CN114062419B - Method for testing shrinkage mismatch degree of multilayer cofired ceramic substrate - Google Patents

Method for testing shrinkage mismatch degree of multilayer cofired ceramic substrate Download PDF

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CN114062419B
CN114062419B CN202111185702.8A CN202111185702A CN114062419B CN 114062419 B CN114062419 B CN 114062419B CN 202111185702 A CN202111185702 A CN 202111185702A CN 114062419 B CN114062419 B CN 114062419B
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sintering
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slurry
ceramic
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CN114062419A (en
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岳帅旗
王娜
徐洋
陈丽丽
张刚
杨宇
黄翠英
肖晖
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CETC 29 Research Institute
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Abstract

The invention discloses a method for testing shrinkage mismatch degree of a multilayer cofired ceramic substrate, which comprises the following steps: s1, manufacturing a pure raw porcelain process sample by using blank raw porcelain, and testing the sintering shrinkage rate of the pure raw porcelain process sample; s2, introducing matched slurry, manufacturing a process sample containing the matched slurry, and testing the sintering shrinkage rate of the process sample after the matched slurry is introduced; and S3, subtracting the sintering shrinkage of the process sample piece after the matched slurry is introduced from the sintering shrinkage of the pure ceramic process sample piece to obtain the shrinkage mismatch degree of the matched slurry and the green ceramic sintering of the multilayer cofiring ceramic substrate. The invention solves the problem that the quantitative test of the shrinkage mismatch degree of the slurry and the green porcelain sintering cannot be realized in the prior art.

Description

Method for testing shrinkage mismatch degree of multilayer cofired ceramic substrate
Technical Field
The invention relates to the technical field of manufacturing of multilayer ceramic circuit substrates, in particular to a method for testing shrinkage mismatch degree of a multilayer cofired ceramic substrate.
Background
Multilayer ceramic circuit boards typically represented by LTCC (low temperature cofired ceramic) are widely used in the aviation and aerospace fields due to their excellent high frequency performance and high integration density. Along with the continuous promotion of miniaturization, multi-functional, high performance demand, the wiring density of multilayer cofired ceramic circuit substrate is higher and higher, cavity structure is more and more complicated, has higher and higher requirement to the size precision, the roughness of substrate simultaneously.
In the manufacturing process of the multilayer cofired ceramic substrate, raw porcelain is used as a main material, and serves as an electric insulating medium in the circuit substrate after sintering, and meanwhile, structural support is provided. The matched slurry mainly comprises conductor slurry, resistor slurry and dielectric slurry, is usually manufactured on raw porcelain in a film layer or through hole mode, and after being co-fired with the raw porcelain integrally, the matched slurry realizes the established functional characteristics to form circuit elements in a substrate.
In the co-firing process of the multilayer ceramic substrate, due to the fact that the matched slurry and the raw ceramic have a certain degree of difference in sintering characteristics and shrinkage behaviors, the problems of warping, plane distortion and the like of the circuit substrate are very easy to occur, particularly in the circuit substrate with a complex structure, through holes and wires are unevenly distributed, the cavity structure further damages the overall symmetry, the problems are particularly remarkable, the quality and the qualification rate of products are seriously affected, therefore, the evaluation of the degree of co-firing shrinkage mismatch of the matched slurry and the raw ceramic is very important, on one hand, the overall shrinkage behavior of the circuit substrate can be predicted according to a test result, necessary process compensation is conducted, the processing quality of the multilayer ceramic circuit substrate is improved, on the other hand, a quantized test method is provided for the research and development improvement of materials, and a support is provided for the improvement of the co-firing matching property of the matched slurry and the raw ceramic.
In recent years, a great deal of research is being conducted in the industry on the multilayer cofired ceramic substrate process technology, and the paper "LTCC process technology research" indicates that the substrate warpage is caused by the asymmetric distribution of the conductors inside the substrate; the paper "LTCC substrate co-firing flatness process research" indicates that the open grid-land and pattern uniform design can improve the flatness of the LTCC substrate; the patent 'a multilayer co-fired ceramic circuit substrate with a structure compensation area and a manufacturing method of the multilayer substrate' provides a process design compensation method for arranging conductor through holes and patterns on the periphery of a product, so that the warp of the substrate in an asymmetric area is restrained, and the flatness of the substrate is improved. Although the shrinkage mismatch problem of the co-firing of the matched slurry and the raw porcelain is mentioned in many related researches, the shrinkage mismatch problem is qualitatively described as an influencing factor in a certain aspect, and quantitative test and evaluation are not performed, so that a test method for testing the shrinkage mismatch degree of the co-firing of the matched slurry and the raw porcelain is urgently needed to be established, the quantitative test for the shrinkage mismatch degree of the sintering of the slurry and the raw porcelain is realized, and the product design, the process design and the raw material optimization improvement are guided.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a method for testing the shrinkage mismatch degree of a multilayer co-fired ceramic substrate, which solves the problem that the quantitative test of the shrinkage mismatch degree of slurry and green ceramic sintering cannot be realized in the prior art.
The invention solves the problems by adopting the following technical scheme:
a method for testing shrinkage mismatch degree of a multilayer co-fired ceramic substrate comprises the following steps:
s1, manufacturing a pure raw porcelain process sample by using blank raw porcelain, and testing the sintering shrinkage rate of the pure raw porcelain process sample;
s2, introducing matched slurry, manufacturing a process sample containing the matched slurry, and testing the sintering shrinkage rate of the process sample after the matched slurry is introduced;
and S3, subtracting the sintering shrinkage of the process sample piece after the matched slurry is introduced from the sintering shrinkage of the pure ceramic process sample piece to obtain the shrinkage mismatch degree of the matched slurry and the green ceramic sintering of the multilayer cofiring ceramic substrate.
As a preferable technical scheme, in step S1, test points are arranged on the pure ceramic process sample, and test marks are manufactured at the positions where the test points are arranged and used for testing the sizes of the pure ceramic process sample before and after sintering.
In step S1, a test mark of a green ceramic process sample is made by punching, hole filling or pattern printing.
As a preferred technical solution, in step S2, a process sample containing the matched slurry is manufactured by using a symmetry design, where the symmetry design refers to: when the matched slurry is arranged, the printed patterns which are completely identical in shape and completely aligned in position are arranged on the front surface and the back surface of the process sample piece, or through holes which are identical in diameter and aligned in position are arranged on each layer of the process sample piece.
As a preferred technical solution, in step S2, a process sample is manufactured, which contains a large-area distribution of the matched slurry, where the large-area distribution of the matched slurry refers to: the conductor slurry is continuously distributed, and a blank raw porcelain area is reserved at the periphery of the matched slurry distribution area.
As a preferable technical scheme, in the step S2, the width of a blank raw porcelain area at the periphery of a matched slurry distribution area is 3-10 mm, and the width difference of the blank raw porcelain at the edge of a process sample piece after the matched slurry is introduced is less than 1mm.
In the step S2, the matched slurry is printed on the front surface of the first layer and the back surface of the last layer of the process sample piece, the length and width of the pattern are 20 mm-60 mm, and the thickness of the printed dry film is 6 mu m-20 mu m; or, arranging through holes on each layer of the raw porcelain, wherein the diameter of the through holes is 0.1-0.3 mm, and the center-to-center distance of the through holes is 2-5 times the diameter of the through holes.
As a preferable technical scheme, the sintering shrinkage rate calculation method of the pure ceramic process sample piece comprises the following steps: (1-the size after sintering of the pure ceramic process sample piece/the size before sintering of the pure ceramic process sample piece) ×100%, wherein the size after sintering of the pure ceramic process sample piece refers to the distance between test marks after sintering of the pure ceramic sample piece, and the size before sintering of the pure ceramic process sample piece refers to the distance between test marks before sintering of the pure ceramic sample piece; the method for calculating the sintering shrinkage of the process sample after the matched slurry is introduced comprises the following steps: (1-post-sintering dimension of the process sample after the introduction of the supporting slurry/pre-sintering dimension of the process sample after the introduction of the supporting slurry) ×100%, wherein the post-sintering dimension of the process sample after the introduction of the supporting slurry refers to the distance between the test marks after the sintering of the sample, and the pre-sintering dimension of the process sample after the introduction of the supporting slurry refers to the distance between the test marks before the sintering of the sample.
As a preferable technical scheme, the number of layers of the arrangement of the process sample piece after the matched slurry is introduced is the same as that of the pure ceramic process sample piece.
As a preferred technical scheme, in step S3, the shrinkage mismatch degree of the supporting slurry and the green ceramic sintering takes the average value of the shrinkage mismatch degrees of the test marks in all directions, and/or the shrinkage mismatch degree of the supporting slurry and the green ceramic sintering of the multilayer co-fired ceramic substrate takes the average value of the shrinkage mismatch degree of the supporting slurry and the green ceramic sintering.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention provides a simple and easy method, which is characterized in that under a certain arrangement rule, the influence degree of matched slurry on the sintering shrinkage of raw porcelain is obtained through the comparison test of process sample pieces, and the shrinkage mismatch degree of the matched slurry and the raw porcelain during co-firing is rapidly obtained, so that the quantitative test of the shrinkage mismatch degree of the matched slurry and the raw porcelain during sintering is realized, the quantitative index is provided for the analysis and evaluation of mismatch problems, and the product design, the process design and the raw material optimization improvement are guided; the process sample adopted by the invention is simple and quick to manufacture, is compatible with the conventional multilayer cofired ceramic substrate technology, and is easy to realize;
(2) Test marks are introduced, so that the sintering shrinkage rate can be conveniently tested;
(3) The test marks are manufactured by punching, hole filling or pattern printing, so that the operation is easy, and the test is convenient;
(4) The symmetrical design is beneficial to avoiding the warpage of the sample piece caused by asymmetric shrinkage in the sintering process, reducing the measurement error and improving the accuracy of the test;
(5) The large-area distribution of the matched slurry can fully show the shrinkage mismatch effect between the slurry and the raw porcelain in the sintering process.
(6) The blank raw porcelain area can effectively inhibit the warpage of the sample in the sintering process, and eliminate interference factors in the shrinkage test.
(7) Reasonable sample size design is convenient for the effective utilization of experimental materials, guarantees lower test relative error simultaneously.
(8) The sintering shrinkage rate is conveniently calculated through the measurement data, and the shrinkage mismatch degree is further calculated;
(9) Further reducing the measurement error and further increasing the accuracy of measurement.
Drawings
FIG. 1 is a schematic diagram of the steps of the present invention;
FIG. 2 is a plan view of a green ceramic process sample prior to sintering;
FIG. 3 is a schematic diagram of sintering shrinkage of a green ceramic process sample;
FIG. 4 is a plan view of a large area distribution process sample of the slurry kit;
FIG. 5 is a cross-sectional view taken along the line A-A' of FIG. 4;
FIG. 6 is a schematic diagram of sintering shrinkage of a large area distribution process sample of the matched slurry.
The reference numerals and corresponding part names in the drawings: 1. the ceramic tile comprises a pure ceramic block body 2, a sintered pure ceramic process sample piece 3, a raw ceramic block body formed after stacking/laminating of raw ceramic printed with symmetrical patterns, and a sintered matched slurry large-area distribution process sample piece 4.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but embodiments of the present invention are not limited thereto.
Example 1
As shown in fig. 1 to 6, a method for testing shrinkage mismatch of a multilayer co-fired ceramic substrate includes the following steps:
s1, manufacturing a pure raw porcelain process sample by using blank raw porcelain, and testing the sintering shrinkage rate of the pure raw porcelain process sample;
s2, introducing matched slurry, manufacturing a process sample containing the matched slurry, and testing the sintering shrinkage rate of the process sample after the matched slurry is introduced;
and S3, subtracting the sintering shrinkage of the process sample piece after the matched slurry is introduced from the sintering shrinkage of the pure ceramic process sample piece to obtain the shrinkage mismatch degree of the matched slurry and the green ceramic sintering of the multilayer cofiring ceramic substrate.
The invention provides a simple and easy method, which is characterized in that under a certain arrangement rule, the influence degree of matched slurry on the sintering shrinkage of raw porcelain is obtained through the comparison test of process sample pieces, and the shrinkage mismatch degree of the matched slurry and the raw porcelain during co-firing is rapidly obtained, so that the quantitative test of the shrinkage mismatch degree of the matched slurry and the raw porcelain during sintering is realized, the quantitative index is provided for the analysis and evaluation of mismatch problems, and the product design, the process design and the raw material optimization improvement are guided. The process sample adopted by the invention is simple and quick to manufacture, is compatible with the conventional multilayer co-fired ceramic substrate technology, and is easy to realize.
As a preferable technical scheme, in step S1, test points are arranged on the pure ceramic process sample, and test marks are manufactured at the positions where the test points are arranged and used for testing the sizes of the pure ceramic process sample before and after sintering.
And a test mark is introduced, so that the sintering shrinkage rate can be conveniently tested.
In step S1, a test mark of a green ceramic process sample is made by punching, hole filling or pattern printing.
The test mark is manufactured by punching, hole filling or pattern printing, so that the operation is easy and the test is convenient.
As a preferred technical solution, in step S2, a process sample containing the matched slurry is manufactured by using a symmetry design, where the symmetry design refers to: when the matched slurry is arranged, the printed patterns which are completely identical in shape and completely aligned in position are arranged on the front surface and the back surface of the process sample piece, or through holes which are identical in diameter and aligned in position are arranged on each layer of the pure ceramic process sample piece.
The symmetry design is favorable for avoiding the warpage of the sample piece caused by asymmetric shrinkage in the sintering process, reducing the measurement error and improving the accuracy of the test.
As a preferred technical solution, in step S2, a process sample is manufactured, which contains a large-area distribution of the matched slurry, where the large-area distribution of the matched slurry refers to: the conductor slurry is continuously distributed, and a blank raw porcelain area is reserved at the periphery of the matched slurry distribution area.
The large-area distribution of the matched slurry can fully show the shrinkage mismatch effect between the slurry and the raw porcelain in the sintering process.
As a preferable technical scheme, in the step S2, the width of a blank raw porcelain area at the periphery of a matched slurry distribution area is 3-10 mm, and the width difference of the blank raw porcelain at the edge of a process sample piece after the matched slurry is introduced is less than 1mm.
The width design is convenient for setting the blank raw porcelain area, can effectively inhibit the warpage of the sample piece in the sintering process, and eliminates interference factors in the shrinkage test.
In the step S2, the matched slurry is printed on the front surface of the first layer and the back surface of the last layer of the process sample piece, the length and width of the pattern are 20 mm-60 mm, and the thickness of the printed dry film is 6 mu m-20 mu m; or, arranging through holes on each layer of the raw porcelain, wherein the diameter of the through holes is 0.1-0.3 mm, and the center-to-center distance of the through holes is 2-5 times the diameter of the through holes.
The size design is convenient for the effective utilization of experimental materials, and simultaneously ensures lower test relative error.
Example 2
As further optimization of embodiment 1, this embodiment includes all the technical features of embodiment 1, as shown in fig. 1 to 6, and in addition, this embodiment further includes the following technical features:
as a preferable technical scheme, the sintering shrinkage rate calculation method of the pure ceramic process sample piece comprises the following steps: (1-the size after sintering of the pure ceramic process sample piece/the size before sintering of the pure ceramic process sample piece) ×100%, wherein the size after sintering of the pure ceramic process sample piece refers to the distance between test marks after sintering of the pure ceramic sample piece, and the size before sintering of the pure ceramic process sample piece refers to the distance between test marks before sintering of the pure ceramic sample piece; the method for calculating the sintering shrinkage of the process sample after the matched slurry is introduced comprises the following steps: (1-post-sintering dimension of the process sample after the introduction of the supporting slurry/pre-sintering dimension of the process sample after the introduction of the supporting slurry) ×100%, wherein the post-sintering dimension of the process sample after the introduction of the supporting slurry refers to the distance between the test marks after the sintering of the sample, and the pre-sintering dimension of the process sample after the introduction of the supporting slurry refers to the distance between the test marks before the sintering of the sample.
This facilitates calculation of the sintering shrinkage and thus the shrinkage mismatch from the measured data.
As a preferable technical scheme, the number of layers of the arrangement of the process sample piece after the matched slurry is introduced is the same as that of the pure ceramic process sample piece.
This further increases the accuracy of the measurement.
As a preferred technical scheme, in step S3, the shrinkage mismatch degree of the co-fired ceramic substrate and the green ceramic sintering is an average value of shrinkage mismatch degrees in all directions, and/or the shrinkage mismatch degree of the multi-layer co-fired ceramic substrate and the green ceramic sintering is an average value of shrinkage mismatch degrees of the co-fired ceramic substrate and the green ceramic sintering.
The adoption of the average value is beneficial to further reducing the measurement error and further increasing the measurement accuracy.
Example 3
As shown in fig. 1 to 6, this embodiment includes all the technical features of embodiment 1 and embodiment 2, and provides a more detailed embodiment on the basis of embodiment 1 and embodiment 2.
The invention is realized by the following technical method:
1) And manufacturing a pure raw porcelain process sample piece by using the blank raw porcelain, and testing the sintering shrinkage rate of the pure raw porcelain process sample piece.
2) And (3) manufacturing a process sample with large-area distribution of the matched slurry by utilizing a symmetry design, and testing the sintering shrinkage rate after the matched slurry is introduced.
3) And subtracting the sintering shrinkage rate of the sample piece of the matched slurry from the sintering shrinkage rate of the sample piece of the pure raw porcelain process to obtain the mismatch degree of the sintering shrinkage of the matched slurry and the raw porcelain.
The blank raw porcelain refers to raw porcelain raw materials which are not processed by any process.
The pure raw porcelain process sample is characterized in that a blank raw porcelain is utilized to manufacture a multi-layer structure through a lamination-sintering method, test marks are manufactured only at test point positions, and no matched slurry is introduced into other areas.
The plane size of the multilayer structure of the pure raw porcelain process sample piece is usually 20-60 mm, the number of layers is usually 2-10, the thickness of a single-layer blank raw porcelain is usually 0.05-0.3 mm, the lamination pressure in the manufacturing process is usually 2000-4000 PSI, and the sintering condition is determined according to the characteristics of the raw porcelain.
The test mark of the green ceramic sample is a mark which is manufactured at a specific position of the sample and has the appearance similar to that of the green ceramic, and is used for testing the size of the sample before and after sintering, and is usually arranged at the vertex position of the sample close to 4 angles.
The test mark of the pure ceramic sample piece can be manufactured by a punching/hole filling or micro pattern printing method, the diameter of a through hole is usually 0.05-0.3 mm, and the hole filling material is hole filling slurry matched with the raw ceramic; the size of the printed micro pattern is usually 0.1 mm-1 mm, the thickness of the printed dry film is 6 mu m-20 mu m, and the printing material is printing slurry matched with raw porcelain.
The method for calculating the sintering shrinkage of the pure ceramic process sample piece comprises the following steps: (1-post-sintering size/pre-sintering size) X100%
The pre-sintering/post-sintering dimensions refer to the distance between the test marks of the green ceramic sample before and after sintering.
The symmetry design is that when the matched slurry is arranged, the printed patterns with the same shape and the same position are arranged on the front surface and the back surface of the sample piece, or through holes with the same diameter and the same position are arranged on each layer, so that the warpage of the sample piece caused by asymmetric shrinkage is avoided.
The number of layers of the distribution and the blank raw porcelain are the same as those of the pure raw porcelain process sample, and the process sample is also manufactured into a multilayer structure by a lamination-sintering method.
The large-area distribution of the matched slurry means that large-area patterns are printed on the front surface of the first layer of raw porcelain and the back surface of the last layer of raw porcelain of the sample piece, the length and width of the patterns are usually 20 mm-60 mm, and the thickness of a printed dry film is 6 mu m-20 mu m; or high-density through holes are arranged on each layer of the raw porcelain, the diameter of the through holes is usually 0.1-0.3 mm, and the center-to-center distance of the through holes is usually 2-5 times the diameter of the through holes. The symmetrical arrangement of the matched slurry is formed by the accurate lamination.
The large-area distribution process sample of the matched slurry is characterized in that a blank raw porcelain area is reserved on the periphery of the large-area distribution area of the matched slurry, the width of the blank raw porcelain area is generally 3-10 mm and is used for arranging test marks and inhibiting the warpage of the edge of the sample, and the blank raw porcelain width difference of four sides of the sample is smaller than 1mm.
The process sample piece matched with the slurry and distributed in a large area adopts the same method as that of the pure ceramic process sample piece, and the test marks are arranged at the vertex positions of the sample piece, which are close to 4 corners.
The method for calculating the sintering shrinkage rate of the matched slurry large-area distribution process sample comprises the following steps: (1-post-sintering size/pre-sintering size). Times.100%.
The shrinkage mismatch degree of the matched slurry and the green porcelain sintering is as follows: the sintering shrinkage rate of the process sample with large-area distribution of the matched slurry, namely the sintering shrinkage rate of the pure ceramic process sample, can be obtained by taking the average value of the whole area and taking the average value according to the direction of the sample, or not taking the average value.
The method comprises the steps of manufacturing a pure ceramic process sample, testing the shrinkage rate of the pure ceramic process sample, manufacturing a matched slurry large-area distribution process sample, testing the shrinkage rate of the matched slurry large-area distribution process sample, calculating the mismatch degree between the slurry and the raw ceramic sintering, and the like.
FIG. 2 is a plan view of a green ceramic process sample before sintering, wherein a green ceramic block 1 is a green ceramic block (green ceramic process sample) formed by laminating/laminating blank green ceramics, 1-m are test marks made on the green ceramics, X 1 、X 2 、Y 1 、Y 2 The distances between the test points before sintering are respectively.
FIG. 3 is a schematic diagram showing sintering shrinkage of a green ceramic process sample, wherein the sintered green ceramic process sample 2 is a sintered green ceramic process sample, 2-m is a test mark after sintering of the green ceramic process sample, and X 11 、X 21 、Y 11 、Y 21 The distances between the test points after sintering are respectively.
FIG. 4 is a plan view of a large-area distribution process sample of the slurry used in the process before sintering, wherein the green ceramic block 3 formed by laminating the green ceramic layer with the symmetrical pattern printed thereon is a green ceramic block formed by laminating the green ceramic layer with the symmetrical pattern printed thereon, and 3-m is an arrangement3-f is matched slurry for large-area printing, 3-P is blank raw porcelain area, a 1 、a 2 、b 1 、b 2 The distances between the test points before sintering are shown in the schematic cross-section, and A-A' are shown in the schematic cross-section.
FIG. 5 is a cross-sectional view of a large area distribution process sample of the matched paste before sintering, 3-f is the large area matched paste symmetrically printed on the upper and lower surfaces, and 3-P is the blank green ceramic area.
FIG. 6 is a schematic diagram showing sintering shrinkage of a large-area distribution process sample of the matched slurry, wherein the sintered matched slurry large-area distribution process sample 4 is a sintered process sample, 4-m is an arranged test mark, 4-f is a film layer formed after sintering the matched slurry, 4-P is a white porcelain region formed after sintering, and a 11 、a 21 、b 11 、b 21 The distances between the test points after sintering are respectively.
As shown in FIG. 2, 6 layers of 9K7 raw porcelain of Dupont company are selected, the thickness of the raw porcelain is 127 mu m, holes are punched/filled in the raw porcelain by using a conventional process, the diameter of each through hole is 0.2mm, the hole filling slurry is matched LL502 hole filling gold slurry, the raw porcelain is laminated/laminated to form a pure raw porcelain block 1, and the filled through holes are used as test marks 1-m.
As shown in FIG. 2, test X 1 、X 2 、Y 1 、Y 2 The length of (2) is: 60.008mm, 60.003mm, 60.005mm, 59.998mm.
As shown in fig. 3, the green ceramic block 1 is sintered to form a sintered green ceramic process sample 2,2-m as a test mark.
As shown in FIG. 3, test X 11 、X 21 、Y 11 、Y 21 The length of (2) is: 54.396mm, 54.393mm, 54.390mm, 54.376mm.
The sintering shrinkage rates of four sides of the pure ceramic process sample piece are calculated as follows:
Figure GDA0004183392990000101
as shown in fig. 4 and 5, 6 layers of 9K7 green porcelain of Dupont company are selected to be made into matched slurry large-area distribution process samples, the thickness of green porcelain batches and blank green porcelain is the same as that of pure green porcelain process samples, large-area patterns 3-f are printed on the top surface and the back surface of each sample, the printing slurry is LL507 wiring gold slurry matched with the 9K7 green porcelain, the thickness of a printing dry film is 11-13 mu m, the pattern size is 35mm multiplied by 35mm, the width of an edge blank green porcelain area is 3-P is 5mm, a green porcelain block body (the green porcelain block body 3 formed after the green porcelain lamination/lamination printed with symmetrical patterns) is formed after lamination/lamination of the green porcelain, 3-m is a test mark, the manufacturing method is the same as that of the pure green porcelain process samples, and the direction of the samples is the same as that of the pure green porcelain process samples.
As shown in fig. 4, test a respectively 1 、b 2 、c 1 、d 2 The length of (2) is: 36.995mm, 37.008mm, 37.003mm, 36.993mm.
As shown in fig. 6, the green ceramic block 3 formed after stacking/laminating the green ceramic printed with the symmetrical patterns is sintered to form a matched slurry large-area distribution process sample (a sintered matched slurry large-area distribution process sample 4), 4-m is a test mark, 4-f is a conductor film layer sintered by printing the large-area pattern 3-f, and is tightly combined with a ceramic body formed after sintering the green ceramic, and 4-P is a blank ceramic region formed after sintering.
As shown in fig. 6, test a respectively 11 、b 21 、c 11 、d 21 The length of (2) is: 33.605 mm,33.650mm,33.686mm,33.650mm.
The sintering shrinkage rates of four sides of a large-area distribution process sample piece of the matched slurry are respectively as follows:
Figure GDA0004183392990000111
calculating the sintering shrinkage mismatch degree of the LL507 matched slurry and the 9K7 green ceramic: and (3) the sintering shrinkage rates of the matched slurry large-area distribution process sample and the pure raw porcelain process sample are respectively averaged according to the direction area, and then the shrinkage rates of the matched slurry large-area distribution process sample and the pure raw porcelain process sample in the same direction are subtracted to obtain the sintering shrinkage mismatch degree.
Figure GDA0004183392990000121
As described above, the present invention can be preferably implemented.
All of the features disclosed in all of the embodiments of this specification, or all of the steps in any method or process disclosed implicitly, except for the mutually exclusive features and/or steps, may be combined and/or expanded and substituted in any way.
The foregoing description of the preferred embodiment of the invention is not intended to limit the invention in any way, but rather to cover all modifications, equivalents, improvements and alternatives falling within the spirit and principles of the invention.

Claims (3)

1. The method for testing the shrinkage mismatch degree of the multilayer cofired ceramic substrate is characterized by comprising the following steps of:
s1, manufacturing a pure raw porcelain process sample by using blank raw porcelain, and testing the sintering shrinkage rate of the pure raw porcelain process sample;
s2, introducing matched slurry, manufacturing a process sample containing the matched slurry, and testing the sintering shrinkage rate of the process sample after the matched slurry is introduced;
s3, subtracting the sintering shrinkage rate of the process sample piece after the matched slurry is introduced from the sintering shrinkage rate of the pure ceramic process sample piece to obtain the shrinkage mismatch degree of the matched slurry and the green ceramic sintering of the multilayer cofiring ceramic substrate;
in the step S1, test points are arranged on the pure-raw porcelain process sample, test marks are manufactured at the positions of the arranged test points and used for testing the sizes of the pure-raw porcelain process sample before and after sintering;
in the step S1, a test mark of a pure ceramic process sample is manufactured by a punching, hole filling or pattern printing method;
in step S2, a process sample containing the matched slurry is manufactured by using a symmetry design, wherein the symmetry design refers to: when the matched slurry is arranged, printing patterns which are completely identical in shape and completely aligned in position are arranged on the front surface and the back surface of the process sample piece, or through holes which are identical in diameter and aligned in position are arranged on each layer of the process sample piece;
in step S2, manufacturing a process sample containing large-area distribution of matched slurry, wherein the large-area distribution of the matched slurry refers to: the conductor sizing agent is continuously distributed, and a blank raw porcelain area is reserved at the periphery of the matched sizing agent distribution area;
in the step S2, the width of a blank raw porcelain area at the periphery of the matched slurry distribution area is 3-10 mm, and the width difference of the blank raw porcelain at the edge of a process sample piece after the matched slurry is introduced is less than 1mm;
in the step S2, printing patterns on the front surface of the first layer and the back surface of the last layer of the process sample piece by using matched slurry, wherein the length and width of the patterns are 20 mm-60 mm, and the thickness of a printing dry film is 6 mu m-20 mu m; or, arranging through holes on each layer of the raw porcelain, wherein the diameter of the through holes is 0.1-0.3 mm, and the center-to-center distance of the through holes is 2-5 times of the diameter of the through holes;
the method for calculating the sintering shrinkage of the pure ceramic process sample piece comprises the following steps: (1-the size after sintering of the pure ceramic process sample piece/the size before sintering of the pure ceramic process sample piece) ×100%, wherein the size after sintering of the pure ceramic process sample piece refers to the distance between test marks after sintering of the pure ceramic sample piece, and the size before sintering of the pure ceramic process sample piece refers to the distance between test marks before sintering of the pure ceramic sample piece; the method for calculating the sintering shrinkage of the process sample after the matched slurry is introduced comprises the following steps: (1-post-sintering dimension of the process sample after the introduction of the supporting slurry/pre-sintering dimension of the process sample after the introduction of the supporting slurry) ×100%, wherein the post-sintering dimension of the process sample after the introduction of the supporting slurry refers to the distance between the test marks after the sintering of the sample, and the pre-sintering dimension of the process sample after the introduction of the supporting slurry refers to the distance between the test marks before the sintering of the sample.
2. The method for testing shrinkage mismatch degree of a multilayer cofired ceramic substrate according to claim 1, wherein the number of layers of the process sample after the introduction of the matched slurry is the same as that of the arrangement layers of the pure ceramic process sample.
3. The method for testing shrinkage mismatch degree of a multilayer cofired ceramic substrate according to claim 2, wherein in step S3, the shrinkage mismatch degree of the mating paste and the green ceramic is an average value in each direction, and/or the shrinkage mismatch degree of the mating paste and the green ceramic of the multilayer cofired ceramic substrate is an average value of the shrinkage mismatch degree of the mating paste and the green ceramic.
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