sintering furnace for sintering: starting to rise from room temperature to 450 ℃ at the speed of 1.2 ℃/min, preserving heat for 2 hours for glue removal, continuing to rise to 850 ℃ at the speed of 7 ℃/min after the glue removal is finished, preserving heat for 15 minutes, and sintering into porcelain; and after sintering, naturally cooling, 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 is measured, and the experiment is repeated for a plurality of times, so that the shrinkage repeatability is +/-0.05%. The visual measurement LTCC ceramic substrate product has the advantages that the surface is smooth, the flatness of the product is 0.05mm through the step profiler test, the repeatability of the flatness is +/-0.05%, and the flatness is good. The test data are given in table 4 below.
TABLE 4
Comparative example 1
A preparation method of an LTCC ceramic substrate comprises the following steps:
s51: preparing an LTCC green porcelain tape (MG 60 of Shanghai crystal new material science and technology Co., ltd.), punching, laminating to obtain an LTCC green porcelain block with the thickness of 0.8mm, and cutting the LTCC green porcelain block with the thickness of 0.8mm into small green porcelain blocks with the thickness of 50mm x 50mm;
s52: placing steel sheets on the small raw porcelain blocks up and down, placing the small raw porcelain blocks on an aluminum foil, vacuumizing and sealing; opening a warm water isostatic pressing machine, preheating to 75 ℃, putting the sealed to-be-sintered object block, performing isostatic pressing according to an isostatic pressing curve, and obtaining a new green porcelain blank after the isostatic pressing is finished; the isostatic pressure curve is: pressurizing at 0MPa for 10min to 10MPa, and maintaining the pressure for 10 min; pressurizing at 10MPa for 20 min to 15MPa, and maintaining the pressure for 20 min; pressurizing for 10 minutes to 20MPa, maintaining the pressure for 2 hours, and finishing isostatic pressing.
And (3) placing the green porcelain blank obtained after isostatic pressing in a sintering furnace for sintering: and starting to rise from room temperature to 450 ℃ at the speed of 1 ℃/min, preserving heat for 2 hours, removing the adhesive, continuing to rise to 850 ℃ at the speed of 6 ℃/min after the adhesive removal is finished, preserving heat for 10 minutes, and sintering into ceramic to obtain the LTCC ceramic substrate product.
The shrinkage on both X/Y sides of the sintered LTCC ceramic substrate product was measured to be 16.3%.
From the comparison, the shrinkage rate of the low-temperature co-fired ceramic substrate obtained by the preparation method provided by the embodiment of the application can be well controlled by controlling the weight of the pressing plate, the process parameters and the like, and the product has a 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 tape (A6 of Ferro corporation, USA), punching, laminating to obtain an LTCC green block with the thickness of 0.8mm, and cutting the LTCC green block with the thickness of 0.8mm into small green blocks with the thickness of 50mm;
s62: placing steel sheets on the small raw porcelain blocks up and down, placing the small raw porcelain blocks on an aluminum foil, vacuumizing and sealing; opening a warm water isostatic pressing machine, preheating to 75 ℃, putting the sealed to-be-sintered object block, performing isostatic pressing according to an isostatic pressing curve, and obtaining a new green porcelain blank after the isostatic pressing is finished; the isostatic pressure curve is: pressurizing at 0MPa for 10min to 10MPa, and maintaining the pressure for 10 min; pressurizing at 10MPa for 20 min to 15MPa, and maintaining the pressure for 20 min; pressurizing for 10 minutes to 20MPa, maintaining the pressure for 2 hours, and finishing isostatic pressing.
And (3) placing the green porcelain blank obtained after isostatic pressing in a sintering furnace for sintering: and starting to rise from room temperature to 450 ℃ at a speed of 1 ℃/min, preserving heat for 2 hours for glue removal, continuing to rise to 850 ℃ at a speed of 6 ℃/min after the glue removal is finished, preserving heat for 10 minutes, and sintering into ceramic to obtain the LTCC ceramic substrate product.
The shrinkage on both X/Y sides of the sintered LTCC ceramic substrate product was measured to be 16%.
From the comparison, the shrinkage rate of the low-temperature co-fired ceramic substrate obtained by the preparation method provided by the embodiment of the application can be well controlled by controlling the weight of the pressing plate, the process parameters and the like, and the product has a 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 tape (951C 2 of DuPont, USA), punching, laminating to obtain an LTCC green block with the thickness of 0.8mm, and cutting the LTCC green block with the thickness of 0.8mm into small green blocks with the thickness of 50mm x 50mm;
s72: placing steel sheets on the small raw porcelain blocks up and down, placing the small raw porcelain blocks on an aluminum foil, and vacuumizing and sealing; opening a warm water isostatic pressing machine, preheating to 75 ℃, putting the sealed to-be-sintered object block, performing isostatic pressing according to an isostatic pressing curve, and obtaining a new green porcelain blank after the isostatic pressing is finished; the isostatic pressure curve is: pressurizing at 0MPa for 10min to 10MPa, and maintaining the pressure for 10 min; pressurizing at 10MPa for 20 min to 15MPa, and maintaining the pressure for 20 min; pressurizing for 10 minutes to 20MPa, maintaining the pressure for 2 hours, and finishing isostatic pressing.
And (3) placing the green porcelain blank obtained after isostatic pressing in a sintering furnace for sintering: and starting to rise from room temperature to 450 ℃ at the speed of 1 ℃/min, preserving heat for 2 hours, removing the adhesive, continuing to rise to 850 ℃ at the speed of 6 ℃/min after the adhesive removal is finished, preserving heat for 10 minutes, and sintering into ceramic to obtain the LTCC ceramic substrate product.
When the sintered LTCC ceramic substrate product is measured, the shrinkage on both sides X/Y is 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 process parameters and the like, and the product has a smooth surface, good flatness and good consistency.
The above description is only a preferred embodiment of the present application and should not be taken as limiting the present application, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. A method for preparing a ceramic substrate is characterized by comprising the following steps:
preparing the raw porcelain strips into raw porcelain blocks;
respectively attaching a first separation layer and a second separation layer to two surfaces of the raw porcelain bar block, then respectively attaching a first protective layer and a second protective layer, and forming a to-be-sintered block by sequentially laminating the second protective layer, the second separation layer, the raw porcelain bar block, the first separation layer and the first protective layer;
sealing the to-be-sintered block, carrying out isostatic pressing treatment, and then respectively attaching a first pressing plate and a second pressing plate to the two surfaces of the to-be-sintered block;
and sintering the to-be-sintered object block attached with the first pressing plate and the second pressing plate to sinter the raw porcelain blocks into the ceramic substrate.
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 of claim 1, wherein the green ceramic bar block has a thickness of 0.8 to 1.2mm; and/or the presence of a gas in the atmosphere,
the thicknesses of the first separation layer and the second separation layer are both 0.08-0.12 mm; and/or the presence of a gas in the atmosphere,
the thickness of the first protective layer and the second protective layer is 0.12-0.30 mm.
4. The method of claim 3, wherein the first separation layer and the second separation layer are the same and are each selected from a carbon-based sacrificial material.
5. The method according to claim 3, wherein the first protective layer and the second protective layer are made of the same material and each is selected from at least one of alumina ceramics, zirconia ceramics, and aluminum nitride ceramics.
6. The method of claim 3, wherein the first and second platens are made of the same material and are each selected from at least one of alumina, zirconia, and corundum-mullite.
7. The method of manufacturing according to claim 6, wherein the first press plate and the second press plate have a weight of 2 to 6kg; and/or the presence of a gas in the gas,
the first pressing plate and the second pressing plate have the porosity of 20-30%, the roughness of less than 0.5 mu m and the flatness of less than 0.1%.
8. The method according to any one of claims 1 to 7, wherein the step of sealing the mass to be sintered and then subjecting it to isostatic pressing comprises: pressurizing the sealed block to be sintered at 70-80 ℃ under the pressure of 0-0.5 MPa: pressurizing for 8-12 minutes to 5-10 MPa, then maintaining the pressure for 8-12 minutes, then continuously pressurizing for 10-20 minutes to 14-16 MPa, then maintaining the pressure for 18-22 minutes, and finally pressurizing for 8-12 minutes to 19-21 MPa, and maintaining the pressure for 1.5-2.5 hours.
9. The production method according to any one of claims 1 to 7, wherein the step of sintering treatment comprises: firstly, the glue is discharged at 450-480 ℃, and then the temperature is raised to 800-900 ℃ for sintering.
10. A low-temperature co-fired ceramic substrate, characterized in that it is prepared by the preparation method of any one of claims 1 to 9.
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